Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Davies, John E.' 'Mays, M.' 'Raithby, Paul R.' 'Sarveswaran, Koshala' 'Solan, Gregory A.' _publ_contact_author_name 'Dr M Mays' _publ_contact_author_address ; Dr M Mays University Chemistry Laboratory Lensfield Road CAMBRIDGE CB2 1EW U.K. ; data_mm9721 _database_code_CSD 154853 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C34 H26 Co O7 P W' _chemical_formula_weight 820.30 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' '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' 'W' 'W' -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 15.501(16) _cell_length_b 12.623(14) _cell_length_c 31.390(14) _cell_angle_alpha 90.00 _cell_angle_beta 91.95(6) _cell_angle_gamma 90.00 _cell_volume 6138.5(97) _cell_formula_units_Z 8 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 20 _cell_measurement_theta_max 30 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.775 _exptl_crystal_density_method ? _exptl_crystal_F_000 3216 _exptl_absorpt_coefficient_mu 4.386 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'R-Axis IIc' _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32480 _diffrn_reflns_av_R_equivalents 0.0689 _diffrn_reflns_av_sigmaI/netI 0.0560 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.30 _diffrn_reflns_theta_max 25.25 _reflns_number_total 10491 _reflns_number_observed 9603 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 35 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0539P)^2^+2.4953P] 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 refU _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10456 _refine_ls_number_parameters 793 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0592 _refine_ls_R_factor_obs 0.0476 _refine_ls_wR_factor_all 0.1150 _refine_ls_wR_factor_obs 0.1017 _refine_ls_goodness_of_fit_all 1.121 _refine_ls_goodness_of_fit_obs 1.119 _refine_ls_restrained_S_all 1.210 _refine_ls_restrained_S_obs 1.119 _refine_ls_shift/esd_max 0.002 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group W1 W 0.58543(2) 0.30845(2) 0.947503(7) 0.02223(8) Uani 1 d . . W2 W 0.365817(15) 0.00735(2) 0.782193(7) 0.02055(8) Uani 1 d . . Co1 Co 0.68789(5) 0.18423(7) 0.99483(3) 0.0242(2) Uani 1 d . . Co2 Co 0.27974(5) 0.17631(6) 0.75388(2) 0.0214(2) Uani 1 d . . P1 P 0.71827(10) 0.22524(13) 0.92899(5) 0.0243(3) Uani 1 d . . P2 P 0.25027(10) 0.10056(13) 0.81430(5) 0.0226(3) Uani 1 d . . O1 O 0.7319(4) 0.5105(4) 0.9973(2) 0.0521(15) Uani 1 d . . O2 O 0.8209(3) 0.3775(4) 1.01448(15) 0.0387(12) Uani 1 d . . O3 O 0.5169(3) 0.2461(4) 1.07396(13) 0.0320(11) Uani 1 d . . O4 O 0.5070(3) 0.2855(4) 1.00427(13) 0.0269(10) Uani 1 d . . O5 O 0.1217(3) 0.0258(4) 0.7096(2) 0.0382(12) Uani 1 d . . O6 O 0.1955(3) -0.1250(4) 0.7185(2) 0.0368(11) Uani 1 d . . O7 O 0.4433(3) 0.0442(3) 0.72655(12) 0.0248(9) Uani 1 d . . O8 O 0.4421(3) 0.1310(3) 0.66464(13) 0.0270(10) Uani 1 d . . O15 O 0.8564(3) 0.1205(5) 1.0307(2) 0.068(2) Uani 1 d . . O16 O 0.5946(3) -0.0169(4) 0.9994(2) 0.0467(13) Uani 1 d . . O17 O 0.5108(3) 0.0884(4) 0.91603(14) 0.0330(11) Uani 1 d . . O49 O 0.1098(3) 0.2699(4) 0.7363(2) 0.0521(14) Uani 1 d . . O50 O 0.3826(3) 0.3641(4) 0.7766(2) 0.0426(12) Uani 1 d . . O51 O 0.4804(3) 0.1840(4) 0.82547(14) 0.0349(11) Uani 1 d . . C1 C 0.9121(5) 0.4477(6) 1.2052(2) 0.045(2) Uani 1 d . . H1 H 0.9523(5) 0.4727(6) 1.2265(2) 0.054 Uiso 1 calc R . C2 C 0.9398(5) 0.3909(7) 1.1708(2) 0.048(2) Uani 1 d . . H2 H 0.9997(5) 0.3776(7) 1.1680(2) 0.058 Uiso 1 calc R . C3 C 0.8815(5) 0.3532(6) 1.1402(2) 0.042(2) Uani 1 d . . H3 H 0.9017(5) 0.3127(6) 1.1171(2) 0.050 Uiso 1 calc R . C4 C 0.7941(4) 0.3734(5) 1.1428(2) 0.0273(14) Uani 1 d . . C5 C 0.7669(4) 0.4305(6) 1.1778(2) 0.037(2) Uani 1 d . . H5 H 0.7070(4) 0.4440(6) 1.1806(2) 0.044 Uiso 1 calc R . C6 C 0.8243(5) 0.4678(6) 1.2084(2) 0.042(2) Uani 1 d . . H6 H 0.8042(5) 0.5074(6) 1.2318(2) 0.051 Uiso 1 calc R . C7 C 0.7348(4) 0.3389(5) 1.1092(2) 0.0271(14) Uani 1 d . . C8 C 0.6891(4) 0.3120(5) 1.0795(2) 0.0272(14) Uani 1 d . . C9 C 0.6435(4) 0.2940(5) 1.0394(2) 0.0261(14) Uani 1 d . . C10 C 0.6742(4) 0.3387(5) 0.9999(2) 0.0253(14) Uani 1 d . . C11 C 0.7434(4) 0.4174(6) 1.0033(2) 0.032(2) Uani 1 d . . C12 C 0.8915(5) 0.4530(8) 1.0201(3) 0.063(3) Uani 1 d . . H12A H 0.9447(5) 0.4150(8) 1.0283(3) 0.076 Uiso 1 calc R . H12B H 0.8778(5) 0.5036(8) 1.0426(3) 0.076 Uiso 1 calc R . H12C H 0.8996(5) 0.4911(8) 0.9934(3) 0.076 Uiso 1 calc R . C13 C 0.5522(4) 0.2739(5) 1.0378(2) 0.0238(13) Uani 1 d . . C14 C 0.4246(4) 0.2220(7) 1.0727(2) 0.042(2) Uani 1 d . . H14A H 0.4069(4) 0.2028(7) 1.1014(2) 0.051 Uiso 1 calc R . H14B H 0.4131(4) 0.1628(7) 1.0532(2) 0.051 Uiso 1 calc R . H14C H 0.3921(4) 0.2844(7) 1.0628(2) 0.051 Uiso 1 calc R . C15 C 0.7912(5) 0.1482(6) 1.0166(2) 0.038(2) Uani 1 d . . C16 C 0.6303(4) 0.0627(5) 0.9977(2) 0.0302(15) Uani 1 d . . C17 C 0.5384(4) 0.1672(6) 0.9284(2) 0.0292(15) Uani 1 d . . C18 C 0.6063(5) 0.4536(6) 0.9058(2) 0.040(2) Uani 1 d . . H18 H 0.6633(5) 0.4770(6) 0.9007(2) 0.048 Uiso 1 calc R . C19 C 0.5531(5) 0.4876(5) 0.9397(2) 0.041(2) Uani 1 d . . H19 H 0.5688(5) 0.5370(5) 0.9614(2) 0.049 Uiso 1 calc R . C20 C 0.4728(5) 0.4343(5) 0.9351(2) 0.036(2) Uani 1 d . . H20 H 0.4253(5) 0.4424(5) 0.9531(2) 0.043 Uiso 1 calc R . C21 C 0.4750(4) 0.3683(5) 0.8997(2) 0.0306(15) Uani 1 d . . H21 H 0.4291(4) 0.3241(5) 0.8896(2) 0.037 Uiso 1 calc R . C22 C 0.5571(4) 0.3771(5) 0.8808(2) 0.033(2) Uani 1 d . . H22 H 0.5758(4) 0.3399(5) 0.8565(2) 0.039 Uiso 1 calc R . C23 C 0.7178(4) 0.1272(5) 0.8866(2) 0.0260(14) Uani 1 d . . C24 C 0.7133(5) 0.1616(6) 0.8444(2) 0.039(2) Uani 1 d . . H24 H 0.7117(5) 0.2354(6) 0.8383(2) 0.047 Uiso 1 calc R . C25 C 0.7112(5) 0.0889(7) 0.8111(2) 0.051(2) Uani 1 d . . H25 H 0.7078(5) 0.1131(7) 0.7824(2) 0.061 Uiso 1 calc R . C26 C 0.7139(5) -0.0176(6) 0.8195(3) 0.046(2) Uani 1 d . . H26 H 0.7129(5) -0.0667(6) 0.7965(3) 0.055 Uiso 1 calc R . C27 C 0.7180(5) -0.0539(6) 0.8607(3) 0.046(2) Uani 1 d . . H27 H 0.7187(5) -0.1278(6) 0.8664(3) 0.055 Uiso 1 calc R . C28 C 0.7210(5) 0.0192(5) 0.8943(2) 0.037(2) Uani 1 d . . H28 H 0.7253(5) -0.0057(5) 0.9229(2) 0.044 Uiso 1 calc R . C29 C 0.8241(4) 0.2846(5) 0.9211(2) 0.0295(15) Uani 1 d . . C30 C 0.8370(5) 0.3888(6) 0.9096(2) 0.045(2) Uani 1 d . . H30 H 0.7887(5) 0.4350(6) 0.9069(2) 0.054 Uiso 1 calc R . C31 C 0.9191(5) 0.4280(7) 0.9019(3) 0.056(2) Uani 1 d . . H31 H 0.9262(5) 0.4996(7) 0.8934(3) 0.067 Uiso 1 calc R . C32 C 0.9900(5) 0.3625(7) 0.9067(2) 0.050(2) Uani 1 d . . H32 H 1.0462(5) 0.3888(7) 0.9017(2) 0.060 Uiso 1 calc R . C33 C 0.9787(5) 0.2596(7) 0.9187(2) 0.049(2) Uani 1 d . . H33 H 1.0275(5) 0.2144(7) 0.9221(2) 0.058 Uiso 1 calc R . C34 C 0.8964(5) 0.2200(6) 0.9259(2) 0.042(2) Uani 1 d . . H34 H 0.8897(5) 0.1481(6) 0.9342(2) 0.050 Uiso 1 calc R . C35 C 0.0592(6) 0.3128(8) 0.5358(3) 0.068(3) Uani 1 d . . H35 H 0.0246(6) 0.3484(8) 0.5148(3) 0.081 Uiso 1 calc R . C36 C 0.1268(6) 0.2503(9) 0.5243(3) 0.076(3) Uani 1 d . . H36 H 0.1373(6) 0.2408(9) 0.4949(3) 0.091 Uiso 1 calc R . C37 C 0.1797(5) 0.2011(7) 0.5540(2) 0.055(2) Uani 1 d . . H37 H 0.2259(5) 0.1580(7) 0.5450(2) 0.066 Uiso 1 calc R . C38 C 0.1662(4) 0.2137(6) 0.5969(2) 0.0298(15) Uani 1 d . . C39 C 0.0964(5) 0.2749(6) 0.6088(2) 0.041(2) Uani 1 d . . H39 H 0.0857(5) 0.2836(6) 0.6382(2) 0.050 Uiso 1 calc R . C40 C 0.0423(5) 0.3233(7) 0.5788(2) 0.053(2) Uani 1 d . . H40 H -0.0060(5) 0.3633(7) 0.5875(2) 0.064 Uiso 1 calc R . C41 C 0.2201(4) 0.1655(5) 0.6293(2) 0.0260(14) Uani 1 d . . C42 C 0.2618(4) 0.1348(5) 0.6593(2) 0.0235(13) Uani 1 d . . C43 C 0.3088(4) 0.0988(5) 0.6973(2) 0.0234(13) Uani 1 d . . C44 C 0.2717(4) 0.0323(5) 0.7305(2) 0.0243(13) Uani 1 d . . C45 C 0.1880(4) -0.0189(5) 0.7191(2) 0.0260(14) Uani 1 d . . C46 C 0.1164(5) -0.1822(6) 0.7081(3) 0.052(2) Uani 1 d . . H46A H 0.1279(5) -0.2585(6) 0.7084(3) 0.062 Uiso 1 calc R . H46B H 0.0946(5) -0.1613(6) 0.6796(3) 0.062 Uiso 1 calc R . H46C H 0.0731(5) -0.1655(6) 0.7291(3) 0.062 Uiso 1 calc R . C47 C 0.4021(4) 0.0909(4) 0.6973(2) 0.0219(13) Uani 1 d . . C48 C 0.5346(4) 0.1136(6) 0.6647(2) 0.031(2) Uani 1 d . . H48A H 0.5584(4) 0.1461(6) 0.6393(2) 0.038 Uiso 1 calc R . H48B H 0.5464(4) 0.0373(6) 0.6646(2) 0.038 Uiso 1 calc R . H48C H 0.5616(4) 0.1455(6) 0.6903(2) 0.038 Uiso 1 calc R . C49 C 0.1760(4) 0.2323(6) 0.7419(2) 0.032(2) Uani 1 d . . C50 C 0.3447(4) 0.2892(5) 0.7660(2) 0.0272(14) Uani 1 d . . C51 C 0.4359(4) 0.1225(5) 0.8091(2) 0.0283(14) Uani 1 d . . C52 C 0.3414(5) -0.1766(5) 0.7865(2) 0.035(2) Uani 1 d . . H52 H 0.2946(5) -0.2109(5) 0.7718(2) 0.042 Uiso 1 calc R . C53 C 0.3404(5) -0.1356(5) 0.8283(2) 0.036(2) Uani 1 d . . H53 H 0.2926(5) -0.1369(5) 0.8464(2) 0.043 Uiso 1 calc R . C54 C 0.4232(4) -0.0921(5) 0.8386(2) 0.033(2) Uani 1 d . . H54 H 0.4407(4) -0.0599(5) 0.8648(2) 0.039 Uiso 1 calc R . C55 C 0.4745(4) -0.1057(5) 0.8026(2) 0.0302(15) Uani 1 d . . H55 H 0.5329(4) -0.0838(5) 0.8004(2) 0.036 Uiso 1 calc R . C56 C 0.4234(4) -0.1580(5) 0.7702(2) 0.033(2) Uani 1 d . . H56 H 0.4416(4) -0.1768(5) 0.7426(2) 0.039 Uiso 1 calc R . C57 C 0.1413(4) 0.0494(5) 0.8190(2) 0.0287(15) Uani 1 d . . C58 C 0.1210(4) -0.0560(5) 0.8108(2) 0.031(2) Uani 1 d . . H58 H 0.1656(4) -0.1039(5) 0.8037(2) 0.037 Uiso 1 calc R . C59 C 0.0362(4) -0.0928(6) 0.8128(2) 0.040(2) Uani 1 d . . H59 H 0.0235(4) -0.1653(6) 0.8074(2) 0.048 Uiso 1 calc R . C60 C -0.0292(4) -0.0228(6) 0.8226(2) 0.038(2) Uani 1 d . . H60 H -0.0871(4) -0.0469(6) 0.8235(2) 0.046 Uiso 1 calc R . C61 C -0.0097(4) 0.0810(6) 0.8309(2) 0.037(2) Uani 1 d . . H61 H -0.0545(4) 0.1286(6) 0.8380(2) 0.044 Uiso 1 calc R . C62 C 0.0736(4) 0.1174(6) 0.8291(2) 0.037(2) Uani 1 d . . H62 H 0.0856(4) 0.1900(6) 0.8348(2) 0.044 Uiso 1 calc R . C63 C 0.2630(4) 0.1774(5) 0.8630(2) 0.0239(13) Uani 1 d . . C64 C 0.2445(4) 0.2849(5) 0.8634(2) 0.0287(14) Uani 1 d . . H64 H 0.2280(4) 0.3193(5) 0.8375(2) 0.034 Uiso 1 calc R . C65 C 0.2498(4) 0.3435(5) 0.9012(2) 0.034(2) Uani 1 d . . H65 H 0.2370(4) 0.4171(5) 0.9011(2) 0.041 Uiso 1 calc R . C66 C 0.2741(5) 0.2917(6) 0.9386(2) 0.041(2) Uani 1 d . . H66 H 0.2776(5) 0.3306(6) 0.9645(2) 0.050 Uiso 1 calc R . C67 C 0.2929(6) 0.1865(6) 0.9390(2) 0.054(2) Uani 1 d . . H67 H 0.3098(6) 0.1525(6) 0.9649(2) 0.064 Uiso 1 calc R . C68 C 0.2874(5) 0.1284(6) 0.9008(2) 0.044(2) Uani 1 d . . H68 H 0.3004(5) 0.0548(6) 0.9010(2) 0.053 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.02667(15) 0.02187(15) 0.01801(13) -0.00092(9) -0.00099(10) -0.00196(10) W2 0.02046(14) 0.02149(14) 0.01951(14) 0.00212(9) -0.00211(10) 0.00081(10) Co1 0.0251(4) 0.0274(5) 0.0200(4) -0.0001(3) -0.0018(3) -0.0020(4) Co2 0.0227(4) 0.0218(4) 0.0196(4) 0.0014(3) -0.0013(3) 0.0010(3) P1 0.0255(8) 0.0254(9) 0.0221(8) -0.0021(7) 0.0007(7) -0.0027(7) P2 0.0232(8) 0.0231(8) 0.0214(8) 0.0009(6) 0.0015(6) 0.0005(7) O1 0.051(3) 0.034(3) 0.071(4) -0.010(3) 0.007(3) -0.013(3) O2 0.030(3) 0.053(3) 0.033(3) -0.007(2) 0.000(2) -0.020(2) O3 0.032(2) 0.046(3) 0.018(2) 0.001(2) 0.005(2) -0.009(2) O4 0.026(2) 0.034(3) 0.020(2) -0.003(2) 0.001(2) -0.007(2) O5 0.020(2) 0.043(3) 0.050(3) 0.003(2) -0.012(2) -0.002(2) O6 0.032(3) 0.024(3) 0.054(3) -0.004(2) -0.009(2) -0.005(2) O7 0.025(2) 0.030(2) 0.020(2) 0.004(2) 0.002(2) 0.001(2) O8 0.027(2) 0.033(3) 0.021(2) 0.003(2) 0.002(2) -0.004(2) O15 0.033(3) 0.089(5) 0.079(4) 0.013(4) -0.021(3) 0.005(3) O16 0.050(3) 0.033(3) 0.057(4) 0.009(2) -0.004(3) -0.004(3) O17 0.040(3) 0.024(3) 0.034(3) -0.004(2) -0.008(2) -0.008(2) O49 0.040(3) 0.055(4) 0.061(4) 0.000(3) -0.007(3) 0.022(3) O50 0.044(3) 0.035(3) 0.048(3) 0.002(2) -0.002(2) -0.014(2) O51 0.036(3) 0.038(3) 0.030(3) -0.002(2) -0.014(2) -0.012(2) C1 0.045(4) 0.059(5) 0.030(4) -0.003(4) -0.009(3) -0.014(4) C2 0.027(4) 0.067(6) 0.050(5) -0.010(4) -0.010(3) -0.012(4) C3 0.039(4) 0.046(5) 0.040(4) -0.011(3) -0.001(3) 0.004(4) C4 0.031(3) 0.031(4) 0.020(3) 0.000(3) -0.003(3) -0.006(3) C5 0.031(4) 0.049(4) 0.031(4) -0.007(3) 0.000(3) -0.009(3) C6 0.040(4) 0.054(5) 0.033(4) -0.016(4) 0.002(3) -0.012(4) C7 0.024(3) 0.032(4) 0.026(3) 0.004(3) 