# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2001 # CCDC Number: 186/2280 data_00srv174 _publ_requested_journal 'test' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H28 Co2 O4 P2' _chemical_formula_weight 716.39 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' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 39.6115(10) _cell_length_b 12.2498(3) _cell_length_c 14.6354(4) _cell_angle_alpha 90 _cell_angle_beta 92.074(2) _cell_angle_gamma 90 _cell_volume 7096.9(3) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description irregular _exptl_crystal_colour clear_red _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.34 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2922 _exptl_absorpt_coefficient_mu 1.061 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min . _exptl_absorpt_correction_T_max . _exptl_absorpt_process_details . _exptl_special_details ; The data collection nominally covered over a full sphere of reciprocal space, by a combination of 5 sets of \w scans, each set at different \f and/or 2\q angles and each scan (10 s exposure) covering 0.3\% in \w. Crystal to detector distance 4.51 cm. PLATON Squeeze was used. Sum-formula, density and mu are calculated without taking the solvent into account. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD 1K area detector' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean 8 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 38965 _diffrn_reflns_av_R_equivalents 0.0269 _diffrn_reflns_av_sigmaI/netI 0.0182 _diffrn_reflns_limit_h_min -54 _diffrn_reflns_limit_h_max 53 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.03 _diffrn_reflns_theta_max 29.02 _reflns_number_total 9374 _reflns_number_gt 8330 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT V5.0 (Bruker, 1998)' _computing_cell_refinement 'SMART-NT V5.0 (Bruker, 1998)' _computing_data_reduction 'SAINT-NT V5.0 (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Ferrugia, 2000)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0340P)^2^+10.9346P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9374 _refine_ls_number_parameters 410 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0389 _refine_ls_R_factor_gt 0.0330 _refine_ls_wR_factor_ref 0.0793 _refine_ls_wR_factor_gt 0.0768 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.085 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.165960(5) 0.287370(17) 0.303110(14) 0.01423(5) Uani 1 1 d . . . Co2 Co 0.103125(5) 0.288766(17) 0.298168(14) 0.01378(5) Uani 1 1 d . . . P1 P 0.173259(10) 0.37536(3) 0.43550(3) 0.01385(8) Uani 1 1 d . . . P2 P 0.096883(10) 0.38597(3) 0.42571(3) 0.01360(8) Uani 1 1 d . . . C22 C 0.09624(4) 0.14609(14) 0.31660(11) 0.0198(3) Uani 1 1 d . . . C12 C 0.17365(4) 0.14491(14) 0.32440(12) 0.0227(3) Uani 1 1 d . . . C121 C 0.17986(4) 0.29986(13) 0.54204(10) 0.0162(3) Uani 1 1 d . . . C5 C 0.13613(4) 0.46196(12) 0.45258(10) 0.0153(3) Uani 1 1 d . . . H5A H 0.1371 0.5258 0.4135 0.018 Uiso 1 1 calc R . . H5B H 0.1362 0.4867 0.5156 0.018 Uiso 1 1 calc R . . C221 C 0.08857(4) 0.32022(13) 0.53558(11) 0.0175(3) Uani 1 1 d . . . C4 C 0.13490(4) 0.38907(13) 0.24120(10) 0.0158(3) Uani 1 1 d . . . H4 H 0.1346(5) 0.4660(19) 0.2285(15) 0.028(6) Uiso 1 1 d . . . O11 O 0.22819(3) 0.34879(12) 0.21532(9) 0.0300(3) Uani 1 1 d . . . C3 C 0.13377(4) 0.29239(13) 0.19715(10) 0.0159(3) Uani 1 1 d . . . C111 C 0.20744(4) 0.47678(13) 0.44107(11) 0.0170(3) Uani 1 1 d . . . C224 C 0.07927(5) 0.22238(17) 0.70582(13) 0.0319(4) Uani 1 1 d . . . H224 H 0.0761 0.1897 0.7622 0.038 Uiso 1 1 calc R . . C34 C 0.13436(4) 0.24328(13) 0.10575(10) 0.0163(3) Uani 1 1 d . . . C124 C 0.19109(5) 0.17833(16) 0.70252(12) 0.0291(4) Uani 1 1 d . . . H124 H 0.1945 0.1373 0.7555 0.035 Uiso 1 1 calc R . . C225 C 0.07477(4) 0.33453(16) 0.69542(12) 0.0255(4) Uani 1 1 d . . . H225 H 0.0687 0.3769 0.7449 0.031 Uiso 1 1 calc R . . C211 C 0.06489(4) 0.49405(13) 0.42081(10) 0.0154(3) Uani 1 1 d . . . C116 C 0.21138(4) 0.54279(14) 0.36431(12) 0.0211(3) Uani 1 1 d . . . H116 H 0.1967 0.5348 0.3138 0.025 Uiso 1 1 calc R . . C123 C 0.17097(5) 0.27064(16) 0.70313(11) 0.0246(4) Uani 1 1 d . . . H123 H 0.1609 0.2918 0.7567 0.029 Uiso 1 1 calc R . . C226 C 0.07945(4) 0.38305(15) 0.61076(11) 0.0201(3) Uani 1 1 d . . . H226 H 0.0765 0.4580 0.6041 0.024 Uiso 1 1 calc R . . C222 C 0.09306(5) 0.20814(15) 0.54689(12) 0.0283(4) Uani 1 1 d . . . H222 H 0.0992 0.1654 0.4976 0.034 Uiso 1 1 calc R . . C122 C 0.16576(4) 0.33184(15) 0.62401(11) 0.0211(3) Uani 1 1 d . . . H122 H 0.1527 0.3949 0.6256 0.025 Uiso 1 1 calc R . . C33 C 0.15823(4) 0.27751(13) 0.04323(11) 0.0181(3) Uani 1 1 d . . . H33 H 0.1737 0.3317 0.0599 0.022 Uiso 1 1 calc R . . C32 C 0.15895(4) 0.23105(14) -0.04330(11) 0.0215(3) Uani 1 1 d . . . H32 H 0.1750 0.2540 -0.0839 0.026 Uiso 1 1 calc R . . C126 C 0.20027(5) 0.20684(15) 0.54227(12) 0.0262(4) Uani 1 1 d . . . H126 H 0.2100 0.1845 0.4885 0.031 Uiso 1 1 calc R . . C212 C 0.03209(4) 0.46436(14) 0.39163(12) 0.0219(3) Uani 1 1 d . . . H212 H 0.0273 0.3919 0.3774 0.026 Uiso 1 1 calc R . . C214 C 0.01339(5) 0.65062(15) 0.40645(13) 0.0262(4) Uani 1 1 d . . . H214 H -0.0037 0.7026 0.4014 0.031 Uiso 1 1 calc R . . C36 C 0.11206(5) 0.11613(14) -0.00867(12) 0.0245(3) Uani 1 1 d . . . H36 H 0.0965 0.0626 -0.0261 0.029 Uiso 1 1 calc R . . C112 C 0.22974(4) 0.48979(15) 0.51674(12) 0.0219(3) Uani 1 1 d . . . H112 H 0.2274 0.4468 0.5685 0.026 Uiso 1 1 calc R . . C216 C 0.07135(4) 0.60330(13) 0.44398(11) 0.0190(3) Uani 1 1 d . . . H216 H 0.0929 0.6243 0.4644 0.023 Uiso 1 1 calc R . . C213 C 0.00672(4) 0.54225(16) 0.38375(14) 0.0285(4) Uani 1 1 d . . . H213 H -0.0149 0.5219 0.3632 0.034 Uiso 1 1 calc R . . C113 C 0.25552(4) 0.56738(15) 0.51437(13) 0.0258(4) Uani 1 1 d . . . H113 H 0.2703 0.5758 0.5646 0.031 Uiso 1 1 calc R . . C215 C 0.04555(4) 0.68071(14) 0.43653(12) 0.0232(3) Uani 1 1 d . . . H215 H 0.0500 0.7531 0.4519 0.028 Uiso 1 1 calc R . . C31 C 0.13582(5) 0.15060(15) -0.06981(11) 0.0239(3) Uani 1 1 d . . . H31 H 0.1363 0.1202 -0.1280 0.029 Uiso 1 1 calc R . . C35 C 0.11142(4) 0.16135(14) 0.07876(11) 0.0215(3) Uani 1 1 d . . . H35 H 0.0956 0.1369 0.1195 0.026 Uiso 1 1 calc R . . C125 C 0.20615(6) 0.14737(17) 0.62231(13) 0.0341(4) Uani 1 1 d . . . H125 H 0.2202 0.0866 0.6221 0.041 Uiso 1 1 calc R . . C115 C 0.23701(5) 0.62023(15) 0.36256(14) 0.0268(4) Uani 1 1 d . . . H115 H 0.2393 0.6640 0.3112 0.032 Uiso 1 1 calc R . . C114 C 0.25918(4) 0.63216(15) 0.43738(14) 0.0269(4) Uani 1 1 d . . . H114 H 0.2765 0.6834 0.4361 0.032 Uiso 1 1 calc R . . C223 C 0.08840(6) 0.15958(17) 0.63204(13) 0.0372(5) Uani 1 1 d . . . H223 H 0.0914 0.0847 0.6391 0.045 Uiso 1 1 calc R . . O22 O 0.09206(4) 0.05364(11) 0.32021(9) 0.0324(3) Uani 1 1 d . . . O21 O 0.04127(4) 0.33401(13) 0.19011(10) 0.0363(3) Uani 1 1 d . . . O12 O 0.17875(4) 0.05389(11) 0.33444(12) 0.0397(4) Uani 1 1 d . . . C11 C 0.20422(4) 0.32307(14) 0.25126(11) 0.0204(3) Uani 1 1 d . . . C21 C 0.06493(4) 0.31808(14) 0.23543(11) 0.0212(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.01724(10) 0.01409(10) 0.01135(10) -0.00120(7) 0.00047(7) 0.00148(7) Co2 0.01707(10) 0.01320(10) 0.01104(10) -0.00051(7) 0.00006(7) 0.00029(7) P1 0.01582(17) 0.01408(17) 0.01162(17) -0.00101(14) 0.00000(13) 0.00098(14) P2 0.01564(17) 0.01321(17) 0.01195(17) -0.00069(13) 0.00051(13) 0.00030(13) C22 0.0256(8) 0.0205(8) 0.0134(7) 0.0010(6) 0.0005(6) -0.0013(6) C12 0.0240(8) 0.0212(8) 0.0226(8) -0.0026(7) -0.0031(6) 0.0013(6) C121 0.0181(7) 0.0164(7) 0.0140(7) 0.0001(6) -0.0008(5) 0.0015(6) C5 0.0168(7) 0.0145(7) 0.0145(7) -0.0017(5) -0.0002(5) 0.0000(5) C221 0.0189(7) 0.0198(7) 0.0139(7) 0.0005(6) -0.0002(5) -0.0019(6) C4 0.0188(7) 0.0149(7) 0.0136(7) 0.0020(6) 0.0002(5) 0.0000(5) O11 0.0244(6) 0.0405(8) 0.0257(7) -0.0018(6) 0.0073(5) 0.0003(6) C3 0.0182(7) 0.0171(7) 0.0124(6) 0.0017(5) 0.0009(5) 0.0000(6) C111 0.0158(7) 0.0158(7) 0.0193(7) -0.0038(6) 0.0012(6) 0.0011(5) C224 0.0418(11) 0.0372(11) 0.0168(8) 0.0083(7) 0.0025(7) -0.0069(8) C34 0.0214(7) 0.0152(7) 0.0123(7) 0.0002(5) 0.0002(5) 0.0038(6) C124 0.0406(11) 0.0289(9) 0.0176(8) 0.0067(7) -0.0035(7) 0.0013(8) C225 0.0246(8) 0.0377(10) 0.0144(7) 0.0000(7) 0.0028(6) 0.0021(7) C211 0.0167(7) 0.0175(7) 0.0121(6) -0.0001(5) 0.0015(5) 0.0021(6) C116 0.0187(7) 0.0205(8) 0.0240(8) 0.0005(6) -0.0017(6) -0.0001(6) C123 0.0254(8) 0.0357(10) 0.0127(7) -0.0004(7) 0.0011(6) 0.0013(7) C226 0.0185(7) 0.0252(8) 0.0168(7) -0.0011(6) 0.0012(6) 0.0022(6) C222 0.0488(12) 0.0190(8) 0.0170(8) -0.0008(6) 0.0005(7) -0.0032(8) C122 0.0224(8) 0.0253(8) 0.0156(7) -0.0014(6) -0.0011(6) 0.0053(6) C33 0.0213(8) 0.0185(7) 0.0143(7) 0.0013(6) -0.0004(6) 0.0015(6) C32 0.0249(8) 0.0254(8) 0.0145(7) 0.0019(6) 0.0041(6) 0.0053(6) C126 0.0370(10) 0.0244(9) 0.0172(8) -0.0009(7) 0.0016(7) 0.0122(7) C212 0.0187(8) 0.0208(8) 0.0261(8) -0.0063(7) 0.0002(6) 0.0000(6) C214 0.0231(8) 0.0245(9) 0.0308(9) -0.0044(7) -0.0019(7) 0.0085(7) C36 0.0341(9) 0.0200(8) 0.0194(8) -0.0057(6) -0.0004(7) -0.0028(7) C112 0.0212(8) 0.0262(8) 0.0184(8) -0.0040(6) -0.0004(6) 0.0002(6) C216 0.0186(7) 0.0193(8) 0.0191(7) -0.0029(6) -0.0006(6) 0.0003(6) C213 0.0171(8) 0.0307(9) 0.0373(10) -0.0091(8) -0.0023(7) 0.0023(7) C113 0.0198(8) 0.0301(9) 0.0271(9) -0.0101(7) -0.0031(6) -0.0021(7) C215 0.0246(8) 0.0186(8) 0.0265(8) -0.0036(7) 0.0006(7) 0.0032(6) C31 0.0345(9) 0.0242(8) 0.0128(7) -0.0034(6) 0.0007(6) 0.0049(7) C35 0.0290(9) 0.0204(8) 0.0153(7) -0.0012(6) 0.0028(6) -0.0025(6) C125 0.0512(12) 0.0278(10) 0.0229(9) 0.0014(8) -0.0030(8) 0.0168(9) C115 0.0256(9) 0.0189(8) 0.0361(10) 0.0034(7) 0.0022(7) -0.0019(7) C114 0.0193(8) 0.0196(8) 0.0418(11) -0.0056(7) 0.0005(7) -0.0040(6) C223 0.0679(15) 0.0216(9) 0.0220(9) 0.0049(7) 0.0013(9) -0.0083(9) O22 0.0517(9) 0.0179(6) 0.0275(7) 0.0022(5) -0.0027(6) -0.0049(6) O21 0.0306(7) 0.0462(9) 0.0312(7) -0.0022(7) -0.0107(6) 0.0087(6) O12 0.0455(9) 0.0188(7) 0.0543(10) 0.0012(6) -0.0068(7) 0.0059(6) C11 0.0227(8) 0.0234(8) 0.0150(7) -0.0034(6) -0.0010(6) 0.0035(6) C21 0.0240(8) 0.0215(8) 0.0181(7) -0.0015(6) 0.0009(6) 0.0017(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 C11 1.7741(17) . ? Co1 C12 1.7968(18) . ? Co1 C4 1.9508(16) . ? Co1 C3 1.9727(15) . ? Co1 P1 2.2269(4) . ? Co1 Co2 2.4875(3) . ? Co2 C21 1.7779(17) . ? Co2 C22 1.7908(17) . ? Co2 C3 1.9470(15) . ? Co2 C4 1.9660(16) . ? Co2 P2 2.2354(4) . ? P1 C121 1.8236(16) . ? P1 C111 1.8373(16) . ? P1 C5 1.8380(15) . ? P2 C211 1.8322(16) . ? P2 C221 1.8387(16) . ? P2 C5 1.8421(15) . ? C22 O22 1.146(2) . ? C12 O12 1.142(2) . ? C121 C126 1.397(2) . ? C121 C122 1.397(2) . ? C221 C222 1.393(2) . ? C221 C226 1.401(2) . ? C4 C3 1.348(2) . ? O11 C11 1.146(2) . ? C3 C34 1.468(2) . ? C111 C116 1.397(2) . ? C111 C112 1.401(2) . ? C224 C223 1.384(3) . ? C224 C225 1.393(3) . ? C34 C35 1.401(2) . ? C34 C33 1.403(2) . ? C124 C123 1.384(3) . ? C124 C125 1.389(3) . ? C225 C226 1.393(2) . ? C211 C212 1.401(2) . ? C211 C216 1.402(2) . ? C116 C115 1.390(2) . ? C123 C122 1.389(2) . ? C222 C223 1.399(3) . ? C33 C32 1.390(2) . ? C32 C31 1.391(3) . ? C126 C125 1.392(3) . ? C212 C213 1.387(2) . ? C214 C215 1.383(3) . ? C214 C213 1.391(3) . ? C36 C31 1.388(3) . ? C36 C35 1.395(2) . ? C112 C113 1.396(2) . ? C216 C215 1.396(2) . ? C113 C114 1.390(3) . ? C115 C114 1.386(3) . ? O21 C21 1.145(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 Co1 C12 99.87(8) . . ? C11 Co1 C4 100.25(7) . . ? C12 Co1 C4 143.21(7) . . ? C11 Co1 C3 101.19(7) . . ? C12 Co1 C3 105.50(7) . . ? C4 Co1 C3 40.19(6) . . ? C11 Co1 P1 99.61(5) . . ? C12 Co1 P1 107.66(6) . . ? C4 Co1 P1 98.91(5) . . ? C3 Co1 P1 136.78(5) . . ? C11 Co1 Co2 148.79(5) . . ? C12 Co1 Co2 100.07(6) . . ? C4 Co1 Co2 50.85(5) . . ? C3 Co1 Co2 50.15(4) . . ? P1 Co1 Co2 96.905(13) . . ? C21 Co2 C22 98.26(8) . . ? C21 Co2 C3 98.37(7) . . ? C22 Co2 C3 103.84(7) . . ? C21 Co2 C4 101.58(7) . . ? C22 Co2 C4 141.00(7) . . ? C3 Co2 C4 40.31(6) . . ? C21 Co2 P2 101.88(6) . . ? C22 Co2 P2 111.84(5) . . ? C3 Co2 P2 135.46(5) . . ? C4 Co2 P2 96.50(5) . . ? C21 Co2 Co1 148.03(6) . . ? C22 Co2 Co1 98.42(6) . . ? C3 Co2 Co1 51.07(5) . . ? C4 Co2 Co1 50.31(5) . . ? P2 Co2 Co1 96.903(13) . . ? C121 P1 C111 102.86(7) . . ? C121 P1 C5 105.49(7) . . ? C111 P1 C5 101.29(7) . . ? C121 P1 Co1 120.57(5) . . ? C111 P1 Co1 115.98(5) . . ? C5 P1 Co1 108.56(5) . . ? C211 P2 C221 101.85(7) . . ? C211 P2 C5 102.73(7) . . ? C221 P2 C5 102.19(7) . . ? C211 P2 Co2 116.71(5) . . ? C221 P2 Co2 121.71(5) . . ? C5 P2 Co2 109.24(5) . . ? O22 C22 Co2 173.93(15) . . ? O12 C12 Co1 177.37(18) . . ? C126 C121 C122 118.41(15) . . ? C126 C121 P1 118.73(12) . . ? C122 C121 P1 122.85(12) . . ? P1 C5 P2 110.64(8) . . ? C222 C221 C226 118.91(15) . . ? C222 C221 P2 120.62(13) . . ? C226 C221 P2 120.37(13) . . ? C3 C4 Co1 70.78(9) . . ? C3 C4 Co2 69.09(9) . . ? Co1 C4 Co2 78.85(6) . . ? C4 C3 C34 142.60(15) . . ? C4 C3 Co2 70.61(9) . . ? C34 C3 Co2 135.54(12) . . ? C4 C3 Co1 69.03(9) . . ? C34 C3 Co1 132.26(11) . . ? Co2 C3 Co1 78.78(6) . . ? C116 C111 C112 118.96(15) . . ? C116 C111 P1 117.34(12) . . ? C112 C111 P1 123.69(13) . . ? C223 C224 C225 119.92(17) . . ? C35 C34 C33 118.40(14) . . ? C35 C34 C3 121.26(14) . . ? C33 C34 C3 120.34(14) . . ? C123 C124 C125 119.59(17) . . ? C226 C225 C224 119.84(17) . . ? C212 C211 C216 118.73(15) . . ? C212 C211 P2 117.18(12) . . ? C216 C211 P2 124.08(12) . . ? C115 C116 C111 120.83(16) . . ? C124 C123 C122 120.27(16) . . ? C225 C226 C221 120.71(16) . . ? C221 C222 C223 120.28(17) . . ? C123 C122 C121 120.83(16) . . ? C32 C33 C34 120.55(15) . . ? C33 C32 C31 120.61(16) . . ? C125 C126 C121 120.54(16) . . ? C213 C212 C211 120.52(16) . . ? C215 C214 C213 119.68(16) . . ? C31 C36 C35 120.38(16) . . ? C113 C112 C111 119.92(16) . . ? C215 C216 C211 120.20(15) . . ? C212 C213 C214 120.37(17) . . ? C114 C113 C112 120.43(16) . . ? C214 C215 C216 120.49(16) . . ? C36 C31 C32 119.40(15) . . ? C36 C35 C34 120.65(16) . . ? C124 C125 C126 120.30(18) . . ? C114 C115 C116 119.96(17) . . ? C115 C114 C113 119.90(16) . . ? C224 C223 C222 120.33(18) . . ? O11 C11 Co1 177.20(16) . . ? O21 C21 Co2 175.51(16) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 29.02 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.609 _refine_diff_density_min -0.400 _refine_diff_density_rms 0.067 data_00srv167 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H33 Co2 N O4 P2' _chemical_formula_weight 759.46 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Co' 'Co' 0.3494 0.9721 '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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _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 14.301(1) _cell_length_b 15.716(1) _cell_length_c 15.727(1) _cell_angle_alpha 90 _cell_angle_beta 98.792(2) _cell_angle_gamma 90 _cell_volume 3493.