Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Prof Andreas Roodt' _publ_contact_author_address ; Deptartment of Chemistry and Biochemistry Rand Afrikaans University P.O. Box 524 Auckland Park 2006 SOUTH AFRICA ; _publ_contact_author_email AROO@RAU.AC.ZA _publ_section_title ; Synthesis, crystal structure and hydroformylation activity of triphenylphosphite modified cobalt catalysts ; loop_ _publ_author_name 'Andreas Roodt' 'Marco Haumann' 'Reinout Meijboom' 'John Moss' data_codimer _database_code_depnum_ccdc_archive 'CCDC 232540' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H30 Co2 O12 P2' _chemical_formula_weight 906.46 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.3422(2) _cell_length_b 11.0745(2) _cell_length_c 12.0715(2) _cell_angle_alpha 63.7430(10) _cell_angle_beta 89.6420(10) _cell_angle_gamma 65.7760(10) _cell_volume 997.70(3) _cell_formula_units_Z 1 _cell_measurement_temperature 203(2) _exptl_crystal_description Cuboidal _exptl_crystal_colour 'Dark red' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas N/A _exptl_crystal_density_diffrn 1.509 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 462 _exptl_absorpt_coefficient_mu 0.975 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(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 'Nonius Kappa CCD diffractometer' _diffrn_measurement_method '1.2\% \f scans and \w scans' _diffrn_reflns_number 8620 _diffrn_reflns_av_R_equivalents 0.0262 _diffrn_reflns_av_sigmaI/netI 0.0461 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.65 _diffrn_reflns_theta_max 27.46 _reflns_number_total 4543 _reflns_number_gt 3538 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (2000)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenberg & Berndt, 1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0216P)^2^+0.2716P] 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 4543 _refine_ls_number_parameters 263 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0501 _refine_ls_R_factor_gt 0.0293 _refine_ls_wR_factor_ref 0.0640 _refine_ls_wR_factor_gt 0.0583 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co Co 0.92780(3) 0.54815(2) 0.38297(2) 0.02227(8) Uani 1 d . . . P P 0.80330(5) 0.62460(5) 0.20029(4) 0.02237(10) Uani 1 d . . . C1 C 0.9735(2) 0.7031(2) 0.33644(17) 0.0319(4) Uani 1 d . . . C2 C 1.0825(2) 0.3755(2) 0.39866(16) 0.0294(4) Uani 1 d . . . C3 C 0.7589(2) 0.5504(2) 0.45280(17) 0.0348(4) Uani 1 d . . . O11 O 0.90407(13) 0.60245(13) 0.09712(11) 0.0267(3) Uani 1 d . . . O13 O 0.68148(13) 0.80086(13) 0.11752(11) 0.0295(3) Uani 1 d . . . O12 O 0.68800(13) 0.55534(13) 0.18791(11) 0.0274(3) Uani 1 d . . . O1 O 1.00229(19) 0.80318(17) 0.30550(14) 0.0512(4) Uani 1 d . . . O2 O 1.18288(17) 0.26683(15) 0.40703(13) 0.0456(4) Uani 1 d . . . O3 O 0.64961(17) 0.5511(2) 0.49681(15) 0.0583(4) Uani 1 d . . . C11 C 1.0374(2) 0.6325(2) 0.07662(15) 0.0258(4) Uani 1 d . . . C21 C 0.7260(2) 0.4014(2) 0.26194(16) 0.0264(4) Uani 1 d . . . C31 C 0.5657(2) 0.87905(18) 0.16866(16) 0.0268(4) Uani 1 d . . . C16 C 1.1843(2) 0.5123(2) 0.10192(17) 0.0334(4) Uani 1 d . . . H16 H 1.1950 0.4139 