0.004(3) -0.006(3) C8 0.028(3) 0.033(4) 0.021(3) -0.001(3) 0.002(3) -0.005(3) C9 0.025(3) 0.029(4) 0.024(3) -0.003(3) -0.001(3) -0.005(3) C10 0.026(3) 0.024(3) 0.026(3) 0.001(3) 0.005(3) -0.006(3) C11 0.033(4) 0.040(4) 0.022(3) -0.010(3) 0.006(3) -0.009(3) C12 0.041(5) 0.077(7) 0.073(6) -0.020(5) 0.003(4) -0.031(5) C13 0.030(3) 0.024(3) 0.018(3) -0.005(2) -0.003(3) -0.006(3) C14 0.030(4) 0.063(5) 0.035(4) -0.004(4) 0.009(3) -0.022(4) C15 0.038(4) 0.045(4) 0.032(4) 0.001(3) 0.000(3) -0.006(4) C16 0.031(4) 0.030(4) 0.029(4) 0.003(3) -0.004(3) -0.001(3) C17 0.028(3) 0.039(4) 0.021(3) 0.009(3) 0.000(3) 0.000(3) C18 0.041(4) 0.035(4) 0.045(4) 0.018(3) 0.000(3) -0.002(3) C19 0.065(5) 0.019(4) 0.038(4) -0.008(3) -0.011(4) 0.007(3) C20 0.045(4) 0.033(4) 0.030(4) 0.007(3) 0.001(3) 0.019(3) C21 0.024(3) 0.032(4) 0.035(4) 0.007(3) -0.009(3) 0.003(3) C22 0.045(4) 0.034(4) 0.020(3) 0.008(3) -0.002(3) 0.004(3) C23 0.027(3) 0.025(3) 0.026(3) -0.003(3) -0.001(3) 0.000(3) C24 0.057(5) 0.034(4) 0.027(4) -0.009(3) 0.002(3) 0.007(4) C25 0.061(5) 0.059(6) 0.032(4) -0.009(4) 0.000(4) 0.003(4) C26 0.043(5) 0.049(5) 0.045(5) -0.026(4) 0.005(4) -0.009(4) C27 0.046(5) 0.028(4) 0.065(6) -0.013(4) 0.016(4) -0.007(3) C28 0.039(4) 0.031(4) 0.041(4) -0.006(3) 0.009(3) -0.004(3) C29 0.032(4) 0.036(4) 0.021(3) -0.011(3) 0.002(3) -0.004(3) C30 0.035(4) 0.046(5) 0.054(5) -0.004(4) 0.016(4) -0.008(4) C31 0.049(5) 0.049(5) 0.071(6) -0.002(4) 0.019(4) -0.019(4) C32 0.032(4) 0.077(6) 0.042(4) -0.018(4) 0.009(3) -0.026(4) C33 0.033(4) 0.073(6) 0.040(4) -0.003(4) 0.000(3) 0.002(4) C34 0.035(4) 0.046(5) 0.045(5) 0.001(4) 0.003(3) -0.001(4) C35 0.053(5) 0.117(9) 0.032(4) 0.019(5) -0.004(4) 0.043(6) C36 0.067(6) 0.138(10) 0.023(4) 0.008(5) 0.005(4) 0.043(7) C37 0.044(5) 0.093(7) 0.026(4) -0.003(4) -0.005(3) 0.029(5) C38 0.024(3) 0.044(4) 0.021(3) 0.002(3) -0.003(3) 0.005(3) C39 0.038(4) 0.061(5) 0.025(4) 0.001(3) 0.000(3) 0.022(4) C40 0.041(4) 0.083(7) 0.035(4) 0.002(4) -0.002(3) 0.031(4) C41 0.028(3) 0.031(3) 0.018(3) -0.003(3) -0.002(3) 0.003(3) C42 0.024(3) 0.025(3) 0.021(3) -0.003(3) 0.001(3) 0.001(3) C43 0.022(3) 0.026(3) 0.022(3) 0.001(3) -0.001(2) 0.002(3) C44 0.020(3) 0.028(3) 0.025(3) -0.005(3) 0.005(3) 0.003(3) C45 0.025(3) 0.032(4) 0.021(3) 0.000(3) -0.002(3) -0.002(3) C46 0.055(5) 0.045(5) 0.055(5) -0.004(4) -0.013(4) -0.022(4) C47 0.026(3) 0.016(3) 0.024(3) -0.007(2) -0.002(3) -0.007(3) C48 0.026(3) 0.041(4) 0.027(3) 0.004(3) 0.006(3) -0.009(3) C49 0.034(4) 0.037(4) 0.025(3) -0.002(3) -0.004(3) 0.005(3) C50 0.025(3) 0.036(4) 0.022(3) 0.003(3) 0.003(3) 0.005(3) C51 0.025(3) 0.038(4) 0.022(3) 0.005(3) -0.001(3) 0.009(3) C52 0.042(4) 0.006(3) 0.056(5) 0.009(3) -0.009(3) -0.005(3) C53 0.039(4) 0.028(4) 0.041(4) 0.020(3) 0.013(3) 0.004(3) C54 0.044(4) 0.032(4) 0.022(3) 0.011(3) -0.006(3) 0.013(3) C55 0.023(3) 0.027(4) 0.040(4) 0.011(3) -0.005(3) 0.011(3) C56 0.042(4) 0.023(3) 0.034(4) -0.002(3) 0.001(3) 0.014(3) C57 0.030(3) 0.036(4) 0.020(3) 0.006(3) 0.002(3) 0.004(3) C58 0.029(3) 0.029(4) 0.035(4) -0.001(3) 0.007(3) 0.002(3) C59 0.036(4) 0.040(4) 0.044(4) 0.002(3) 0.000(3) -0.014(3) C60 0.023(3) 0.053(5) 0.038(4) 0.011(4) 0.003(3) -0.004(3) C61 0.025(3) 0.044(4) 0.041(4) 0.005(3) 0.004(3) 0.006(3) C62 0.032(4) 0.036(4) 0.042(4) 0.002(3) 0.004(3) -0.004(3) C63 0.020(3) 0.030(3) 0.022(3) 0.002(3) 0.001(2) 0.001(3) C64 0.027(3) 0.034(4) 0.026(3) 0.001(3) 0.002(3) -0.001(3) C65 0.037(4) 0.027(4) 0.040(4) -0.009(3) 0.008(3) -0.003(3) C66 0.045(4) 0.052(5) 0.026(4) -0.015(3) 0.004(3) -0.004(4) C67 0.082(6) 0.053(5) 0.025(4) -0.003(4) -0.001(4) 0.019(5) C68 0.064(5) 0.037(4) 0.031(4) 0.000(3) 0.001(4) 0.021(4) _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 W1 C17 2.010(7) . ? W1 C10 2.142(7) . ? W1 O4 2.210(4) . ? W1 C18 2.281(7) . ? W1 C22 2.294(6) . ? W1 C19 2.327(7) . ? W1 C21 2.362(6) . ? W1 C20 2.383(7) . ? W1 P1 2.400(3) . ? W1 Co1 2.651(2) . ? W2 C51 1.986(7) . ? W2 C44 2.167(6) . ? W2 O7 2.203(4) . ? W2 C55 2.283(6) . ? W2 C56 2.306(6) . ? W2 C54 2.323(6) . ? W2 C53 2.354(6) . ? W2 C52 2.357(6) . ? W2 P2 2.394(2) . ? W2 Co2 2.653(2) . ? Co1 C15 1.778(8) . ? Co1 C16 1.779(7) . ? Co1 C10 1.968(7) . ? Co1 C9 2.102(6) . ? Co1 P1 2.197(2) . ? Co2 C50 1.778(7) . ? Co2 C49 1.785(7) . ? Co2 C44 1.962(7) . ? Co2 C43 2.089(6) . ? Co2 P2 2.186(2) . ? P1 C23 1.817(6) . ? P1 C29 1.828(7) . ? P2 C63 1.815(6) . ? P2 C57 1.820(7) . ? O1 C11 1.203(8) . ? O2 C11 1.338(8) . ? O2 C12 1.459(8) . ? O3 C13 1.325(7) . ? O3 C14 1.461(7) . ? O4 C13 1.252(7) . ? O5 C45 1.200(8) . ? O6 C45 1.344(8) . ? O6 C46 1.452(8) . ? O7 C47 1.247(7) . ? O8 C47 1.318(7) . ? O8 C48 1.450(7) . ? O15 C15 1.145(9) . ? O16 C16 1.149(8) . ? O17 C17 1.146(8) . ? O49 C49 1.140(8) . ? O50 C50 1.155(8) . ? O51 C51 1.148(8) . ? C1 C2 1.379(10) . ? C1 C6 1.391(10) . ? C1 H1 0.95 . ? C2 C3 1.380(10) . ? C2 H2 0.95 . ? C3 C4 1.384(9) . ? C3 H3 0.95 . ? C4 C5 1.392(9) . ? C4 C7 1.444(9) . ? C5 C6 1.370(9) . ? C5 H5 0.95 . ? C6 H6 0.95 . ? C7 C8 1.199(9) . ? C8 C9 1.441(9) . ? C9 C13 1.437(8) . ? C9 C10 1.457(8) . ? C10 C11 1.464(9) . ? C12 H12A 0.98 . ? C12 H12B 0.98 . ? C12 H12C 0.98 . ? C14 H14A 0.98 . ? C14 H14B 0.98 . ? C14 H14C 0.98 . ? C18 C19 1.434(10) . ? C18 C22 1.445(10) . ? C18 H18 0.95 . ? C19 C20 1.418(10) . ? C19 H19 0.95 . ? C20 C21 1.390(9) . ? C20 H20 0.95 . ? C21 C22 1.425(9) . ? C21 H21 0.95 . ? C22 H22 0.95 . ? C23 C28 1.384(9) . ? C23 C24 1.394(9) . ? C24 C25 1.392(10) . ? C24 H24 0.95 . ? C25 C26 1.370(11) . ? C25 H25 0.95 . ? C26 C27 1.372(11) . ? C26 H26 0.95 . ? C27 C28 1.402(10) . ? C27 H27 0.95 . ? C28 H28 0.95 . ? C29 C30 1.380(10) . ? C29 C34 1.390(10) . ? C30 C31 1.394(10) . ? C30 H30 0.95 . ? C31 C32 1.379(12) . ? C31 H31 0.95 . ? C32 C33 1.365(12) . ? C32 H32 0.95 . ? C33 C34 1.396(10) . ? C33 H33 0.95 . ? C34 H34 0.95 . ? C35 C36 1.370(12) . ? C35 C40 1.390(11) . ? C35 H35 0.95 . ? C36 C37 1.370(11) . ? C36 H36 0.95 . ? C37 C38 1.379(9) . ? C37 H37 0.95 . ? C38 C39 1.390(9) . ? C38 C41 1.431(9) . ? C39 C40 1.382(10) . ? C39 H39 0.95 . ? C40 H40 0.95 . ? C41 C42 1.188(8) . ? C42 C43 1.450(8) . ? C43 C47 1.450(8) . ? C43 C44 1.470(8) . ? C44 C45 1.483(9) . ? C46 H46A 0.98 . ? C46 H46B 0.98 . ? C46 H46C 0.98 . ? C48 H48A 0.98 . ? C48 H48B 0.98 . ? C48 H48C 0.98 . ? C52 C56 1.405(10) . ? C52 C53 1.411(10) . ? C52 H52 0.95 . ? C53 C54 1.423(10) . ? C53 H53 0.95 . ? C54 C55 1.414(9) . ? C54 H54 0.95 . ? C55 C56 1.431(9) . ? C55 H55 0.95 . ? C56 H56 0.95 . ? C57 C58 1.388(10) . ? C57 C62 1.400(9) . ? C58 C59 1.398(9) . ? C58 H58 0.95 . ? C59 C60 1.387(10) . ? C59 H59 0.95 . ? C60 C61 1.369(10) . ? C60 H60 0.95 . ? C61 C62 1.375(9) . ? C61 H61 0.95 . ? C62 H62 0.95 . ? C63 C68 1.380(9) . ? C63 C64 1.387(9) . ? C64 C65 1.396(9) . ? C64 H64 0.95 . ? C65 C66 1.385(10) . ? C65 H65 0.95 . ? C66 C67 1.360(10) . ? C66 H66 0.95 . ? C67 C68 1.406(10) . ? C67 H67 0.95 . ? C68 H68 0.95 . ? 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 C17 W1 C10 127.2(2) . . ? C17 W1 O4 85.5(2) . . ? C10 W1 O4 76.2(2) . . ? C17 W1 C18 126.7(3) . . ? C10 W1 C18 101.4(3) . . ? O4 W1 C18 131.3(2) . . ? C17 W1 C22 90.4(3) . . ? C10 W1 C22 137.0(2) . . ? O4 W1 C22 133.7(2) . . ? C18 W1 C22 36.8(2) . . ? C17 W1 C19 139.1(3) . . ? C10 W1 C19 92.2(3) . . ? O4 W1 C19 95.1(2) . . ? C18 W1 C19 36.2(3) . . ? C22 W1 C19 60.2(2) . . ? C17 W1 C21 81.1(3) . . ? C10 W1 C21 149.7(2) . . ? O4 W1 C21 98.5(2) . . ? C18 W1 C21 59.5(3) . . ? C22 W1 C21 35.6(2) . . ? C19 W1 C21 58.2(3) . . ? C17 W1 C20 106.6(3) . . ? C10 W1 C20 117.1(3) . . ? O4 W1 C20 78.4(2) . . ? C18 W1 C20 59.2(3) . . ? C22 W1 C20 58.8(2) . . ? C19 W1 C20 35.0(3) . . ? C21 W1 C20 34.1(2) . . ? C17 W1 P1 81.1(2) . . ? C10 W1 P1 74.3(2) . . ? O4 W1 P1 129.64(13) . . ? C18 W1 P1 94.2(2) . . ? C22 W1 P1 94.8(2) . . ? C19 W1 P1 125.7(2) . . ? C21 W1 P1 126.5(2) . . ? C20 W1 P1 151.9(2) . . ? C17 W1 Co1 81.2(2) . . ? C10 W1 Co1 47.0(2) . . ? O4 W1 Co1 78.84(13) . . ? C18 W1 Co1 134.6(2) . . ? C22 W1 Co1 145.8(2) . . ? C19 W1 Co1 139.2(2) . . ? C21 W1 Co1 162.3(2) . . ? C20 W1 Co1 155.2(2) . . ? P1 W1 Co1 51.27(6) . . ? C51 W2 C44 123.8(3) . . ? C51 W2 O7 83.0(2) . . ? C44 W2 O7 75.4(2) . . ? C51 W2 C55 87.1(3) . . ? C44 W2 C55 140.6(2) . . ? O7 W2 C55 86.4(2) . . ? C51 W2 C56 121.5(3) . . ? C44 W2 C56 105.3(2) . . ? O7 W2 C56 80.6(2) . . ? C55 W2 C56 36.3(2) . . ? C51 W2 C54 83.2(3) . . ? C44 W2 C54 151.6(3) . . ? O7 W2 C54 120.9(2) . . ? C55 W2 C54 35.7(2) . . ? C56 W2 C54 59.7(2) . . ? C51 W2 C53 113.6(3) . . ? C44 W2 C53 116.7(3) . . ? O7 W2 C53 139.1(2) . . ? C55 W2 C53 59.1(2) . . ? C56 W2 C53 58.7(2) . . ? C54 W2 C53 35.4(2) . . ? C51 W2 C52 141.6(3) . . ? C44 W2 C52 94.6(2) . . ? O7 W2 C52 110.2(2) . . ? C55 W2 C52 59.1(2) . . ? C56 W2 C52 35.1(2) . . ? C54 W2 C52 58.8(3) . . ? C53 W2 C52 34.9(2) . . ? C51 W2 P2 82.4(2) . . ? C44 W2 P2 75.5(2) . . ? O7 W2 P2 131.76(12) . . ? C55 W2 P2 138.1(2) . . ? C56 W2 P2 144.4(2) . . ? C54 W2 P2 102.5(2) . . ? C53 W2 P2 88.6(2) . . ? C52 W2 P2 109.7(2) . . ? C51 W2 Co2 79.4(2) . . ? C44 W2 Co2 46.7(2) . . ? O7 W2 Co2 81.16(12) . . ? C55 W2 Co2 162.6(2) . . ? C56 W2 Co2 150.0(2) . . ? C54 W2 Co2 149.9(2) . . ? C53 W2 Co2 136.8(2) . . ? C52 W2 Co2 137.0(2) . . ? P2 W2 Co2 51.02(5) . . ? C15 Co1 C16 101.9(3) . . ? C15 Co1 C10 108.7(3) . . ? C16 Co1 C10 142.6(3) . . ? C15 Co1 C9 103.0(3) . . ? C16 Co1 C9 111.0(3) . . ? C10 Co1 C9 41.8(2) . . ? C15 Co1 P1 101.7(2) . . ? C16 Co1 P1 112.0(2) . . ? C10 Co1 P1 82.5(2) . . ? C9 Co1 P1 123.8(2) . . ? C15 Co1 W1 151.7(2) . . ? C16 Co1 W1 104.3(2) . . ? C10 Co1 W1 52.8(2) . . ? C9 Co1 W1 77.3(2) . . ? P1 Co1 W1 58.47(7) . . ? C50 Co2 C49 103.1(3) . . ? C50 Co2 C44 148.3(3) . . ? C49 Co2 C44 104.0(3) . . ? C50 Co2 C43 114.9(3) . . ? C49 Co2 C43 103.0(3) . . ? C44 Co2 C43 42.4(2) . . ? C50 Co2 P2 107.4(2) . . ? C49 Co2 P2 98.2(2) . . ? C44 Co2 P2 84.6(2) . . ? C43 Co2 P2 126.1(2) . . ? C50 Co2 W2 107.3(2) . . ? C49 Co2 W2 145.9(2) . . ? C44 Co2 W2 53.5(2) . . ? C43 Co2 W2 77.7(2) . . ? P2 Co2 W2 58.35(6) . . ? C23 P1 C29 99.3(3) . . ? C23 P1 Co1 122.2(2) . . ? C29 P1 Co1 116.5(2) . . ? C23 P1 W1 119.6(2) . . ? C29 P1 W1 129.4(2) . . ? Co1 P1 W1 70.27(7) . . ? C63 P2 C57 101.4(3) . . ? C63 P2 Co2 118.5(2) . . ? C57 P2 Co2 116.6(2) . . ? C63 P2 W2 123.7(2) . . ? C57 P2 W2 124.7(2) . . ? Co2 P2 W2 70.63(7) . . ? C11 O2 C12 116.7(6) . . ? C13 O3 C14 117.7(5) . . ? C13 O4 W1 112.6(4) . . ? C45 O6 C46 115.2(6) . . ? C47 O7 W2 113.8(4) . . ? C47 O8 C48 115.6(5) . . ? C2 C1 C6 118.8(7) . . ? C2 C1 H1 120.6(4) . . ? C6 C1 H1 120.6(4) . . ? C1 C2 C3 120.7(7) . . ? C1 C2 H2 119.7(4) . . ? C3 C2 H2 119.7(4) . . ? C2 C3 C4 121.0(7) . . ? C2 C3 H3 119.5(4) . . ? C4 C3 H3 119.5(4) . . ? C3 C4 C5 117.8(6) . . ? C3 C4 C7 120.1(6) . . ? C5 C4 C7 122.1(6) . . ? C6 C5 C4 121.6(7) . . ? C6 C5 H5 119.2(4) . . ? C4 C5 H5 119.2(4) . . ? C5 C6 C1 120.1(7) . . ? C5 C6 H6 119.9(4) . . ? C1 C6 H6 119.9(4) . . ? C8 C7 C4 176.2(6) . . ? C7 C8 C9 169.1(7) . . ? C13 C9 C8 120.9(5) . . ? C13 C9 C10 112.8(5) . . ? C8 C9 C10 121.2(5) . . ? C13 C9 Co1 101.8(4) . . ? C8 C9 Co1 121.5(5) . . ? C10 C9 Co1 64.2(3) . . ? C9 C10 C11 117.4(6) . . ? C9 C10 Co1 74.0(4) . . ? C11 C10 Co1 126.7(5) . . ? C9 C10 W1 111.4(4) . . ? C11 C10 W1 128.8(5) . . ? Co1 C10 W1 80.2(2) . . ? O1 C11 O2 122.4(6) . . ? O1 C11 C10 123.2(7) . . ? O2 C11 C10 114.3(6) . . ? O2 C12 H12A 109.5(5) . . ? O2 C12 H12B 109.5(4) . . ? H12A C12 H12B 109.5 . . ? O2 C12 H12C 109.5(4) . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O4 C13 O3 121.0(5) . . ? O4 C13 C9 122.1(5) . . ? O3 C13 C9 116.8(5) . . ? O3 C14 H14A 109.5(3) . . ? O3 C14 H14B 109.5(4) . . ? H14A C14 H14B 109.5 . . ? O3 C14 H14C 109.5(4) . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O15 C15 Co1 177.0(7) . . ? O16 C16 Co1 178.6(6) . . ? O17 C17 W1 177.5(5) . . ? C19 C18 C22 107.2(6) . . ? C19 C18 W1 73.6(4) . . ? C22 C18 W1 72.1(4) . . ? C19 C18 H18 126.4(4) . . ? C22 C18 H18 126.4(4) . . ? W1 C18 H18 119.8(2) . . ? C20 C19 C18 107.9(6) . . ? C20 C19 W1 74.7(4) . . ? C18 C19 W1 70.1(4) . . ? C20 C19 H19 126.1(4) . . ? C18 C19 H19 126.1(4) . . ? W1 C19 H19 120.9(2) . . ? C21 C20 C19 108.7(6) . . ? C21 C20 W1 72.1(4) . . ? C19 C20 W1 70.3(4) . . ? C21 C20 H20 125.6(4) . . ? C19 C20 H20 125.6(4) . . ? W1 C20 H20 123.5(2) . . ? C20 C21 C22 109.4(6) . . ? C20 C21 W1 73.8(4) . . ? C22 C21 W1 69.6(4) . . ? C20 C21 H21 125.3(4) . . ? C22 C21 H21 125.3(4) . . ? W1 C21 H21 122.9(2) . . ? C21 C22 C18 106.8(6) . . ? C21 C22 W1 74.8(4) . . ? C18 C22 W1 71.1(4) . . ? C21 C22 H22 126.6(4) . . ? C18 C22 H22 126.6(4) . . ? W1 C22 H22 119.4(2) . . ? C28 C23 C24 118.2(6) . . ? C28 C23 P1 122.9(5) . . ? C24 C23 P1 118.8(5) . . ? C25 C24 C23 120.5(7) . . ? C25 C24 H24 119.7(5) . . ? C23 C24 H24 119.7(4) . . ? C26 C25 C24 120.2(7) . . ? C26 C25 H25 119.9(5) . . ? C24 C25 H25 119.9(5) . . ? C25 C26 C27 120.6(7) . . ? C25 C26 H26 119.7(5) . . ? C27 C26 H26 119.7(4) . . ? C26 C27 C28 119.3(7) . . ? C26 C27 H27 120.3(4) . . ? C28 C27 H27 120.3(5) . . ? C23 C28 C27 121.1(7) . . ? C23 C28 H28 119.5(4) . . ? C27 C28 H28 119.5(5) . . ? C30 C29 C34 117.7(6) . . ? C30 C29 P1 124.4(5) . . ? C34 C29 P1 117.9(5) . . ? C29 C30 C31 121.6(8) . . ? C29 C30 H30 119.2(4) . . ? C31 C30 H30 119.2(5) . . ? C32 C31 C30 119.8(8) . . ? C32 C31 H31 120.1(5) . . ? C30 C31 H31 120.1(5) . . ? C33 C32 C31 119.5(7) . . ? C33 C32 H32 120.3(5) . . ? C31 C32 H32 120.3(5) . . ? C32 C33 C34 120.8(8) . . ? C32 C33 H33 119.6(5) . . ? C34 C33 H33 119.6(5) . . ? C29 C34 C33 120.6(8) . . ? C29 C34 H34 119.7(4) . . ? C33 C34 H34 119.7(5) . . ? C36 C35 C40 118.8(7) . . ? C36 C35 H35 120.6(5) . . ? C40 C35 H35 120.6(5) . . ? C35 C36 C37 121.8(8) . . ? C35 C36 H36 119.1(5) . . ? C37 C36 H36 119.1(5) . . ? C36 C37 C38 120.4(7) . . ? C36 C37 H37 119.8(5) . . ? C38 C37 H37 119.8(4) . . ? C37 C38 C39 118.1(6) . . ? C37 C38 C41 122.8(6) . . ? C39 C38 C41 119.1(6) . . ? C40 C39 C38 121.5(7) . . ? C40 C39 H39 119.2(4) . . ? C38 C39 H39 119.2(4) . . ? C39 C40 C35 119.3(7) . . ? C39 C40 H40 120.3(4) . . ? C35 C40 H40 120.3(5) . . ? C42 C41 C38 172.2(7) . . ? C41 C42 C43 176.9(6) . . ? C42 C43 C47 119.6(5) . . ? C42 C43 C44 124.4(5) . . ? C47 C43 C44 112.0(5) . . ? C42 C43 Co2 115.8(4) . . ? C47 C43 Co2 106.0(4) . . ? C44 C43 Co2 64.2(3) . . ? C43 C44 C45 115.9(5) . . ? C43 C44 Co2 73.4(4) . . ? C45 C44 Co2 122.6(4) . . ? C43 C44 W2 110.1(4) . . ? C45 C44 W2 132.8(4) . . ? Co2 C44 W2 79.8(2) . . ? O5 C45 O6 122.6(6) . . ? O5 C45 C44 126.1(6) . . ? O6 C45 C44 111.2(5) . . ? O6 C46 H46A 109.5(4) . . ? O6 C46 H46B 109.5(4) . . ? H46A C46 H46B 109.5 . . ? O6 C46 H46C 109.5(4) . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? O7 C47 O8 120.7(5) . . ? O7 C47 C43 121.2(5) . . ? O8 C47 C43 118.0(5) . . ? O8 C48 H48A 109.5(3) . . ? O8 C48 H48B 109.5(3) . . ? H48A C48 H48B 109.5 . . ? O8 C48 H48C 109.5(3) . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? O49 C49 Co2 176.4(6) . . ? O50 C50 Co2 174.5(5) . . ? O51 C51 W2 175.4(5) . . ? C56 C52 C53 108.4(6) . . ? C56 C52 W2 70.5(3) . . ? C53 C52 W2 72.5(4) . . ? C56 C52 H52 125.8(4) . . ? C53 C52 H52 125.8(4) . . ? W2 C52 H52 122.9(2) . . ? C52 C53 C54 108.4(6) . . ? C52 C53 W2 72.7(3) . . ? C54 C53 W2 71.1(3) . . ? C52 C53 H53 125.8(4) . . ? C54 C53 H53 125.8(4) . . ? W2 C53 H53 122.1(2) . . ? C55 C54 C53 107.4(6) . . ? C55 C54 W2 70.6(3) . . ? C53 C54 W2 73.5(4) . . ? C55 C54 H54 126.3(4) . . ? C53 C54 H54 126.3(4) . . ? W2 C54 H54 121.3(2) . . ? C54 C55 C56 108.1(6) . . ? C54 C55 W2 73.6(3) . . ? C56 C55 W2 72.7(4) . . ? C54 C55 H55 125.9(4) . . ? C56 C55 H55 125.9(4) . . ? W2 C55 H55 119.6(2) . . ? C52 C56 C55 107.7(6) . . ? C52 C56 W2 74.5(3) . . ? C55 C56 W2 71.0(3) . . ? C52 C56 H56 126.1(4) . . ? C55 C56 H56 126.1(4) . . ? W2 C56 H56 120.2(2) . . ? C58 C57 C62 117.6(6) . . ? C58 C57 P2 122.0(5) . . ? C62 C57 P2 120.3(5) . . ? C57 C58 C59 121.1(6) . . ? C57 C58 H58 119.4(4) . . ? C59 C58 H58 119.4(4) . . ? C60 C59 C58 119.6(7) . . ? C60 C59 H59 120.2(4) . . ? C58 C59 H59 120.2(4) . . ? C61 C60 C59 119.7(7) . . ? C61 C60 H60 120.2(4) . . ? C59 C60 H60 120.2(4) . . ? C60 C61 C62 120.9(7) . . ? C60 C61 H61 119.6(4) . . ? C62 C61 H61 119.6(4) . . ? C61 C62 C57 121.1(7) . . ? C61 C62 H62 119.5(4) . . ? C57 C62 H62 119.5(4) . . ? C68 C63 C64 118.7(6) . . ? C68 C63 P2 120.2(5) . . ? C64 C63 P2 121.0(5) . . ? C63 C64 C65 121.4(6) . . ? C63 C64 H64 119.3(4) . . ? C65 C64 H64 119.3(4) . . ? C66 C65 C64 118.4(7) . . ? C66 C65 H65 120.8(4) . . ? C64 C65 H65 120.8(4) . . ? C67 C66 C65 121.3(7) . . ? C67 C66 H66 119.3(5) . . ? C65 C66 H66 119.3(4) . . ? C66 C67 C68 119.7(7) . . ? C66 C67 H67 120.1(5) . . ? C68 C67 H67 120.1(4) . . ? C63 C68 C67 120.4(7) . . ? C63 C68 H68 119.8(4) . . ? C67 C68 H68 119.8(4) . . ? 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 C17 W1 Co1 C15 135.8(5) . . . . ? C10 W1 Co1 C15 -55.7(5) . . . . ? O4 W1 Co1 C15 -137.2(5) . . . . ? C18 W1 Co1 C15 1.5(6) . . . . ? C22 W1 Co1 C15 58.2(6) . . . . ? C19 W1 Co1 C15 -52.3(6) . . . . ? C21 W1 Co1 C15 139.9(7) . . . . ? C20 W1 Co1 C15 -113.5(7) . . . . ? P1 W1 Co1 C15 50.2(5) . . . . ? C17 W1 Co1 C16 -21.7(3) . . . . ? C10 W1 Co1 C16 146.8(3) . . . . ? O4 W1 Co1 C16 65.3(2) . . . . ? C18 W1 Co1 C16 -156.0(3) . . . . ? C22 W1 Co1 C16 -99.3(4) . . . . ? C19 W1 Co1 C16 150.2(4) . . . . ? C21 W1 Co1 C16 -17.6(6) . . . . ? C20 W1 Co1 C16 89.0(5) . . . . ? P1 W1 Co1 C16 -107.3(2) . . . . ? C17 W1 Co1 C10 -168.5(3) . . . . ? C10 W1 Co1 C10 0.000(3) . . . . ? O4 W1 Co1 C10 -81.4(2) . . . . ? C18 W1 Co1 C10 57.2(3) . . . . ? C22 W1 Co1 C10 114.0(4) . . . . ? C19 W1 Co1 C10 3.5(4) . . . . ? C21 W1 Co1 C10 -164.4(6) . . . . ? C20 W1 Co1 C10 -57.7(5) . . . . ? P1 W1 Co1 C10 105.9(2) . . . . ? C17 W1 Co1 C9 -130.5(2) . . . . ? C10 W1 Co1 C9 38.0(3) . . . . ? O4 W1 Co1 C9 -43.4(2) . . . . ? C18 W1 Co1 C9 95.2(3) . . . . ? C22 W1 Co1 C9 152.0(4) . . . . ? C19 W1 Co1 C9 41.4(3) . . . . ? C21 W1 Co1 C9 -126.4(5) . . . . ? C20 W1 Co1 C9 -19.7(5) . . . . ? P1 W1 Co1 C9 143.9(2) . . . . ? C17 W1 Co1 P1 85.6(2) . . . . ? C10 W1 Co1 P1 -105.9(2) . . . . ? O4 W1 Co1 P1 172.66(12) . . . . ? C18 W1 Co1 P1 -48.7(3) . . . . ? C22 W1 Co1 P1 8.1(3) . . . . ? C19 W1 Co1 P1 -102.4(3) . . . . ? C21 W1 Co1 P1 89.7(5) . . . . ? C20 W1 Co1 P1 -163.6(4) . . . . ? P1 W1 Co1 P1 0.0 . . . . ? C51 W2 Co2 C50 11.3(3) . . . . ? C44 W2 Co2 C50 -151.3(3) . . . . ? O7 W2 Co2 C50 -73.1(2) . . . . ? C55 W2 Co2 C50 -28.3(6) . . . . ? C56 W2 Co2 C50 -126.3(4) . . . . ? C54 W2 Co2 C50 67.0(4) . . . . ? C53 W2 Co2 C50 124.6(3) . . . . ? C52 W2 Co2 C50 176.6(3) . . . . ? P2 W2 Co2 C50 100.1(2) . . . . ? C51 W2 Co2 C49 -141.1(4) . . . . ? C44 W2 Co2 C49 56.3(4) . . . . ? O7 W2 Co2 C49 134.5(4) . . . . ? C55 W2 Co2 C49 179.3(7) . . . . ? C56 W2 Co2 C49 81.3(5) . . . . ? C54 W2 Co2 C49 -85.4(5) . . . . ? C53 W2 Co2 C49 -27.8(5) . . . . ? C52 W2 Co2 C49 24.2(5) . . . . ? P2 W2 Co2 C49 -52.3(4) . . . . ? C51 W2 Co2 C44 162.6(3) . . . . ? C44 W2 Co2 C44 0.000(2) . . . . ? O7 W2 Co2 C44 78.2(2) . . . . ? C55 W2 Co2 C44 123.0(6) . . . . ? C56 W2 Co2 C44 25.0(4) . . . . ? C54 W2 Co2 C44 -141.7(4) . . . . ? C53 W2 Co2 C44 -84.1(3) . . . . ? C52 W2 Co2 C44 -32.1(3) . . . . ? P2 W2 Co2 C44 -108.6(2) . . . . ? C51 W2 Co2 C43 123.8(2) . . . . ? C44 W2 Co2 C43 -38.8(3) . . . . ? O7 W2 Co2 C43 39.4(2) . . . . ? C55 W2 Co2 C43 84.2(6) . . . . ? C56 W2 Co2 C43 -13.8(4) . . . . ? C54 W2 Co2 C43 179.5(4) . . . . ? C53 W2 Co2 C43 -122.9(3) . . . . ? C52 W2 Co2 C43 -70.9(3) . . . . ? P2 W2 Co2 C43 -147.4(2) . . . . ? C51 W2 Co2 P2 -88.8(2) . . . . ? C44 W2 Co2 P2 108.6(2) . . . . ? O7 W2 Co2 P2 -173.20(12) . . . . ? C55 W2 Co2 P2 -128.4(6) . . . . ? C56 W2 Co2 P2 133.6(4) . . . . ? C54 W2 Co2 P2 -33.1(4) . . . . ? C53 W2 Co2 P2 24.5(3) . . . . ? C52 W2 Co2 P2 76.5(3) . . . . ? P2 W2 Co2 P2 0.0 . . . . ? C15 Co1 P1 C23 88.6(3) . . . . ? C16 Co1 P1 C23 -19.6(3) . . . . ? C10 Co1 P1 C23 -163.7(3) . . . . ? C9 Co1 P1 C23 -157.0(3) . . . . ? W1 Co1 P1 C23 -113.2(3) . . . . ? C15 Co1 P1 C29 -33.2(4) . . . . ? C16 Co1 P1 C29 -141.3(3) . . . . ? C10 Co1 P1 C29 74.5(3) . . . . ? C9 Co1 P1 C29 81.3(3) . . . . ? W1 Co1 P1 C29 125.1(3) . . . . ? C15 Co1 P1 W1 -158.2(3) . . . . ? C16 Co1 P1 W1 93.6(2) . . . . ? C10 Co1 P1 W1 -50.6(2) . . . . ? C9 Co1 P1 W1 -43.8(2) . . . . ? W1 Co1 P1 W1 0.0 . . . . ? C17 W1 P1 C23 30.7(3) . . . . ? C10 W1 P1 C23 163.5(3) . . . . ? O4 W1 P1 C23 107.2(3) . . . . ? C18 W1 P1 C23 -95.9(3) . . . . ? C22 W1 P1 C23 -58.9(3) . . . . ? C19 W1 P1 C23 -115.3(3) . . . . ? C21 W1 P1 C23 -41.2(3) . . . . ? C20 W1 P1 C23 -78.0(5) . . . . ? Co1 W1 P1 C23 116.5(3) . . . . ? C17 W1 P1 C29 165.6(3) . . . . ? C10 W1 P1 C29 -61.6(3) . . . . ? O4 W1 P1 C29 -117.9(3) . . . . ? C18 W1 P1 C29 39.0(3) . . . . ? C22 W1 P1 C29 76.0(3) . . . . ? C19 W1 P1 C29 19.6(4) . . . . ? C21 W1 P1 C29 93.7(3) . . . . ? C20 W1 P1 C29 56.9(5) . . . . ? Co1 W1 P1 C29 -108.5(3) . . . . ? C17 W1 P1 Co1 -85.8(2) . . . . ? C10 W1 P1 Co1 46.9(2) . . . . ? O4 W1 P1 Co1 -9.4(2) . . . . ? C18 W1 P1 Co1 147.6(2) . . . . ? C22 W1 P1 Co1 -175.5(2) . . . . ? C19 W1 P1 Co1 128.2(2) . . . . ? C21 W1 P1 Co1 -157.8(2) . . . . ? C20 W1 P1 Co1 165.5(4) . . . . ? Co1 W1 P1 Co1 0.0 . . . . ? C50 Co2 P2 C63 18.6(3) . . . . ? C49 Co2 P2 C63 -88.0(3) . . . . ? C44 Co2 P2 C63 168.6(3) . . . . ? C43 Co2 P2 C63 159.3(3) . . . . ? W2 Co2 P2 C63 118.6(2) . . . . ? C50 Co2 P2 C57 140.0(3) . . . . ? C49 Co2 P2 C57 33.4(3) . . . . ? C44 Co2 P2 C57 -70.0(3) . . . . ? C43 Co2 P2 C57 -79.3(3) . . . . ? W2 Co2 P2 C57 -119.9(3) . . . . ? C50 Co2 P2 W2 -100.0(2) . . . . ? C49 Co2 P2 W2 153.4(2) . . . . ? C44 Co2 P2 W2 49.9(2) . . . . ? C43 Co2 P2 W2 40.6(2) . . . . ? W2 Co2 P2 W2 0.0 . . . . ? C51 W2 P2 C63 -29.4(3) . . . . ? C44 W2 P2 C63 -157.3(3) . . . . ? O7 W2 P2 C63 -102.9(3) . . . . ? C55 W2 P2 C63 47.6(4) . . . . ? C56 W2 P2 C63 106.6(4) . . . . ? C54 W2 P2 C63 51.8(3) . . . . ? C53 W2 P2 C63 84.6(3) . . . . ? C52 W2 P2 C63 112.9(3) . . . . ? Co2 W2 P2 C63 -111.9(3) . . . . ? C51 W2 P2 C57 -168.1(3) . . . . ? C44 W2 P2 C57 64.0(3) . . . . ? O7 W2 P2 C57 118.5(3) . . . . ? C55 W2 P2 C57 -91.1(4) . . . . ? C56 W2 P2 C57 -32.1(4) . . . . ? C54 W2 P2 C57 -86.8(3) . . . . ? C53 W2 P2 C57 -54.0(3) . . . . ? C52 W2 P2 C57 -25.8(3) . . . . ? Co2 W2 P2 C57 109.4(3) . . . . ? C51 W2 P2 Co2 82.5(2) . . . . ? C44 W2 P2 Co2 -45.5(2) . . . . ? O7 W2 P2 Co2 9.0(2) . . . . ? C55 W2 P2 Co2 159.5(3) . . . . ? C56 W2 P2 Co2 -141.5(3) . . . . ? C54 W2 P2 Co2 163.7(2) . . . . ? C53 W2 P2 Co2 -163.5(2) . . . . ? C52 W2 P2 Co2 -135.2(2) . . . . ? Co2 W2 P2 Co2 0.0 . . . . ? C17 W1 O4 C13 113.3(5) . . . . ? C10 W1 O4 C13 -16.8(4) . . . . ? C18 W1 O4 C13 -109.8(5) . . . . ? C22 W1 O4 C13 -160.5(4) . . . . ? C19 W1 O4 C13 -107.7(5) . . . . ? C21 W1 O4 C13 -166.4(4) . . . . ? C20 W1 O4 C13 -138.7(5) . . . . ? P1 W1 O4 C13 38.8(5) . . . . ? Co1 W1 O4 C13 31.4(4) . . . . ? C51 W2 O7 C47 -107.6(4) . . . . ? C44 W2 O7 C47 20.1(4) . . . . ? C55 W2 O7 C47 164.8(4) . . . . ? C56 W2 O7 C47 128.7(4) . . . . ? C54 W2 O7 C47 174.7(4) . . . . ? C53 W2 O7 C47 134.1(4) . . . . ? C52 W2 O7 C47 109.6(4) . . . . ? P2 W2 O7 C47 -34.4(5) . . . . ? Co2 W2 O7 C47 -27.4(4) . . . . ? C6 C1 C2 C3 -0.9(12) . . . . ? C1 C2 C3 C4 1.5(13) . . . . ? C2 C3 C4 C5 -1.7(11) . . . . ? C2 C3 C4 C7 176.1(7) . . . . ? C3 C4 C5 C6 1.3(11) . . . . ? C7 C4 C5 C6 -176.4(7) . . . . ? C4 C5 C6 C1 -0.8(12) . . . . ? C2 C1 C6 C5 0.6(12) . . . . ? C3 C4 C7 C8 -39.6(111) . . . . ? C5 C4 C7 C8 138.1(107) . . . . ? C4 C7 C8 C9 -25.2(136) . . . . ? C7 C8 C9 C13 -142.8(34) . . . . ? C7 C8 C9 C10 10.1(40) . . . . ? C7 C8 C9 Co1 87.0(37) . . . . ? C15 Co1 C9 C13 -146.5(4) . . . . ? C16 Co1 C9 C13 -38.1(5) . . . . ? C10 Co1 C9 C13 109.8(6) . . . . ? P1 Co1 C9 C13 99.7(4) . . . . ? W1 Co1 C9 C13 62.5(4) . . . . ? C15 Co1 C9 C8 -8.6(6) . . . . ? C16 Co1 C9 C8 99.9(5) . . . . ? C10 Co1 C9 C8 -112.3(6) . . . . ? P1 Co1 C9 C8 -122.4(5) . . . . ? W1 Co1 C9 C8 -159.6(5) . . . . ? C15 Co1 C9 C10 103.7(4) . . . . ? C16 Co1 C9 C10 -147.9(4) . . . . ? C10 Co1 C9 C10 0.000(5) . . . . ? P1 Co1 C9 C10 -10.1(4) . . . . ? W1 Co1 C9 C10 -47.3(3) . . . . ? C13 