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rectangular-prism _exptl_crystal_colour metallic_dark_red _exptl_crystal_size_max 0.65 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.444 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1560 _exptl_absorpt_coefficient_mu 1.083 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min . _exptl_absorpt_correction_T_max . _exptl_absorpt_process_details . _exptl_special_details ; The data collection nominally covered over a full sphere of reciprocal space, by a combination of 5 sets of \w scans, each set at different \f and/or 2\q angles and each scan (10 s exposure) covering 0.3\% in \w. Crystal to detector distance 4.51 cm. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD 1K area detector' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean 8 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 35790 _diffrn_reflns_av_R_equivalents 0.0585 _diffrn_reflns_av_sigmaI/netI 0.0296 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 27.51 _reflns_number_total 8011 _reflns_number_gt 7247 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT V5.0 (Bruker, 1998)' _computing_cell_refinement 'SMART-NT V5.0 (Bruker, 1998)' _computing_data_reduction 'SAINT-NT V5.0 (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Ferrugia, 2000)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0240P)^2^+3.9673P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8011 _refine_ls_number_parameters 441 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0396 _refine_ls_R_factor_gt 0.0338 _refine_ls_wR_factor_ref 0.0820 _refine_ls_wR_factor_gt 0.0761 _refine_ls_goodness_of_fit_ref 1.116 _refine_ls_restrained_S_all 1.116 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co2 Co 0.783095(17) 0.054852(15) 0.233354(15) 0.01475(7) Uani 1 1 d . . . Co1 Co 0.636309(18) -0.020895(16) 0.174856(15) 0.01600(7) Uani 1 1 d . . . P2 P 0.73495(3) 0.12289(3) 0.34227(3) 0.01445(9) Uani 1 1 d . . . P1 P 0.55049(3) 0.02682(3) 0.27166(3) 0.01479(10) Uani 1 1 d . . . N N 0.95056(12) -0.23428(11) -0.06851(11) 0.0225(3) Uani 1 1 d . . . O22 O 0.74214(11) 0.18679(10) 0.10132(10) 0.0270(3) Uani 1 1 d . . . O21 O 0.98955(11) 0.06142(12) 0.26305(12) 0.0381(4) Uani 1 1 d . . . O12 O 0.58211(12) 0.06756(12) 0.00948(10) 0.0350(4) Uani 1 1 d . . . O11 O 0.54848(12) -0.18769(10) 0.13941(11) 0.0333(4) Uani 1 1 d . . . C4 C 0.74338(14) -0.06139(12) 0.25756(12) 0.0187(4) Uani 1 1 d . . . H4 H 0.7484(17) -0.0998(16) 0.3035(15) 0.023(6) Uiso 1 1 d . . . C3 C 0.77016(13) -0.05647(12) 0.17904(12) 0.0178(3) Uani 1 1 d . . . C5 C 0.60470(13) 0.11905(12) 0.33471(11) 0.0160(3) Uani 1 1 d . . . H5B H 0.5781 0.1711 0.3081 0.019 Uiso 1 1 d R . . H5A H 0.5884 0.1164 0.3923 0.019 Uiso 1 1 d R . . C22 C 0.75958(13) 0.13555(12) 0.15299(12) 0.0182(4) Uani 1 1 d . . . C21 C 0.90843(14) 0.05860(13) 0.25452(12) 0.0217(4) Uani 1 1 d . . . C12 C 0.60205(14) 0.03389(14) 0.07443(13) 0.0228(4) Uani 1 1 d . . . C11 C 0.58006(15) -0.12108(14) 0.15208(12) 0.0233(4) Uani 1 1 d . . . C34 C 0.81944(13) -0.10248(12) 0.11805(11) 0.0175(3) Uani 1 1 d . . . C35 C 0.86627(14) -0.05927(12) 0.05874(12) 0.0197(4) Uani 1 1 d . . . H35 H 0.8670 -0.0001 0.0589 0.024 Uiso 1 1 d R . . C36 C 0.91142(14) -0.10258(13) -0.00001(12) 0.0203(4) Uani 1 1 d . . . H36 H 0.9428 -0.0720 -0.0377 0.024 Uiso 1 1 d R . . C31 C 0.91069(13) -0.19217(12) -0.00374(12) 0.0180(4) Uani 1 1 d . . . C32 C 0.86433(15) -0.23566(12) 0.05624(13) 0.0228(4) Uani 1 1 d . . . H32 H 0.8632 -0.2948 0.0560 0.027 Uiso 1 1 d R . . C33 C 0.82026(15) -0.19164(13) 0.11585(13) 0.0230(4) Uani 1 1 d . . . H33 H 0.7907 -0.2220 0.1550 0.028 Uiso 1 1 d R . . C42 C 1.04235(18) -0.20569(17) -0.08597(16) 0.0359(5) Uani 1 1 d . . . H42B H 1.0421(5) -0.1452(11) -0.0913(12) 0.054 Uiso 1 1 d R . . H42C H 1.0552(7) -0.2307(11) -0.1382(12) 0.054 Uiso 1 1 d R . . H42A H 1.0901(9) -0.2223(11) -0.0398(10) 0.054 Uiso 1 1 d R . . C41 C 0.9406(2) -0.32581(15) -0.07420(19) 0.0426(6) Uani 1 1 d . . . H41A H 0.9803(14) -0.3523(5) -0.0249(12) 0.064 Uiso 1 1 d R . . H41C H 0.9606(15) -0.3459(4) -0.1277(12) 0.064 Uiso 1 1 d R . . H41B H 0.8742(13) -0.3413(4) -0.0739(14) 0.064 Uiso 1 1 d R . . C221 C 0.76434(13) 0.23713(11) 0.34882(11) 0.0165(3) Uani 1 1 d . . . C226 C 0.70353(14) 0.30070(13) 0.36938(12) 0.0212(4) Uani 1 1 d . . . H226 H 0.6433 0.2867 0.3802 0.025 Uiso 1 1 d R . . C225 C 0.73344(16) 0.38594(13) 0.37373(13) 0.0256(4) Uani 1 1 d . . . H225 H 0.6927 0.4282 0.3874 0.031 Uiso 1 1 d R . . C224 C 0.82268(16) 0.40765(13) 0.35797(12) 0.0249(4) Uani 1 1 d . . . H224 H 0.8413 0.4644 0.3600 0.030 Uiso 1 1 d R . . C223 C 0.88490(15) 0.34466(14) 0.33911(13) 0.0247(4) Uani 1 1 d . . . H223 H 0.9457 0.3590 0.3301 0.030 Uiso 1 1 d R . . C222 C 0.85524(14) 0.25980(13) 0.33377(12) 0.0217(4) Uani 1 1 d . . . H222 H 0.8963 0.2178 0.3201 0.026 Uiso 1 1 d R . . C211 C 0.77783(13) 0.09032(12) 0.45341(11) 0.0161(3) Uani 1 1 d . . . C212 C 0.74243(14) 0.12948(12) 0.52230(12) 0.0193(4) Uani 1 1 d . . . H212 H 0.6959 0.1711 0.5114 0.023 Uiso 1 1 d R . . C213 C 0.77675(14) 0.10616(13) 0.60693(12) 0.0211(4) Uani 1 1 d . . . H213 H 0.7529 0.1321 0.6523 0.025 Uiso 1 1 d R . . C214 C 0.84654(14) 0.04417(13) 0.62351(12) 0.0208(4) Uani 1 1 d . . . H214 H 0.8695 0.0288 0.6799 0.025 Uiso 1 1 d R . . C215 C 0.88193(14) 0.00517(13) 0.55573(12) 0.0219(4) Uani 1 1 d . . . H215 H 0.9286 -0.0363 0.5670 0.026 Uiso 1 1 d R . . C216 C 0.84762(14) 0.02805(12) 0.47065(12) 0.0183(4) Uani 1 1 d . . . H216 H 0.8714 0.0017 0.4255 0.022 Uiso 1 1 d R . . C121 C 0.43013(13) 0.06793(12) 0.24117(12) 0.0175(3) Uani 1 1 d . . . C122 C 0.40348(15) 0.10228(14) 0.15871(13) 0.0253(4) Uani 1 1 d . . . H122 H 0.4451 0.0996 0.1187 0.030 Uiso 1 1 d R . . C123 C 0.31520(16) 0.14040(16) 0.13619(14) 0.0309(5) Uani 1 1 d . . . H123 H 0.2985 0.1632 0.0814 0.037 Uiso 1 1 d R . . C124 C 0.25194(15) 0.14460(14) 0.19498(14) 0.0265(4) Uani 1 1 d . . . H124 H 0.1932 0.1703 0.1798 0.032 Uiso 1 1 d R . . C125 C 0.27748(15) 0.10994(13) 0.27682(13) 0.0243(4) Uani 1 1 d . . . H125 H 0.2355 0.1126 0.3165 0.029 Uiso 1 1 d R . . C126 C 0.36520(15) 0.07145(13) 0.29953(12) 0.0219(4) Uani 1 1 d . . . H126 H 0.3811 0.0478 0.3540 0.026 Uiso 1 1 d R . . C111 C 0.53463(13) -0.05767(12) 0.34823(11) 0.0170(3) Uani 1 1 d . . . C116 C 0.46592(14) -0.11961(13) 0.32137(12) 0.0205(4) Uani 1 1 d . . . H116 H 0.4251 -0.1123 0.2699 0.025 Uiso 1 1 d R . . C115 C 0.45809(16) -0.19184(13) 0.37078(13) 0.0253(4) Uani 1 1 d . . . H115 H 0.4119 -0.2322 0.3524 0.030 Uiso 1 1 d R . . C114 C 0.51921(17) -0.20388(14) 0.44763(13) 0.0278(4) Uani 1 1 d . . . H114 H 0.5144 -0.2525 0.4804 0.033 Uiso 1 1 d R . . C113 C 0.58738(18) -0.14297(14) 0.47515(13) 0.0292(5) Uani 1 1 d . . . H113 H 0.6281 -0.1508 0.5266 0.035 Uiso 1 1 d R . . C112 C 0.59537(15) -0.06969(13) 0.42602(12) 0.0238(4) Uani 1 1 d . . . H112 H 0.6410 -0.0290 0.4451 0.029 Uiso 1 1 d 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 Co2 0.01548(13) 0.01493(12) 0.01322(11) -0.00029(8) 0.00016(9) 0.00076(9) Co1 0.01753(13) 0.01757(13) 0.01238(11) -0.00142(9) 0.00066(9) -0.00226(9) P2 0.0154(2) 0.0142(2) 0.0128(2) -0.00085(15) -0.00060(16) 0.00034(16) P1 0.0153(2) 0.0157(2) 0.0126(2) 0.00047(16) -0.00037(16) -0.00059(17) N 0.0220(8) 0.0191(8) 0.0278(8) -0.0017(6) 0.0082(7) 0.0028(7) O22 0.0253(8) 0.0252(7) 0.0294(7) 0.0099(6) 0.0010(6) 0.0001(6) O21 0.0172(8) 0.0486(11) 0.0457(10) 0.0054(8) -0.0041(7) 0.0067(7) O12 0.0309(9) 0.0520(11) 0.0200(7) 0.0122(7) -0.0032(6) -0.0112(8) O11 0.0368(9) 0.0274(8) 0.0355(8) -0.0112(7) 0.0054(7) -0.0108(7) C4 0.0205(9) 0.0166(9) 0.0182(8) 0.0012(7) 0.0011(7) -0.0001(7) C3 0.0181(9) 0.0156(8) 0.0187(8) -0.0005(7) -0.0003(7) -0.0004(7) C5 0.0138(8) 0.0170(8) 0.0160(8) -0.0017(6) -0.0015(6) -0.0002(7) C22 0.0147(9) 0.0194(9) 0.0206(9) -0.0012(7) 0.0028(7) -0.0010(7) C21 0.0208(10) 0.0224(10) 0.0206(9) 0.0001(7) -0.0011(7) 0.0040(7) C12 0.0161(9) 0.0306(10) 0.0210(9) -0.0012(8) 0.0004(7) -0.0079(8) C11 0.0238(10) 0.0274(10) 0.0187(9) -0.0048(7) 0.0033(7) -0.0019(8) C34 0.0186(9) 0.0171(9) 0.0162(8) -0.0006(6) 0.0001(7) 0.0004(7) C35 0.0234(10) 0.0139(8) 0.0210(9) 0.0012(7) 0.0007(7) 0.0006(7) C36 0.0222(10) 0.0199(9) 0.0195(9) 0.0027(7) 0.0049(7) -0.0006(7) C31 0.0155(9) 0.0196(9) 0.0182(8) -0.0007(7) 0.0009(7) 0.0016(7) C32 0.0267(10) 0.0144(9) 0.0282(10) -0.0003(7) 0.0075(8) 0.0005(7) C33 0.0293(11) 0.0168(9) 0.0246(9) 0.0032(7) 0.0096(8) -0.0007(8) C42 0.0367(13) 0.0398(13) 0.0355(12) -0.0075(10) 0.0199(10) -0.0067(10) C41 0.0578(17) 0.0230(11) 0.0556(16) -0.0079(10) 0.0368(14) -0.0004(11) C221 0.0217(9) 0.0142(8) 0.0121(8) -0.0004(6) -0.0024(6) -0.0005(7) C226 0.0226(10) 0.0193(9) 0.0210(9) 0.0010(7) 0.0013(7) 0.0008(7) C225 0.0346(12) 0.0179(9) 0.0230(9) -0.0024(7) 0.0006(8) 0.0032(8) C224 0.0373(12) 0.0159(9) 0.0195(9) -0.0002(7) -0.0016(8) -0.0047(8) C223 0.0252(10) 0.0254(10) 0.0222(9) 0.0003(8) 0.0001(7) -0.0086(8) C222 0.0216(10) 0.0213(9) 0.0214(9) -0.0031(7) 0.0002(7) 0.0000(7) C211 0.0158(8) 0.0163(8) 0.0151(8) 0.0002(6) -0.0010(6) -0.0011(7) C212 0.0209(9) 0.0189(9) 0.0172(8) -0.0011(7) -0.0002(7) 0.0040(7) C213 0.0244(10) 0.0240(10) 0.0147(8) -0.0014(7) 0.0025(7) 0.0019(8) C214 0.0213(9) 0.0247(10) 0.0151(8) 0.0028(7) -0.0008(7) -0.0011(8) C215 0.0220(10) 0.0224(9) 0.0201(9) 0.0035(7) -0.0003(7) 0.0057(8) C216 0.0183(9) 0.0199(9) 0.0160(8) -0.0007(7) 0.0008(7) 0.0017(7) C121 0.0144(8) 0.0179(9) 0.0187(8) -0.0007(7) -0.0024(7) -0.0021(7) C122 0.0220(10) 0.0324(11) 0.0209(9) 0.0071(8) 0.0012(7) 0.0006(8) C123 0.0255(11) 0.0405(13) 0.0248(10) 0.0103(9) -0.0020(8) 0.0050(9) C124 0.0203(10) 0.0255(10) 0.0315(11) 0.0007(8) -0.0035(8) 0.0032(8) C125 0.0226(10) 0.0230(10) 0.0280(10) -0.0012(8) 0.0062(8) 0.0018(8) C126 0.0245(10) 0.0222(9) 0.0192(9) 0.0013(7) 0.0035(7) 0.0028(8) C111 0.0198(9) 0.0169(9) 0.0149(8) 0.0001(6) 0.0038(7) 0.0011(7) C116 0.0190(9) 0.0222(9) 0.0199(9) 0.0017(7) 0.0015(7) 0.0011(7) C115 0.0290(11) 0.0216(10) 0.0268(10) 0.0006(8) 0.0085(8) -0.0035(8) C114 0.0419(13) 0.0204(10) 0.0228(9) 0.0051(8) 0.0106(9) 0.0027(9) C113 0.0427(13) 0.0261(11) 0.0170(9) 0.0036(8) -0.0010(8) 0.0009(9) C112 0.0291(11) 0.0233(10) 0.0175(9) 0.0017(7) -0.0013(8) -0.0024(8) _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 Co2 C21 1.773(2) . ? Co2 C22 1.7858(19) . ? Co2 C3 1.9434(19) . ? Co2 C4 1.9674(19) . ? Co2 P2 2.2163(5) . ? Co2 Co1 2.4657(4) . ? Co1 C11 1.779(2) . ? Co1 C12 1.800(2) . ? Co1 C4 1.9577(19) . ? Co1 C3 1.9857(19) . ? Co1 P1 2.2266(5) . ? P2 C211 1.8346(18) . ? P2 C221 1.8431(19) . ? P2 C5 1.8493(19) . ? P1 C111 1.8299(19) . ? P1 C121 1.8323(19) . ? P1 C5 1.8575(18) . ? N C31 1.407(2) . ? N C41 1.447(3) . ? N C42 1.453(3) . ? O22 C22 1.144(2) . ? O21 C21 1.148(3) . ? O12 C12 1.147(3) . ? O11 C11 1.145(3) . ? C4 C3 1.350(3) . ? C3 C34 1.465(3) . ? C34 C33 1.402(3) . ? C34 C35 1.404(3) . ? C35 C36 1.384(3) . ? C36 C31 1.409(3) . ? C31 C32 1.410(3) . ? C32 C33 1.391(3) . ? C221 C226 1.395(3) . ? C221 C222 1.402(3) . ? C226 C225 1.405(3) . ? C225 C224 1.380(3) . ? C224 C223 1.393(3) . ? C223 C222 1.398(3) . ? C211 C216 1.394(3) . ? C211 C212 1.406(3) . ? C212 C213 1.395(3) . ? C213 C214 1.391(3) . ? C214 C215 1.390(3) . ? C215 C216 1.400(3) . ? C121 C122 1.403(3) . ? C121 C126 1.403(3) . ? C122 C123 1.393(3) . ? C123 C124 1.390(3) . ? C124 C125 1.394(3) . ? C125 C126 1.389(3) . ? C111 C112 1.401(3) . ? C111 C116 1.402(3) . ? C116 C115 1.390(3) . ? C115 C114 1.392(3) . ? C114 C113 1.387(3) . ? C113 C112 1.401(3) . ? 