0.1347 0.040 Uiso 1 calc R . . C22 C 0.8530(2) 0.2914(2) 0.24916(18) 0.0343(4) Uani 1 d . . . H22 H 0.9200 0.3166 0.1943 0.041 Uiso 1 calc R . . C12 C 1.0180(2) 0.7773(2) 0.02720(18) 0.0359(4) Uani 1 d . . . H12 H 0.9162 0.8581 0.0089 0.043 Uiso 1 calc R . . C26 C 0.6247(2) 0.3683(2) 0.33951(19) 0.0390(5) Uani 1 d . . . H26 H 0.5379 0.4452 0.3463 0.047 Uiso 1 calc R . . C32 C 0.4367(2) 0.8505(2) 0.19565(19) 0.0365(4) Uani 1 d . . . H32 H 0.4262 0.7761 0.1835 0.044 Uiso 1 calc R . . C36 C 0.5827(2) 0.9878(2) 0.1847(2) 0.0395(5) Uani 1 d . . . H36 H 0.6715 1.0067 0.1654 0.047 Uiso 1 calc R . . C14 C 1.2997(2) 0.6844(3) 0.0300(2) 0.0449(5) Uani 1 d . . . H14 H 1.3898 0.7021 0.0147 0.054 Uiso 1 calc R . . C33 C 0.3219(2) 0.9329(2) 0.2412(2) 0.0465(5) Uani 1 d . . . H33 H 0.2331 0.9140 0.2603 0.056 Uiso 1 calc R . . C34 C 0.3369(3) 1.0418(2) 0.2585(2) 0.0471(5) Uani 1 d . . . H34 H 0.2588 1.0971 0.2897 0.057 Uiso 1 calc R . . C35 C 0.4660(3) 1.0696(2) 0.2302(2) 0.0498(6) Uani 1 d . . . H35 H 0.4759 1.1447 0.2417 0.060 Uiso 1 calc R . . C23 C 0.8800(3) 0.1431(2) 0.3187(2) 0.0464(5) Uani 1 d . . . H23 H 0.9671 0.0662 0.3121 0.056 Uiso 1 calc R . . C13 C 1.1512(3) 0.8023(3) 0.0048(2) 0.0463(5) Uani 1 d . . . H13 H 1.1402 0.9008 -0.0281 0.056 Uiso 1 calc R . . C15 C 1.3159(2) 0.5401(3) 0.07775(19) 0.0418(5) Uani 1 d . . . H15 H 1.4172 0.4597 0.0941 0.050 Uiso 1 calc R . . C24 C 0.7804(3) 0.1071(3) 0.3974(2) 0.0525(6) Uani 1 d . . . H24 H 0.7993 0.0061 0.4443 0.063 Uiso 1 calc R . . C25 C 0.6527(3) 0.2195(3) 0.4075(2) 0.0533(6) Uani 1 d . . . H25 H 0.5843 0.1948 0.4610 0.064 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co 0.02420(13) 0.02237(13) 0.02026(13) -0.01145(10) 0.00378(9) -0.00929(10) P 0.0227(2) 0.0226(2) 0.0203(2) -0.01100(18) 0.00358(16) -0.00834(18) C1 0.0382(10) 0.0310(10) 0.0250(9) -0.0141(8) 0.0034(8) -0.0137(9) C2 0.0364(10) 0.0301(10) 0.0221(9) -0.0131(8) 0.0039(7) -0.0150(9) C3 0.0347(11) 0.0446(11) 0.0271(10) -0.0199(9) 0.0032(8) -0.0167(9) O11 0.0284(6) 0.0330(7) 0.0253(6) -0.0186(5) 0.0094(5) -0.0149(5) O13 0.0294(7) 0.0231(6) 0.0246(6) -0.0087(5) 0.0046(5) -0.0050(5) O12 0.0254(6) 0.0278(6) 0.0276(6) -0.0125(5) 0.0014(5) -0.0118(5) O1 0.0745(11) 0.0398(8) 0.0479(9) -0.0179(7) 0.0087(8) -0.0371(8) O2 0.0496(9) 0.0316(8) 0.0450(9) -0.0233(7) 0.0042(7) -0.0038(7) O3 0.0387(8) 0.1019(14) 0.0480(9) -0.0426(10) 0.0226(7) -0.0369(9) C11 0.0277(9) 0.0328(10) 0.0209(8) -0.0162(8) 0.0084(7) -0.0137(8) C21 0.0298(9) 0.0301(9) 0.0225(9) -0.0131(7) 0.0022(7) -0.0158(8) C31 0.0259(9) 0.0219(9) 0.0228(9) -0.0086(7) 0.0011(7) -0.0048(7) C16 0.0334(10) 0.0316(10) 0.0292(10) -0.0144(8) 0.0083(8) -0.0100(8) C22 0.0359(10) 0.0370(11) 0.0375(11) -0.0224(9) 0.0104(8) -0.0183(9) C12 0.0369(11) 0.0342(11) 0.0402(11) -0.0219(9) 0.0151(8) -0.0151(9) C26 0.0390(11) 0.0458(12) 0.0392(11) -0.0223(10) 0.0150(9) -0.0236(10) C32 0.0305(10) 0.0345(11) 0.0487(12) -0.0257(9) 0.0056(8) -0.0121(8) C36 0.0332(10) 0.0255(10) 0.0560(13) -0.0180(9) 0.0056(9) -0.0117(8) C14 0.0421(12) 0.0703(16) 0.0476(13) -0.0387(12) 0.0217(10) -0.0364(12) C33 0.0317(11) 0.0457(13) 