C9 C10 C11 144.1(6) . . . . ? C8 C9 C10 C11 -10.8(9) . . . . ? Co1 C9 C10 C11 -123.5(6) . . . . ? C13 C9 C10 Co1 -92.4(5) . . . . ? C8 C9 C10 Co1 112.7(6) . . . . ? Co1 C9 C10 Co1 0.000(3) . . . . ? C13 C9 C10 W1 -20.0(7) . . . . ? C8 C9 C10 W1 -174.9(5) . . . . ? Co1 C9 C10 W1 72.4(3) . . . . ? C15 Co1 C10 C9 -88.6(4) . . . . ? C16 Co1 C10 C9 54.7(6) . . . . ? C9 Co1 C10 C9 0.000(5) . . . . ? P1 Co1 C10 C9 171.5(4) . . . . ? W1 Co1 C10 C9 115.8(4) . . . . ? C15 Co1 C10 C11 23.9(6) . . . . ? C16 Co1 C10 C11 167.3(5) . . . . ? C9 Co1 C10 C11 112.6(7) . . . . ? P1 Co1 C10 C11 -75.9(5) . . . . ? W1 Co1 C10 C11 -131.7(6) . . . . ? C15 Co1 C10 W1 155.6(3) . . . . ? C16 Co1 C10 W1 -61.0(5) . . . . ? C9 Co1 C10 W1 -115.8(4) . . . . ? P1 Co1 C10 W1 55.77(13) . . . . ? W1 Co1 C10 W1 0.000(2) . . . . ? C17 W1 C10 C9 -54.1(5) . . . . ? O4 W1 C10 C9 19.1(4) . . . . ? C18 W1 C10 C9 149.2(5) . . . . ? C22 W1 C10 C9 160.3(4) . . . . ? C19 W1 C10 C9 113.8(5) . . . . ? C21 W1 C10 C9 102.2(6) . . . . ? C20 W1 C10 C9 88.1(5) . . . . ? P1 W1 C10 C9 -119.6(5) . . . . ? Co1 W1 C10 C9 -68.5(4) . . . . ? C17 W1 C10 C11 144.1(5) . . . . ? O4 W1 C10 C11 -142.7(6) . . . . ? C18 W1 C10 C11 -12.6(6) . . . . ? C22 W1 C10 C11 -1.5(7) . . . . ? C19 W1 C10 C11 -48.0(6) . . . . ? C21 W1 C10 C11 -59.6(8) . . . . ? C20 W1 C10 C11 -73.7(6) . . . . ? P1 W1 C10 C11 78.6(6) . . . . ? Co1 W1 C10 C11 129.7(6) . . . . ? C17 W1 C10 Co1 14.3(3) . . . . ? O4 W1 C10 Co1 87.5(2) . . . . ? C18 W1 C10 Co1 -142.4(2) . . . . ? C22 W1 C10 Co1 -131.2(3) . . . . ? C19 W1 C10 Co1 -177.7(2) . . . . ? C21 W1 C10 Co1 170.6(3) . . . . ? C20 W1 C10 Co1 156.5(2) . . . . ? P1 W1 C10 Co1 -51.18(13) . . . . ? Co1 W1 C10 Co1 0.000(2) . . . . ? C12 O2 C11 O1 1.2(9) . . . . ? C12 O2 C11 C10 -177.4(6) . . . . ? C9 C10 C11 O1 -106.2(8) . . . . ? Co1 C10 C11 O1 163.8(5) . . . . ? W1 C10 C11 O1 54.7(9) . . . . ? C9 C10 C11 O2 72.5(7) . . . . ? Co1 C10 C11 O2 -17.5(8) . . . . ? W1 C10 C11 O2 -126.6(5) . . . . ? W1 O4 C13 O3 -171.5(4) . . . . ? W1 O4 C13 C9 11.2(7) . . . . ? C14 O3 C13 O4 4.4(9) . . . . ? C14 O3 C13 C9 -178.1(6) . . . . ? C8 C9 C13 O4 160.8(6) . . . . ? C10 C9 C13 O4 5.8(9) . . . . ? Co1 C9 C13 O4 -60.9(7) . . . . ? C8 C9 C13 O3 -16.7(9) . . . . ? C10 C9 C13 O3 -171.7(5) . . . . ? Co1 C9 C13 O3 121.6(5) . . . . ? C16 Co1 C15 O15 3.5(129) . . . . ? C10 Co1 C15 O15 161.7(128) . . . . ? C9 Co1 C15 O15 118.6(128) . . . . ? P1 Co1 C15 O15 -112.3(128) . . . . ? W1 Co1 C15 O15 -154.2(125) . . . . ? C15 Co1 C16 O16 -31.0(226) . . . . ? C10 Co1 C16 O16 -175.7(1000) . . . . ? C9 Co1 C16 O16 -140.1(225) . . . . ? P1 Co1 C16 O16 77.0(226) . . . . ? W1 Co1 C16 O16 138.3(225) . . . . ? C10 W1 C17 O17 -160.9(122) . . . . ? O4 W1 C17 O17 130.2(123) . . . . ? C18 W1 C17 O17 -9.9(124) . . . . ? C22 W1 C17 O17 -3.7(123) . . . . ? C19 W1 C17 O17 37.6(125) . . . . ? C21 W1 C17 O17 30.9(123) . . . . ? C20 W1 C17 O17 53.7(124) . . . . ? P1 W1 C17 O17 -98.5(123) . . . . ? Co1 W1 C17 O17 -150.4(123) . . . . ? C17 W1 C18 C19 125.2(5) . . . . ? C10 W1 C18 C19 -78.0(5) . . . . ? O4 W1 C18 C19 3.5(6) . . . . ? C22 W1 C18 C19 114.8(6) . . . . ? C19 W1 C18 C19 0.000(6) . . . . ? C21 W1 C18 C19 76.7(5) . . . . ? C20 W1 C18 C19 36.9(4) . . . . ? P1 W1 C18 C19 -152.8(4) . . . . ? Co1 W1 C18 C19 -116.8(4) . . . . ? C17 W1 C18 C22 10.4(5) . . . . ? C10 W1 C18 C22 167.3(4) . . . . ? O4 W1 C18 C22 -111.2(4) . . . . ? C22 W1 C18 C22 0.000(3) . . . . ? C19 W1 C18 C22 -114.8(6) . . . . ? C21 W1 C18 C22 -38.0(4) . . . . ? C20 W1 C18 C22 -77.8(4) . . . . ? P1 W1 C18 C22 92.4(4) . . . . ? Co1 W1 C18 C22 128.4(4) . . . . ? C22 C18 C19 C20 -0.9(8) . . . . ? W1 C18 C19 C20 -65.7(5) . . . . ? C22 C18 C19 W1 64.7(5) . . . . ? W1 C18 C19 W1 0.000(3) . . . . ? C17 W1 C19 C20 27.6(6) . . . . ? C10 W1 C19 C20 -137.7(4) . . . . ? O4 W1 C19 C20 -61.4(4) . . . . ? C18 W1 C19 C20 116.0(6) . . . . ? C22 W1 C19 C20 77.1(4) . . . . ? C21 W1 C19 C20 35.5(4) . . . . ? C20 W1 C19 C20 0.0 . . . . ? P1 W1 C19 C20 150.1(3) . . . . ? Co1 W1 C19 C20 -140.2(3) . . . . ? C17 W1 C19 C18 -88.4(6) . . . . ? C10 W1 C19 C18 106.4(5) . . . . ? O4 W1 C19 C18 -177.3(4) . . . . ? C18 W1 C19 C18 0.000(5) . . . . ? C22 W1 C19 C18 -38.9(4) . . . . ? C21 W1 C19 C18 -80.5(5) . . . . ? C20 W1 C19 C18 -116.0(6) . . . . ? P1 W1 C19 C18 34.1(5) . . . . ? Co1 W1 C19 C18 103.8(4) . . . . ? C18 C19 C20 C21 0.4(8) . . . . ? W1 C19 C20 C21 -62.3(5) . . . . ? C18 C19 C20 W1 62.7(5) . . . . ? W1 C19 C20 W1 0.0 . . . . ? C17 W1 C20 C21 -43.3(4) . . . . ? C10 W1 C20 C21 167.3(4) . . . . ? O4 W1 C20 C21 -124.9(4) . . . . ? C18 W1 C20 C21 80.0(4) . . . . ? C22 W1 C20 C21 36.8(4) . . . . ? C19 W1 C20 C21 118.2(6) . . . . ? C21 W1 C20 C21 0.000(7) . . . . ? P1 W1 C20 C21 59.1(6) . . . . ? Co1 W1 C20 C21 -148.7(4) . . . . ? C17 W1 C20 C19 -161.5(4) . . . . ? C10 W1 C20 C19 49.1(5) . . . . ? O4 W1 C20 C19 116.8(4) . . . . ? C18 W1 C20 C19 -38.2(4) . . . . ? C22 W1 C20 C19 -81.5(4) . . . . ? C19 W1 C20 C19 0.0 . . . . ? C21 W1 C20 C19 -118.2(6) . . . . ? P1 W1 C20 C19 -59.1(6) . . . . ? Co1 W1 C20 C19 93.1(5) . . . . ? C19 C20 C21 C22 0.3(8) . . . . ? W1 C20 C21 C22 -60.8(5) . . . . ? C19 C20 C21 W1 61.1(5) . . . . ? W1 C20 C21 W1 0.000(4) . . . . ? C17 W1 C21 C20 138.3(4) . . . . ? C10 W1 C21 C20 -22.8(7) . . . . ? O4 W1 C21 C20 54.3(4) . . . . ? C18 W1 C21 C20 -79.1(5) . . . . ? C22 W1 C21 C20 -118.5(6) . . . . ? C19 W1 C21 C20 -36.5(4) . . . . ? C20 W1 C21 C20 0.000(7) . . . . ? P1 W1 C21 C20 -149.8(4) . . . . ? Co1 W1 C21 C20 134.2(5) . . . . ? C17 W1 C21 C22 -103.2(4) . . . . ? C10 W1 C21 C22 95.7(5) . . . . ? O4 W1 C21 C22 172.8(4) . . . . ? C18 W1 C21 C22 39.4(4) . . . . ? C22 W1 C21 C22 0.000(4) . . . . ? C19 W1 C21 C22 82.0(4) . . . . ? C20 W1 C21 C22 118.5(6) . . . . ? P1 W1 C21 C22 -31.3(5) . . . . ? Co1 W1 C21 C22 -107.4(6) . . . . ? C20 C21 C22 C18 -0.9(7) . . . . ? W1 C21 C22 C18 -64.4(4) . . . . ? C20 C21 C22 W1 63.5(5) . . . . ? W1 C21 C22 W1 0.000(3) . . . . ? C19 C18 C22 C21 1.1(7) . . . . ? W1 C18 C22 C21 66.9(4) . . . . ? C19 C18 C22 W1 -65.8(5) . . . . ? W1 C18 C22 W1 0.000(2) . . . . ? C17 W1 C22 C21 74.1(4) . . . . ? C10 W1 C22 C21 -132.7(4) . . . . ? O4 W1 C22 C21 -9.9(5) . . . . ? C18 W1 C22 C21 -114.2(6) . . . . ? C19 W1 C22 C21 -76.0(4) . . . . ? C21 W1 C22 C21 0.000(4) . . . . ? C20 W1 C22 C21 -35.1(4) . . . . ? P1 W1 C22 C21 155.2(4) . . . . ? Co1 W1 C22 C21 148.9(3) . . . . ? C17 W1 C22 C18 -171.6(4) . . . . ? C10 W1 C22 C18 -18.5(6) . . . . ? O4 W1 C22 C18 104.3(4) . . . . ? C18 W1 C22 C18 0.000(3) . . . . ? C19 W1 C22 C18 38.2(4) . . . . ? C21 W1 C22 C18 114.2(6) . . . . ? C20 W1 C22 C18 79.1(5) . . . . ? P1 W1 C22 C18 -90.6(4) . . . . ? Co1 W1 C22 C18 -96.9(5) . . . . ? C29 P1 C23 C28 112.2(6) . . . . ? Co1 P1 C23 C28 -17.4(7) . . . . ? W1 P1 C23 C28 -101.5(6) . . . . ? C29 P1 C23 C24 -68.4(6) . . . . ? Co1 P1 C23 C24 162.0(5) . . . . ? W1 P1 C23 C24 77.9(6) . . . . ? C28 C23 C24 C25 0.7(11) . . . . ? P1 C23 C24 C25 -178.7(6) . . . . ? C23 C24 C25 C26 -0.3(12) . . . . ? C24 C25 C26 C27 0.6(13) . . . . ? C25 C26 C27 C28 -1.2(12) . . . . ? C24 C23 C28 C27 -1.3(11) . . . . ? P1 C23 C28 C27 178.1(5) . . . . ? C26 C27 C28 C23 1.6(11) . . . . ? C23 P1 C29 C30 116.5(6) . . . . ? Co1 P1 C29 C30 -110.3(6) . . . . ? W1 P1 C29 C30 -24.9(7) . . . . ? C23 P1 C29 C34 -61.6(6) . . . . ? Co1 P1 C29 C34 71.5(5) . . . . ? W1 P1 C29 C34 157.0(4) . . . . ? C34 C29 C30 C31 1.6(11) . . . . ? P1 C29 C30 C31 -176.5(6) . . . . ? C29 C30 C31 C32 -1.5(13) . . . . ? C30 C31 C32 C33 0.5(12) . . . . ? C31 C32 C33 C34 0.3(12) . . . . ? C30 C29 C34 C33 -0.8(10) . . . . ? P1 C29 C34 C33 177.5(6) . . . . ? C32 C33 C34 C29 -0.1(12) . . . . ? C40 C35 C36 C37 -2.4(18) . . . . ? C35 C36 C37 C38 -0.2(17) . . . . ? C36 C37 C38 C39 1.9(14) . . . . ? C36 C37 C38 C41 -179.1(9) . . . . ? C37 C38 C39 C40 -0.9(13) . . . . ? C41 C38 C39 C40 180.0(8) . . . . ? C38 C39 C40 C35 -1.6(14) . . . . ? C36 C35 C40 C39 3.2(16) . . . . ? C37 C38 C41 C42 155.2(48) . . . . ? C39 C38 C41 C42 -25.7(54) . . . . ? C38 C41 C42 C43 41.0(160) . . . . ? C41 C42 C43 C47 -160.2(123) . . . . ? C41 C42 C43 C44 43.9(128) . . . . ? C41 C42 C43 Co2 -31.3(127) . . . . ? C50 Co2 C43 C42 -90.4(5) . . . . ? C49 Co2 C43 C42 20.9(5) . . . . ? C44 Co2 C43 C42 117.6(6) . . . . ? P2 Co2 C43 C42 131.4(4) . . . . ? W2 Co2 C43 C42 166.0(5) . . . . ? C50 Co2 C43 C47 44.9(5) . . . . ? C49 Co2 C43 C47 156.2(4) . . . . ? C44 Co2 C43 C47 -107.1(5) . . . . ? P2 Co2 C43 C47 -93.3(4) . . . . ? W2 Co2 C43 C47 -58.8(4) . . . . ? C50 Co2 C43 C44 152.0(4) . . . . ? C49 Co2 C43 C44 -96.7(4) . . . . ? C44 Co2 C43 C44 0.000(2) . . . . ? P2 Co2 C43 C44 13.8(4) . . . . ? W2 Co2 C43 C44 48.4(3) . . . . ? C42 C43 C44 C45 13.9(9) . . . . ? C47 C43 C44 C45 -143.5(5) . . . . ? Co2 C43 C44 C45 118.7(5) . . . . ? C42 C43 C44 Co2 -104.8(6) . . . . ? C47 C43 C44 Co2 97.8(5) . . . . ? Co2 C43 C44 Co2 0.000(2) . . . . ? C42 C43 C44 W2 -177.0(5) . . . . ? C47 C43 C44 W2 25.6(6) . . . . ? Co2 C43 C44 W2 -72.2(3) . . . . ? C50 Co2 C44 C43 -54.1(6) . . . . ? C49 Co2 C44 C43 94.0(4) . . . . ? C43 Co2 C44 C43 0.000(2) . . . . ? P2 Co2 C44 C43 -168.8(3) . . . . ? W2 Co2 C44 C43 -114.7(4) . . . . ? C50 Co2 C44 C45 -164.7(5) . . . . ? C49 Co2 C44 C45 -16.5(6) . . . . ? C43 Co2 C44 C45 -110.5(6) . . . . ? P2 Co2 C44 C45 80.6(5) . . . . ? W2 Co2 C44 C45 134.8(6) . . . . ? C50 Co2 C44 W2 60.6(5) . . . . ? C49 Co2 C44 W2 -151.3(2) . . . . ? C43 Co2 C44 W2 114.7(4) . . . . ? P2 Co2 C44 W2 -54.14(13) . . . . ? W2 Co2 C44 W2 0.000(2) . . . . ? C51 W2 C44 C43 47.3(5) . . . . ? O7 W2 C44 C43 -23.6(4) . . . . ? C55 W2 C44 C43 -88.8(5) . . . . ? C56 W2 C44 C43 -99.3(4) . . . . ? C54 W2 C44 C43 -152.9(4) . . . . ? C53 W2 C44 C43 -161.6(4) . . . . ? C52 W2 C44 C43 -133.3(4) . . . . ? P2 W2 C44 C43 117.6(4) . . . . ? Co2 W2 C44 C43 68.0(4) . . . . ? C51 W2 C44 C45 -146.1(5) . . . . ? O7 W2 C44 C45 143.0(6) . . . . ? C55 W2 C44 C45 77.8(7) . . . . ? C56 W2 C44 C45 67.3(6) . . . . ? C54 W2 C44 C45 13.7(9) . . . . ? C53 W2 C44 C45 5.0(6) . . . . ? C52 W2 C44 C45 33.3(6) . . . . ? P2 W2 C44 C45 -75.8(6) . . . . ? Co2 W2 C44 C45 -125.4(6) . . . . ? C51 W2 C44 Co2 -20.7(3) . . . . ? O7 W2 C44 Co2 -91.6(2) . . . . ? C55 W2 C44 Co2 -156.8(3) . . . . ? C56 W2 C44 Co2 -167.3(2) . . . . ? C54 W2 C44 Co2 139.1(4) . . . . ? C53 W2 C44 Co2 130.4(2) . . . . ? C52 W2 C44 Co2 158.7(2) . . . . ? P2 W2 C44 Co2 49.56(13) . . . . ? Co2 W2 C44 Co2 0.000(2) . . . . ? C46 O6 C45 O5 -3.3(9) . . . . ? C46 O6 C45 C44 179.3(5) . . . . ? C43 C44 C45 O5 -61.4(9) . . . . ? Co2 C44 C45 O5 24.8(9) . . . . ? W2 C44 C45 O5 132.6(6) . . . . ? C43 C44 C45 O6 115.8(6) . . . . ? Co2 C44 C45 O6 -157.9(4) . . . . ? W2 C44 C45 O6 -50.2(8) . . . . ? W2 O7 C47 O8 170.6(4) . . . . ? W2 O7 C47 C43 -12.0(7) . . . . ? C48 O8 C47 O7 2.0(8) . . . . ? C48 O8 C47 C43 -175.4(5) . . . . ? C42 C43 C47 O7 -168.0(6) . . . . ? C44 C43 C47 O7 -9.4(8) . . . . ? Co2 C43 C47 O7 58.7(6) . . . . ? C42 C43 C47 O8 9.4(8) . . . . ? C44 C43 C47 O8 168.0(5) . . . . ? Co2 C43 C47 O8 -123.9(5) . . . . ? C50 Co2 C49 O49 -63.4(109) . . . . ? C44 Co2 C49 O49 133.2(108) . . . . ? C43 Co2 C49 O49 176.9(1000) . . . . ? P2 Co2 C49 O49 46.7(109) . . . . ? W2 Co2 C49 O49 89.6(109) . . . . ? C49 Co2 C50 O50 62.0(63) . . . . ? C44 Co2 C50 O50 -149.8(60) . . . . ? C43 Co2 C50 O50 173.2(62) . . . . ? P2 Co2 C50 O50 -41.2(63) . . . . ? W2 Co2 C50 O50 -102.6(63) . . . . ? C44 W2 C51 O51 -156.6(66) . . . . ? O7 W2 C51 O51 -89.4(67) . . . . ? C55 W2 C51 O51 -2.7(67) . . . . ? C56 W2 C51 O51 -15.0(68) . . . . ? C54 W2 C51 O51 33.0(67) . . . . ? C53 W2 C51 O51 51.6(67) . . . . ? C52 W2 C51 O51 24.5(69) . . . . ? P2 W2 C51 O51 136.7(67) . . . . ? Co2 W2 C51 O51 -171.7(67) . . . . ? C51 W2 C52 C56 -70.6(6) . . . . ? C44 W2 C52 C56 110.2(4) . . . . ? O7 W2 C52 C56 34.1(5) . . . . ? C55 W2 C52 C56 -38.5(4) . . . . ? C56 W2 C52 C56 0.000(1) . . . . ? C54 W2 C52 C56 -80.5(4) . . . . ? C53 W2 C52 C56 -117.6(6) . . . . ? P2 W2 C52 C56 -173.6(4) . . . . ? Co2 W2 C52 C56 133.0(4) . . . . ? C51 W2 C52 C53 