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 C21 Co2 C22 100.65(9) . . ? C21 Co2 C3 97.93(9) . . ? C22 Co2 C3 109.47(8) . . ? C21 Co2 C4 107.93(9) . . ? C22 Co2 C4 140.14(8) . . ? C3 Co2 C4 40.38(8) . . ? C21 Co2 P2 105.27(7) . . ? C22 Co2 P2 99.04(6) . . ? C3 Co2 P2 138.95(6) . . ? C4 Co2 P2 99.53(6) . . ? C21 Co2 Co1 149.83(7) . . ? C22 Co2 Co1 91.22(6) . . ? C3 Co2 Co1 51.90(6) . . ? C4 Co2 Co1 50.91(6) . . ? P2 Co2 Co1 100.020(16) . . ? C11 Co1 C12 101.11(9) . . ? C11 Co1 C4 97.45(9) . . ? C12 Co1 C4 144.97(9) . . ? C11 Co1 C3 99.29(9) . . ? C12 Co1 C3 107.19(8) . . ? C4 Co1 C3 40.03(8) . . ? C11 Co1 P1 98.99(7) . . ? C12 Co1 P1 109.53(7) . . ? C4 Co1 P1 96.44(6) . . ? C3 Co1 P1 134.55(5) . . ? C11 Co1 Co2 146.64(7) . . ? C12 Co1 Co2 101.45(6) . . ? C4 Co1 Co2 51.26(6) . . ? C3 Co1 Co2 50.37(5) . . ? P1 Co1 Co2 96.262(16) . . ? C211 P2 C221 100.28(8) . . ? C211 P2 C5 103.82(8) . . ? C221 P2 C5 104.73(8) . . ? C211 P2 Co2 120.24(6) . . ? C221 P2 Co2 114.71(6) . . ? C5 P2 Co2 111.31(6) . . ? C111 P1 C121 102.83(9) . . ? C111 P1 C5 107.37(8) . . ? C121 P1 C5 99.40(8) . . ? C111 P1 Co1 110.02(6) . . ? C121 P1 Co1 122.26(6) . . ? C5 P1 Co1 113.52(6) . . ? C31 N C41 117.74(17) . . ? C31 N C42 117.99(17) . . ? C41 N C42 112.29(19) . . ? C3 C4 Co1 71.10(11) . . ? C3 C4 Co2 68.85(11) . . ? Co1 C4 Co2 77.83(7) . . ? C4 C3 C34 143.41(18) . . ? C4 C3 Co2 70.77(11) . . ? C34 C3 Co2 135.17(14) . . ? C4 C3 Co1 68.87(12) . . ? C34 C3 Co1 132.46(13) . . ? Co2 C3 Co1 77.73(7) . . ? P2 C5 P1 113.20(9) . . ? O22 C22 Co2 178.28(17) . . ? O21 C21 Co2 175.94(18) . . ? O12 C12 Co1 178.1(2) . . ? O11 C11 Co1 176.2(2) . . ? C33 C34 C35 117.42(17) . . ? C33 C34 C3 121.08(17) . . ? C35 C34 C3 121.49(17) . . ? C36 C35 C34 121.62(17) . . ? C35 C36 C31 121.18(18) . . ? N C31 C36 119.94(17) . . ? N C31 C32 122.73(17) . . ? C36 C31 C32 117.24(17) . . ? C33 C32 C31 121.17(18) . . ? C32 C33 C34 121.35(18) . . ? C226 C221 C222 118.95(17) . . ? C226 C221 P2 124.46(15) . . ? C222 C221 P2 116.57(14) . . ? C221 C226 C225 119.90(19) . . ? C224 C225 C226 120.7(2) . . ? C225 C224 C223 120.07(19) . . ? C224 C223 C222 119.53(19) . . ? C223 C222 C221 120.84(19) . . ? C216 C211 C212 119.26(16) . . ? C216 C211 P2 120.40(14) . . ? C212 C211 P2 120.32(14) . . ? C213 C212 C211 120.30(18) . . ? C214 C213 C212 120.05(18) . . ? C215 C214 C213 120.00(17) . . ? C214 C215 C216 120.27(18) . . ? C211 C216 C215 120.13(17) . . ? C122 C121 C126 118.44(18) . . ? C122 C121 P1 119.29(15) . . ? C126 C121 P1 122.14(14) . . ? C123 C122 C121 120.53(19) . . ? C124 C123 C122 120.52(19) . . ? C123 C124 C125 119.3(2) . . ? C126 C125 C124 120.42(19) . . ? C125 C126 C121 120.73(18) . . ? C112 C111 C116 118.82(17) . . ? C112 C111 P1 123.37(15) . . ? C116 C111 P1 117.22(14) . . ? C115 C116 C111 120.76(18) . . ? C116 C115 C114 120.2(2) . . ? C113 C114 C115 119.68(19) . . ? C114 C113 C112 120.50(19) . . ? C111 C112 C113 120.04(19) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.533 _refine_diff_density_min -0.447 _refine_diff_density_rms 0.070 data_00srv196 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H27 Co2 N O6 P2' _chemical_formula_weight 761.4 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbcm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x, -y+1/2, -z' '-x, -y, -z' 'x, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x, y-1/2, z' _cell_length_a 14.4825(11) _cell_length_b 13.6742(10) _cell_length_c 16.8860(14) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3344.1(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour clear_intense_red _exptl_crystal_size_max 0.86 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.512 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1552 _exptl_absorpt_coefficient_mu 1.136 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min . _exptl_absorpt_correction_T_max . _exptl_absorpt_process_details . _exptl_special_details ; The data collection nominally covered over a full sphere of reciprocal space, by a combination of 5 sets of \w scans, each set at different \f and/or 2\q angles and each scan (10 s exposure) covering 0.3\% in \w. Crystal to detector distance 4.51 cm. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD 1K area detector' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean 8 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 39675 _diffrn_reflns_av_R_equivalents 0.1189 _diffrn_reflns_av_sigmaI/netI 0.0442 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 29.04 _reflns_number_total 4608 _reflns_number_gt 4242 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT V5.0 (Bruker, 1998)' _computing_cell_refinement 'SMART-NT V5.0 (Bruker, 1998)' _computing_data_reduction 'SAINT-NT V5.0 (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Ferrugia, 2000)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0349P)^2^+1.9035P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef 1.14 _refine_ls_number_reflns 4608 _refine_ls_number_parameters 238 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0353 _refine_ls_R_factor_gt 0.0322 _refine_ls_wR_factor_ref 0.0794 _refine_ls_wR_factor_gt 0.0765 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.426837(12) 0.028353(12) 0.323877(10) 0.01151(7) Uani 1 1 d . . . P1 P 0.27502(2) 0.04313(2) 0.340021(19) 0.01099(8) Uani 1 1 d . . . C4 C 0.44380(13) 0.13753(13) 0.2500 0.0136(3) Uani 1 2 d S . . C111 C 0.21944(9) -0.03010(9) 0.41846(8) 0.0137(2) Uani 1 1 d . . . C34 C 0.62009(12) 0.08305(14) 0.2500 0.0149(3) Uani 1 2 d S . . C3 C 0.51948(12) 0.07912(13) 0.2500 0.0143(3) Uani 1 2 d S . . C5 C 0.21222(12) 0.00378(13) 0.2500 0.0122(3) Uani 1 2 d S . . H5A H 0.1508 0.0320 0.2500 0.015 Uiso 1 2 calc SR . . H5B H 0.2060 -0.0669 0.2500 0.015 Uiso 1 2 calc SR . . O11 O 0.49888(8) 0.11455(8) 0.47049(7) 0.0277(2) Uani 1 1 d . . . C12 C 0.45393(10) -0.09828(10) 0.34193(8) 0.0167(2) Uani 1 1 d . . . C121 C 0.23136(9) 0.16674(9) 0.36085(7) 0.0138(2) Uani 1 1 d . . . O12 O 0.47571(9) -0.17770(8) 0.35337(7) 0.0276(2) Uani 1 1 d . . . C32 C 0.76155(14) 0.17896(16) 0.2500 0.0200(4) Uani 1 2 d S . . H32 H 0.7918 0.2390 0.2500 0.024 Uiso 1 2 calc SR . . O1 O 0.95744(12) 0.02113(15) 0.2500 0.0392(4) Uani 1 2 d S . . C11 C 0.46906(9) 0.08024(10) 0.41408(8) 0.0171(2) Uani 1 1 d . . . C112 C 0.12390(10) -0.04717(11) 0.42228(9) 0.0193(3) Uani 1 1 d . . . H112 H 0.0855 -0.0232 0.3827 0.023 Uiso 1 1 calc R . . O2 O 0.94829(12) 0.17953(15) 0.2500 0.0346(4) Uani 1 2 d S . . C124 C 0.16623(11) 0.35314(10) 0.40401(10) 0.0237(3) Uani 1 1 d . . . H124 H 0.1445 0.4143 0.4192 0.028 Uiso 1 1 calc R . . C35 C 0.67289(14) -0.00326(15) 0.2500 0.0200(4) Uani 1 2 d S . . H35 H 0.6433 -0.0636 0.2500 0.024 Uiso 1 2 calc SR . . C116 C 0.27566(9) -0.06834(10) 0.47848(8) 0.0169(3) Uani 1 1 d . . . H116 H 0.3391 -0.0581 0.4765 0.020 Uiso 1 1 calc R . . C114 C 0.14301(11) -0.13741(10) 0.54484(8) 0.0206(3) Uani 1 1 d . . . H114 H 0.1175 -0.1726 0.5866 0.025 Uiso 1 1 calc R . . N1 N 0.91204(12) 0.09760(16) 0.2500 0.0255(4) Uani 1 2 d S . . C36 C 0.76896(14) 0.00078(17) 0.2500 0.0212(4) Uani 1 2 d S . . H36 H 0.8039 -0.0563 0.2500 0.025 Uiso 1 2 calc SR . . C113 C 0.08637(10) -0.10007(11) 0.48544(9) 0.0214(3) Uani 1 1 d . . . H113 H 0.0230 -0.1104 0.4878 0.026 Uiso 1 1 calc R . . C31 C 0.81137(13) 0.09174(16) 0.2500 0.0197(4) Uani 1 2 d S . . C123 C 0.25968(10) 0.33084(10) 0.41073(9) 0.0219(3) Uani 1 1 d . . . H123 H 0.3006 0.3776 0.4300 0.026 Uiso 1 1 calc R . . C33 C 0.66591(13) 0.17419(15) 0.2500 0.0178(4) Uani 1 2 d S . . H33 H 0.6316 0.2317 0.2500 0.021 Uiso 1 2 calc SR . . C115 C 0.23789(11) -0.12183(11) 0.54148(9) 0.0214(3) Uani 1 1 d . . . H115 H 0.2761 -0.1468 0.5809 0.026 Uiso 1 1 calc R . . C122 C 0.29230(9) 0.23864(10) 0.38874(8) 0.0176(3) Uani 1 1 d . . . H122 H 0.3550 0.2248 0.3926 0.021 Uiso 1 1 calc R . . C126 C 0.13758(10) 0.19026(11) 0.35332(9) 0.0212(3) Uani 1 1 d . . . H126 H 0.0964 0.1437 0.3342 0.025 Uiso 1 1 calc R . . C125 C 0.10554(10) 0.28303(11) 0.37429(10) 0.0257(3) Uani 1 1 d . . . H125 H 0.0433 0.2981 0.3684 0.031 Uiso 1 1 calc R . . H4 H 0.4244(18) 0.206(2) 0.2500 0.026(7) Uiso 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.01077(10) 0.01315(10) 0.01063(10) -0.00007(6) -0.00054(5) 0.00059(6) P1 0.01105(15) 0.01186(15) 0.01006(14) -0.00001(10) -0.00005(11) 0.00025(11) C4 0.0139(7) 0.0144(8) 0.0126(8) 0.000 0.000 -0.0009(6) C111 0.0163(6) 0.0132(5) 0.0116(5) -0.0006(4) 0.0012(4) -0.0009(4) C34 0.0118(8) 0.0205(9) 0.0123(8) 0.000 0.000 -0.0001(7) C3 0.0126(8) 0.0165(8) 0.0137(8) 0.000 0.000 -0.0016(6) C5 0.0127(7) 0.0132(7) 0.0108(7) 0.000 0.000 0.0000(6) O11 0.0336(6) 0.0274(5) 0.0220(5) -0.0051(4) -0.0110(5) 0.0013(5) C12 0.0185(6) 0.0198(6) 0.0119(5) -0.0019(5) -0.0009(5) 0.0023(5) C121 0.0165(6) 0.0129(5) 0.0119(5) -0.0006(4) 0.0010(4) 0.0019(4) O12 0.0410(7) 0.0189(5) 0.0228(5) -0.0021(4) -0.0045(5) 0.0092(5) C32 0.0158(8) 0.0251(10) 0.0192(9) 0.000 0.000 -0.0049(7) O1 0.0170(8) 0.0516(12) 0.0491(12) 0.000 0.000 0.0086(7) C11 0.0168(6) 0.0174(6) 0.0172(6) 0.0020(5) -0.0021(5) 0.0015(5) C112 0.0162(6) 0.0244(6) 0.0174(6) 0.0020(5) -0.0002(5) -0.0031(5) O2 0.0169(7) 0.0503(11) 0.0364(9) 0.000 0.000 -0.0104(7) C124 0.0284(7) 0.0165(6) 0.0260(7) -0.0043(5) 0.0032(6) 0.0051(5) C35 0.0157(8) 0.0206(9) 0.0237(10) 0.000 0.000 0.0013(7) C116 0.0173(6) 0.0193(6) 0.0142(6) 0.0018(5) 0.0002(5) -0.0002(5) C114 0.0294(7) 0.0183(6) 0.0142(6) 0.0007(5) 0.0041(5) -0.0071(5) N1 0.0142(7) 0.0451(11) 0.0172(8) 0.000 0.000 0.0005(8) C36 0.0155(9) 0.0268(10) 0.0212(9) 0.000 0.000 0.0045(8) C113 0.0203(6) 0.0251(7) 0.0189(7) -0.0009(5) 0.0026(5) -0.0078(5) C31 0.0124(8) 0.0336(11) 0.0130(8) 0.000 0.000 -0.0008(7) C123 0.0260(7) 0.0151(6) 0.0247(7) -0.0035(5) 0.0007(6) -0.0020(5) C33 0.0155(8) 0.0204(9) 0.0174(8) 0.000 0.000 -0.0004(7) C115 0.0263(7) 0.0226(7) 0.0152(6) 0.0049(5) -0.0003(5) -0.0001(5) C122 0.0188(6) 0.0156(6) 0.0184(6) -0.0010(5) -0.0003(5) -0.0005(5) C126 0.0171(6) 0.0202(7) 0.0262(7) -0.0061(5) -0.0013(5) 0.0024(5) C125 0.0197(6) 0.0230(7) 0.0345(8) -0.0067(6) -0.0003(6) 0.0073(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 Co1 C11 1.7881(14) . ? Co1 C12 1.8014(14) . ? Co1 C3 1.9591(14) . ? Co1 C4 1.9609(14) . ? Co1 P1 2.2248(4) . ? Co1 Co1 2.4950(4) 6_556 ? P1 C121 1.8385(13) . ? P1 C111 1.8453(13) . ? P1 C5 1.8514(11) . ? C4 C3 1.356(3) . ? C4 Co1 1.9609(14) 6_556 ? C111 C116 1.4013(18) . ? C111 C112 1.4047(18) . ? C34 C35 1.406(3) . ? C34 C33 1.412(3) . ? C34 C3 1.458(3) . ? C3 Co1 1.9591(14) 6_556 ? C5 P1 1.8514(11) 6_556 ? O11 C11 1.1462(18) . ? C12 O12 1.1473(18) . ? C121 C126 1.4015(18) . ? C121 C122 1.4026(18) . ? C32 C33 1.387(3) . ? C32 C31 1.394(3) . ? O1 N1 1.235(3) . ? C112 C113 1.399(2) . ? O2 N1 1.237(3) . ? C124 C123 1.392(2) . ? C124 C125 1.394(2) . ? C35 C36 1.392(3) . ? C116 C115 1.4022(19) . ? C114 C115 1.392(2) . ? C114 C113 1.393(2) . ? N1 C31 1.460(2) . ? C36 C31 1.387(3) . ? C123 C122 1.3966(19) . ? C126 C125 1.396(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 Co1 C12 99.37(6) . . ? C11 Co1 C3 99.65(6) . . ? C12 Co1 C3 107.41(7) . . ? C11 Co1 C4 101.36(6) . . ? C12 Co1 C4 144.30(6) . . ? C3 Co1 C4 40.48(7) . . ? C11 Co1 P1 101.40(4) . . ? C12 Co1 P1 106.37(5) . . ? C3 Co1 P1 136.27(5) . . ? C4 Co1 P1 97.62(5) . . ? C11 Co1 Co1 148.41(4) . 6_556 ? C12 Co1 Co1 99.74(4) . 6_556 ? C3 Co1 Co1 50.45(3) . 6_556 ? C4 Co1 Co1 50.49(3) . 6_556 ? P1 Co1 Co1 97.038(10) . 6_556 ? C121 P1 C111 102.21(6) . . ? C121 P1 C5 104.79(7) . . ? C111 P1 C5 102.55(6) . . ? C121 P1 Co1 116.54(4) . . ? C111 P1 Co1 118.02(4) . . ? C5 P1 Co1 111.01(5) . . ? C3 C4 Co1 69.69(9) . 6_556 ? C3 C4 Co1 69.69(9) . . ? Co1 C4 Co1 79.01(7) 6_556 . ? C116 C111 C112 118.50(12) . . ? C116 C111 P1 117.92(10) . . ? C112 C111 P1 123.56(10) . . ? C35 C34 C33 119.03(17) . . ? C35 C34 C3 120.83(17) . . ? C33 C34 C3 120.14(17) . . ? C4 C3 C34 141.81(17) . . ? C4 C3 Co1 69.83(9) . 6_556 ? C34 C3 Co1 134.22(7) . 6_556 ? C4 C3 Co1 69.83(9) . . ? C34 C3 Co1 134.22(7) . . ? Co1 C3 Co1 79.10(7) 6_556 . ? P1 C5 P1 110.39(9) . 6_556 ? O12 C12 Co1 176.63(13) . . ? C126 C121 C122 118.64(12) . . ? C126 C121 P1 121.80(10) . . ? C122 C121 P1 119.49(10) . . ? C33 C32 C31 118.47(18) . . ? O11 C11 Co1 177.57(13) . . ? C113 C112 C111 120.24(13) . . ? C123 C124 C125 119.45(13) . . ? C36 C35 C34 120.67(19) . . ? C111 C116 C115 121.11(13) . . ? C115 C114 C113 119.74(13) . . ? O1 N1 O2 122.73(19) . . ? O1 N1 C31 119.0(2) . . ? O2 N1 C31 118.26(19) . . ? C31 C36 C35 118.55(19) . . ? C114 C113 C112 120.66(13) . . ? C36 C31 C32 122.55(18) . . ? C36 C31 N1 119.43(19) . . ? C32 C31 N1 118.03(19) . . ? C124 C123 C122 120.33(13) . . ? C32 C33 C34 120.73(18) . . ? C114 C115 C116 119.73(13) . . ? C123 C122 C121 120.62(13) . . ? C125 C126 C121 120.50(13) . . ? C124 C125 C126 120.43(14) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 1.41 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.733 _refine_diff_density_min -1.002 _refine_diff_density_rms 0.106 data_00srv218 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H27 Co2 N O4 P2' _chemical_formula_weight 741.