47.0(6) . . . . ? C44 W2 C52 C53 -132.2(4) . . . . ? O7 W2 C52 C53 151.7(4) . . . . ? C55 W2 C52 C53 79.0(4) . . . . ? C56 W2 C52 C53 117.6(6) . . . . ? C54 W2 C52 C53 37.1(4) . . . . ? C53 W2 C52 C53 0.000(3) . . . . ? P2 W2 C52 C53 -56.0(4) . . . . ? Co2 W2 C52 C53 -109.4(4) . . . . ? C56 C52 C53 C54 -0.8(7) . . . . ? W2 C52 C53 C54 -62.5(4) . . . . ? C56 C52 C53 W2 61.7(4) . . . . ? W2 C52 C53 W2 0.000(2) . . . . ? C51 W2 C53 C52 -150.3(4) . . . . ? C44 W2 C53 C52 55.7(5) . . . . ? O7 W2 C53 C52 -42.8(6) . . . . ? C55 W2 C53 C52 -79.3(4) . . . . ? C56 W2 C53 C52 -36.6(4) . . . . ? C54 W2 C53 C52 -117.1(6) . . . . ? C52 W2 C53 C52 0.000(3) . . . . ? P2 W2 C53 C52 128.7(4) . . . . ? Co2 W2 C53 C52 109.8(4) . . . . ? C51 W2 C53 C54 -33.2(5) . . . . ? C44 W2 C53 C54 172.9(4) . . . . ? O7 W2 C53 C54 74.3(5) . . . . ? C55 W2 C53 C54 37.8(4) . . . . ? C56 W2 C53 C54 80.6(4) . . . . ? C54 W2 C53 C54 0.000(1) . . . . ? C52 W2 C53 C54 117.1(6) . . . . ? P2 W2 C53 C54 -114.2(4) . . . . ? Co2 W2 C53 C54 -133.0(3) . . . . ? C52 C53 C54 C55 0.6(7) . . . . ? W2 C53 C54 C55 -62.9(4) . . . . ? C52 C53 C54 W2 63.5(4) . . . . ? W2 C53 C54 W2 0.0 . . . . ? C51 W2 C54 C55 -94.6(4) . . . . ? C44 W2 C54 C55 102.2(6) . . . . ? O7 W2 C54 C55 -17.0(5) . . . . ? C55 W2 C54 C55 0.000(5) . . . . ? C56 W2 C54 C55 38.3(4) . . . . ? C53 W2 C54 C55 115.8(6) . . . . ? C52 W2 C54 C55 79.3(4) . . . . ? P2 W2 C54 C55 -175.2(4) . . . . ? Co2 W2 C54 C55 -149.4(3) . . . . ? C51 W2 C54 C53 149.7(4) . . . . ? C44 W2 C54 C53 -13.5(7) . . . . ? O7 W2 C54 C53 -132.7(4) . . . . ? C55 W2 C54 C53 -115.8(6) . . . . ? C56 W2 C54 C53 -77.5(4) . . . . ? C53 W2 C54 C53 0.000(1) . . . . ? C52 W2 C54 C53 -36.5(4) . . . . ? P2 W2 C54 C53 69.1(4) . . . . ? Co2 W2 C54 C53 94.8(5) . . . . ? C53 C54 C55 C56 -0.2(7) . . . . ? W2 C54 C55 C56 -65.0(4) . . . . ? C53 C54 C55 W2 64.8(4) . . . . ? W2 C54 C55 W2 0.000(3) . . . . ? C51 W2 C55 C54 82.3(4) . . . . ? C44 W2 C55 C54 -132.9(4) . . . . ? O7 W2 C55 C54 165.5(4) . . . . ? C56 W2 C55 C54 -115.5(6) . . . . ? C54 W2 C55 C54 0.000(5) . . . . ? C53 W2 C55 C54 -37.5(4) . . . . ? C52 W2 C55 C54 -78.4(4) . . . . ? P2 W2 C55 C54 7.1(5) . . . . ? Co2 W2 C55 C54 121.2(6) . . . . ? C51 W2 C55 C56 -162.1(4) . . . . ? C44 W2 C55 C56 -17.4(6) . . . . ? O7 W2 C55 C56 -79.0(4) . . . . ? C56 W2 C55 C56 0.000(4) . . . . ? C54 W2 C55 C56 115.5(6) . . . . ? C53 W2 C55 C56 78.0(4) . . . . ? C52 W2 C55 C56 37.2(4) . . . . ? P2 W2 C55 C56 122.6(4) . . . . ? Co2 W2 C55 C56 -123.3(6) . . . . ? C53 C52 C56 C55 0.7(7) . . . . ? W2 C52 C56 C55 63.6(4) . . . . ? C53 C52 C56 W2 -62.9(4) . . . . ? W2 C52 C56 W2 0.0 . . . . ? C54 C55 C56 C52 -0.3(7) . . . . ? W2 C55 C56 C52 -65.9(4) . . . . ? C54 C55 C56 W2 65.7(4) . . . . ? W2 C55 C56 W2 0.000(2) . . . . ? C51 W2 C56 C52 136.6(4) . . . . ? C44 W2 C56 C52 -75.8(4) . . . . ? O7 W2 C56 C52 -147.8(4) . . . . ? C55 W2 C56 C52 115.5(6) . . . . ? C54 W2 C56 C52 77.9(5) . . . . ? C53 W2 C56 C52 36.4(4) . . . . ? C52 W2 C56 C52 0.000(1) . . . . ? P2 W2 C56 C52 10.4(6) . . . . ? Co2 W2 C56 C52 -94.4(5) . . . . ? C51 W2 C56 C55 21.1(5) . . . . ? C44 W2 C56 C55 168.7(4) . . . . ? O7 W2 C56 C55 96.8(4) . . . . ? C55 W2 C56 C55 0.000(4) . . . . ? C54 W2 C56 C55 -37.6(4) . . . . ? C53 W2 C56 C55 -79.1(4) . . . . ? C52 W2 C56 C55 -115.5(6) . . . . ? P2 W2 C56 C55 -105.1(4) . . . . ? Co2 W2 C56 C55 150.1(3) . . . . ? C63 P2 C57 C58 -134.3(5) . . . . ? Co2 P2 C57 C58 95.6(5) . . . . ? W2 P2 C57 C58 11.6(6) . . . . ? C63 P2 C57 C62 48.8(6) . . . . ? Co2 P2 C57 C62 -81.3(6) . . . . ? W2 P2 C57 C62 -165.3(4) . . . . ? C62 C57 C58 C59 -0.3(10) . . . . ? P2 C57 C58 C59 -177.3(5) . . . . ? C57 C58 C59 C60 0.8(10) . . . . ? C58 C59 C60 C61 -1.1(11) . . . . ? C59 C60 C61 C62 0.9(11) . . . . ? C60 C61 C62 C57 -0.4(11) . . . . ? C58 C57 C62 C61 0.1(10) . . . . ? P2 C57 C62 C61 177.1(5) . . . . ? C57 P2 C63 C68 83.2(6) . . . . ? Co2 P2 C63 C68 -147.9(5) . . . . ? W2 P2 C63 C68 -63.1(6) . . . . ? C57 P2 C63 C64 -93.6(5) . . . . ? Co2 P2 C63 C64 35.3(6) . . . . ? W2 P2 C63 C64 120.0(5) . . . . ? C68 C63 C64 C65 -0.3(10) . . . . ? P2 C63 C64 C65 176.6(5) . . . . ? C63 C64 C65 C66 0.0(10) . . . . ? C64 C65 C66 C67 0.4(11) . . . . ? C65 C66 C67 C68 -0.4(13) . . . . ? C64 C63 C68 C67 0.2(11) . . . . ? P2 C63 C68 C67 -176.7(6) . . . . ? C66 C67 C68 C63 0.1(13) . . . . ? _refine_diff_density_max 1.096 _refine_diff_density_min -2.668 _refine_diff_density_rms 0.173 data_mm9805 _database_code_CSD 154854 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C36 H32 Cl2 Co O4 P W' _chemical_formula_weight 873.27 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'W' 'W' -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.451(5) _cell_length_b 9.870(5) _cell_length_c 35.906(18) _cell_angle_alpha 90.00 _cell_angle_beta 91.59(3) _cell_angle_gamma 90.00 _cell_volume 3348.1(20) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 46 _cell_measurement_theta_min 10 _cell_measurement_theta_max 15 _exptl_crystal_description 'block' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.732 _exptl_crystal_density_method ? _exptl_crystal_F_000 1720 _exptl_absorpt_coefficient_mu 4.174 _exptl_absorpt_correction_type 'Semi-empirical psi scans' _exptl_absorpt_correction_T_min 0.249 _exptl_absorpt_correction_T_max 0.313 _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(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 'Stoe Diffractometer' _diffrn_measurement_method 'omega-theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 90 _diffrn_standards_decay_% ? _diffrn_reflns_number 5886 _diffrn_reflns_av_R_equivalents 0.0381 _diffrn_reflns_av_sigmaI/netI 0.0477 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 3.51 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5875 _reflns_number_observed 4714 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Stoe DIF4' _computing_cell_refinement 'Stoe DIF4' _computing_data_reduction 'Stoe REDU4' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics SHELXTL-Plus _computing_publication_material SHELXL-93 _refine_special_details ; Refinement on F^2^ for ALL reflections except for 36 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0339P)^2^+20.9588P] 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 'Riding Model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5839 _refine_ls_number_parameters 394 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0656 _refine_ls_R_factor_obs 0.0462 _refine_ls_wR_factor_all 0.1178 _refine_ls_wR_factor_obs 0.0974 _refine_ls_goodness_of_fit_all 1.167 _refine_ls_goodness_of_fit_obs 1.155 _refine_ls_restrained_S_all 1.243 _refine_ls_restrained_S_obs 1.155 _refine_ls_shift/esd_max 0.025 _refine_ls_shift/esd_mean 0.003 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group W1 W 0.00655(3) 0.05206(3) 0.191915(8) 0.02443(11) Uani 1 d . . Co1 Co 0.17384(11) 0.24954(11) 0.16621(3) 0.0248(2) Uani 1 d . . P1 P -0.0007(2) 0.3461(2) 0.08319(5) 0.0258(4) Uani 1 d . . O1 O 0.4286(7) 0.2365(7) 0.2119(2) 0.052(2) Uani 1 d . . O2 O 0.2425(8) 0.0258(8) 0.2547(2) 0.053(2) Uani 1 d . . O3 O 0.1850(9) 0.5415(7) 0.1649(2) 0.058(2) Uani 1 d . . O4 O -0.0739(7) 0.2647(7) 0.2530(2) 0.049(2) Uani 1 d . . C1 C 0.3303(9) 0.2412(9) 0.1926(2) 0.032(2) Uani 1 d . . C2 C 0.1633(9) 0.0346(9) 0.2300(2) 0.034(2) Uani 1 d . . C3 C 0.1794(10) 0.4269(10) 0.1657(2) 0.036(2) Uani 1 d . . C4 C -0.0430(9) 0.1914(10) 0.2294(3) 0.038(2) Uani 1 d . . C5 C 0.1760(8) 0.0454(8) 0.1502(2) 0.025(2) Uani 1 d . . C6 C 0.1482(8) 0.1258(8) 0.1183(2) 0.024(2) Uani 1 d . . H6A H 0.2173(8) 0.1302(8) 0.0978(2) 0.029 Uiso 1 calc R . C7 C 0.0372(8) 0.2214(8) 0.1205(2) 0.023(2) Uani 1 d . . C8 C -0.0377(8) 0.2180(8) 0.1544(2) 0.025(2) Uani 1 d . . C11 C -0.1033(8) 0.2436(8) 0.0497(2) 0.026(2) Uani 1 d . . C12 C -0.1499(9) 0.3077(9) 0.0167(2) 0.033(2) Uani 1 d . . H12A H -0.1265(9) 0.3999(9) 0.0125(2) 0.039 Uiso 1 calc R . C13 C -0.2296(10) 0.2376(10) -0.0096(2) 0.039(2) Uani 1 d . . H13A H -0.2589(10) 0.2816(10) -0.0320(2) 0.047 Uiso 1 calc R . C14 C -0.2671(11) 0.1065(10) -0.0039(3) 0.045(2) Uani 1 d . . H14 H -0.3235(11) 0.0593(10) -0.0219(3) 0.054 Uiso 1 calc R . C15 C -0.2221(11) 0.0431(11) 0.0285(3) 0.049(3) Uani 1 d . . H15A H -0.2485(11) -0.0483(11) 0.0327(3) 0.058 Uiso 1 calc R . C16 C -0.1394(10) 0.1099(9) 0.0547(2) 0.037(2) Uani 1 d . . H16A H -0.1071(10) 0.0634(9) 0.0765(2) 0.045 Uiso 1 calc R . C21 C 0.1708(8) 0.3557(8) 0.0608(2) 0.026(2) Uani 1 d . . C22 C 0.2599(9) 0.4588(9) 0.0715(2) 0.036(2) Uani 1 d . . H22A H 0.2284(9) 0.5235(9) 0.0890(2) 0.043 Uiso 1 calc R . C23 C 0.3950(10) 0.4719(10) 0.0576(3) 0.046(2) Uani 1 d . . H23A H 0.4544(10) 0.5452(10) 0.0651(3) 0.056 Uiso 1 calc R . C24 C 0.4416(10) 0.3760(11) 0.0324(3) 0.047(3) Uani 1 d . . H24A H 0.5344(10) 0.3815(11) 0.0230(3) 0.056 Uiso 1 calc R . C25 C 0.3527(10) 0.2738(11) 0.0213(3) 0.047(2) Uani 1 d . . H25A H 0.3851(10) 0.2080(11) 0.0042(3) 0.056 Uiso 1 calc R . C26 C 0.2171(9) 0.2637(9) 0.0343(2) 0.037(2) Uani 1 d . . H26A H 0.1555(9) 0.1944(9) 0.0251(2) 0.044 Uiso 1 calc R . C31 C -0.1597(9) 0.3140(8) 0.1579(2) 0.027(2) Uani 1 d . . C32 C -0.1551(10) 0.4298(10) 0.1804(2) 0.039(2) Uani 1 d . . H32A H -0.0715(10) 0.4499(10) 0.1947(2) 0.047 Uiso 1 calc R . C33 C -0.2706(11) 0.5153(10) 0.1822(3) 0.046(3) Uani 1 d . . H33A H -0.2659(11) 0.5935(10) 0.1976(3) 0.055 Uiso 1 calc R . C34 C -0.3930(11) 0.4872(11) 0.1615(3) 0.052(3) Uani 1 d . . H34A H -0.4729(11) 0.5452(11) 0.1630(3) 0.062 Uiso 1 calc R . C35 C -0.3979(10) 0.3756(11) 0.1391(3) 0.047(3) Uani 1 d . . H35A H -0.4814(10) 0.3564(11) 0.1247(3) 0.057 Uiso 1 calc R . C36 C -0.2822(9) 0.2901(9) 0.1371(2) 0.035(2) Uani 1 d . . H36A H -0.2873(9) 0.2134(9) 0.1211(2) 0.041 Uiso 1 calc R . C41 C -0.1275(10) -0.1010(10) 0.2234(3) 0.042(2) Uani 1 d . . H41A H -0.1323(10) -0.1097(10) 0.2511(3) 0.051 Uiso 1 calc R . C42 C -0.0374(10) -0.1743(9) 0.2003(3) 0.039(2) Uani 1 d . . H42A H 0.0333(10) -0.2442(9) 0.2086(3) 0.047 Uiso 1 calc R . C43 C -0.0799(10) -0.1462(10) 0.1630(3) 0.040(2) Uani 1 d . . H43A H -0.0409(10) -0.1897(10) 0.1403(3) 0.049 Uiso 1 calc R . C44 C -0.1876(10) -0.0536(10) 0.1634(3) 0.042(2) Uani 1 d . . H44A H -0.2414(10) -0.0193(10) 0.1409(3) 0.050 Uiso 1 calc R . C45 C -0.2184(10) -0.0244(10) 0.2005(3) 0.045(2) Uani 1 d . . H45A H -0.2997(10) 0.0315(10) 0.2090(3) 0.054 Uiso 1 calc R . C51 C 0.3023(8) -0.0534(9) 0.1455(2) 0.031(2) Uani 1 d . . C52 C 0.2553(10) -0.1632(9) 0.1173(3) 0.040(2) Uani 1 d . . H52A H 0.3361(18) -0.2212(39) 0.1118(13) 0.060 Uiso 1 calc R . H52B H 0.2197(60) -0.1200(9) 0.0943(7) 0.060 Uiso 1 calc R . H52C H 0.1801(46) -0.2181(40) 0.1280(7) 0.060 Uiso 1 calc R . C53 C 0.4320(9) 0.0181(10) 0.1298(3) 0.044(2) Uani 1 d . . H53A H 0.5085(25) -0.0478(17) 0.1269(17) 0.066 Uiso 1 calc R . H53B H 0.4636(42) 0.0899(44) 0.1469(9) 0.066 Uiso 1 calc R . H53C H 0.4067(20) 0.0577(57) 0.1055(9) 0.066 Uiso 1 calc R . C54 C 0.3522(10) -0.1255(10) 0.1809(3) 0.045(2) Uani 1 d . . H54A H 0.4268(50) -0.1904(48) 0.1750(4) 0.067 Uiso 1 calc R . H54B H 0.2725(19) -0.1738(55) 0.1917(10) 0.067 Uiso 1 calc R . H54C H 0.3895(63) -0.0589(12) 0.1989(7) 0.067 Uiso 1 calc R . Cl1 Cl -0.0705(3) -0.2898(3) 0.06305(7) 0.0526(6) Uiso 1 d . . Cl2 Cl -0.3554(3) -0.2495(3) 0.08838(7) 0.0490(6) Uiso 1 d . . C10 C -0.2210(11) -0.3674(11) 0.0806(3) 0.052(3) Uiso 1 d . . H10A H -0.1955(11) -0.4136(11) 0.1043(3) 0.063 Uiso 1 calc R . H10B H -0.2563(11) -0.4367(11) 0.0627(3) 0.063 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.0276(2) 0.0254(2) 0.0204(2) 0.00209(15) 0.00280(11) -0.0034(2) Co1 0.0286(6) 0.0230(6) 0.0227(5) -0.0007(5) 0.0015(4) -0.0030(5) P1 0.0322(11) 0.0215(10) 0.0237(10) 0.0020(9) 0.0042(8) 0.0014(9) O1 0.045(4) 0.056(5) 0.053(4) 0.001(4) -0.019(3) -0.005(3) O2 0.057(4) 0.071(5) 0.029(3) 0.010(3) -0.010(3) -0.002(4) O3 0.101(6) 0.028(4) 0.043(4) 0.001(3) -0.001(4) -0.009(4) O4 0.067(5) 0.050(4) 0.030(3) -0.011(3) 0.007(3) 0.005(4) C1 0.032(5) 0.026(5) 0.039(5) -0.001(4) 0.002(4) -0.006(4) C2 0.039(5) 0.032(5) 0.030(4) 0.002(4) -0.001(4) -0.004(4) C3 0.053(6) 0.039(6) 0.016(4) 0.003(4) -0.001(4) -0.004(4) C4 0.040(5) 0.039(5) 0.036(5) 0.004(4) 0.020(4) -0.002(4) C5 0.025(4) 0.027(4) 0.022(4) 0.001(4) 0.000(3) -0.005(4) C6 0.030(4) 0.026(4) 0.017(4) -0.004(3) 0.001(3) 0.001(3) C7 0.029(4) 0.022(4) 0.018(4) 0.002(3) 0.002(3) 0.001(3) C8 0.028(4) 0.024(4) 0.022(4) 0.003(3) 0.003(3) -0.006(3) C11 0.031(4) 0.031(5) 0.016(4) -0.003(3) 0.004(3) 0.001(4) C12 0.037(5) 0.030(5) 0.031(5) 0.006(4) 0.006(4) 0.004(4) C13 0.047(5) 0.047(6) 0.023(4) 0.005(4) 0.000(4) 0.007(5) C14 0.054(6) 0.047(6) 0.033(5) -0.004(4) -0.012(4) 0.001(5) C15 0.063(6) 0.041(6) 0.041(5) 0.002(5) -0.013(5) -0.019(5) C16 0.056(6) 0.029(5) 0.026(4) 0.001(4) -0.012(4) -0.001(4) C21 0.032(4) 0.023(4) 0.024(4) 0.005(3) 0.006(3) 0.002(4) C22 0.049(5) 0.028(5) 0.031(4) -0.001(4) 0.008(4) 0.002(4) C23 0.045(6) 0.039(6) 0.055(6) 0.007(5) 0.004(5) -0.014(5) C24 0.031(5) 0.061(7) 0.050(6) 0.008(5) 0.015(4) -0.002(5) C25 0.039(5) 0.051(6) 0.052(6) -0.007(5) 0.015(5) 0.004(5) C26 0.036(5) 0.038(5) 0.037(5) -0.008(4) 0.009(4) -0.006(4) C31 0.033(4) 0.022(4) 0.028(4) 0.008(3) 0.012(4) 0.002(3) C32 0.046(5) 0.042(6) 0.031(5) 0.006(4) 0.013(4) -0.002(4) C33 0.053(6) 0.035(6) 0.051(6) 0.002(4) 0.030(5) 0.011(5) C34 0.037(6) 0.044(6) 0.075(8) 0.017(6) 0.029(5) 0.018(5) C35 0.035(5) 0.053(7) 0.055(6) 0.023(5) 0.010(4) 0.004(5) C36 0.029(5) 0.036(5) 0.039(5) 0.009(4) 0.012(4) -0.002(4) C41 0.050(6) 0.035(5) 0.041(5) 0.014(4) 0.007(4) -0.010(4) C42 0.039(5) 0.017(4) 0.060(6) 0.001(4) -0.006(4) -0.001(4) C43 0.040(5) 0.045(6) 0.037(5) -0.008(4) 0.005(4) -0.023(5) C44 0.038(5) 0.036(5) 0.051(6) 0.005(5) -0.011(4) -0.017(5) C45 0.034(5) 0.045(6) 0.055(6) 0.002(5) 0.009(4) -0.010(4) C51 0.031(4) 0.025(4) 0.036(4) 0.001(4) 0.002(3) 0.004(4) C52 0.040(5) 0.032(5) 0.047(5) -0.007(4) -0.005(4) 0.007(4) C53 0.027(5) 0.043(6) 0.062(6) -0.003(5) 0.008(4) 0.006(4) C54 0.043(5) 0.041(6) 0.050(6) 0.008(5) -0.011(4) 0.016(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 W1 C4 1.991(9) . ? W1 C2 1.996(9) . ? W1 C8 2.154(8) . ? W1 C5 2.224(7) . ? W1 C45 2.285(9) . ? W1 C42 2.294(8) . ? W1 C41 2.291(9) . ? W1 C44 2.324(8) . ? W1 C43 2.351(9) . ? W1 Co1 2.6892(12) . ? Co1 C1 1.735(9) . ? Co1 C3 1.751(9) . ? Co1 C8 2.056(8) . ? Co1 C7 2.078(8) . ? Co1 C5 2.096(8) . ? Co1 C6 2.117(7) . ? P1 C11 1.828(8) . ? P1 C21 1.831(8) . ? P1 C7 1.847(8) . ? O1 C1 1.145(10) . ? O2 C2 1.147(10) . ? O3 C3 1.133(11) . ? O4 C4 1.156(10) . ? C5 C6 1.411(11) . ? C5 C51 1.554(11) . ? C6 C7 1.415(11) . ? C7 C8 1.424(10) . ? C8 C31 1.500(11) . ? C11 C16 1.376(12) . ? C11 C12 1.403(11) . ? C12 C13 1.377(12) . ? C13 C14 1.358(14) . ? C14 C15 1.376(13) . ? C15 C16 1.376(12) . ? C21 C22 1.369(12) . ? C21 C26 1.397(11) . ? C22 C23 1.390(12) . ? C23 C24 1.389(14) . ? C24 C25 1.365(14) . ? C25 C26 1.380(12) . ? C31 C36 1.380(12) . ? C31 C32 1.401(12) . ? C32 C33 1.382(13) . ? C33 C34 1.385(15) . ? C34 C35 1.365(15) . ? C35 C36 1.385(12) . ? C41 C45 1.397(13) . ? C41 C42 1.407(13) . ? C42 C43 1.413(13) . ? C43 C44 1.368(14) . ? C44 C45 1.402(13) . ? C51 C54 1.521(12) . ? C51 C53 1.535(12) . ? C51 C52 1.540(12) . ? Cl1 C10 1.749(10) . ? Cl2 C10 1.750(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 C4 W1 C2 77.3(4) . . ? C4 W1 C8 81.5(3) . . ? C2 W1 C8 128.5(3) . . ? C4 W1 C5 131.6(3) . . ? C2 W1 C5 85.7(3) . . ? C8 W1 C5 74.5(3) . . ? C4 W1 C45 84.2(4) . . ? C2 W1 C45 123.7(4) . . ? C8 W1 C45 99.8(3) . . ? C5 W1 C45 140.4(3) . . ? C4 W1 C42 122.5(3) . . ? C2 W1 C42 87.7(3) . . ? C8 W1 C42 142.1(3) . . ? C5 W1 C42 101.3(3) . . ? C45 W1 C42 59.2(3) . . ? C4 W1 C41 88.7(4) . . ? C2 W1 C41 90.8(3) . . ? C8 W1 C41 135.2(3) . . ? C5 W1 C41 137.0(3) . . ? C45 W1 C41 35.5(3) . . ? C42 W1 C41 35.8(3) . . ? C4 W1 C44 114.3(4) . . ? C2 W1 C44 145.6(3) . . ? C8 W1 C44 85.9(3) . . ? C5 W1 C44 105.3(3) . . ? C45 W1 C44 35.4(3) . . ? C42 W1 C44 58.4(3) . . ? C41 W1 C44 58.8(3) . . ? C4 W1 C43 142.1(3) . . ? C2 W1 C43 118.2(4) . . ? C8 W1 C43 107.3(3) . . ? C5 W1 C43 85.8(3) . . ? C45 W1 C43 58.1(3) . . ? C42 W1 C43 35.4(3) . . ? C41 W1 C43 58.6(3) . . ? C44 W1 C43 34.0(3) . . ? C4 W1 Co1 83.3(2) . . ? C2 W1 Co1 82.3(2) . . ? C8 W1 Co1 48.7(2) . . ? C5 W1 Co1 49.4(2) . . ? C45 W1 Co1 147.5(3) . . ? C42 W1 Co1 149.5(2) . . ? C41 W1 Co1 170.4(3) . . ? C44 W1 Co1 129.7(2) . . ? C43 W1 Co1 130.7(2) . . ? C1 Co1 C3 91.6(4) . . ? C1 Co1 C8 156.1(3) . . ? C3 Co1 C8 100.3(4) . . ? C1 Co1 C7 157.8(4) . . ? C3 Co1 C7 98.3(4) . . ? C8 Co1 C7 40.3(3) . . ? C1 Co1 C5 95.1(4) . . ? C3 Co1 C5 163.2(3) . . ? C8 Co1 C5 79.3(3) . . ? C7 Co1 C5 70.5(3) . . ? C1 Co1 C6 119.5(4) . . ? C3 Co1 C6 124.8(3) . . ? C8 Co1 C6 69.9(3) . . ? C7 Co1 C6 39.4(3) . . ? C5 Co1 C6 39.1(3) . . ? C1 Co1 W1 106.2(3) . . ? C3 Co1 W1 138.3(3) . . ? C8 Co1 W1 51.9(2) . . ? C7 Co1 W1 79.4(2) . . ? C5 Co1 W1 53.7(2) . . ? C6 Co1 W1 78.8(2) . . ? C11 P1 C21 101.5(4) . . ? C11 P1 C7 101.4(4) . . ? C21 P1 C7 101.4(3) . . ? O1 C1 Co1 175.7(8) . . ? O2 C2 W1 172.7(8) . . ? O3 C3 Co1 178.8(9) . . ? O4 C4 W1 175.0(8) . . ? C6 C5 C51 113.0(6) . . ? C6 C5 Co1 71.2(5) . . ? C51 C5 Co1 130.2(5) . . ? C6 C5 W1 114.1(5) . . ? C51 C5 W1 131.4(5) . . ? Co1 C5 W1 76.9(3) . . ? C7 C6 C5 116.8(7) . . ? C7 C6 Co1 68.8(4) . . ? C5 C6 Co1 69.6(4) . . ? C6 C7 C8 114.7(7) . . ? C6 C7 P1 122.2(6) . . ? C8 C7 P1 123.0(6) . . ? C6 C7 Co1 71.8(4) . . ? C8 C7 Co1 69.0(4) . . ? P1 C7 Co1 126.0(4) . . ? C7 C8 C31 117.2(7) . . ? C7 C8 Co1 70.7(4) . . ? C31 C8 Co1 129.2(6) . . ? C7 C8 W1 117.4(6) . . ? C31 C8 W1 124.4(5) . . ? Co1 C8 W1 79.4(3) . . ? C16 C11 C12 118.0(8) . . ? C16 C11 P1 125.0(6) . . ? C12 C11 P1 117.0(6) . . ? C13 C12 C11 120.3(8) . . ? C14 C13 C12 121.0(9) . . ? C13 C14 C15 119.0(9) . . ? C14 C15 C16 121.1(9) . . ? C11 C16 C15 120.5(8) . . ? C22 C21 C26 118.2(7) . . ? C22 C21 P1 117.4(6) . . ? C26 C21 P1 124.3(6) . . ? C21 C22 C23 122.1(8) . . ? C22 C23 C24 118.8(9) . . ? C25 C24 C23 119.4(8) . . ? C24 C25 C26 121.6(9) . . ? C25 C26 C21 119.7(9) . . ? C36 C31 C32 117.6(8) . . ? C36 C31 C8 118.8(7) . . ? C32 C31 C8 123.5(8) . . ? C33 C32 C31 120.8(9) . . ? C34 C33 C32 120.2(10) . . ? C35 C34 C33 119.5(9) . . ? C34 C35 C36 120.5(10) . . ? C31 C36 C35 121.3(9) . . ? C45 C41 C42 107.6(9) . . ? C45 C41 W1 72.0(5) . . ? C42 C41 W1 72.3(5) . . ? C41 C42 C43 107.3(8) . . ? C41 C42 W1 72.0(5) . . ? C43 C42 W1 74.5(5) . . ? C44 C43 C42 108.3(8) . . ? C44 C43 W1 71.9(5) . . ? C42 C43 W1 70.1(5) . . ? C43 C44 C45 108.7(9) . . ? C43 C44 W1 74.1(5) . . ? C45 C44 W1 70.8(5) . . ? C41 C45 C44 108.0(9) . . ? C41 C45 W1 72.5(5) . . ? C44 C45 W1 73.8(5) . . ? C54 C51 C53 106.9(7) . . ? C54 C51 C52 107.3(8) . . ? C53 C51 C52 107.5(7) . . ? C54 C51 C5 115.1(7) . . ? C53 C51 C5 112.0(7) . . ? C52 C51 C5 107.7(6) . . ? Cl1 C10 Cl2 111.6(6) . . ? _refine_diff_density_max 1.606 _refine_diff_density_min -1.638 _refine_diff_density_rms 0.153 data_mm9806 _database_code_CSD 154855 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C39 H30 Co Fe O8 P W' _chemical_formula_weight 956.23 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 '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' 'W' 'W' -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.688(6) _cell_length_b 17.919(9) _cell_length_c 17.359(9) _cell_angle_alpha 90.00 _cell_angle_beta 103.54(2) _cell_angle_gamma 90.00 _cell_volume 3534.6(31) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 48 _cell_measurement_theta_min 10 _cell_measurement_theta_max 12.5 _exptl_crystal_description 'block' _exptl_crystal_colour red _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.797 _exptl_crystal_density_method ? _exptl_crystal_F_000 1880 _exptl_absorpt_coefficient_mu 4.214 _exptl_absorpt_correction_type 'semi-empirical psi scans' _exptl_absorpt_correction_T_min 0.285 _exptl_absorpt_correction_T_max 0.361 _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(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 'Stoe diffractometer' _diffrn_measurement_method 'omega-theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 90 _diffrn_standards_decay_% ? _diffrn_reflns_number 4644 _diffrn_reflns_av_R_equivalents 0.0288 _diffrn_reflns_av_sigmaI/netI 0.0336 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 22.50 _reflns_number_total 4605 _reflns_number_observed 4011 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Stoe DIF4' _computing_cell_refinement 'Stoe DIF4' _computing_data_reduction 'Stoe REDU4' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics SHELXTL-Plus _computing_publication_material SHELXL-93 _refine_special_details ; Refinement on F^2^ for ALL reflections except for 11 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0360P)^2^+11.6976P] 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 'Riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4594 _refine_ls_number_parameters 463 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0404 _refine_ls_R_factor_obs 0.0308 _refine_ls_wR_factor_all 0.0864 _refine_ls_wR_factor_obs 0.0780 _refine_ls_goodness_of_fit_all 1.122 _refine_ls_goodness_of_fit_obs 1.125 _refine_ls_restrained_S_all 1.154 _refine_ls_restrained_S_obs 1.125 _refine_ls_shift/esd_max 0.015 _refine_ls_shift/esd_mean 0.001 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group W1 W 0.43220(2) 0.16372(2) 0.33169(2) 0.02232(11) Uani 1 d . . Co1 Co 0.48002(8) 0.17252(5) 0.49026(5) 0.0240(2) Uani 1 d . . Fe1 Fe 0.36842(9) 0.38909(6) 0.60532(6) 0.0264(2) Uani 1 d . . P1 P 0.26169(15) 0.30652(10) 0.51889(10) 0.0216(4) Uani 1 d . . C1 C 0.4682(7) 0.3149(5) 0.6434(4) 0.032(2) Uani 1 d . . O1 O 0.5301(5) 0.2678(3) 0.6709(3) 0.0463(15) Uani 1 d . . C2 C 0.3663(7) 0.4493(4) 0.5233(5) 0.036(2) Uani 1 d . . O2 O 0.3642(5) 0.4885(3) 0.4705(3) 0.052(2) Uani 1 d . . C3 C 0.2504(7) 0.4015(4) 0.6535(5) 0.039(2) Uani 1 d . . O3 O 0.1778(6) 0.4095(3) 0.6864(4) 0.058(2) Uani 1 d . . C4 C 0.4646(7) 0.4518(4) 0.6696(4) 0.035(2) Uani 1 d . . O4 O 0.5295(6) 0.4901(3) 0.7103(4) 0.059(2) Uani 1 d . . C5 C 0.5848(7) 0.1085(4) 0.3571(5) 0.034(2) Uani 1 d . . O5 O 0.6683(5) 0.0727(3) 0.3661(4) 0.053(2) Uani 1 d . . C6 C 0.3795(6) 0.0598(5) 0.3493(4) 0.032(2) Uani 1 d . . O6 O 0.3506(5) -0.0001(3) 0.3537(4) 0.0486(15) Uani 1 d . . C7 C 0.6253(7) 0.1492(5) 0.5336(5) 0.048(2) Uani 1 d . . O7 O 0.7185(5) 0.1286(4) 0.5596(5) 0.090(3) Uani 1 d . . C8 C 0.4388(6) 0.1183(4) 0.5626(4) 0.031(2) Uani 1 d . . O8 O 0.4210(4) 0.0833(3) 0.6140(3) 0.0442(14) Uani 1 d . . C9 C 0.3192(5) 0.1897(4) 0.4118(4) 0.0209(15) Uani 1 d . . C10 C 0.3486(5) 0.2550(4) 0.4606(4) 0.0194(15) Uani 1 d . . C11 C 0.4588(5) 0.2859(4) 0.4590(4) 0.022(2) Uani 1 d . . H11A H 0.4945(5) 0.3255(4) 0.4978(4) 0.027 Uiso 1 calc R . C12 C 0.5263(5) 0.2505(4) 0.4118(4) 0.0209(15) Uani 1 d . . C20 C 0.6471(6) 0.2902(4) 0.4170(4) 0.028(2) Uani 1 d . . C21 C 0.6164(7) 0.3626(4) 0.3697(4) 0.035(2) Uani 1 d . . H21A H 0.6883(9) 0.3915(13) 0.3722(24) 0.053 Uiso 1 calc R . H21B H 0.5615(33) 0.3919(13) 0.3923(18) 0.053 Uiso 1 calc R . H21C H 0.5797(38) 0.3506(4) 0.3144(7) 0.053 Uiso 1 calc R . C22 C 0.7337(6) 0.2457(4) 0.3814(5) 0.037(2) Uani 1 d . . H22A H 0.8026(20) 0.2766(10) 0.3809(26) 0.055 Uiso 1 calc R . H22B H 0.6955(15) 0.2310(23) 0.3271(11) 0.055 Uiso 1 calc R . H22C H 0.7585(33) 0.2010(15) 0.4134(17) 0.055 Uiso 1 calc R . C23 C 0.7106(6) 0.3134(5) 0.5011(4) 0.037(2) Uani 1 d . . H23A H 0.7849(21) 0.3380(25) 0.4997(6) 0.055 Uiso 1 calc R . H23B H 0.7267(38) 0.2690(5) 0.5349(8) 0.055 Uiso 1 calc R . H23C H 0.6607(19) 0.3479(21) 0.5224(12) 0.055 Uiso 1 calc R . C31 C 0.4066(7) 0.1340(5) 0.2005(4) 0.043(2) Uani 1 d . . H31A H 0.4306(7) 0.0862(5) 0.1791(4) 0.052 Uiso 1 calc R . C32 C 0.4729(6) 0.2002(5) 0.2130(4) 0.034(2) Uani 1 d . . H32A H 0.5531(6) 0.2072(5) 0.2030(4) 0.040 Uiso 1 calc R . C33 C 0.4015(6) 0.2568(4) 0.2333(4) 0.030(2) Uani 1 d . . H33A H 0.4240(6) 0.3105(4) 0.2421(4) 0.036 Uiso 1 calc R . C34 C 0.2924(6) 0.2268(4) 0.2344(4) 0.031(2) Uani 1 d . . H34A H 0.2235(6) 0.2554(4) 0.2438(4) 0.037 Uiso 1 calc R . C35 C 0.2918(7) 0.1502(5) 0.2145(4) 