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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)/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 9.3295(2) _cell_length_b 16.6546(4) _cell_length_c 11.1253(3) _cell_angle_alpha 90 _cell_angle_beta 92.212(10) _cell_angle_gamma 90 _cell_volume 1727.35(7) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour clear_light_red _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.425 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 756 _exptl_absorpt_coefficient_mu 1.093 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5951 _exptl_absorpt_correction_T_max 0.7458 _exptl_absorpt_process_details 'SADABS (G.M.Sheldrick,1998), R(int)=0.0453 before correction' _exptl_special_details ; The data collection nominally covered over a full sphere of reciprocal space, by a combination of 5 sets of \w scans, each set at different \f and/or 2\q angles and each scan (10 s exposure) covering 0.3\% in \w. Crystal to detector distance 4.51 cm. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD 1K area detector' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean 8 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 21205 _diffrn_reflns_av_R_equivalents 0.0293 _diffrn_reflns_av_sigmaI/netI 0.0175 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 29 _reflns_number_total 4731 _reflns_number_gt 4424 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT V5.0 (Bruker, 1998)' _computing_cell_refinement 'SMART-NT V5.0 (Bruker, 1998)' _computing_data_reduction 'SAINT-NT V5.0 (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Ferrugia, 2000)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0323P)^2^+1.0165P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4731 _refine_ls_number_parameters 232 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0283 _refine_ls_R_factor_gt 0.0258 _refine_ls_wR_factor_ref 0.0676 _refine_ls_wR_factor_gt 0.0661 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.468413(17) 0.175825(10) 0.626855(14) 0.01334(6) Uani 1 1 d . . . P1 P 0.33030(3) 0.158593(19) 0.78356(3) 0.01335(7) Uani 1 1 d . . . C51 C 0.9600(2) 0.2500 0.1617(2) 0.0283(4) Uani 1 2 d S . . O11 O 0.62744(13) 0.02496(7) 0.60939(11) 0.0339(3) Uani 1 1 d . . . O12 O 0.25979(12) 0.15540(6) 0.42483(9) 0.0258(2) Uani 1 1 d . . . C3 C 0.61497(19) 0.2500 0.57362(16) 0.0165(3) Uani 1 2 d S . . C4 C 0.6140(2) 0.2500 0.69504(17) 0.0174(3) Uani 1 2 d S . . C5 C 0.22478(19) 0.2500 0.80950(16) 0.0150(3) Uani 1 2 d S . . H5A H 0.1402 0.2500 0.7560 0.018 Uiso 1 2 calc SR . . H5B H 0.1932 0.2500 0.8916 0.018 Uiso 1 2 calc SR . . C11 C 0.56426(15) 0.08330(8) 0.61879(12) 0.0208(3) Uani 1 1 d . . . C12 C 0.34068(14) 0.16222(8) 0.50428(12) 0.0174(2) Uani 1 1 d . . . C31 C 0.8754(2) 0.2500 0.26756(18) 0.0219(4) Uani 1 2 d S . . C32 C 0.9406(2) 0.2500 0.3823(2) 0.0253(4) Uani 1 2 d S . . H32 H 1.0401 0.2500 0.3916 0.030 Uiso 1 2 calc SR . . C33 C 0.8566(2) 0.2500 0.48297(18) 0.0216(4) Uani 1 2 d S . . H33 H 0.9003 0.2500 0.5595 0.026 Uiso 1 2 calc SR . . C34 C 0.70631(19) 0.2500 0.46960(16) 0.0168(3) Uani 1 2 d S . . C35 C 0.6433(2) 0.2500 0.35313(18) 0.0237(4) Uani 1 2 d S . . H35 H 0.5438 0.2500 0.3433 0.028 Uiso 1 2 calc SR . . C36 C 0.7260(2) 0.2500 0.25232(18) 0.0230(4) Uani 1 2 d S . . H36 H 0.6828 0.2500 0.1756 0.028 Uiso 1 2 calc SR . . N1 N 1.0245(2) 0.2500 0.0753(2) 0.0381(5) Uani 1 2 d S . . C111 C 0.41669(14) 0.13533(7) 0.93022(11) 0.0157(2) Uani 1 1 d . . . C112 C 0.34209(16) 0.14064(9) 1.03694(12) 0.0227(3) Uani 1 1 d . . . H112 H 0.2485 0.1599 1.0349 0.027 Uiso 1 1 calc R . . C113 C 0.40759(17) 0.11721(10) 1.14598(12) 0.0271(3) Uani 1 1 d . . . H113 H 0.3573 0.1206 1.2164 0.033 Uiso 1 1 calc R . . C114 C 0.54731(17) 0.08878(9) 1.15009(12) 0.0261(3) Uani 1 1 d . . . H114 H 0.5902 0.0726 1.2230 0.031 Uiso 1 1 calc R . . C115 C 0.62324(16) 0.08440(9) 1.04550(13) 0.0248(3) Uani 1 1 d . . . H115 H 0.7174 0.0660 1.0484 0.030 Uiso 1 1 calc R . . C116 C 0.55817(15) 0.10766(8) 0.93581(12) 0.0202(3) Uani 1 1 d . . . H116 H 0.6094 0.1047 0.8659 0.024 Uiso 1 1 calc R . . C121 C 0.18699(14) 0.08309(8) 0.76807(11) 0.0174(2) Uani 1 1 d . . . C122 C 0.06925(16) 0.08164(10) 0.84296(14) 0.0279(3) Uani 1 1 d . . . H122 H 0.0616 0.1201 0.9030 0.033 Uiso 1 1 calc R . . C123 C -0.03622(18) 0.02278(11) 0.82776(16) 0.0357(4) Uani 1 1 d . . . H123 H -0.1133 0.0219 0.8783 0.043 Uiso 1 1 calc R . . C124 C -0.02705(18) -0.03450(10) 0.73776(16) 0.0337(4) Uani 1 1 d . . . H124 H -0.0976 -0.0737 0.7282 0.040 Uiso 1 1 calc R . . C125 C 0.08755(18) -0.03309(9) 0.66219(14) 0.0282(3) Uani 1 1 d . . . H125 H 0.0935 -0.0711 0.6014 0.034 Uiso 1 1 calc R . . C126 C 0.19385(15) 0.02523(8) 0.67712(12) 0.0205(3) Uani 1 1 d . . . H126 H 0.2704 0.0257 0.6260 0.025 Uiso 1 1 calc R . . H4 H 0.678(3) 0.2500 0.763(2) 0.029(7) Uiso 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.01500(9) 0.01425(9) 0.01084(8) -0.00031(5) 0.00163(6) 0.00097(6) P1 0.01553(14) 0.01330(14) 0.01129(14) -0.00035(10) 0.00136(11) -0.00082(11) C51 0.0275(10) 0.0256(10) 0.0327(11) 0.000 0.0138(9) 0.000 O11 0.0386(6) 0.0274(6) 0.0358(6) -0.0036(5) 0.0009(5) 0.0144(5) O12 0.0311(5) 0.0242(5) 0.0216(5) -0.0039(4) -0.0080(4) 0.0018(4) C3 0.0140(8) 0.0189(8) 0.0167(8) 0.000 0.0016(6) 0.000 C4 0.0163(8) 0.0189(8) 0.0169(8) 0.000 0.0004(6) 0.000 C5 0.0151(8) 0.0159(8) 0.0142(7) 0.000 0.0028(6) 0.000 C11 0.0233(6) 0.0225(6) 0.0168(6) -0.0005(5) 0.0020(5) 0.0012(5) C12 0.0209(6) 0.0148(6) 0.0166(6) -0.0013(4) 0.0032(5) 0.0009(5) C31 0.0241(9) 0.0159(8) 0.0265(10) 0.000 0.0128(8) 0.000 C32 0.0159(8) 0.0278(10) 0.0328(11) 0.000 0.0080(8) 0.000 C33 0.0169(8) 0.0244(9) 0.0236(9) 0.000 0.0013(7) 0.000 C34 0.0157(8) 0.0159(8) 0.0190(8) 0.000 0.0041(6) 0.000 C35 0.0169(8) 0.0352(11) 0.0194(9) 0.000 0.0044(7) 0.000 C36 0.0249(9) 0.0268(10) 0.0178(9) 0.000 0.0064(7) 0.000 N1 0.0353(11) 0.0439(12) 0.0367(11) 0.000 0.0215(9) 0.000 C111 0.0204(6) 0.0137(5) 0.0128(5) 0.0006(4) 0.0003(4) -0.0005(4) C112 0.0255(7) 0.0269(7) 0.0157(6) 0.0017(5) 0.0025(5) 0.0039(5) C113 0.0346(8) 0.0333(8) 0.0136(6) 0.0019(5) 0.0025(5) 0.0036(6) C114 0.0367(8) 0.0254(7) 0.0156(6) 0.0030(5) -0.0061(5) 0.0029(6) C115 0.0254(7) 0.0269(7) 0.0218(7) 0.0008(5) -0.0044(5) 0.0055(6) C116 0.0225(6) 0.0222(6) 0.0160(6) -0.0005(5) 0.0006(5) 0.0016(5) C121 0.0191(6) 0.0163(6) 0.0167(6) -0.0001(4) 0.0000(4) -0.0031(5) C122 0.0264(7) 0.0298(8) 0.0281(7) -0.0093(6) 0.0085(6) -0.0105(6) C123 0.0288(8) 0.0384(9) 0.0406(9) -0.0086(7) 0.0115(7) -0.0141(7) C124 0.0317(8) 0.0312(8) 0.0382(9) -0.0055(7) 0.0004(6) -0.0163(7) C125 0.0363(8) 0.0224(7) 0.0257(7) -0.0060(5) -0.0005(6) -0.0080(6) C126 0.0255(6) 0.0177(6) 0.0184(6) -0.0007(5) 0.0008(5) -0.0025(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 Co1 C11 1.7856(14) . ? Co1 C12 1.7904(14) . ? Co1 C3 1.9516(14) . ? Co1 C4 1.9662(15) . ? Co1 P1 2.2261(3) . ? Co1 Co1 2.4707(3) 4_565 ? P1 C111 1.8331(13) . ? P1 C121 1.8387(13) . ? P1 C5 1.8417(10) . ? C51 N1 1.154(3) . ? C51 C31 1.443(3) . ? O11 C11 1.1433(18) . ? O12 C12 1.1455(17) . ? C3 C4 1.351(3) . ? C3 C34 1.463(2) . ? C3 Co1 1.9516(14) 4_565 ? C4 Co1 1.9662(15) 4_565 ? C5 P1 1.8417(10) 4_565 ? C31 C32 1.392(3) . ? C31 C36 1.397(3) . ? C32 C33 1.392(3) . ? C33 C34 1.405(3) . ? C34 C35 1.402(3) . ? C35 C36 1.386(3) . ? C111 C116 1.3972(18) . ? C111 C112 1.4021(18) . ? C112 C113 1.3929(19) . ? C113 C114 1.386(2) . ? C114 C115 1.387(2) . ? C115 C116 1.3966(19) . ? C121 C126 1.4005(18) . ? C121 C122 1.4044(19) . ? C122 C123 1.395(2) . ? C123 C124 1.388(2) . ? C124 C125 1.386(2) . ? C125 C126 1.393(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 Co1 C12 99.93(6) . . ? C11 Co1 C3 99.96(6) . . ? C12 Co1 C3 107.61(7) . . ? C11 Co1 C4 102.82(6) . . ? C12 Co1 C4 143.40(6) . . ? C3 Co1 C4 40.35(7) . . ? C11 Co1 P1 103.55(4) . . ? C12 Co1 P1 101.06(4) . . ? C3 Co1 P1 138.83(5) . . ? C4 Co1 P1 101.00(5) . . ? C11 Co1 Co1 149.65(5) . 4_565 ? C12 Co1 Co1 97.27(4) . 4_565 ? C3 Co1 Co1 50.73(3) . 4_565 ? C4 Co1 Co1 51.07(3) . 4_565 ? P1 Co1 Co1 97.407(9) . 4_565 ? C111 P1 C121 103.42(6) . . ? C111 P1 C5 104.75(7) . . ? C121 P1 C5 100.89(6) . . ? C111 P1 Co1 118.45(4) . . ? C121 P1 Co1 117.10(4) . . ? C5 P1 Co1 110.20(5) . . ? N1 C51 C31 178.3(3) . . ? C4 C3 C34 144.82(17) . . ? C4 C3 Co1 70.41(9) . 4_565 ? C34 C3 Co1 132.54(8) . 4_565 ? C4 C3 Co1 70.41(9) . . ? C34 C3 Co1 132.54(8) . . ? Co1 C3 Co1 78.54(7) 4_565 . ? C3 C4 Co1 69.25(9) . . ? C3 C4 Co1 69.25(9) . 4_565 ? Co1 C4 Co1 77.85(7) . 4_565 ? P1 C5 P1 111.50(9) 4_565 . ? O11 C11 Co1 177.35(13) . . ? O12 C12 Co1 178.28(12) . . ? C32 C31 C36 120.62(17) . . ? C32 C31 C51 120.98(19) . . ? C36 C31 C51 118.4(2) . . ? C33 C32 C31 119.90(18) . . ? C32 C33 C34 120.37(19) . . ? C35 C34 C33 118.64(17) . . ? C35 C34 C3 119.64(16) . . ? C33 C34 C3 121.72(17) . . ? C36 C35 C34 121.40(18) . . ? C35 C36 C31 119.08(19) . . ? C116 C111 C112 118.82(12) . . ? C116 C111 P1 119.44(9) . . ? C112 C111 P1 121.66(10) . . ? C113 C112 C111 120.29(13) . . ? C114 C113 C112 120.33(13) . . ? C113 C114 C115 120.02(13) . . ? C114 C115 C116 119.97(13) . . ? C115 C116 C111 120.56(12) . . ? C126 C121 C122 118.38(12) . . ? C126 C121 P1 119.01(10) . . ? C122 C121 P1 122.60(10) . . ? C123 C122 C121 120.30(14) . . ? C124 C123 C122 120.51(15) . . ? C125 C124 C123 119.78(14) . . ? C124 C125 C126 120.11(14) . . ? C125 C126 C121 120.90(13) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 1.83 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.405 _refine_diff_density_min -0.373 _refine_diff_density_rms 0.056 data_00srv184 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84 H72 Cl2 Co2 O4 P4 Ru Si' _chemical_formula_weight 1587.22 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' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 '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' 'Si' 'Si' 0.0817 0.0704 '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 19.4088(9) _cell_length_b 19.2738(9) _cell_length_c 20.0688(10) _cell_angle_alpha 90 _cell_angle_beta 97.390(1) _cell_angle_gamma 90 _cell_volume 7445.0(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour clear_red _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.124 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4884 _exptl_absorpt_coefficient_mu 1.298 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min . _exptl_absorpt_correction_T_max . _exptl_absorpt_process_details . _exptl_special_details ; The data collection nominally covered over a full sphere of reciprocal space, by a combination of 5 sets of \w scans, each set at different \f and/or 2\q angles and each scan (10 s exposure) covering 0.3\% in \w. Crystal to detector distance 4.51 cm. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD 1K area detector' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean 8 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 58747 _diffrn_reflns_av_R_equivalents 0.0374 _diffrn_reflns_av_sigmaI/netI 0.0348 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 29.05 _reflns_number_total 19733 _reflns_number_gt 15810 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT V5.0 (Bruker, 1998)' _computing_cell_refinement 'SMART-NT V5.0 (Bruker, 1998)' _computing_data_reduction 'SAINT-NT V5.0 (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Ferrugia, 2000)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0487P)^2^+12.7466P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 19733 _refine_ls_number_parameters 886 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0581 _refine_ls_R_factor_gt 0.041 _refine_ls_wR_factor_ref 0.1133 _refine_ls_wR_factor_gt 0.1008 _refine_ls_goodness_of_fit_ref 1.04 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru Ru 0.052363(10) 0.113510(10) 1.138246(9) 0.01534(5) Uani 1 1 d . . . Co1 Co 0.046307(17) 0.286996(17) 0.650963(16) 0.01624(7) Uani 1 1 d . . . Co2 Co 0.165751(17) 0.235422(17) 0.656558(16) 0.01575(7) Uani 1 1 d . . . P1 P 0.21787(3) 0.32546(3) 0.71253(3) 0.01616(12) Uani 1 1 d . . . P2 P 0.07397(3) 0.38149(3) 0.71296(3) 0.01657(12) Uani 1 1 d . . . P3 P 0.16207(3) 0.07225(3) 1.16985(3) 0.01783(12) Uani 1 1 d . . . P4 P 0.07299(3) 0.23051(3) 1.15272(3) 0.01703(12) Uani 1 1 d . . . Si Si 0.03810(4) 0.11098(4) 0.60167(4) 0.02071(14) Uani 1 1 d . . . O1 O 0.19872(12) 0.24075(12) 0.51739(10) 0.0331(5) Uani 1 1 d . . . O2 O 0.25295(11) 0.11784(11) 0.70496(11) 0.0295(4) Uani 1 1 d . . . C1W C 0.1890(3) 0.4906(3) 0.9959(3) 0.0680(13) Uani 1 1 d . . . H1W1 H 0.1986 0.4544 1.0308 0.082 Uiso 1 1 calc R . . H1W2 H 0.1829 0.5352 1.0188 0.082 Uiso 1 1 calc R . . Cl1W Cl 0.11220(10) 0.47010(8) 0.94458(12) 0.1251(8) Uani 1 1 d . . . Cl2W Cl 