0.038(2) Uani 1 d . . H35A H 0.2224(7) 0.1159(5) 0.2048(4) 0.046 Uiso 1 calc R . C41 C 0.1792(6) 0.2396(4) 0.5645(4) 0.025(2) Uani 1 d . . C42 C 0.0619(6) 0.2212(4) 0.5300(4) 0.027(2) Uani 1 d . . H42A H 0.0205(6) 0.2447(4) 0.4827(4) 0.032 Uiso 1 calc R . C43 C 0.0076(7) 0.1674(4) 0.5671(4) 0.034(2) Uani 1 d . . H43A H -0.0726(7) 0.1554(4) 0.5451(4) 0.040 Uiso 1 calc R . C44 C 0.0662(7) 0.1315(4) 0.6341(4) 0.033(2) Uani 1 d . . H44A H 0.0274(7) 0.0943(4) 0.6577(4) 0.040 Uiso 1 calc R . C45 C 0.1820(7) 0.1495(4) 0.6675(4) 0.035(2) Uani 1 d . . H45A H 0.2237(7) 0.1241(4) 0.7135(4) 0.042 Uiso 1 calc R . C46 C 0.2372(6) 0.2045(4) 0.6340(4) 0.032(2) Uani 1 d . . H46A H 0.3156(6) 0.2185(4) 0.6587(4) 0.038 Uiso 1 calc R . C51 C 0.1539(6) 0.3546(4) 0.4438(4) 0.023(2) Uani 1 d . . C52 C 0.0552(6) 0.3877(4) 0.4626(5) 0.036(2) Uani 1 d . . H52A H 0.0429(6) 0.3831(4) 0.5146(5) 0.043 Uiso 1 calc R . C53 C -0.0249(7) 0.4275(4) 0.4052(5) 0.042(2) Uani 1 d . . H53A H -0.0920(7) 0.4497(4) 0.4178(5) 0.051 Uiso 1 calc R . C54 C -0.0066(7) 0.4346(4) 0.3301(5) 0.045(2) Uani 1 d . . H54A H -0.0624(7) 0.4606(4) 0.2907(5) 0.054 Uiso 1 calc R . C55 C 0.0898(7) 0.4049(4) 0.3118(5) 0.041(2) Uani 1 d . . H55A H 0.1026(7) 0.4114(4) 0.2601(5) 0.049 Uiso 1 calc R . C56 C 0.1695(7) 0.3653(4) 0.3673(4) 0.032(2) Uani 1 d . . H56A H 0.2369(7) 0.3448(4) 0.3534(4) 0.039 Uiso 1 calc R . C61 C 0.2043(6) 0.1496(4) 0.4061(4) 0.023(2) Uani 1 d . . C62 C 0.1940(6) 0.0827(4) 0.4431(4) 0.026(2) Uani 1 d . . H62A H 0.2616(6) 0.0602(4) 0.4760(4) 0.031 Uiso 1 calc R . C63 C 0.0851(7) 0.0482(4) 0.4323(4) 0.034(2) Uani 1 d . . H63A H 0.0796(7) 0.0023(4) 0.4587(4) 0.041 Uiso 1 calc R . C64 C -0.0132(6) 0.0775(4) 0.3857(4) 0.033(2) Uani 1 d . . H64A H -0.0868(6) 0.0529(4) 0.3793(4) 0.040 Uiso 1 calc R . C65 C -0.0048(7) 0.1435(4) 0.3477(4) 0.036(2) Uani 1 d . . H65A H -0.0735(7) 0.1650(4) 0.3150(4) 0.043 Uiso 1 calc R . C66 C 0.1026(6) 0.1795(4) 0.3560(4) 0.026(2) Uani 1 d . . H66A H 0.1072(6) 0.2244(4) 0.3279(4) 0.031 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.0183(2) 0.0247(2) 0.0254(2) 0.00056(13) 0.00807(12) 0.00071(13) Co1 0.0164(5) 0.0298(5) 0.0256(5) 0.0071(4) 0.0044(4) 0.0010(4) Fe1 0.0233(5) 0.0299(6) 0.0258(5) -0.0022(4) 0.0052(4) -0.0042(4) P1 0.0173(9) 0.0266(10) 0.0218(9) 0.0003(8) 0.0060(7) -0.0013(8) C1 0.022(4) 0.044(5) 0.031(4) -0.013(4) 0.008(3) -0.008(4) O1 0.027(3) 0.051(4) 0.050(4) -0.009(3) -0.013(3) 0.008(3) C2 0.035(5) 0.034(4) 0.036(5) -0.005(4) 0.004(4) -0.016(4) O2 0.067(4) 0.046(4) 0.042(3) 0.009(3) 0.008(3) -0.021(3) C3 0.044(5) 0.037(5) 0.034(4) -0.006(4) 0.009(4) 0.001(4) O3 0.058(4) 0.067(4) 0.063(4) -0.007(3) 0.041(4) 0.006(3) C4 0.041(5) 0.031(4) 0.030(4) 0.004(4) 0.002(4) 0.001(4) O4 0.070(4) 0.043(4) 0.050(4) 0.000(3) -0.016(3) -0.018(3) C5 0.024(4) 0.037(5) 0.046(5) 0.000(4) 0.017(4) -0.004(4) O5 0.028(3) 0.042(3) 0.093(5) 0.011(3) 0.022(3) 0.014(3) C6 0.026(4) 0.034(5) 0.042(5) -0.005(4) 0.016(4) 0.008(4) O6 0.051(4) 0.028(3) 0.076(4) 0.000(3) 0.034(3) 0.001(3) C7 0.026(5) 0.057(6) 0.062(6) 0.033(5) 0.012(4) 0.002(4) O7 0.019(4) 0.104(6) 0.143(7) 0.087(5) 0.009(4) 0.008(4) C8 0.021(4) 0.041(5) 0.030(4) 0.003(4) 0.006(3) 0.001(3) O8 0.034(3) 0.054(4) 0.048(3) 0.024(3) 0.017(3) 0.008(3) C9 0.013(3) 0.024(4) 0.026(4) 0.005(3) 0.005(3) 0.005(3) C10 0.019(4) 0.023(4) 0.017(3) 0.002(3) 0.005(3) 0.001(3) C11 0.013(3) 0.026(4) 0.025(4) 0.005(3) 0.000(3) -0.002(3) C12 0.017(3) 0.023(4) 0.023(4) 0.004(3) 0.006(3) 0.000(3) C20 0.019(4) 0.035(4) 0.031(4) 0.001(3) 0.007(3) -0.003(3) C21 0.033(4) 0.043(5) 0.031(4) 0.009(4) 0.008(3) -0.006(4) C22 0.022(4) 0.046(5) 0.048(5) -0.007(4) 0.021(4) -0.011(4) C23 0.022(4) 0.052(5) 0.035(4) 0.005(4) 0.003(3) -0.013(4) C31 0.054(6) 0.052(5) 0.025(4) -0.008(4) 0.013(4) 0.015(5) C32 0.023(4) 0.053(5) 0.027(4) 0.004(4) 0.010(3) 0.002(4) C33 0.030(4) 0.038(4) 0.022(4) 0.007(3) 0.004(3) -0.003(4) C34 0.024(4) 0.043(5) 0.023(4) 0.008(3) 0.000(3) 0.008(3) C35 0.030(4) 0.052(5) 0.028(4) -0.005(4) -0.002(3) -0.007(4) C41 0.022(4) 0.026(4) 0.027(4) -0.004(3) 0.009(3) -0.001(3) C42 0.022(4) 0.030(4) 0.029(4) -0.006(3) 0.008(3) 0.001(3) C43 0.027(4) 0.041(5) 0.037(4) -0.009(4) 0.015(3) -0.010(4) C44 0.043(5) 0.028(4) 0.037(5) -0.005(4) 0.026(4) -0.007(4) C45 0.043(5) 0.038(5) 0.027(4) 0.005(3) 0.015(4) 0.006(4) C46 0.028(4) 0.039(4) 0.031(4) 0.007(4) 0.011(3) 0.005(4) C51 0.014(4) 0.023(4) 0.031(4) -0.004(3) 0.002(3) -0.001(3) C52 0.027(4) 0.038(5) 0.039(4) 0.005(4) 0.002(4) 0.002(4) C53 0.024(4) 0.037(5) 0.063(6) 0.001(4) 0.003(4) 0.006(4) C54 0.041(5) 0.031(5) 0.050(6) 0.011(4) -0.013(4) -0.003(4) C55 0.044(5) 0.042(5) 0.033(4) 0.014(4) 0.003(4) 0.002(4) C56 0.035(4) 0.028(4) 0.034(4) 0.011(3) 0.006(4) 0.002(3) C61 0.017(4) 0.028(4) 0.027(4) -0.005(3) 0.008(3) -0.001(3) C62 0.022(4) 0.030(4) 0.027(4) 0.002(3) 0.009(3) 0.002(3) C63 0.040(5) 0.029(4) 0.040(4) -0.006(4) 0.022(4) -0.012(4) C64 0.017(4) 0.039(5) 0.045(5) -0.013(4) 0.010(4) -0.010(3) C65 0.028(4) 0.049(5) 0.029(4) -0.013(4) 0.002(3) -0.002(4) C66 0.020(4) 0.033(4) 0.026(4) -0.003(3) 0.010(3) 0.000(3) _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 W1 C5 1.997(8) . ? W1 C6 2.007(8) . ? W1 C9 2.181(6) . ? W1 C12 2.201(7) . ? W1 C31 2.288(7) . ? W1 C35 2.307(7) . ? W1 C32 2.315(7) . ? W1 C34 2.347(7) . ? W1 C33 2.354(7) . ? W1 Co1 2.682(2) . ? Co1 C7 1.739(8) . ? Co1 C8 1.742(8) . ? Co1 C9 2.070(6) . ? Co1 C11 2.103(7) . ? Co1 C12 2.108(6) . ? Co1 C10 2.106(6) . ? Fe1 C2 1.781(8) . ? Fe1 C3 1.786(9) . ? Fe1 C4 1.785(8) . ? Fe1 C1 1.790(9) . ? Fe1 P1 2.263(2) . ? P1 C51 1.805(7) . ? P1 C41 1.830(7) . ? P1 C10 1.842(6) . ? C1 O1 1.142(9) . ? C2 O2 1.151(9) . ? C3 O3 1.138(9) . ? C4 O4 1.138(9) . ? C5 O5 1.148(9) . ? C6 O6 1.133(9) . ? C7 O7 1.138(9) . ? C8 O8 1.148(8) . ? C9 C10 1.437(9) . ? C9 C61 1.506(9) . ? C10 C11 1.408(9) . ? C11 C12 1.414(9) . ? C12 C20 1.564(9) . ? C20 C23 1.532(10) . ? C20 C22 1.528(10) . ? C20 C21 1.532(10) . ? C31 C32 1.405(11) . ? C31 C35 1.447(11) . ? C32 C33 1.410(10) . ? C33 C34 1.389(10) . ? C34 C35 1.413(11) . ? C41 C46 1.389(10) . ? C41 C42 1.402(9) . ? C42 C43 1.391(10) . ? C43 C44 1.366(11) . ? C44 C45 1.381(11) . ? C45 C46 1.378(10) . ? C51 C56 1.395(10) . ? C51 C52 1.403(10) . ? C52 C53 1.393(11) . ? C53 C54 1.375(12) . ? C54 C55 1.350(11) . ? C55 C56 1.370(10) . ? C61 C62 1.379(9) . ? C61 C66 1.404(9) . ? C62 C63 1.388(10) . ? C63 C64 1.347(11) . ? C64 C65 1.368(11) . ? C65 C66 1.388(10) . ? 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 C5 W1 C6 78.3(3) . . ? C5 W1 C9 127.5(3) . . ? C6 W1 C9 81.3(3) . . ? C5 W1 C12 85.5(3) . . ? C6 W1 C12 133.3(3) . . ? C9 W1 C12 74.6(2) . . ? C5 W1 C31 90.4(3) . . ? C6 W1 C31 87.8(3) . . ? C9 W1 C31 136.6(3) . . ? C12 W1 C31 136.3(3) . . ? C5 W1 C35 123.8(3) . . ? C6 W1 C35 81.8(3) . . ? C9 W1 C35 99.9(3) . . ? C12 W1 C35 141.1(3) . . ? C31 W1 C35 36.7(3) . . ? C5 W1 C32 88.7(3) . . ? C6 W1 C32 122.1(3) . . ? C9 W1 C32 142.1(2) . . ? C12 W1 C32 100.8(3) . . ? C31 W1 C32 35.5(3) . . ? C35 W1 C32 59.8(3) . . ? C5 W1 C34 146.4(3) . . ? C6 W1 C34 111.7(3) . . ? C9 W1 C34 86.1(2) . . ? C12 W1 C34 106.0(3) . . ? C31 W1 C34 59.3(3) . . ? C35 W1 C34 35.3(3) . . ? C32 W1 C34 58.5(3) . . ? C5 W1 C33 119.2(3) . . ? C6 W1 C33 140.1(3) . . ? C9 W1 C33 107.4(2) . . ? C12 W1 C33 85.8(2) . . ? C31 W1 C33 58.7(3) . . ? C35 W1 C33 58.6(3) . . ? C32 W1 C33 35.1(3) . . ? C34 W1 C33 34.4(2) . . ? C5 W1 Co1 80.9(2) . . ? C6 W1 Co1 84.0(2) . . ? C9 W1 Co1 49.1(2) . . ? C12 W1 Co1 50.0(2) . . ? C31 W1 Co1 169.1(2) . . ? C35 W1 Co1 147.7(2) . . ? C32 W1 Co1 149.3(2) . . ? C34 W1 Co1 130.8(2) . . ? C33 W1 Co1 131.5(2) . . ? C7 Co1 C8 87.8(3) . . ? C7 Co1 C9 164.7(4) . . ? C8 Co1 C9 101.3(3) . . ? C7 Co1 C11 112.9(3) . . ? C8 Co1 C11 133.6(3) . . ? C9 Co1 C11 69.6(3) . . ? C7 Co1 C12 93.8(3) . . ? C8 Co1 C12 172.4(3) . . ? C9 Co1 C12 78.9(2) . . ? C11 Co1 C12 39.2(2) . . ? C7 Co1 C10 148.9(4) . . ? C8 Co1 C10 105.0(3) . . ? C9 Co1 C10 40.2(2) . . ? C11 Co1 C10 39.1(2) . . ? C12 Co1 C10 70.1(2) . . ? C7 Co1 W1 112.2(3) . . ? C8 Co1 W1 132.9(2) . . ? C9 Co1 W1 52.7(2) . . ? C11 Co1 W1 78.9(2) . . ? C12 Co1 W1 53.1(2) . . ? C10 Co1 W1 79.9(2) . . ? C2 Fe1 C3 115.5(4) . . ? C2 Fe1 C4 90.4(3) . . ? C3 Fe1 C4 94.1(4) . . ? C2 Fe1 C1 129.1(3) . . ? C3 Fe1 C1 115.3(3) . . ? C4 Fe1 C1 88.7(3) . . ? C2 Fe1 P1 87.9(2) . . ? C3 Fe1 P1 91.4(3) . . ? C4 Fe1 P1 174.4(3) . . ? C1 Fe1 P1 88.2(2) . . ? C51 P1 C41 106.0(3) . . ? C51 P1 C10 102.9(3) . . ? C41 P1 C10 108.9(3) . . ? C51 P1 Fe1 110.5(2) . . ? C41 P1 Fe1 113.9(2) . . ? C10 P1 Fe1 113.8(2) . . ? O1 C1 Fe1 176.8(7) . . ? O2 C2 Fe1 179.4(7) . . ? O3 C3 Fe1 177.8(7) . . ? O4 C4 Fe1 177.4(7) . . ? O5 C5 W1 173.9(7) . . ? O6 C6 W1 174.9(7) . . ? O7 C7 Co1 174.8(9) . . ? O8 C8 Co1 174.3(6) . . ? C10 C9 C61 120.9(5) . . ? C10 C9 Co1 71.2(4) . . ? C61 C9 Co1 129.1(5) . . ? C10 C9 W1 116.9(4) . . ? C61 C9 W1 121.3(4) . . ? Co1 C9 W1 78.2(2) . . ? C11 C10 C9 113.8(6) . . ? C11 C10 P1 116.0(5) . . ? C9 C10 P1 130.2(5) . . ? C11 C10 Co1 70.3(4) . . ? C9 C10 Co1 68.5(3) . . ? P1 C10 Co1 133.0(3) . . ? C12 C11 C10 118.1(6) . . ? C12 C11 Co1 70.6(4) . . ? C10 C11 Co1 70.6(4) . . ? C11 C12 C20 112.4(6) . . ? C11 C12 Co1 70.2(4) . . ? C20 C12 Co1 128.9(4) . . ? C11 C12 W1 114.8(4) . . ? C20 C12 W1 131.9(5) . . ? Co1 C12 W1 76.9(2) . . ? C23 C20 C22 107.9(6) . . ? C23 C20 C21 106.3(6) . . ? C22 C20 C21 108.6(6) . . ? C23 C20 C12 114.1(6) . . ? C22 C20 C12 114.5(6) . . ? C21 C20 C12 105.0(5) . . ? C32 C31 C35 107.7(7) . . ? C32 C31 W1 73.3(4) . . ? C35 C31 W1 72.4(4) . . ? C33 C32 C31 108.0(6) . . ? C33 C32 W1 74.0(4) . . ? C31 C32 W1 71.2(4) . . ? C34 C33 C32 108.9(7) . . ? C34 C33 W1 72.5(4) . . ? C32 C33 W1 70.9(4) . . ? C33 C34 C35 108.9(7) . . ? C33 C34 W1 73.1(4) . . ? C35 C34 W1 70.8(4) . . ? C34 C35 C31 106.5(7) . . ? C34 C35 W1 73.9(4) . . ? C31 C35 W1 70.9(4) . . ? C46 C41 C42 119.6(6) . . ? C46 C41 P1 118.3(5) . . ? C42 C41 P1 122.1(5) . . ? C43 C42 C41 118.2(7) . . ? C44 C43 C42 121.9(7) . . ? C43 C44 C45 119.6(7) . . ? C46 C45 C44 120.0(7) . . ? C45 C46 C41 120.6(7) . . ? C56 C51 C52 117.5(6) . . ? C56 C51 P1 121.9(5) . . ? C52 C51 P1 120.5(5) . . ? C53 C52 C51 120.1(7) . . ? C54 C53 C52 119.9(7) . . ? C55 C54 C53 120.7(7) . . ? C54 C55 C56 120.4(8) . . ? C55 C56 C51 121.5(7) . . ? C62 C61 C66 117.8(6) . . ? C62 C61 C9 124.0(6) . . ? C66 C61 C9 118.2(6) . . ? C61 C62 C63 120.2(7) . . ? C64 C63 C62 122.2(7) . . ? C63 C64 C65 118.6(7) . . ? C64 C65 C66 121.1(7) . . ? C65 C66 C61 120.1(7) . . ? _refine_diff_density_max 0.729 _refine_diff_density_min -0.603 _refine_diff_density_rms 0.108 data_mm9814 _database_code_CSD 154856 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H34 Co O4 P W' _chemical_formula_weight 756.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'W' 'W' -0.8490 6.8722 '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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.990(5) _cell_length_b 12.809(5) _cell_length_c 21.080(5) _cell_angle_alpha 90.00 _cell_angle_beta 102.81(4) _cell_angle_gamma 90.00 _cell_volume 2893.6(19) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour 'v dark' _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.736 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1496 _exptl_absorpt_coefficient_mu 4.636 _exptl_absorpt_correction_type spherical _exptl_absorpt_correction_T_min 0.6061 _exptl_absorpt_correction_T_max 0.6542 _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(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 RAXIS-IIC _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23089 _diffrn_reflns_av_R_equivalents 0.0632 _diffrn_reflns_av_sigmaI/netI 0.0817 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.53 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4999 _reflns_number_gt 3822 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00301(18) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4999 _refine_ls_number_parameters 359 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0583 _refine_ls_R_factor_gt 0.0352 _refine_ls_wR_factor_ref 0.0709 _refine_ls_wR_factor_gt 0.0663 _refine_ls_goodness_of_fit_ref 0.981 _refine_ls_restrained_S_all 0.981 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.01058(2) 0.203360(16) 0.295871(11) 0.01921(9) Uani 1 d . . . Co1 Co 0.10398(6) 0.19428(5) 0.42473(3) 0.01745(17) Uani 1 d . . . P1 P 0.26845(13) 0.14485(10) 0.31913(7) 0.0177(3) Uani 1 d . . . C1 C -0.1158(6) 0.0965(5) 0.3056(3) 0.0263(14) Uani 1 d . . . O1 O -0.1898(4) 0.0343(3) 0.3058(2) 0.0439(13) Uani 1 d . . . C2 C 0.1497(5) 0.1923(4) 0.5098(3) 0.0262(13) Uani 1 d . . . O2 O 0.1743(4) 0.1892(4) 0.5656(2) 0.0409(11) Uani 1 d . . . C3 C 0.0553(6) 0.0659(4) 0.4240(3) 0.0271(14) Uani 1 d . . . O3 O 0.0258(5) -0.0208(3) 0.4279(2) 0.0450(13) Uani 1 d . . . O4 O 0.1522(3) 0.0811(3) 0.28609(19) 0.0220(9) Uani 1 d . . . C4 C -0.0958(8) 0.1889(6) 0.1880(3) 0.056(2) Uani 1 d . . . H4 H -0.1337 0.1248 0.1716 0.067 Uiso 1 calc R . . C5 C -0.1522(6) 0.2675(6) 0.2183(4) 0.049(2) Uani 1 d . . . H5 H -0.2339 0.2661 0.2264 0.059 Uiso 1 calc R . . C6 C -0.0649(6) 0.3480(5) 0.2342(3) 0.0353(16) Uani 1 d . . . H6 H -0.0770 0.4114 0.2554 0.042 Uiso 1 calc R . . C7 C 0.0440(6) 0.3194(4) 0.2137(3) 0.0262(14) Uani 1 d . . . H7 H 0.1174 0.3604 0.2180 0.031 Uiso 1 calc R . . C8 C 0.0252(7) 0.2205(5) 0.1860(3) 0.0380(17) Uani 1 d . . . H8 H 0.0839 0.1814 0.1688 0.046 Uiso 1 calc R . . C9 C 0.3504(5) 0.1953(4) 0.2597(3) 0.0197(11) Uani 1 d . . . C10 C 0.3704(5) 0.3015(4) 0.2534(3) 0.0227(12) Uani 1 d . . . H10 H 0.3393 0.3493 0.2804 0.027 Uiso 1 calc R . . C11 C 0.4342(6) 0.3389(5) 0.2088(3) 0.0310(15) Uani 1 d . . . H11 H 0.4477 0.4117 0.2055 0.037 Uiso 1 calc R . . C12 C 0.4788(6) 0.2689(5) 0.1687(3) 0.0341(16) Uani 1 d . . . H12 H 0.5228 0.2937 0.1377 0.041 Uiso 1 calc R . . C13 C 0.4586(7) 0.1626(5) 0.1744(4) 0.0401(17) Uani 1 d . . . H13 H 0.4890 0.1147 0.1472 0.048 Uiso 1 calc R . . C14 C 0.3941(6) 0.1260(4) 0.2197(3) 0.0286(14) Uani 1 d . . . H14 H 0.3801 0.0533 0.2231 0.034 Uiso 1 calc R . . C15 C 0.3781(5) 0.0562(4) 0.3691(3) 0.0227(13) Uani 1 d . . . C16 C 0.5061(5) 0.0668(4) 0.3754(3) 0.0235(13) Uani 1 d . . . H16 H 0.5381 0.1235 0.3551 0.028 Uiso 1 calc R . . C17 C 0.5871(6) -0.0049(4) 0.4113(3) 0.0290(14) Uani 1 d . . . H17 H 0.6746 0.0017 0.4153 0.035 Uiso 1 calc R . . C18 C 0.5395(6) -0.0866(5) 0.4415(3) 0.0341(16) Uani 1 d . . . H18 H 0.5951 -0.1352 0.4669 0.041 Uiso 1 calc R . . C19 C 0.4128(6) -0.0982(5) 0.4353(3) 0.0313(15) Uani 1 d . . . H19 H 0.3815 -0.1548 0.4561 0.038 Uiso 1 calc R . . C20 C 0.3312(6) -0.0275(4) 0.3987(3) 0.0286(14) Uani 1 d . . . H20 H 0.2437 -0.0359 0.3937 0.034 Uiso 1 calc R . . C21 C -0.2002(7) 0.4344(6) 0.3616(4) 0.057(2) Uani 1 d . . . H21A H -0.2765 0.4532 0.3758 0.085 Uiso 1 calc R . . H21B H -0.2190 0.4267 0.3142 0.085 Uiso 1 calc R . . H21C H -0.1377 0.4895 0.3745 0.085 Uiso 1 calc R . . C22 C -0.2493(7) 0.2471(6) 0.3769(5) 0.071(3) Uani 1 d . . . H22A H -0.3191 0.2644 0.3969 0.107 Uiso 1 calc R . . H22B H -0.2137 0.1797 0.3936 0.107 Uiso 1 calc R . . H22C H -0.2792 0.2427 0.3295 0.107 Uiso 1 calc R . . C23 C -0.1327(7) 0.3489(7) 0.4684(4) 0.056(2) Uani 1 d . . . H23A H -0.2124 0.3710 0.4777 0.084 Uiso 1 calc R . . H23B H -0.0697 0.4030 0.4830 0.084 Uiso 1 calc R . . H23C H -0.1057 0.2835 0.4913 0.084 Uiso 1 calc R . . C24 C -0.1493(5) 0.3318(4) 0.3933(3) 0.0290(15) Uani 1 d . . . C25 C -0.0272(5) 0.3016(4) 0.3733(3) 0.0223(12) Uani 1 d . . . C26 C 0.0806(5) 0.3543(4) 0.4080(3) 0.0198(12) Uani 1 d . . . H26 H 0.0729 0.4098 0.4368 0.024 Uiso 1 calc R . . C27 C 0.2031(5) 0.3228(4) 0.3994(3) 0.0159(12) Uani 1 d . . . C28 C 0.1924(5) 0.2430(4) 0.3528(3) 0.0164(12) Uani 1 d . . . C29 C 0.3208(5) 0.3794(4) 0.4373(3) 0.0197(12) Uani 1 d . . . C30 C 0.3225(5) 0.3945(5) 0.5094(3) 0.0288(14) Uani 1 d . . . H30A H 0.3288 0.3263 0.5310 0.043 Uiso 1 calc R . . H30B H 0.2454 0.4292 0.5139 0.043 Uiso 1 calc R . . H30C H 0.3943 0.4376 0.5295 0.043 Uiso 1 calc R . . C31 C 0.4389(5) 0.3195(4) 0.4321(3) 0.0250(13) Uani 1 d . . . H31A H 0.4357 0.2489 0.4497 0.038 Uiso 1 calc R . . H31B H 0.5125 0.3561 0.4570 0.038 Uiso 1 calc R . . H31C H 0.4440 0.3150 0.3864 0.038 Uiso 1 calc R . . C32 C 0.3216(6) 0.4875(4) 0.4037(4) 0.0330(16) Uani 1 d . . . H32A H 0.3924 0.5288 0.4272 0.049 Uiso 1 calc R . . H32B H 0.2436 0.5244 0.4040 0.049 Uiso 1 calc R . . H32C H 0.3293 0.4774 0.3587 0.049 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.01720(13) 0.02103(13) 0.01813(14) 0.00071(11) 0.00121(8) -0.00400(10) Co1 0.0173(4) 0.0184(3) 0.0174(4) 0.0003(3) 0.0055(3) -0.0012(3) P1 0.0185(7) 0.0181(6) 0.0175(8) -0.0014(5) 0.0061(6) -0.0027(6) C1 0.029(3) 0.031(3) 0.018(3) -0.003(2) 0.002(3) -0.003(3) O1 0.039(3) 0.040(2) 0.057(4) -0.012(2) 0.019(3) -0.023(2) C2 0.021(3) 0.028(3) 0.031(4) 0.000(3) 0.010(3) -0.008(3) O2 0.045(3) 0.059(3) 0.019(3) 0.003(2) 0.007(2) -0.010(2) C3 0.031(4) 0.036(3) 0.016(3) -0.002(3) 0.009(3) -0.002(3) O3 0.070(4) 0.024(2) 0.045(3) 0.000(2) 0.020(3) -0.015(2) O4 0.020(2) 0.0215(19) 0.024(2) -0.0006(16) 0.0042(17) -0.0022(16) C4 0.076(6) 0.056(5) 0.021(4) 0.008(3) -0.021(4) -0.033(4) C5 0.021(4) 0.077(6) 0.041(5) 0.024(4) -0.011(3) 0.007(3) C6 0.036(4) 0.038(3) 0.030(4) 0.017(3) 0.001(3) 0.011(3) C7 0.033(3) 0.028(3) 0.018(3) 0.008(2) 0.006(3) 0.003(3) C8 0.061(5) 0.039(4) 0.015(3) 0.007(3) 0.010(3) 0.007(3) C9 0.021(3) 0.018(2) 0.020(3) 0.000(2) 0.005(2) 0.002(2) C10 0.021(3) 0.022(3) 0.026(3) 0.009(3) 0.008(2) 0.005(3) C11 0.029(3) 0.035(3) 0.031(4) 0.009(3) 0.013(3) -0.003(3) C12 0.027(3) 0.040(3) 0.041(4) 0.013(3) 0.019(3) 0.003(3) C13 0.049(5) 0.043(4) 0.035(4) 0.002(3) 0.023(3) 0.014(3) C14 0.038(4) 0.026(3) 0.025(4) 0.000(2) 0.014(3) 0.002(3) C15 0.033(3) 0.016(3) 0.020(3) 0.000(2) 0.008(3) -0.005(2) C16 0.026(3) 0.020(3) 0.025(4) 0.000(2) 0.008(3) -0.001(2) C17 0.031(4) 0.027(3) 0.030(4) 0.002(3) 0.009(3) 0.005(3) C18 0.040(4) 0.029(3) 0.031(4) 0.006(3) 0.004(3) 0.012(3) C19 0.041(4) 0.029(3) 0.026(4) 0.005(3) 0.011(3) 0.003(3) C20 0.033(4) 0.031(3) 0.023(4) -0.006(3) 0.009(3) -0.006(3) C21 0.055(5) 0.060(5) 0.062(6) 0.019(4) 0.027(4) 0.036(4) C22 0.028(4) 0.067(5) 0.132(9) -0.047(5) 0.043(5) -0.016(4) C23 0.034(4) 0.092(6) 0.048(5) 0.008(4) 0.021(4) 0.025(4) C24 0.011(3) 0.024(3) 0.051(5) -0.007(3) 0.004(3) 0.003(2) C25 0.021(3) 0.018(2) 0.027(3) 0.002(3) 0.004(2) 0.002(2) C26 0.025(3) 0.015(2) 0.021(3) 0.003(2) 0.007(2) 0.001(2) C27 0.018(3) 0.014(2) 0.016(3) 0.000(2) 0.004(2) 0.001(2) C28 0.014(3) 0.018(2) 0.017(3) 0.006(2) 0.003(2) -0.002(2) C29 0.020(3) 0.013(2) 0.025(3) -0.005(2) 0.002(2) -0.005(2) C30 0.024(3) 0.032(3) 0.027(4) -0.010(3) -0.002(3) -0.008(3) C31 0.010(3) 0.035(3) 0.028(4) -0.007(3) 0.001(2) -0.001(2) C32 0.023(3) 0.017(3) 0.055(5) -0.002(3) 0.000(3) -0.004(3) _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 W1 C1 1.993(6) . ? W1 C28 2.151(5) . ? W1 C25 2.172(6) . ? W1 O4 2.250(4) . ? W1 C5 2.291(6) . ? W1 C6 2.309(6) . ? W1 C4 2.322(7) . ? W1 C8 2.367(6) . ? W1 C7 2.372(6) . ? W1 Co1 2.6851(12) . ? W1 P1 2.8666(19) . ? Co1 C3 1.728(6) . ? Co1 C2 1.751(6) . ? Co1 C28 2.070(5) . ? Co1 C26 2.086(5) . ? Co1 C27 2.107(5) . ? Co1 C25 2.110(5) . ? P1 O4 1.546(4) . ? P1 C28 1.745(5) . ? P1 C15 1.814(6) . ? P1 C9 1.816(6) . ? C1 O1 1.139(7) . ? C2 O2 1.149(7) . ? C3 O3 1.165(7) . ? C4 C8 1.399(11) . ? C4 C5 1.408(11) . ? C5 C6 1.397(10) . ? C6 C7 1.409(9) . ? C7 C8 1.390(8) . ? C9 C14 1.383(8) . ? C9 C10 1.388(7) . ? C10 C11 1.377(8) . ? C11 C12 1.394(9) . ? C12 C13 1.389(9) . ? C13 C14 1.390(9) . ? C15 C16 1.390(8) . ? C15 C20 1.395(8) . ? C16 C17 1.382(8) . ? C17 C18 1.386(8) . ? C18 C19 1.377(9) . ? C19 C20 1.384(8) . ? C21 C24 1.524(8) . ? C22 C24 1.528(9) . ? C23 C24 1.568(10) . ? C24 C25 1.543(8) . ? C25 C26 1.418(7) . ? C26 C27 1.455(7) . ? C27 C28 1.405(7) . ? C27 C29 1.542(7) . ? C29 C30 1.527(8) . ? C29 C31 1.532(7) . ? C29 C32 1.557(7) . ? 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 C1 W1 C28 133.4(2) . . ? C1 W1 C25 93.9(2) . . ? C28 W1 C25 75.7(2) . . ? C1 W1 O4 92.47(19) . . ? C28 W1 O4 68.87(17) . . ? C25 W1 O4 136.35(18) . . ? C1 W1 C5 82.4(3) . . ? C28 W1 C5 142.7(2) . . ? C25 W1 C5 94.5(3) . . ? O4 W1 C5 129.1(2) . . ? C1 W1 C6 115.9(2) . . ? C28 W1 C6 107.3(2) . . ? C25 W1 C6 81.5(2) . . ? O4 W1 C6 132.6(2) . . ? C5 W1 C6 35.4(2) . . ? C1 W1 C4 80.5(3) . . ? C28 W1 C4 140.3(3) . . ? C25 W1 C4 130.0(3) . . ? O4 W1 C4 93.6(3) . . ? C5 W1 C4 35.5(3) . . ? C6 W1 C4 58.2(3) . . ? C1 W1 C8 111.3(2) . . ? C28 W1 C8 105.5(2) . . ? C25 W1 C8 138.3(2) . . ? O4 W1 C8 77.10(19) . . ? C5 W1 C8 58.7(3) . . ? C6 W1 C8 57.9(2) . . ? C4 W1 C8 34.7(3) . . ? C1 W1 C7 136.9(2) . . ? C28 W1 C7 89.1(2) . . ? C25 W1 C7 105.8(2) . . ? O4 W1 C7 98.45(18) . . ? C5 W1 C7 58.5(2) . . ? C6 W1 C7 35.0(2) . . ? C4 W1 C7 57.4(2) . . ? C8 W1 C7 34.1(2) . . ? C1 W1 Co1 89.16(17) . . ? C28 W1 Co1 49.19(15) . . ? C25 W1 Co1 50.14(14) . . ? O4 W1 Co1 86.88(10) . . ? C5 W1 Co1 143.1(2) . . ? C6 W1 Co1 127.82(18) . . ? C4 W1 Co1 169.62(19) . . ? C8 W1 Co1 154.20(18) . . ? C7 W1 Co1 132.81(15) . . ? C1 W1 P1 119.20(17) . . ? C28 W1 P1 37.39(14) . . ? C25 W1 P1 111.67(15) . . ? O4 W1 P1 32.41(9) . . ? C5 W1 P1 143.3(2) . . ? C6 W1 P1 121.63(18) . . ? C4 W1 P1 114.2(2) . . ? C8 W1 P1 85.00(18) . . ? C7 W1 P1 88.93(16) . . ? Co1 W1 P1 70.97(5) . . ? C3 Co1 C2 90.7(3) . . ? C3 Co1 C28 118.4(2) . . ? C2 Co1 C28 132.8(2) . . ? C3 Co1 C26 155.1(3) . . ? C2 Co1 C26 100.6(2) . . ? C28 Co1 C26 68.9(2) . . ? C3 Co1 C27 156.6(2) . . ? C2 Co1 C27 102.9(2) . . ? C28 Co1 C27 39.3(2) . . ? C26 Co1 C27 40.6(2) . . ? C3 Co1 C25 116.1(2) . . ? C2 Co1 C25 123.0(3) . . ? C28 Co1 C25 78.7(2) . . ? C26 Co1 C25 39.5(2) . . ? C27 Co1 C25 72.1(2) . . ? C3 Co1 W1 89.1(2) . . ? C2 Co1 W1 174.11(19) . . ? C28 Co1 W1 51.83(15) . . ? C26 Co1 W1 77.38(16) . . ? C27 Co1 W1 79.24(15) . . ? C25 Co1 W1 52.21(16) . . ? O4 P1 C28 98.1(2) . . ? O4 P1 C15 107.9(2) . . ? C28 P1 C15 122.1(3) . . ? O4 P1 C9 111.3(2) . . ? C28 P1 C9 112.3(2) . . ? C15 P1 C9 104.8(3) . . ? O4 P1 W1 51.27(14) . . ? C28 P1 W1 48.44(18) . . ? C15 P1 W1 140.1(2) . . ? C9 P1 W1 114.31(18) . . ? O1 C1 W1 174.5(5) . . ? O2 C2 Co1 176.8(5) . . ? O3 C3 Co1 175.5(5) . . ? P1 O4 W1 96.31(17) . . ? C8 C4 C5 108.9(6) . . ? C8 C4 W1 74.4(4) . . ? C5 C4 W1 71.1(4) . . ? C6 C5 C4 106.8(7) . . ? C6 C5 W1 73.0(4) . . ? C4 C5 W1 73.4(4) . . ? C5 C6 C7 108.6(6) . . ? C5 C6 W1 71.6(4) . . ? C7 C6 W1 75.0(3) . . ? C8 C7 C6 107.9(6) . . ? C8 C7 W1 72.7(3) . . ? C6 C7 W1 70.0(3) . . ? C7 C8 C4 107.8(6) . . ? C7 C8 W1 73.1(4) . . ? C4 C8 W1 70.9(4) . . ? C14 C9 C10 119.1(5) . . ? C14 C9 P1 119.0(4) . . ? C10 C9 P1 121.8(4) . . ? C11 C10 C9 121.4(6) . . ? C10 C11 C12 119.4(6) . . ? C13 C12 C11 119.5(6) . . ? C12 C13 C14 120.4(6) . . ? C9 C14 C13 120.1(6) . . ? C16 C15 C20 119.9(5) . . ? C16 C15 P1 121.5(4) . . ? C20 C15 P1 118.5(5) . . ? C17 C16 C15 120.2(5) . . ? C16 C17 C18 119.4(6) . . ? C19 C18 C17 120.9(6) . . ? C18 C19 C20 120.0(6) . . ? C19 C20 C15 119.6(6) . . ? C21 C24 C22 109.7(6) . . ? C21 C24 C25 110.6(5) . . ? C22 C24 C25 112.7(5) . . ? C21 C24 C23 105.7(6) . . ? C22 C24 C23 104.2(6) . . ? C25 C24 C23 113.5(5) . . ? C26 C25 C24 114.7(5) . . ? C26 C25 Co1 69.3(3) . . ? C24 C25 Co1 124.0(4) . . ? C26 C25 W1 112.8(4) . . ? C24 C25 W1 132.3(4) . . ? Co1 C25 W1 77.65(18) . . ? C25 C26 C27 119.6(5) . . ? C25 C26 Co1 71.2(3) . . ? C27 C26 Co1 70.5(3) . . ? C28 C27 C26 110.6(5) . . ? C28 C27 C29 129.4(5) . . ? C26 C27 C29 119.9(4) . . ? C28 C27 Co1 68.9(3) . . ? C26 C27 Co1 68.9(3) . . ? C29 C27 Co1 131.1(4) . . ? C27 C28 P1 146.6(4) . . ? C27 C28 Co1 71.8(3) . . ? P1 C28 Co1 115.2(2) . . ? C27 C28 W1 119.1(4) . . ? P1 C28 W1 94.2(2) . . ? Co1 C28 W1 78.98(18) . . ? C30 C29 C31 108.1(5) . . ? C30 C29 C27 113.5(5) . . ? C31 C29 C27 110.7(4) . . ? C30 C29 C32 109.9(5) . . ? C31 C29 C32 108.8(5) . . ? C27 C29 C32 105.7(4) . . ? _diffrn_measured_fraction_theta_max 0.935 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.935 _refine_diff_density_max 0.892 _refine_diff_density_min -1.409 _refine_diff_density_rms 0.217