0.26133(9) 0.49732(7) 0.95043(7) 0.0854(4) Uani 1 1 d . . . O11 O 0.03115(12) 0.31787(12) 0.50663(10) 0.0349(5) Uani 1 1 d . . . O12 O -0.09531(11) 0.27588(12) 0.68568(11) 0.0339(5) Uani 1 1 d . . . C1 C 0.06954(13) 0.12735(13) 1.04287(12) 0.0188(5) Uani 1 1 d . . . C2 C 0.07108(13) 0.13771(14) 0.98322(13) 0.0208(5) Uani 1 1 d . . . C3 C 0.09191(12) 0.21384(13) 0.71045(12) 0.0169(4) Uani 1 1 d . . . C4 C 0.07326(13) 0.18859(13) 0.64749(12) 0.0174(4) Uani 1 1 d . . . C5 C 0.15857(13) 0.36849(13) 0.76373(12) 0.0178(5) Uani 1 1 d . . . H5A H 0.1529 0.3396 0.8034 0.021 Uiso 1 1 calc R . . H5B H 0.1781 0.4138 0.7798 0.021 Uiso 1 1 calc R . . C11 C 0.03666(14) 0.30889(14) 0.56349(13) 0.0230(5) Uani 1 1 d . . . C12 C -0.04086(14) 0.28104(14) 0.67010(13) 0.0225(5) Uani 1 1 d . . . C21 C 0.18590(14) 0.24114(14) 0.57165(13) 0.0211(5) Uani 1 1 d . . . C22 C 0.22123(13) 0.16537(14) 0.68608(12) 0.0200(5) Uani 1 1 d . . . C31 C 0.07634(13) 0.15587(13) 0.91489(12) 0.0188(5) Uani 1 1 d . . . C32 C 0.01889(13) 0.15073(13) 0.86436(12) 0.0199(5) Uani 1 1 d . . . H32 H -0.0245 0.1349 0.8758 0.024 Uiso 1 1 calc R . . C33 C 0.02462(13) 0.16829(13) 0.79847(12) 0.0197(5) Uani 1 1 d . . . H33 H -0.0147 0.1638 0.7652 0.024 Uiso 1 1 calc R . . C34 C 0.08785(13) 0.19269(12) 0.77996(12) 0.0173(4) Uani 1 1 d . . . C35 C 0.14500(13) 0.19806(13) 0.82991(12) 0.0174(4) Uani 1 1 d . . . H35 H 0.1882 0.2143 0.8184 0.021 Uiso 1 1 calc R . . C36 C 0.13954(13) 0.18005(13) 0.89594(12) 0.0199(5) Uani 1 1 d . . . H36 H 0.1791 0.1841 0.9289 0.024 Uiso 1 1 calc R . . C41 C -0.05804(17) 0.1063(2) 0.6042(2) 0.0429(8) Uani 1 1 d . . . H41A H -0.0672 0.1038 0.6511 0.064 Uiso 1 1 calc R . . H41B H -0.0768 0.0649 0.5800 0.064 Uiso 1 1 calc R . . H41C H -0.0803 0.1478 0.5830 0.064 Uiso 1 1 calc R . . C42 C 0.05377(19) 0.11557(18) 0.51179(15) 0.0366(7) Uani 1 1 d . . . H42A H 0.0336 0.1585 0.4916 0.055 Uiso 1 1 calc R . . H42B H 0.0320 0.0756 0.4873 0.055 Uiso 1 1 calc R . . H42C H 0.1039 0.1151 0.5093 0.055 Uiso 1 1 calc R . . C43 C 0.08107(19) 0.03267(16) 0.64313(17) 0.0383(7) Uani 1 1 d . . . H43A H 0.1312 0.0349 0.6409 0.057 Uiso 1 1 calc R . . H43B H 0.0619 -0.0092 0.6200 0.057 Uiso 1 1 calc R . . H43C H 0.0727 0.0312 0.6902 0.057 Uiso 1 1 calc R . . C51 C -0.05731(14) 0.12144(15) 1.16161(16) 0.0283(6) Uani 1 1 d . . . H51 H -0.0793 0.1648 1.1666 0.034 Uiso 1 1 calc R . . C52 C -0.01920(15) 0.08223(15) 1.21445(14) 0.0262(6) Uani 1 1 d . . . H52 H -0.0114 0.0945 1.2607 0.031 Uiso 1 1 calc R . . C53 C 0.00484(14) 0.02161(14) 1.18482(13) 0.0235(5) Uani 1 1 d . . . H53 H 0.0318 -0.0141 1.2081 0.028 Uiso 1 1 calc R . . C54 C -0.01802(14) 0.02295(14) 1.11459(14) 0.0239(5) Uani 1 1 d . . . H54 H -0.0091 -0.0112 1.0827 0.029 Uiso 1 1 calc R . . C55 C -0.05672(14) 0.08517(15) 1.10114(15) 0.0266(6) Uani 1 1 d . . . H55 H -0.0785 0.0997 1.0583 0.032 Uiso 1 1 calc R . . C111 C 0.24733(13) 0.39861(13) 0.66469(12) 0.0181(5) Uani 1 1 d . . . C112 C 0.29342(13) 0.44812(14) 0.69523(13) 0.0219(5) Uani 1 1 d . . . H112 H 0.3120 0.4430 0.7411 0.026 Uiso 1 1 calc R . . C113 C 0.31243(14) 0.50516(14) 0.65886(15) 0.0248(5) Uani 1 1 d . . . H113 H 0.3438 0.5387 0.6800 0.030 Uiso 1 1 calc R . . C114 C 0.28538(15) 0.51290(15) 0.59173(15) 0.0279(6) Uani 1 1 d . . . H114 H 0.2986 0.5516 0.5669 0.033 Uiso 1 1 calc R . . C115 C 0.23926(16) 0.46432(15) 0.56097(14) 0.0288(6) Uani 1 1 d . . . H115 H 0.2207 0.4698 0.5151 0.035 Uiso 1 1 calc R . . C116 C 0.21997(15) 0.40725(14) 0.59732(13) 0.0236(5) Uani 1 1 d . . . H116 H 0.1881 0.3742 0.5761 0.028 Uiso 1 1 calc R . . C121 C 0.29408(13) 0.30928(13) 0.77476(12) 0.0187(5) Uani 1 1 d . . . C122 C 0.34753(13) 0.26812(13) 0.75530(13) 0.0205(5) Uani 1 1 d . . . H122 H 0.3425 0.2481 0.7117 0.025 Uiso 1 1 calc R . . C123 C 0.40801(14) 0.25625(15) 0.79917(14) 0.0253(5) Uani 1 1 d . . . H123 H 0.4441 0.2286 0.7852 0.030 Uiso 1 1 calc R . . C124 C 0.41581(15) 0.28468(16) 0.86325(14) 0.0274(6) Uani 1 1 d . . . H124 H 0.4571 0.2766 0.8931 0.033 Uiso 1 1 calc R . . C125 C 0.36275(15) 0.32519(17) 0.88361(14) 0.0310(6) Uani 1 1 d . . . H125 H 0.3678 0.3446 0.9275 0.037 Uiso 1 1 calc R . . C126 C 0.30229(15) 0.33724(16) 0.83965(13) 0.0268(6) Uani 1 1 d . . . H126 H 0.2663 0.3647 0.8539 0.032 Uiso 1 1 calc R . . C211 C 0.08071(13) 0.46524(13) 0.67167(12) 0.0182(5) Uani 1 1 d . . . C212 C 0.12451(14) 0.51877(14) 0.69834(14) 0.0244(5) Uani 1 1 d . . . H212 H 0.1549 0.5113 0.7387 0.029 Uiso 1 1 calc R . . C213 C 0.12392(16) 0.58260(14) 0.66641(15) 0.0279(6) Uani 1 1 d . . . H213 H 0.1548 0.6181 0.6843 0.033 Uiso 1 1 calc R . . C214 C 0.07830(16) 0.59484(15) 0.60828(15) 0.0285(6) Uani 1 1 d . . . H214 H 0.0774 0.6390 0.5871 0.034 Uiso 1 1 calc R . . C215 C 0.03429(15) 0.54298(14) 0.58129(14) 0.0258(5) Uani 1 1 d . . . H215 H 0.0026 0.5515 0.5420 0.031 Uiso 1 1 calc R . . C216 C 0.03650(13) 0.47765(14) 0.61217(13) 0.0210(5) Uani 1 1 d . . . H216 H 0.0076 0.4414 0.5924 0.025 Uiso 1 1 calc R . . C221 C 0.02017(13) 0.40270(14) 0.77939(13) 0.0218(5) Uani 1 1 d . . . C222 C -0.01012(16) 0.46741(17) 0.78600(16) 0.0324(6) Uani 1 1 d . . . H222 H -0.0046 0.5030 0.7544 0.039 Uiso 1 1 calc R . . C223 C -0.0487(2) 0.48026(19) 0.8389(2) 0.0460(9) Uani 1 1 d . . . H223 H -0.0694 0.5245 0.8430 0.055 Uiso 1 1 calc R . . C224 C -0.05674(19) 0.4289(2) 0.88529(19) 0.0438(8) Uani 1 1 d . . . H224 H -0.0825 0.4381 0.9215 0.053 Uiso 1 1 calc R . . C225 C -0.02728(18) 0.36376(19) 0.87908(17) 0.0372(7) Uani 1 1 d . . . H225 H -0.0330 0.3284 0.9109 0.045 Uiso 1 1 calc R . . C226 C 0.01051(15) 0.35073(16) 0.82623(14) 0.0281(6) Uani 1 1 d . . . H226 H 0.0301 0.3061 0.8217 0.034 Uiso 1 1 calc R . . C311 C 0.23985(13) 0.08953(14) 1.12872(13) 0.0216(5) Uani 1 1 d . . . C312 C 0.30118(15) 0.05374(16) 1.15177(16) 0.0314(6) Uani 1 1 d . . . H312 H 0.3028 0.0253 1.1906 0.038 Uiso 1 1 calc R . . C313 C 0.35919(16) 0.05922(17) 1.11899(18) 0.0347(7) Uani 1 1 d . . . H313 H 0.4003 0.0346 1.1353 0.042 Uiso 1 1 calc R . . C314 C 0.35751(15) 0.10093(17) 1.06191(16) 0.0310(6) Uani 1 1 d . . . H314 H 0.3972 0.1045 1.0390 0.037 Uiso 1 1 calc R . . C315 C 0.29761(15) 0.13699(16) 1.03912(14) 0.0275(6) Uani 1 1 d . . . H315 H 0.2964 0.1658 1.0005 0.033 Uiso 1 1 calc R . . C316 C 0.23880(14) 0.13153(15) 1.07233(13) 0.0237(5) Uani 1 1 d . . . H316 H 0.1979 0.1567 1.0563 0.028 Uiso 1 1 calc R . . C321 C 0.16488(13) -0.02317(14) 1.15927(13) 0.0215(5) Uani 1 1 d . . . C322 C 0.17891(16) -0.07159(16) 1.21089(16) 0.0307(6) Uani 1 1 d . . . H322 H 0.1853 -0.0566 1.2563 0.037 Uiso 1 1 calc R . . C323 C 0.18365(19) -0.14217(18) 1.19598(19) 0.0425(8) Uani 1 1 d . . . H323 H 0.1914 -0.1751 1.2313 0.051 Uiso 1 1 calc R . . C324 C 0.17704(19) -0.16406(17) 1.1298(2) 0.0439(9) Uani 1 1 d . . . H324 H 0.1821 -0.2118 1.1198 0.053 Uiso 1 1 calc R . . C325 C 0.16296(17) -0.11637(16) 1.07804(17) 0.0351(7) Uani 1 1 d . . . H325 H 0.1586 -0.1315 1.0326 0.042 Uiso 1 1 calc R . . C326 C 0.15520(15) -0.04657(15) 1.09258(14) 0.0256(5) Uani 1 1 d . . . H326 H 0.1433 -0.0144 1.0571 0.031 Uiso 1 1 calc R . . C331 C 0.19452(15) 0.08656(15) 1.25889(13) 0.0259(6) Uani 1 1 d . . . C332 C 0.25240(18) 0.12791(16) 1.27948(17) 0.0363(7) Uani 1 1 d . . . H332 H 0.2793 0.1460 1.2471 0.044 Uiso 1 1 calc R . . C333 C 0.2709(2) 0.1428(2) 1.3478(2) 0.0530(11) Uani 1 1 d . . . H333 H 0.3104 0.1709 1.3614 0.064 Uiso 1 1 calc R . . C334 C 0.2322(2) 0.1170(2) 1.39562(18) 0.0556(12) Uani 1 1 d . . . H334 H 0.2445 0.1281 1.4417 0.067 Uiso 1 1 calc R . . C335 C 0.1761(2) 0.0756(2) 1.37612(16) 0.0508(10) Uani 1 1 d . . . H335 H 0.1503 0.0567 1.4090 0.061 Uiso 1 1 calc R . . C336 C 0.15633(17) 0.06070(19) 1.30858(14) 0.0348(7) Uani 1 1 d . . . H336 H 0.1165 0.0327 1.2958 0.042 Uiso 1 1 calc R . . C411 C 0.13982(14) 0.27188(14) 1.10888(13) 0.0222(5) Uani 1 1 d . . . C412 C 0.20760(15) 0.27815(15) 1.14184(14) 0.0257(5) Uani 1 1 d . . . H412 H 0.2177 0.2639 1.1874 0.031 Uiso 1 1 calc R . . C413 C 0.26036(16) 0.30504(18) 1.10873(17) 0.0355(7) Uani 1 1 d . . . H413 H 0.3057 0.3107 1.1322 0.043 Uiso 1 1 calc R . . C414 C 0.24693(18) 0.32356(19) 1.04178(18) 0.0421(8) Uani 1 1 d . . . H414 H 0.2832 0.3411 1.0189 0.051 Uiso 1 1 calc R . . C415 C 0.18051(19) 0.31654(19) 1.00816(17) 0.0392(8) Uani 1 1 d . . . H415 H 0.1714 0.3286 0.9620 0.047 Uiso 1 1 calc R . . C416 C 0.12637(16) 0.29175(16) 1.04182(14) 0.0291(6) Uani 1 1 d . . . H416 H 0.0806 0.2886 1.0188 0.035 Uiso 1 1 calc R . . C421 C -0.00676(13) 0.27927(13) 1.12039(13) 0.0197(5) Uani 1 1 d . . . C422 C -0.04488(14) 0.25819(14) 1.05957(14) 0.0246(5) Uani 1 1 d . . . H422 H -0.0271 0.2227 1.0337 0.030 Uiso 1 1 calc R . . C423 C -0.10860(16) 0.28892(16) 1.03692(15) 0.0299(6) Uani 1 1 d . . . H423 H -0.1341 0.2741 0.9958 0.036 Uiso 1 1 calc R . . C424 C -0.13497(16) 0.34085(17) 1.07399(17) 0.0337(7) Uani 1 1 d . . . H424 H -0.1788 0.3610 1.0587 0.040 Uiso 1 1 calc R . . C425 C -0.09765(16) 0.36332(16) 1.13316(16) 0.0319(6) Uani 1 1 d . . . H425 H -0.1155 0.3994 1.1582 0.038 Uiso 1 1 calc R . . C426 C -0.03355(14) 0.33313(14) 1.15639(14) 0.0245(5) Uani 1 1 d . . . H426 H -0.0079 0.3492 1.1970 0.029 Uiso 1 1 calc R . . C431 C 0.09488(13) 0.26715(14) 1.23760(13) 0.0198(5) Uani 1 1 d . . . C432 C 0.11679(16) 0.33594(15) 1.24815(14) 0.0282(6) Uani 1 1 d . . . H432 H 0.1222 0.3647 1.2107 0.034 Uiso 1 1 calc R . . C433 C 0.13071(18) 0.36258(17) 1.31300(16) 0.0358(7) Uani 1 1 d . . . H433 H 0.1450 0.4095 1.3195 0.043 Uiso 1 1 calc R . . C434 C 0.12376(16) 0.32094(17) 1.36805(14) 0.0316(6) Uani 1 1 d . . . H434 H 0.1329 0.3394 1.4122 0.038 Uiso 1 1 calc R . . C435 C 0.10347(15) 0.25262(16) 1.35860(13) 0.0262(6) Uani 1 1 d . . . H435 H 0.0996 0.2238 1.3963 0.031 Uiso 1 1 calc R . . C436 C 0.08861(13) 0.22575(14) 1.29364(13) 0.0219(5) Uani 1 1 d . . . H436 H 0.0741 0.1788 1.2875 0.026 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru 0.01523(9) 0.01912(10) 0.01185(9) 0.00101(7) 0.00240(6) -0.00046(7) Co1 0.01628(16) 0.01881(16) 0.01304(15) 0.00149(12) -0.00042(12) -0.00092(12) Co2 0.01661(16) 0.01859(16) 0.01180(14) 0.00093(12) 0.00090(11) -0.00057(12) P1 0.0158(3) 0.0194(3) 0.0129(3) 0.0008(2) 0.0007(2) -0.0005(2) P2 0.0164(3) 0.0189(3) 0.0141(3) 0.0004(2) 0.0009(2) -0.0002(2) P3 0.0170(3) 0.0214(3) 0.0149(3) 0.0006(2) 0.0016(2) 0.0008(2) P4 0.0171(3) 0.0202(3) 0.0137(3) 0.0016(2) 0.0017(2) -0.0010(2) Si 0.0219(3) 0.0216(3) 0.0182(3) -0.0025(3) 0.0008(3) -0.0034(3) O1 0.0402(12) 0.0420(12) 0.0183(9) 0.0008(9) 0.0081(8) 0.0027(10) O2 0.0252(10) 0.0271(10) 0.0349(11) 0.0045(8) -0.0007(8) 0.0041(8) C1W 0.068(3) 0.052(3) 0.082(3) -0.014(2) 0.004(3) -0.005(2) Cl1W 0.1158(14) 0.0513(7) 0.184(2) 0.0095(10) -0.0735(14) -0.0044(8) Cl2W 0.1196(12) 0.0651(8) 0.0802(9) -0.0071(7) 0.0464(9) 0.0096(8) O11 0.0452(13) 0.0411(12) 0.0177(9) 0.0054(9) 0.0014(9) 0.0128(10) O12 0.0218(10) 0.0425(12) 0.0378(12) 0.0042(10) 0.0059(9) -0.0031(9) C1 0.0167(11) 0.0217(12) 0.0179(11) -0.0004(9) 0.0018(9) -0.0002(9) C2 0.0213(12) 0.0243(12) 0.0168(11) 0.0010(9) 0.0028(9) 0.0003(10) C3 0.0154(11) 0.0193(11) 0.0158(11) 0.0017(9) 0.0018(8) -0.0017(9) C4 0.0166(11) 0.0193(11) 0.0161(11) 0.0014(9) 0.0016(8) -0.0014(9) C5 0.0183(11) 0.0210(11) 0.0136(10) -0.0013(9) 0.0002(9) -0.0002(9) C11 0.0240(13) 0.0234(12) 0.0208(12) 0.0024(10) -0.0006(10) 0.0044(10) C12 0.0250(13) 0.0218(12) 0.0193(12) 0.0020(10) -0.0022(10) -0.0006(10) C21 0.0217(12) 0.0228(12) 0.0182(11) 0.0008(9) 0.0004(9) 0.0002(10) C22 0.0199(12) 0.0231(12) 0.0169(11) -0.0009(9) 0.0016(9) -0.0030(10) C31 0.0216(12) 0.0196(11) 0.0153(11) 0.0008(9) 0.0026(9) 0.0022(9) C32 0.0201(12) 0.0227(12) 0.0169(11) 0.0019(9) 0.0024(9) -0.0018(9) C33 0.0199(12) 0.0229(12) 0.0157(11) 0.0016(9) -0.0001(9) -0.0021(9) C34 0.0208(12) 0.0169(11) 0.0141(10) 0.0020(8) 0.0017(9) 0.0011(9) C35 0.0165(11) 0.0201(11) 0.0155(11) 0.0012(9) 0.0020(8) 0.0009(9) C36 0.0196(12) 0.0239(12) 0.0153(11) 0.0009(9) -0.0010(9) 0.0009(9) C41 0.0276(16) 0.048(2) 0.054(2) -0.0191(17) 0.0069(15) -0.0115(14) C42 0.050(2) 0.0384(17) 0.0212(14) -0.0072(12) 0.0033(13) -0.0081(15) C43 0.050(2) 0.0221(14) 0.0407(18) 0.0024(13) -0.0015(15) -0.0003(13) C51 0.0193(13) 0.0268(14) 0.0413(16) 0.0005(12) 0.0138(12) -0.0021(10) C52 0.0266(14) 0.0340(15) 0.0204(12) -0.0029(11) 0.0117(10) -0.0110(11) C53 0.0211(12) 0.0265(13) 0.0234(13) 0.0067(10) 0.0049(10) -0.0032(10) C54 0.0251(13) 0.0252(13) 0.0220(12) -0.0013(10) 0.0049(10) -0.0058(10) C55 0.0177(12) 0.0320(14) 0.0291(14) 0.0072(11) -0.0007(10) -0.0061(11) C111 0.0173(11) 0.0198(11) 0.0175(11) 0.0018(9) 0.0036(9) 0.0000(9) C112 0.0197(12) 0.0249(13) 0.0206(12) -0.0005(10) 0.0007(9) -0.0006(10) C113 0.0196(12) 0.0221(13) 0.0321(14) 0.0007(11) 0.0013(10) -0.0024(10) C114 0.0293(14) 0.0236(13) 0.0317(15) 0.0071(11) 0.0074(12) -0.0018(11) C115 0.0378(16) 0.0273(14) 0.0211(13) 0.0059(11) 0.0031(11) -0.0015(12) C116 0.0283(14) 0.0229(12) 0.0190(12) 0.0027(10) 0.0013(10) -0.0030(10) C121 0.0174(11) 0.0207(11) 0.0170(11) 0.0025(9) -0.0016(9) -0.0008(9) C122 0.0188(12) 0.0222(12) 0.0201(12) -0.0011(9) 0.0014(9) -0.0029(9) C123 0.0181(12) 0.0288(14) 0.0284(14) 0.0017(11) 0.0005(10) -0.0003(10) C124 0.0202(13) 0.0359(15) 0.0244(13) 0.0035(11) -0.0044(10) -0.0010(11) C125 0.0274(14) 0.0454(18) 0.0184(12) -0.0027(12) -0.0044(11) 0.0029(13) C126 0.0228(13) 0.0381(15) 0.0190(12) -0.0035(11) 0.0008(10) 0.0033(11) C211 0.0179(11) 0.0183(11) 0.0183(11) 0.0005(9) 0.0018(9) 0.0001(9) C212 0.0249(13) 0.0227(13) 0.0234(13) -0.0013(10) -0.0048(10) 0.0011(10) C213 0.0313(15) 0.0208(13) 0.0296(14) -0.0022(11) -0.0036(11) -0.0035(11) C214 0.0366(16) 0.0206(13) 0.0270(14) 0.0030(11) -0.0012(12) 0.0004(11) C215 0.0294(14) 0.0259(13) 0.0204(12) 0.0040(10) -0.0037(10) 0.0012(11) C216 0.0203(12) 0.0215(12) 0.0204(12) -0.0011(10) -0.0009(9) -0.0010(10) C221 0.0187(12) 0.0277(13) 0.0188(12) -0.0021(10) 0.0021(9) -0.0010(10) C222 0.0314(15) 0.0328(15) 0.0351(16) 0.0006(12) 0.0123(12) 0.0051(12) C223 0.048(2) 0.0395(18) 0.056(2) -0.0040(16) 0.0274(18) 0.0141(16) C224 0.045(2) 0.049(2) 0.0430(19) -0.0051(16) 0.0271(16) 0.0040(16) C225 0.0370(17) 0.0446(18) 0.0336(16) 0.0042(14) 0.0182(14) 0.0011(14) C226 0.0292(14) 0.0296(14) 0.0271(14) 0.0008(11) 0.0097(11) 0.0019(11) C311 0.0170(12) 0.0235(12) 0.0249(12) -0.0037(10) 0.0048(9) -0.0014(9) C312 0.0246(14) 0.0328(15) 0.0379(16) 0.0095(13) 0.0074(12) 0.0049(12) C313 0.0201(13) 0.0375(17) 0.0475(18) 0.0058(14) 0.0079(12) 0.0061(12) C314 0.0198(13) 0.0417(17) 0.0327(15) -0.0048(13) 0.0082(11) -0.0023(12) C315 0.0231(13) 0.0391(16) 0.0203(12) -0.0003(11) 0.0031(10) -0.0043(12) C316 0.0187(12) 0.0324(14) 0.0198(12) -0.0026(10) 0.0017(9) -0.0001(10) C321 0.0166(11) 0.0237(12) 0.0239(12) 0.0005(10) 0.0013(9) 0.0008(9) C322 0.0304(15) 0.0293(15) 0.0302(15) 0.0061(12) -0.0042(12) 0.0008(12) C323 0.046(2) 0.0298(16) 0.0461(19) 0.0139(14) -0.0162(16) 0.0023(14) C324 0.045(2) 0.0233(15) 0.057(2) -0.0049(14) -0.0181(17) 0.0061(14) C325 0.0358(17) 0.0303(15) 0.0360(16) -0.0084(13) -0.0077(13) 0.0042(13) C326 0.0261(13) 0.0279(14) 0.0226(13) -0.0023(10) 0.0021(10) 0.0007(11) C331 0.0277(14) 0.0297(14) 0.0191(12) -0.0036(10) -0.0025(10) 0.0082(11) C332 0.0398(18) 0.0296(15) 0.0348(16) -0.0071(12) -0.0136(13) 0.0078(13) C333 0.064(3) 0.0369(19) 0.049(2) -0.0173(16) -0.0313(19) 0.0145(18) C334 0.079(3) 0.059(2) 0.0227(16) -0.0165(16) -0.0193(18) 0.034(2) C335 0.063(3) 0.069(3) 0.0181(14) 0.0000(15) -0.0002(15) 0.029(2) C336 0.0358(16) 0.0497(19) 0.0178(13) 0.0016(12) -0.0004(11) 0.0122(14) C411 0.0233(13) 0.0220(12) 0.0217(12) 0.0009(10) 0.0048(10) -0.0031(10) C412 0.0239(13) 0.0298(14) 0.0232(13) 0.0034(11) 0.0023(10) -0.0023(11) C413 0.0234(14) 0.0412(17) 0.0421(18) 0.0035(14) 0.0051(13) -0.0075(13) C414 0.0374(18) 0.049(2) 0.0428(19) 0.0095(16) 0.0158(15) -0.0140(15) C415 0.0462(19) 0.0461(19) 0.0271(15) 0.0072(14) 0.0109(13) -0.0086(15) C416 0.0313(15) 0.0341(15) 0.0216(13) 0.0046(11) 0.0019(11) -0.0051(12) C421 0.0182(12) 0.0216(12) 0.0192(11) 0.0039(9) 0.0024(9) 0.0006(9) C422 0.0245(13) 0.0244(13) 0.0241(13) 0.0000(10) -0.0001(10) 0.0016(10) C423 0.0273(14) 0.0325(15) 0.0271(14) 0.0029(12) -0.0071(11) 0.0033(12) C424 0.0245(14) 0.0368(16) 0.0386(17) 0.0051(13) -0.0006(12) 0.0116(12) C425 0.0312(15) 0.0298(15) 0.0354(16) 0.0011(12) 0.0073(12) 0.0080(12) C426 0.0248(13) 0.0256(13) 0.0231(12) 0.0013(10) 0.0031(10) -0.0007(10) C431 0.0180(11) 0.0234(12) 0.0179(11) -0.0010(9) 0.0019(9) -0.0005(9) C432 0.0356(15) 0.0252(13) 0.0241(13) -0.0002(11) 0.0052(11) -0.0054(12) C433 0.0443(18) 0.0311(15) 0.0324(16) -0.0098(13) 0.0064(13) -0.0118(14) C434 0.0330(15) 0.0418(17) 0.0195(13) -0.0093(12) 0.0017(11) -0.0068(13) C435 0.0256(13) 0.0367(15) 0.0163(12) -0.0002(11) 0.0023(10) -0.0030(11) C436 0.0187(12) 0.0279(13) 0.0192(12) 0.0001(10) 0.0023(9) -0.0005(10) _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 Ru C1 2.003(2) . ? Ru C55 2.220(3) . ? Ru C54 2.230(3) . ? Ru C51 2.243(3) . ? Ru C53 2.255(3) . ? Ru C52 2.275(2) . ? Ru P3 2.2849(7) . ? Ru P4 2.3021(7) . ? Co1 C12 1.786(3) . ? Co1 C11 1.792(3) . ? Co1 C4 1.971(3) . ? Co1 C3 1.981(2) . ? Co1 P2 2.2319(7) . ? Co1 Co2 2.5116(5) . ? Co2 C22 1.780(3) . ? Co2 C21 1.800(3) . ? Co2 C3 1.948(2) . ? Co2 C4 1.997(2) . ? Co2 P1 2.2370(7) . ? P1 C121 1.836(3) . ? P1 C5 1.837(2) . ? P1 C111 1.838(3) . ? P2 C211 1.827(3) . ? P2 C5 1.835(3) . ? P2 C221 1.842(3) . ? P3 C331 1.838(3) . ? P3 C311 1.842(3) . ? P3 C321 1.853(3) . ? P4 C411 1.840(3) . ? P4 C431 1.842(3) . ? P4 C421 1.855(3) . ? Si C4 1.841(3) . ? Si C43 1.867(3) . ? Si C42 1.870(3) . ? Si C41 1.875(3) . ? O1 C21 1.148(3) . ? O2 C22 1.141(3) . ? C1W Cl1W 1.745(5) . ? C1W Cl2W 1.774(5) . ? O11 C11 1.146(3) . ? O12 C12 1.144(3) . ? C1 C2 1.218(4) . ? C2 C31 1.432(3) . ? C3 C4 1.359(3) . ? C3 C34 1.465(3) . ? C31 C36 1.410(4) . ? C31 C32 1.411(3) . ? C32 C33 1.383(3) . ? C33 C34 1.408(3) . ? C34 C35 1.400(3) . ? C35 C36 1.387(3) . ? C51 C55 1.402(4) . ? C51 C52 1.429(4) . ? C52 C53 1.417(4) . ? C53 C54 1.422(4) . ? C54 C55 1.422(4) . ? C111 C112 1.395(4) . ? C111 C116 1.398(3) . ? C112 C113 1.395(4) . ? C113 C114 1.390(4) . ? C114 C115 1.384(4) . ? C115 C116 1.397(4) . ? C121 C126 1.399(4) . ? C121 C122 1.401(4) . ? C122 C123 1.393(4) . ? C123 C124 1.388(4) . ? C124 C125 1.395(4) . ? C125 C126 1.394(4) . ? C211 C216 1.399(3) . ? C211 C212 1.399(4) . ? C212 C213 1.387(4) . ? C213 C214 1.391(4) . ? C214 C215 1.379(4) . ? C215 C216 1.402(4) . ? C221 C222 1.392(4) . ? C221 C226 1.403(4) . ? C222 C223 1.398(4) . ? C223 C224 1.381(5) . ? C224 C225 1.392(5) . ? C225 C226 1.388(4) . ? C311 C316 1.390(4) . ? C311 C312 1.402(4) . ? C312 C313 1.379(4) . ? C313 C314 1.396(5) . ? C314 C315 1.381(4) . ? C315 C316 1.398(4) . ? C321 C322 1.395(4) . ? C321 C326 1.402(4) . ? C322 C323 1.398(5) . ? C323 C324 1.383(5) . ? C324 C325 1.388(5) . ? C325 C326 1.389(4) . ? C331 C332 1.396(4) . ? C331 C336 1.408(4) . ? C332 C333 1.401(5) . ? C333 C334 1.385(7) . ? C334 C335 1.366(7) . ? C335 C336 1.390(4) . ? C411 C416 1.391(4) . ? C411 C412 1.400(4) . ? C412 C413 1.391(4) . ? C413 C414 1.382(5) . ? C414 C415 1.383(5) . ? C415 C416 1.404(4) . ? C421 C426 1.402(4) . ? C421 C422 1.403(4) . ? C422 C423 1.394(4) . ? C423 C424 1.384(4) . ? C424 C425 1.379(5) . ? C425 C426 1.398(4) . ? C431 C436 1.397(4) . ? C431 C432 1.400(4) . ? C432 C433 1.393(4) . ? C433 C434 1.386(4) . ? C434 C435 1.380(4) . ? C435 C436 1.398(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ru C55 88.91(10) . . ? C1 Ru C54 94.22(10) . . ? C55 Ru C54 37.28(11) . . ? C1 Ru C51 118.02(11) . . ? C55 Ru C51 36.60(11) . . ? C54 Ru C51 61.70(10) . . ? C1 Ru C53 128.92(10) . . ? C55 Ru C53 61.48(10) . . ? C54 Ru C53 36.98(10) . . ? C51 Ru C53 61.13(10) . . ? C1 Ru C52 150.31(10) . . ? C55 Ru C52 61.45(10) . . ? C54 Ru C52 61.67(10) . . ? C51 Ru C52 36.86(11) . . ? C53 Ru C52 36.45(10) . . ? C1 Ru P3 92.75(7) . . ? C55 Ru P3 145.27(8) . . ? C54 Ru P3 108.07(8) . . ? C51 Ru P3 147.27(8) . . ? C53 Ru P3 91.59(7) . . ? C52 Ru P3 110.41(8) . . ? C1 Ru P4 86.70(7) . . ? C55 Ru P4 115.22(8) . . ? C54 Ru P4 152.32(8) . . ? C51 Ru P4 93.51(8) . . ? C53 Ru P4 142.28(7) . . ? C52 Ru P4 106.62(8) . . ? P3 Ru P4 99.50(2) . . ? C12 Co1 C11 104.08(12) . . ? C12 Co1 C4 102.05(11) . . ? C11 Co1 C4 100.76(11) . . ? C12 Co1 C3 100.77(11) . . ? C11 Co1 C3 137.76(11) . . ? C4 Co1 C3 40.22(10) . . ? C12 Co1 P2 95.69(9) . . ? C11 Co1 P2 109.96(9) . . ? C4 Co1 P2 139.38(7) . . ? C3 Co1 P2 100.83(7) . . ? C12 Co1 Co2 149.24(9) . . ? C11 Co1 Co2 96.69(9) . . ? C4 Co1 Co2 51.18(7) . . ? C3 Co1 Co2 49.69(7) . . ? P2 Co1 Co2 98.25(2) . . ? C22 Co2 C21 99.53(12) . . ? C22 Co2 C3 96.31(11) . . ? C21 Co2 C3 143.47(11) . . ? C22 Co2 C4 100.71(11) . . ? C21 Co2 C4 104.10(11) . . ? C3 Co2 C4 40.28(10) . . ? C22 Co2 P1 101.90(8) . . ? C21 Co2 P1 106.77(9) . . ? C3 Co2 P1 101.79(7) . . ? C4 Co2 P1 137.70(7) . . ? C22 Co2 Co1 146.14(8) . . ? C21 Co2 Co1 104.19(8) . . ? C3 Co2 Co1 50.85(7) . . ? C4 Co2 Co1 50.28(7) . . ? P1 Co2 Co1 94.05(2) . . ? C121 P1 C5 101.79(11) . . ? C121 P1 C111 102.01(11) . . ? C5 P1 C111 101.85(11) . . ? C121 P1 Co2 118.85(9) . . ? C5 P1 Co2 110.84(8) . . ? C111 P1 Co2 118.93(8) . . ? C211 P2 C5 105.15(12) . . ? C211 P2 C221 102.26(12) . . ? C5 P2 C221 100.28(11) . . ? C211 P2 Co1 119.62(8) . . ? C5 P2 Co1 109.40(8) . . ? C221 P2 Co1 117.81(9) . . ? C331 P3 C311 102.15(13) . . ? C331 P3 C321 104.41(13) . . ? C311 P3 C321 95.17(12) . . ? C331 P3 Ru 114.10(9) . . ? C311 P3 Ru 126.94(9) . . ? C321 P3 Ru 110.71(8) . . ? C411 P4 C431 100.55(12) . . ? C411 P4 C421 102.76(12) . . ? C431 P4 C421 102.23(12) . . ? C411 P4 Ru 119.08(9) . . ? C431 P4 Ru 120.52(9) . . ? C421 P4 Ru 109.17(9) . . ? C4 Si C43 108.58(13) . . ? C4 Si C42 110.34(13) . . ? C43 Si C42 110.46(16) . . ? C4 Si C41 109.35(14) . . ? C43 Si C41 109.76(18) . . ? C42 Si C41 108.34(17) . . ? Cl1W C1W Cl2W 112.7(3) . . ? C2 C1 Ru 171.7(2) . . ? C1 C2 C31 174.6(3) . . ? C4 C3 C34 138.2(2) . . ? C4 C3 Co2 71.78(14) . . ? C34 C3 Co2 136.19(18) . . ? C4 C3 Co1 69.48(15) . . ? C34 C3 Co1 134.20(18) . . ? Co2 C3 Co1 79.46(9) . . ? C3 C4 Si 142.5(2) . . ? C3 C4 Co1 70.29(15) . . ? Si C4 Co1 135.79(14) . . ? C3 C4 Co2 67.94(14) . . ? Si C4 Co2 133.17(14) . . ? Co1 C4 Co2 78.54(9) . . ? P2 C5 P1 109.36(12) . . ? O11 C11 Co1 175.0(3) . . ? O12 C12 Co1 176.3(2) . . ? O1 C21 Co2 176.1(2) . . ? O2 C22 Co2 175.5(2) . . ? C36 C31 C32 117.6(2) . . ? C36 C31 C2 120.7(2) . . ? C32 C31 C2 121.6(2) . . ? C33 C32 C31 121.1(2) . . ? C32 C33 C34 120.9(2) . . ? C35 C34 C33 118.2(2) . . ? C35 C34 C3 121.8(2) . . ? C33 C34 C3 120.0(2) . . ? C36 C35 C34 121.0(2) . . ? C35 C36 C31 121.1(2) . . ? C55 C51 C52 108.5(3) . . ? C55 C51 Ru 70.82(15) . . ? C52 C51 Ru 72.80(15) . . ? C53 C52 C51 107.0(2) . . ? C53 C52 Ru 70.98(14) . . ? C51 C52 Ru 70.34(15) . . ? C52 C53 C54 108.9(2) . . ? C52 C53 Ru 72.57(15) . . ? C54 C53 Ru 70.55(15) . . ? C55 C54 C53 107.1(2) . . ? C55 C54 Ru 71.01(15) . . ? C53 C54 Ru 72.47(15) . . ? C51 C55 C54 108.6(3) . . ? C51 C55 Ru 72.58(16) . . ? C54 C55 Ru 71.71(15) . . ? C112 C111 C116 119.1(2) . . ? C112 C111 P1 121.36(19) . . ? C116 C111 P1 119.45(19) . . ? C111 C112 C113 120.5(2) . . ? C114 C113 C112 120.0(3) . . ? C115 C114 C113 120.1(3) . . ? C114 C115 C116 120.1(3) . . ? C115 C116 C111 120.3(3) . . ? C126 C121 C122 118.5(2) . . ? C126 C121 P1 123.6(2) . . ? C122 C121 P1 117.86(19) . . ? C123 C122 C121 120.7(2) . . ? C124 C123 C122 120.2(3) . . ? C123 C124 C125 119.7(3) . . ? C126 C125 C124 120.1(3) . . ? C125 C126 C121 120.7(3) . . ? C216 C211 C212 118.5(2) . . ? C216 C211 P2 117.81(19) . . ? C212 C211 P2 123.6(2) . . ? C213 C212 C211 120.6(2) . . ? C212 C213 C214 120.3(3) . . ? C215 C214 C213 120.1(3) . . ? C214 C215 C216 119.7(2) . . ? C211 C216 C215 120.8(2) . . ? C222 C221 C226 118.8(3) . . ? C222 C221 P2 123.6(2) . . ? C226 C221 P2 117.6(2) . . ? C221 C222 C223 120.3(3) . . ? C224 C223 C222 120.2(3) . . ? C223 C224 C225 120.2(3) . . ? C226 C225 C224 119.7(3) . . ? C225 C226 C221 120.8(3) . . ? C316 C311 C312 118.6(2) . . ? C316 C311 P3 122.9(2) . . ? C312 C311 P3 118.3(2) . . ? C313 C312 C311 121.0(3) . . ? C312 C313 C314 120.1(3) . . ? C315 C314 C313 119.4(3) . . ? C314 C315 C316 120.6(3) . . ? C311 C316 C315 120.3(3) . . ? C322 C321 C326 118.9(3) . . ? C322 C321 P3 125.8(2) . . ? C326 C321 P3 115.2(2) . . ? C321 C322 C323 120.3(3) . . ? C324 C323 C322 120.1(3) . . ? C323 C324 C325 120.1(3) . . ? C324 C325 C326 120.0(3) . . ? C325 C326 C321 120.5(3) . . ? C332 C331 C336 118.0(3) . . ? C332 C331 P3 122.4(2) . . ? C336 C331 P3 119.3(2) . . ? C331 C332 C333 120.1(4) . . ? C334 C333 C332 120.8(4) . . ? C335 C334 C333 119.6(3) . . ? C334 C335 C336 120.6(4) . . ? C335 C336 C331 120.9(4) . . ? C416 C411 C412 118.8(3) . . ? C416 C411 P4 121.7(2) . . ? C412 C411 P4 119.3(2) . . ? C413 C412 C411 120.8(3) . . ? C414 C413 C412 120.2(3) . . ? C413 C414 C415 119.8(3) . . ? C414 C415 C416 120.5(3) . . ? C411 C416 C415 120.0(3) . . ? C426 C421 C422 118.3(2) . . ? C426 C421 P4 122.9(2) . . ? C422 C421 P4 118.7(2) . . ? C423 C422 C421 120.5(3) . . ? C424 C423 C422 120.4(3) . . ? C425 C424 C423 120.0(3) . . ? C424 C425 C426 120.2(3) . . ? C425 C426 C421 120.6(3) . . ? C436 C431 C432 118.4(2) . . ? C436 C431 P4 119.5(2) . . ? C432 C431 P4 122.2(2) . . ? C433 C432 C431 120.6(3) . . ? C434 C433 C432 120.3(3) . . ? C435 C434 C433 119.9(3) . . ? C434 C435 C436 120.2(3) . . ? C431 C436 C435 120.7(3) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 1.37 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.049 _refine_diff_density_min -2.093 _refine_diff_density_rms 0.096 data_00srv154 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C77 H66 Co2 O4 P4 Ru Si' _chemical_formula_weight 1426.2 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' 'Si' 'Si' 0.0817 0.0704 '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' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 13.7464(7) _cell_length_b 19.9035(6) _cell_length_c 24.8998(8) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 6812.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour dark_red _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.391 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2928 _exptl_absorpt_coefficient_mu 0.861 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min . _exptl_absorpt_correction_T_max . _exptl_absorpt_process_details . _exptl_special_details ; The data collection nominally covered over a full sphere of reciprocal space, by a combination of 5 sets of \w scans, each set at different \f and/or 2\q angles and each scan (10 s exposure) covering 0.3\% in \w. Crystal to detector distance 4.51 cm. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD 1K area detector' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean 8 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 86568 _diffrn_reflns_av_R_equivalents 0.0452 _diffrn_reflns_av_sigmaI/netI 0.0306 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.31 _diffrn_reflns_theta_max 29 _reflns_number_total 18038 _reflns_number_gt 16925 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT V5.0 (Bruker, 1998)' _computing_cell_refinement 'SMART-NT V5.0 (Bruker, 1998)' _computing_data_reduction 'SAINT-NT V5.0 (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Ferrugia, 2000)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0259P)^2^+3.6095P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.002 _refine_ls_number_reflns 18038 _refine_ls_number_parameters 811 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0324 _refine_ls_R_factor_gt 0.028 _refine_ls_wR_factor_ref 0.0635 _refine_ls_wR_factor_gt 0.0613 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru Ru 0.524073(11) 0.469860(8) -0.024279(6) 0.01194(3) Uani 1 1 d . . . Co1 Co 0.42306(2) 0.504793(15) 0.218256(11) 0.01399(6) Uani 1 1 d . . . Co2 Co 0.31392(2) 0.413237(15) 0.185831(12) 0.01451(6) Uani 1 1 d . . . P1 P 0.34611(4) 0.52892(3) 0.29456(2) 0.01317(10) Uani 1 1 d . . . Si Si 0.21573(4) 0.57329(3) 0.14911(2) 0.01777(12) Uani 1 1 d . . . P2 P 0.25411(4) 0.39816(3) 0.26761(2) 0.01384(10) Uani 1 1 d . . . P3 P 0.60923(4) 0.56813(3) -0.01773(2) 0.01289(10) Uani 1 1 d . . . P4 P 0.64272(4) 0.39340(3) -0.00286(2) 0.01362(10) Uani 1 1 d . . . O16 O 0.58818(13) 0.41260(10) 0.22787(7) 0.0291(4) Uani 1 1 d . . . O17 O 0.52533(16) 0.63110(10) 0.20015(9) 0.0399(5) Uani 1 1 d . . . O18 O 0.44116(15) 0.29826(10) 0.16374(8) 0.0372(5) Uani 1 1 d . . . O19 O 0.14086(16) 0.37850(11) 0.12437(9) 0.0433(5) Uani 1 1 d . . . C1 C 0.48127(15) 0.47772(10) 0.05274(8) 0.0148(4) Uani 1 1 d . . . C2 C 0.43626(15) 0.48152(10) 0.09502(8) 0.0156(4) Uani 1 1 d . . . C3 C 0.38477(15) 0.48293(11) 0.14397(8) 0.0158(4) Uani 1 1 d . . . C4 C 0.30794(15) 0.51110(11) 0.17066(8) 0.0158(4) Uani 1 1 d . . . C8 C 0.09640(17) 0.56657(14) 0.18523(10) 0.0271(5) Uani 1 1 d . . . H8A H 0.0742(8) 0.5206(8) 0.1842(7) 0.041(5) Uiso 1 1 d R . . H8B H 0.0491(9) 0.5951(9) 0.1679(6) 0.041(5) Uiso 1 1 d R . . H8C H 0.1046(4) 0.5805(9) 0.2221(7) 0.041(5) Uiso 1 1 d R . . C9 C 0.1908(2) 0.55735(14) 0.07675(10) 0.0293(5) Uani 1 1 d . . . H9A H 0.2500(11) 0.5535(10) 0.0580(4) 0.043(5) Uiso 1 1 d R . . H9B H 0.1544(14) 0.5932(8) 0.0624(3) 0.043(5) Uiso 1 1 d R . . H9C H 0.1552(14) 0.5172(9) 0.07320(14) 0.043(5) Uiso 1 1 d R . . C10 C 0.2649(2) 0.65968(13) 0.15842(10) 0.0276(5) Uani 1 1 d . . . H10A H 0.2718(14) 0.6688(4) 0.1959(7) 0.046(6) Uiso 1 1 d R . . H10B H 0.2213(11) 0.6915(6) 0.1428(8) 0.046(6) Uiso 1 1 d R . . H10C H 0.3270(14) 0.6630(3) 0.1413(8) 0.046(6) Uiso 1 1 d R . . C54 C 0.45657(16) 0.50588(13) -0.10052(9) 0.0210(5) Uani 1 1 d . . . H54 H 0.4768 0.5449 -0.1177 0.025 Uiso 1 1 calc R . . C55 C 0.38297(16) 0.50194(12) -0.05970(9) 0.0203(4) Uani 1 1 d . . . H55 H 0.3471 0.5375 -0.0458 0.024 Uiso 1 1 calc R . . C51 C 0.37553(16) 0.43265(12) -0.04457(9) 0.0202(4) Uani 1 1 d . . . H51 H 0.3334 0.4153 -0.0188 0.024 Uiso 1 1 calc R . . C52 C 0.44276(17) 0.39516(13) -0.07522(9) 0.0218(5) Uani 1 1 d . . . H52 H 0.4525 0.3490 -0.0730 0.026 Uiso 1 1 calc R . . C53 C 0.49339(16) 0.44015(13) -0.11026(9) 0.0219(5) Uani 1 1 d . . . H53 H 0.5415 0.4286 -0.1349 0.026 Uiso 1 1 calc R . . C16 C 0.52333(17) 0.44907(11) 0.22725(8) 0.0195(4) Uani 1 1 d . . . C17 C 0.48520(18) 0.58167(12) 0.20779(9) 0.0232(5) Uani 1 1 d . . . C18 C 0.39271(17) 0.34305(12) 0.17343(9) 0.0223(5) Uani 1 1 d . . . C19 C 0.20903(18) 0.39158(13) 0.14821(10) 0.0244(5) Uani 1 1 d . . . C5 C 0.23171(14) 0.48063(10) 0.29778(8) 0.0137(4) Uani 1 1 d . . . H5B H 0.2112 0.4755 0.3348 0.018 Uiso 1 1 calc R . . H5A H 0.1808 0.5039 0.2783 0.018 Uiso 1 1 calc R . . C111 C 0.30411(16) 0.61553(11) 0.30545(8) 0.0154(4) Uani 1 1 d . . . C116 C 0.37276(17) 0.66750(12) 0.30431(10) 0.0225(5) Uani 1 1 d . . . H116 H 0.4380 0.6576 0.2985 0.027 Uiso 1 1 calc R . . C115 C 0.34412(19) 0.73362(12) 0.31181(12) 0.0297(6) Uani 1 1 d . . . H115 H 0.3903 0.7677 0.3105 0.036 Uiso 1 1 calc R . . C114 C 0.2472(2) 0.74950(12) 0.32125(11) 0.0284(5) Uani 1 1 d . . . H114 H 0.2285 0.7940 0.3261 0.034 Uiso 1 1 calc R . . C113 C 0.17862(18) 0.69854(12) 0.32335(10) 0.0247(5) Uani 1 1 d . . . H113 H 0.1137 0.7087 0.3299 0.030 Uiso 1 1 calc R . . C112 C 0.20705(16) 0.63210(11) 0.31559(9) 0.0191(4) Uani 1 1 d . . . H112 H 0.1606 0.5982 0.3172 0.023 Uiso 1 1 calc R . . C121 C 0.40130(15) 0.51134(10) 0.36015(8) 0.0139(4) Uani 1 1 d . . . C126 C 0.35354(15) 0.53200(12) 0.40675(8) 0.0170(4) Uani 1 1 d . . . H126 H 0.2947 0.5549 0.4041 0.020 Uiso 1 1 calc R . . C125 C 0.39268(17) 0.51885(12) 0.45703(9) 0.0206(5) Uani 1 1 d . . . H125 H 0.3607 0.5335 0.4878 0.025 Uiso 1 1 calc R . . C124 C 0.47975(17) 0.48372(11) 0.46143(8) 0.0200(4) Uani 1 1 d . . . H124 H 0.5059 0.4745 0.4951 0.024 Uiso 1 1 calc R . . C123 C 0.52749(16) 0.46246(12) 0.41531(9) 0.0205(4) Uani 1 1 d . . . H123 H 0.5858 0.4390 0.4181 0.025 Uiso 1 1 calc R . . C122 C 0.48867(15) 0.47596(11) 0.36511(8) 0.0180(4) Uani 1 1 d . . . H122 H 0.5210 0.4614 0.3344 0.022 Uiso 1 1 calc R . . C221 C 0.32343(15) 0.35465(11) 0.32003(9) 0.0162(4) Uani 1 1 d . . . C226 C 0.29272(17) 0.35767(12) 0.37379(10) 0.0217(5) Uani 1 1 d . . . H226 H 0.2359 0.3805 0.3825 0.026 Uiso 1 1 calc R . . C225 C 0.34655(19) 0.32680(13) 0.41406(10) 0.0269(5) Uani 1 1 d . . . H225 H 0.3265 0.3301 0.4496 0.032 Uiso 1 1 calc R . . C224 C 0.43013(19) 0.29105(12) 0.40146(11) 0.0273(5) Uani 1 1 d . . . H224 H 0.4662 0.2708 0.4286 0.033 Uiso 1 1 calc R . . C223 C 0.45996(18) 0.28554(12) 0.34836(11) 0.0251(5) Uani 1 1 d . . . H223 H 0.5149 0.2605 0.3397 0.030 Uiso 1 1 calc R . . C222 C 0.40701(16) 0.31782(11) 0.30788(10) 0.0194(4) Uani 1 1 d . . . H222 H 0.4278 0.3147 0.2724 0.023 Uiso 1 1 calc R . . C211 C 0.13587(16) 0.35549(11) 0.27375(8) 0.0172(4) Uani 1 1 d . . . C212 C 0.13293(19) 0.28592(13) 0.27781(11) 0.0297(6) Uani 1 1 d . . . H212 H 0.1907 0.2617 0.2797 0.036 Uiso 1 1 calc R . . C213 C 0.0445(2) 0.25207(15) 0.27910(13) 0.0387(7) Uani 1 1 d . . . H213 H 0.0437 0.2055 0.2816 0.046 Uiso 1 1 calc R . . C214 C -0.0424(2) 0.28730(16) 0.27664(10) 0.0348(7) Uani 1 1 d . . . H214 H -0.1015 0.2646 0.2780 0.042 Uiso 1 1 calc R . . C215 C -0.04034(18) 0.35621(15) 0.27220(11) 0.0323(6) Uani 1 1 d . . . H215 H -0.0984 0.3801 0.2704 0.039 Uiso 1 1 calc R . . C216 C 0.04791(17) 0.39043(13) 0.27044(10) 0.0259(5) Uani 1 1 d . . . H216 H 0.0483 0.4370 0.2670 0.031 Uiso 1 1 calc R . . C311 C 0.52065(15) 0.63821(10) -0.02102(9) 0.0162(4) Uani 1 1 d . . . C312 C 0.44417(15) 0.64073(11) 0.01648(9) 0.0173(4) Uani 1 1 d . . . H312 H 0.4414 0.6092 0.0440 0.021 Uiso 1 1 calc R . . C313 C 0.37242(16) 0.69012(12) 0.01283(9) 0.0200(5) Uani 1 1 d . . . H313 H 0.3230 0.6918 0.0383 0.024 Uiso 1 1 calc R . . C314 C 0.37433(17) 0.73683(12) -0.02874(10) 0.0255(5) Uani 1 1 d . . . H314 H 0.3266 0.7698 -0.0310 0.031 Uiso 1 1 calc R . . C315 C 0.44751(19) 0.73386(14) -0.06650(11) 0.0301(6) Uani 1 1 d . . . H315 H 0.4484 0.7646 -0.0946 0.036 Uiso 1 1 calc R . . C316 C 0.52032(19) 0.68509(12) -0.06283(10) 0.0245(5) Uani 1 1 d . . . H316 H 0.5693 0.6838 -0.0886 0.029 Uiso 1 1 calc R . . C331 C 0.68867(16) 0.58904(11) 0.03922(8) 0.0158(4) Uani 1 1 d . . . C336 C 0.65504(17) 0.62268(12) 0.08502(9) 0.0213(5) Uani 1 1 d . . . H336 H 0.5901 0.6356 0.0873 0.026 Uiso 1 1 calc R . . C335 C 0.71855(18) 0.63688(14) 0.12704(10) 0.0253(5) Uani 1 1 d . . . H335 H 0.6957 0.6592 0.1573 0.030 Uiso 1 1 calc R . . C334 C 0.81527(18) 0.61813(12) 0.12434(9) 0.0220(5) Uani 1 1 d . . . H334 H 0.8573 0.6283 0.1525 0.026 Uiso 1 1 calc R . . C333 C 0.84935(16) 0.58406(12) 0.07940(9) 0.0202(4) Uani 1 1 d . . . H333 H 0.9141 0.5708 0.0776 0.024 Uiso 1 1 calc R . . C332 C 0.78687(16) 0.56988(11) 0.03743(9) 0.0174(4) Uani 1 1 d . . . H332 H 0.8103 0.5472 0.0074 0.021 Uiso 1 1 calc R . . C321 C 0.69034(15) 0.59123(11) -0.07366(8) 0.0150(4) Uani 1 1 d . . . C322 C 0.74417(17) 0.65118(11) -0.07148(9) 0.0193(4) Uani 1 1 d . . . H322 H 0.7423 0.6773 -0.0406 0.023 Uiso 1 1 calc R . . C323 C 0.79984(17) 0.67179(12) -0.11460(10) 0.0219(5) Uani 1 1 d . . . H323 H 0.8349 0.7117 -0.1126 0.026 Uiso 1 1 calc R . . C324 C 0.80364(17) 0.63286(13) -0.16122(9) 0.0226(5) Uani 1 1 d . . . H324 H 0.8401 0.6471 -0.1906 0.027 Uiso 1 1 calc R . . C325 C 0.75298(17) 0.57306(13) -0.16345(9) 0.0211(5) Uani 1 1 d . . . H325 H 0.7565 0.5466 -0.1942 0.025 Uiso 1 1 calc R . . C326 C 0.69639(15) 0.55202(12) -0.11993(9) 0.0170(4) Uani 1 1 d . . . H326 H 0.6626 0.5116 -0.1219 0.020 Uiso 1 1 calc R . . C411 C 0.59714(15) 0.31244(11) 0.02244(9) 0.0168(4) Uani 1 1 d . . . C416 C 0.49897(16) 0.30290(12) 0.03490(9) 0.0202(5) Uani 1 1 d . . . H416 H 0.4555 0.3385 0.0317 0.024 Uiso 1 1 calc R . . C415 C 0.46594(17) 0.24020(12) 0.05210(9) 0.0222(5) Uani 1 1 d . . . H415 H 0.4004 0.2341 0.0601 0.027 Uiso 1 1 calc R . . C414 C 0.52983(19) 0.18715(12) 0.05730(10) 0.0240(5) Uani 1 1 d . . . H414 H 0.5074 0.1452 0.0681 0.029 Uiso 1 1 calc R . . C413 C 0.62828(19) 0.19692(13) 0.04626(11) 0.0280(5) Uani 1 1 d . . . H413 H 0.6717 0.1615 0.0505 0.034 Uiso 1 1 calc R . . C412 C 0.66187(16) 0.25869(12) 0.02904(11) 0.0245(5) Uani 1 1 d . . . H412 H 0.7277 0.2646 0.0218 0.029 Uiso 1 1 calc R . . C421 C 0.70658(15) 0.36666(11) -0.06444(9) 0.0169(4) Uani 1 1 d . . . C426 C 0.67356(18) 0.31091(12) -0.09384(10) 0.0227(5) Uani 1 1 d . . . H426 H 0.6247 0.2837 -0.0799 0.027 Uiso 1 1 calc R . . C425 C 0.7137(2) 0.29615(13) -0.14375(11) 0.0297(6) Uani 1 1 d . . . H425 H 0.6906 0.2595 -0.1631 0.036 Uiso 1 1 calc R . . C424 C 0.7878(2) 0.33551(14) -0.16504(11) 0.0303(6) Uani 1 1 d . . . H424 H 0.8143 0.3254 -0.1984 0.036 Uiso 1 1 calc R . . C423 C 0.82168(18) 0.39000(13) -0.13587(10) 0.0252(5) Uani 1 1 d . . . H423 H 0.8720 0.4162 -0.1495 0.030 Uiso 1 1 calc R . . C422 C 0.78084(16) 0.40580(12) -0.08625(9) 0.0196(4) Uani 1 1 d . . . H422 H 0.8034 0.4430 -0.0674 0.023 Uiso 1 1 calc R . . C431 C 0.73886(15) 0.40734(11) 0.04702(9) 0.0161(4) Uani 1 1 d . . . C432 C 0.83607(16) 0.38903(12) 0.03938(10) 0.0229(5) Uani 1 1 d . . . H432 H 0.8559 0.3721 0.0063 0.027 Uiso 1 1 calc R . . C433 C 0.90351(17) 0.39582(13) 0.08078(11) 0.0285(5) Uani 1 1 d . . . H433 H 0.9681 0.3837 0.0753 0.034 Uiso 1 1 calc R . . C434 C 0.87414(19) 0.42059(13) 0.13009(10) 0.0281(5) Uani 1 1 d . . . H434 H 0.9191 0.4250 0.1578 0.034 Uiso 1 1 calc R . . C435 C 0.77772(18) 0.43894(13) 0.13849(10) 0.0258(5) Uani 1 1 d . . . H435 H 0.7584 0.4556 0.1717 0.031 Uiso 1 1 calc R . . C436 C 0.71022(16) 0.43230(12) 0.09718(9) 0.0193(4) Uani 1 1 d . . . H436 H 0.6457 0.4445 0.1029 0.023 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru 0.01078(7) 0.01438(7) 0.01067(7) -0.00061(6) -0.00084(6) 0.00026(6) Co1 0.01259(13) 0.01637(14) 0.01303(13) -0.00056(11) 0.00101(10) -0.00119(10) Co2 0.01426(13) 0.01521(14) 0.01405(13) -0.00155(11) 0.00080(10) -0.00050(10) P1 0.0129(2) 0.0138(2) 0.0129(2) -0.0003(2) 0.00040(17) -0.0006(2) Si 0.0185(3) 0.0198(3) 0.0150(3) 0.0002(2) -0.0011(2) 0.0036(2) P2 0.0136(2) 0.0134(3) 0.0146(2) -0.0006(2) 0.00036(19) -0.00102(19) P3 0.0129(2) 0.0133(2) 0.0124(2) 0.0002(2) 0.00074(19) 0.00130(18) P4 0.0122(2) 0.0137(2) 0.0149(2) -0.0004(2) -0.00055(19) -0.00005(19) O16 0.0227(8) 0.0387(10) 0.0259(9) 0.0006(8) 0.0015(7) 0.0116(8) O17 0.0434(11) 0.0277(10) 0.0486(12) 0.0032(9) 0.0149(10) -0.0133(9) O18 0.0352(11) 0.0383(11) 0.0382(11) -0.0156(9) -0.0033(8) 0.0146(9) O19 0.0349(11) 0.0418(12) 0.0532(13) -0.0018(10) -0.0221(10) -0.0064(9) C1 0.0129(8) 0.0147(10) 0.0169(9) 0.0018(8) -0.0020(8) 0.0012(8) C2 0.0168(9) 0.0153(10) 0.0146(9) -0.0013(8) -0.0019(7) 0.0008(7) C3 0.0151(9) 0.0180(11) 0.0143(9) 0.0010(8) -0.0004(7) -0.0009(7) C4 0.0160(9) 0.0178(10) 0.0136(9) -0.0009(8) 0.0007(7) 0.0001(8) C8 0.0192(11) 0.0375(14) 0.0245(12) 0.0004(11) 0.0003(9) 0.0068(10) C9 0.0326(13) 0.0346(14) 0.0207(12) 0.0006(11) -0.0062(10) 0.0034(11) C10 0.0376(14) 0.0211(12) 0.0241(12) 0.0046(10) -0.0025(11) 0.0028(10) C54 0.0182(11) 0.0288(12) 0.0160(10) 0.0035(9) -0.0061(8) -0.0022(9) C55 0.0146(10) 0.0247(12) 0.0216(11) -0.0014(9) -0.0060(8) 0.0014(9) C51 0.0158(10) 0.0249(12) 0.0200(10) 0.0008(9) -0.0056(8) -0.0039(9) C52 0.0217(11) 0.0236(12) 0.0199(11) -0.0049(9) -0.0081(8) -0.0015(9) C53 0.0196(11) 0.0327(13) 0.0136(10) -0.0047(9) -0.0037(8) -0.0021(9) C16 0.0192(10) 0.0261(11) 0.0133(9) -0.0011(8) 0.0019(8) -0.0017(9) C17 0.0228(11) 0.0251(12) 0.0217(11) 0.0015(9) 0.0035(9) -0.0020(9) C18 0.0224(11) 0.0257(12) 0.0187(11) -0.0053(9) 0.0002(9) 0.0007(9) C19 0.0243(12) 0.0238(12) 0.0251(12) -0.0016(10) -0.0029(9) -0.0009(9) C5 0.0122(9) 0.0134(10) 0.0156(9) -0.0013(8) -0.0001(7) -0.0011(7) C111 0.0204(10) 0.0151(10) 0.0105(9) 0.0011(8) -0.0016(8) 0.0014(8) C116 0.0206(11) 0.0213(11) 0.0257(12) 0.0009(9) -0.0031(9) -0.0018(9) C115 0.0320(13) 0.0163(11) 0.0406(15) -0.0024(11) -0.0070(12) -0.0043(10) C114 0.0391(14) 0.0139(11) 0.0323(13) -0.0011(10) -0.0041(11) 0.0065(10) C113 0.0250(12) 0.0234(12) 0.0258(12) 0.0009(10) 0.0024(9) 0.0079(9) C112 0.0195(10) 0.0181(10) 0.0196(11) 0.0014(9) 0.0012(8) -0.0012(8) C121 0.0149(9) 0.0141(10) 0.0128(9) -0.0002(7) 0.0000(7) -0.0033(7) C126 0.0169(9) 0.0169(10) 0.0173(10) 0.0009(9) 0.0009(8) 0.0012(8) C125 0.0247(11) 0.0229(12) 0.0142(9) -0.0001(9) 0.0022(8) 0.0019(9) C124 0.0226(10) 0.0223(11) 0.0152(9) 0.0009(8) -0.0037(8) -0.0003(9) C123 0.0157(9) 0.0243(11) 0.0216(10) -0.0015(9) -0.0028(8) 0.0047(9) C122 0.0171(9) 0.0195(11) 0.0174(9) -0.0040(9) 0.0008(8) 0.0003(8) C221 0.0148(9) 0.0135(10) 0.0203(10) 0.0009(8) -0.0017(8) -0.0013(7) C226 0.0208(11) 0.0205(11) 0.0236(12) 0.0035(9) -0.0003(9) -0.0006(9) C225 0.0306(13) 0.0276(13) 0.0226(12) 0.0079(10) -0.0037(10) -0.0060(10) C224 0.0288(13) 0.0209(12) 0.0321(13) 0.0067(10) -0.0130(11) -0.0025(10) C223 0.0214(11) 0.0172(11) 0.0367(14) -0.0007(10) -0.0076(10) 0.0016(9) C222 0.0169(10) 0.0170(10) 0.0243(11) -0.0018(9) -0.0019(9) 0.0016(8) C211 0.0174(10) 0.0220(11) 0.0121(10) -0.0003(8) 0.0002(8) -0.0060(8) C212 0.0255(12) 0.0248(12) 0.0386(15) 0.0050(11) -0.0107(11) -0.0078(10) C213 0.0380(16) 0.0306(14) 0.0476(17) 0.0104(13) -0.0139(13) -0.0202(12) C214 0.0272(13) 0.0553(18) 0.0219(12) 0.0003(12) -0.0027(10) -0.0253(12) C215 0.0158(11) 0.0474(16) 0.0337(14) -0.0123(12) 0.0031(10) -0.0071(11) C216 0.0190(11) 0.0277(12) 0.0310(13) -0.0068(11) 0.0006(9) -0.0027(9) C311 0.0168(9) 0.0146(9) 0.0172(9) -0.0014(8) -0.0013(9) 0.0021(8) C312 0.0167(9) 0.0170(10) 0.0181(11) 0.0008(8) -0.0008(8) 0.0011(8) C313 0.0175(10) 0.0221(11) 0.0205(11) -0.0032(9) 0.0008(8) 0.0029(8) C314 0.0250(11) 0.0233(12) 0.0281(12) 0.0012(10) -0.0006(10) 0.0120(9) C315 0.0348(14) 0.0276(13) 0.0278(13) 0.0095(11) 0.0050(10) 0.0119(11) C316 0.0244(11) 0.0260(12) 0.0231(11) 0.0062(9) 0.0049(10) 0.0088(10) C331 0.0184(10) 0.0132(9) 0.0157(10) 0.0005(8) -0.0015(8) -0.0015(8) C336 0.0182(10) 0.0264(12) 0.0194(11) -0.0049(9) 0.0008(8) 0.0016(9) C335 0.0244(12) 0.0331(14) 0.0185(11) -0.0078(10) 0.0001(9) -0.0005(10) C334 0.0214(11) 0.0262(12) 0.0183(11) -0.0014(9) -0.0043(9) -0.0044(9) C333 0.0150(10) 0.0210(11) 0.0245(11) 0.0032(9) -0.0007(8) -0.0011(8) C332 0.0190(10) 0.0170(10) 0.0161(10) 0.0002(8) 0.0003(8) -0.0003(8) C321 0.0135(9) 0.0160(10) 0.0155(10) 0.0033(8) 0.0013(7) 0.0042(8) C322 0.0213(11) 0.0164(11) 0.0202(11) 0.0004(9) 0.0025(9) 0.0030(8) C323 0.0206(11) 0.0187(11) 0.0264(12) 0.0061(9) 0.0059(9) 0.0004(9) C324 0.0208(11) 0.0273(12) 0.0197(11) 0.0079(9) 0.0054(9) 0.0037(9) C325 0.0207(10) 0.0286(12) 0.0140(10) -0.0005(9) 0.0018(8) 0.0056(9) C326 0.0149(9) 0.0210(11) 0.0151(10) 0.0011(8) 0.0004(8) 0.0007(8) C411 0.0185(10) 0.0150(10) 0.0170(10) -0.0003(9) -0.0023(8) -0.0016(7) C416 0.0215(11) 0.0189(11) 0.0203(11) -0.0013(9) 0.0002(8) 0.0002(8) C415 0.0206(11) 0.0207(11) 0.0253(11) -0.0006(9) 0.0020(9) -0.0060(9) C414 0.0291(12) 0.0167(10) 0.0262(12) 0.0030(9) 0.0008(10) -0.0058(10) C413 0.0261(12) 0.0197(12) 0.0382(14) 0.0065(11) -0.0007(11) 0.0009(9) C412 0.0173(10) 0.0219(11) 0.0342(13) 0.0047(11) 0.0008(10) 0.0009(8) C421 0.0155(10) 0.0164(10) 0.0188(10) 0.0005(8) 0.0020(8) 0.0027(8) C426 0.0260(12) 0.0189(11) 0.0233(12) -0.0025(9) 0.0020(9) -0.0002(9) C425 0.0392(15) 0.0233(12) 0.0267(13) -0.0082(10) 0.0034(11) 0.0018(11) C424 0.0379(15) 0.0288(13) 0.0241(12) -0.0008(11) 0.0101(11) 0.0081(11) C423 0.0249(12) 0.0244(12) 0.0265(12) 0.0053(10) 0.0103(10) 0.0032(9) C422 0.0186(10) 0.0176(11) 0.0225(11) 0.0000(9) 0.0023(8) 0.0020(8) C431 0.0151(10) 0.0138(10) 0.0194(10) 0.0026(8) -0.0027(8) -0.0010(8) C432 0.0199(11) 0.0222(11) 0.0266(12) 0.0005(9) -0.0021(9) 0.0015(9) C433 0.0158(11) 0.0290(13) 0.0408(15) 0.0047(12) -0.0089(10) 0.0000(9) C434 0.0276(12) 0.0299(14) 0.0267(12) 0.0078(11) -0.0125(10) -0.0085(10) C435 0.0292(12) 0.0296(13) 0.0186(11) 0.0043(10) -0.0056(9) -0.0072(10) C436 0.0167(10) 0.0231(11) 0.0182(10) 0.0024(9) -0.0008(8) -0.0021(8) _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 Ru C1 2.012(2) . ? Ru C55 2.224(2) . ? Ru C51 2.230(2) . ? Ru C54 2.231(2) . ? Ru C52 2.251(2) . ? Ru C53 2.261(2) . ? Ru P3 2.2853(6) . ? Ru P4 2.2935(6) . ? Co1 C17 1.772(2) . ? Co1 C16 1.783(2) . ? Co1 C3 1.972(2) . ? Co1 C4 1.981(2) . ? Co1 P1 2.2269(6) . ? Co1 Co2 2.4947(4) . ? Co2 C19 1.773(2) . ? Co2 C18 1.794(2) . ? Co2 C4 1.986(2) . ? Co2 C3 1.990(2) . ? Co2 P2 2.2165(6) . ? P1 C121 1.834(2) . ? P1 C111 1.838(2) . ? P1 C5 1.845(2) . ? Si C4 1.851(2) . ? Si C9 1.862(3) . ? Si C10 1.862(3) . ? Si C8 1.875(2) . ? P2 C5 1.831(2) . ? P2 C221 1.833(2) . ? P2 C211 1.840(2) . ? P3 C331 1.837(2) . ? P3 C321 1.842(2) . ? P3 C311 1.853(2) . ? P4 C431 1.835(2) . ? P4 C411 1.840(2) . ? P4 C421 1.845(2) . ? O16 C16 1.150(3) . ? O17 C17 1.144(3) . ? O18 C18 1.139(3) . ? O19 C19 1.139(3) . ? C1 C2 1.223(3) . ? C2 C3 1.410(3) . ? C3 C4 1.368(3) . ? C54 C53 1.423(3) . ? C54 C55 1.436(3) . ? C55 C51 1.433(3) . ? C51 C52 1.412(3) . ? C52 C53 1.431(3) . ? C111 C112 1.397(3) . ? C111 C116 1.400(3) . ? C116 C115 1.386(3) . ? C115 C114 1.389(4) . ? C114 C113 1.386(4) . ? C113 C112 1.392(3) . ? C121 C126 1.395(3) . ? C121 C122 1.398(3) . ? C126 C125 1.387(3) . ? C125 C124 1.391(3) . ? C124 C123 1.389(3) . ? C123 C122 1.386(3) . ? C221 C222 1.396(3) . ? C221 C226 1.405(3) . ? C226 C225 1.389(3) . ? C225 C224 1.387(4) . ? C224 C223 1.389(4) . ? C223 C222 1.399(3) . ? C211 C212 1.389(3) . ? C211 C216 1.397(3) . ? C212 C213 1.390(3) . ? C213 C214 1.387(4) . ? C214 C215 1.376(4) . ? C215 C216 1.392(3) . ? C311 C316 1.398(3) . ? C311 C312 1.407(3) . ? C312 C313 1.396(3) . ? C313 C314 1.392(3) . ? C314 C315 1.378(3) . ? C315 C316 1.397(3) . ? C331 C336 1.401(3) . ? C331 C332 1.403(3) . ? C336 C335 1.392(3) . ? C335 C334 1.383(3) . ? C334 C333 1.390(3) . ? C333 C332 1.382(3) . ? C321 C326 1.394(3) . ? C321 C322 1.405(3) . ? C322 C323 1.381(3) . ? C323 C324 1.396(3) . ? C324 C325 1.380(4) . ? C325 C326 1.398(3) . ? C411 C416 1.398(3) . ? C411 C412 1.401(3) . ? C416 C415 1.395(3) . ? C415 C414 1.379(3) . ? C414 C413 1.395(4) . ? C413 C412 1.382(3) . ? C421 C422 1.394(3) . ? C421 C426 1.405(3) . ? C426 C425 1.391(3) . ? C425 C424 1.391(4) . ? C424 C423 1.386(4) . ? C423 C422 1.393(3) . ? C431 C432 1.398(3) . ? C431 C436 1.401(3) . ? C432 C433 1.393(3) . ? C433 C434 1.383(4) . ? C434 C435 1.391(4) . ? C435 C436 1.391(3) . ? 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 Ru C55 95.77(8) . . ? C1 Ru C51 88.51(8) . . ? C55 Ru C51 37.54(8) . . ? C1 Ru C54 131.63(9) . . ? C55 Ru C54 37.61(8) . . ? C51 Ru C54 62.18(8) . . ? C1 Ru C52 116.30(9) . . ? C55 Ru C52 62.18(9) . . ? C51 Ru C52 36.72(9) . . ? C54 Ru C52 61.73(9) . . ? C1 Ru C53 150.27(8) . . ? C55 Ru C53 62.41(8) . . ? C51 Ru C53 61.82(8) . . ? C54 Ru C53 36.94(9) . . ? C52 Ru C53 36.98(9) . . ? C1 Ru P3 90.87(6) . . ? C55 Ru P3 103.26(6) . . ? C51 Ru P3 140.30(6) . . ? C54 Ru P3 89.93(6) . . ? C52 Ru P3 149.29(6) . . ? C53 Ru P3 112.77(6) . . ? C1 Ru P4 92.17(6) . . ? C55 Ru P4 154.52(6) . . ? C51 Ru P4 118.91(6) . . ? C54 Ru P4 134.97(6) . . ? C52 Ru P4 92.63(6) . . ? C53 Ru P4 100.33(6) . . ? P3 Ru P4 100.78(2) . . ? C17 Co1 C16 100.54(11) . . ? C17 Co1 C3 100.44(10) . . ? C16 Co1 C3 100.77(9) . . ? C17 Co1 C4 104.03(10) . . ? C16 Co1 C4 137.05(9) . . ? C3 Co1 C4 40.49(8) . . ? C17 Co1 P1 99.69(8) . . ? C16 Co1 P1 113.21(7) . . ? C3 Co1 P1 136.15(6) . . ? C4 Co1 P1 96.74(6) . . ? C17 Co1 Co2 150.84(8) . . ? C16 Co1 Co2 92.93(7) . . ? C3 Co1 Co2 51.29(6) . . ? C4 Co1 Co2 51.11(6) . . ? P1 Co1 Co2 98.509(18) . . ? C19 Co2 C18 102.17(11) . . ? C19 Co2 C4 95.99(10) . . ? C18 Co2 C4 139.10(10) . . ? C19 Co2 C3 106.91(10) . . ? C18 Co2 C3 99.04(10) . . ? C4 Co2 C3 40.25(8) . . ? C19 Co2 P2 98.68(8) . . ? C18 Co2 P2 106.06(8) . . ? C4 Co2 P2 106.99(6) . . ? C3 Co2 P2 139.22(6) . . ? C19 Co2 Co1 146.91(8) . . ? C18 Co2 Co1 105.15(8) . . ? C4 Co2 Co1 50.95(6) . . ? C3 Co2 Co1 50.65(6) . . ? P2 Co2 Co1 91.411(18) . . ? C121 P1 C111 100.22(9) . . ? C121 P1 C5 102.38(9) . . ? C111 P1 C5 102.38(9) . . ? C121 P1 Co1 121.47(7) . . ? C111 P1 Co1 118.51(7) . . ? C5 P1 Co1 109.25(7) . . ? C4 Si C9 107.02(11) . . ? C4 Si C10 109.44(11) . . ? C9 Si C10 110.17(12) . . ? C4 Si C8 114.35(11) . . ? C9 Si C8 106.90(12) . . ? C10 Si C8 108.90(12) . . ? C5 P2 C221 102.64(10) . . ? C5 P2 C211 103.36(10) . . ? C221 P2 C211 100.48(10) . . ? C5 P2 Co2 108.53(7) . . ? C221 P2 Co2 121.68(7) . . ? C211 P2 Co2 117.80(7) . . ? C331 P3 C321 99.62(10) . . ? C331 P3 C311 104.72(10) . . ? C321 P3 C311 100.15(10) . . ? C331 P3 Ru 123.60(7) . . ? C321 P3 Ru 118.01(7) . . ? C311 P3 Ru 107.72(7) . . ? C431 P4 C411 98.39(10) . . ? C431 P4 C421 105.27(10) . . ? C411 P4 C421 101.18(10) . . ? C431 P4 Ru 124.70(7) . . ? C411 P4 Ru 114.74(7) . . ? C421 P4 Ru 109.66(7) . . ? C2 C1 Ru 166.61(18) . . ? C1 C2 C3 177.6(2) . . ? C4 C3 C2 144.7(2) . . ? C4 C3 Co1 70.13(12) . . ? C2 C3 Co1 132.96(16) . . ? C4 C3 Co2 69.72(13) . . ? C2 C3 Co2 133.21(16) . . ? Co1 C3 Co2 78.06(8) . . ? C3 C4 Si 131.45(17) . . ? C3 C4 Co1 69.38(12) . . ? Si C4 Co1 139.70(12) . . ? C3 C4 Co2 70.03(13) . . ? Si C4 Co2 137.68(12) . . ? Co1 C4 Co2 77.94(8) . . ? C53 C54 C55 108.7(2) . . ? C53 C54 Ru 72.65(13) . . ? C55 C54 Ru 70.93(12) . . ? C51 C55 C54 106.8(2) . . ? C51 C55 Ru 71.45(13) . . ? C54 C55 Ru 71.46(12) . . ? C52 C51 C55 108.6(2) . . ? C52 C51 Ru 72.46(13) . . ? C55 C51 Ru 71.01(13) . . ? C51 C52 C53 108.5(2) . . ? C51 C52 Ru 70.82(13) . . ? C53 C52 Ru 71.86(13) . . ? C54 C53 C52 107.4(2) . . ? C54 C53 Ru 70.41(12) . . ? C52 C53 Ru 71.16(12) . . ? O16 C16 Co1 173.56(19) . . ? O17 C17 Co1 178.9(2) . . ? O18 C18 Co2 177.5(2) . . ? O19 C19 Co2 178.9(3) . . ? P2 C5 P1 107.81(10) . . ? C112 C111 C116 118.2(2) . . ? C112 C111 P1 123.22(17) . . ? C116 C111 P1 118.56(17) . . ? C115 C116 C111 120.5(2) . . ? C116 C115 C114 120.7(2) . . ? C113 C114 C115 119.5(2) . . ? C114 C113 C112 119.9(2) . . ? C113 C112 C111 121.1(2) . . ? C126 C121 C122 118.64(19) . . ? C126 C121 P1 119.32(16) . . ? C122 C121 P1 122.01(16) . . ? C125 C126 C121 120.8(2) . . ? C126 C125 C124 120.0(2) . . ? C123 C124 C125 119.7(2) . . ? C122 C123 C124 120.3(2) . . ? C123 C122 C121 120.56(19) . . ? C222 C221 C226 118.4(2) . . ? C222 C221 P2 121.43(17) . . ? C226 C221 P2 120.13(17) . . ? C225 C226 C221 120.6(2) . . ? C224 C225 C226 120.3(2) . . ? C225 C224 C223 120.0(2) . . ? C224 C223 C222 119.7(2) . . ? C221 C222 C223 120.9(2) . . ? C212 C211 C216 118.4(2) . . ? C212 C211 P2 119.47(18) . . ? C216 C211 P2 121.98(18) . . ? C211 C212 C213 120.7(3) . . ? C214 C213 C212 120.5(3) . . ? C215 C214 C213 119.3(2) . . ? C214 C215 C216 120.6(3) . . ? C215 C216 C211 120.6(2) . . ? C316 C311 C312 117.9(2) . . ? C316 C311 P3 122.51(17) . . ? C312 C311 P3 119.23(16) . . ? C313 C312 C311 120.7(2) . . ? C314 C313 C312 120.4(2) . . ? C315 C314 C313 119.5(2) . . ? C314 C315 C316 120.5(2) . . ? C315 C316 C311 121.0(2) . . ? C336 C331 C332 118.2(2) . . ? C336 C331 P3 122.71(17) . . ? C332 C331 P3 119.05(16) . . ? C335 C336 C331 120.1(2) . . ? C334 C335 C336 120.8(2) . . ? C335 C334 C333 119.7(2) . . ? C332 C333 C334 119.9(2) . . ? C333 C332 C331 121.2(2) . . ? C326 C321 C322 118.4(2) . . ? C326 C321 P3 121.41(17) . . ? C322 C321 P3 120.10(16) . . ? C323 C322 C321 120.9(2) . . ? C322 C323 C324 120.1(2) . . ? C325 C324 C323 119.6(2) . . ? C324 C325 C326 120.5(2) . . ? C321 C326 C325 120.4(2) . . ? C416 C411 C412 118.9(2) . . ? C416 C411 P4 121.58(17) . . ? C412 C411 P4 119.50(16) . . ? C415 C416 C411 120.2(2) . . ? C414 C415 C416 120.4(2) . . ? C415 C414 C413 119.5(2) . . ? C412 C413 C414 120.6(2) . . ? C413 C412 C411 120.2(2) . . ? C422 C421 C426 118.4(2) . . ? C422 C421 P4 120.71(17) . . ? C426 C421 P4 120.48(17) . . ? C425 C426 C421 120.3(2) . . ? C426 C425 C424 120.8(2) . . ? C423 C424 C425 119.2(2) . . ? C424 C423 C422 120.4(2) . . ? C423 C422 C421 121.0(2) . . ? C432 C431 C436 118.8(2) . . ? C432 C431 P4 123.85(18) . . ? C436 C431 P4 117.05(16) . . ? C433 C432 C431 120.7(2) . . ? C434 C433 C432 119.8(2) . . ? C433 C434 C435 120.3(2) . . ? C434 C435 C436 120.0(2) . . ? C435 C436 C431 120.4(2) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 1.31 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.536 _refine_diff_density_min -0.229 _refine_diff_density_rms 0.061