0.0617(15) -0.0289(11) 0.0156(10) -0.0140(10) C34 0.0427(12) 0.0403(12) 0.0535(14) -0.0299(11) 0.0116(10) -0.0067(10) C35 0.0498(13) 0.0341(12) 0.0682(16) -0.0325(11) 0.0032(11) -0.0128(10) C23 0.0506(13) 0.0344(12) 0.0550(14) -0.0242(10) 0.0064(10) -0.0171(10) C13 0.0595(14) 0.0475(13) 0.0557(14) -0.0335(11) 0.0280(11) -0.0356(11) C15 0.0283(10) 0.0528(13) 0.0370(11) -0.0234(10) 0.0079(8) -0.0102(9) C24 0.0687(16) 0.0364(12) 0.0485(14) -0.0109(10) 0.0012(11) -0.0309(12) C25 0.0622(15) 0.0605(15) 0.0440(13) -0.0178(12) 0.0202(11) -0.0418(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co C3 1.780(2) . ? Co C1 1.785(2) . ? Co C2 1.7874(19) . ? Co P 2.1224(4) . ? Co Co 2.6722(4) 2_766 ? P O12 1.5977(12) . ? P O11 1.6012(12) . ? P O13 1.6029(11) . ? C1 O1 1.148(2) . ? C2 O2 1.143(2) . ? C3 O3 1.147(2) . ? O11 C11 1.409(2) . ? O13 C31 1.413(2) . ? O12 C21 1.411(2) . ? C11 C12 1.371(3) . ? C11 C16 1.377(2) . ? C21 C26 1.370(3) . ? C21 C22 1.376(2) . ? C31 C32 1.370(3) . ? C31 C36 1.370(3) . ? C16 C15 1.385(3) . ? C22 C23 1.382(3) . ? C12 C13 1.382(3) . ? C26 C25 1.381(3) . ? C32 C33 1.385(3) . ? C36 C35 1.391(3) . ? C14 C13 1.374(3) . ? C14 C15 1.376(3) . ? C33 C34 1.371(3) . ? C34 C35 1.369(3) . ? C23 C24 1.372(3) . ? C24 C25 1.379(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 C3 Co C1 119.61(9) . . ? C3 Co C2 120.61(9) . . ? C1 Co C2 117.47(8) . . ? C3 Co P 93.88(6) . . ? C1 Co P 95.48(6) . . ? C2 Co P 95.87(6) . . ? C3 Co Co 83.44(6) . 2_766 ? C1 Co Co 85.98(6) . 2_766 ? C2 Co Co 85.42(5) . 2_766 ? P Co Co 177.319(19) . 2_766 ? O12 P O11 98.57(6) . . ? O12 P O13 99.18(6) . . ? O11 P O13 99.00(6) . . ? O12 P Co 118.79(5) . . ? O11 P Co 119.18(5) . . ? O13 P Co 118.00(5) . . ? O1 C1 Co 179.43(17) . . ? O2 C2 Co 178.57(17) . . ? O3 C3 Co 179.11(17) . . ? C11 O11 P 123.16(10) . . ? C31 O13 P 121.59(10) . . ? C21 O12 P 123.29(10) . . ? C12 C11 C16 122.04(17) . . ? C12 C11 O11 120.61(15) . . ? C16 C11 O11 117.27(16) . . ? C26 C21 C22 121.97(18) . . ? C26 C21 O12 117.10(16) . . ? C22 C21 O12 120.77(16) . . ? C32 C31 C36 121.48(17) . . ? C32 C31 O13 120.22(16) . . ? C36 C31 O13 118.23(16) . . ? C11 C16 C15 118.28(18) . . ? C21 C22 C23 118.59(19) . . ? C11 C12 C13 118.66(18) . . ? C21 C26 C25 118.60(19) . . ? C31 C32 C33 118.96(18) . . ? C31 C36 C35 118.69(19) . . ? C13 C14 C15 119.74(19) . . ? C34 C33 C32 120.6(2) . . ? C35 C34 C33 119.71(19) . . ? C34 C35 C36 120.60(19) . . ? C24 C23 C22 120.5(2) . . ? C14 C13 C12 120.6(2) . . ? C14 C15 C16 120.67(18) . . ? C23 C24 C25 119.9(2) . . ? C24 C25 C26 120.5(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3 Co P O12 -42.25(8) . . . . ? C1 Co P O12 -162.51(8) . . . . ? C2 Co P O12 79.08(8) . . . . ? Co Co P O12 -39.6(4) 2_766 . . . ? C3 Co P O11 -162.36(8) . . . . ? C1 Co P O11 77.38(8) . . . . ? C2 Co P O11 -41.03(8) . . . . ? Co Co P O11 -159.7(4) 2_766 . . . ? C3 Co P O13 77.65(8) . . . . ? C1 Co P O13 -42.61(8) . . . . ? C2 Co P O13 -161.02(8) . . . . ? Co Co P O13 80.3(4) 2_766 . . . ? C3 Co C1 O1 -97(16) . . . . ? C2 Co C1 O1 100(16) . . . . ? P Co C1 O1 0(16) . . . . ? Co Co C1 O1 -178(100) 2_766 . . . ? C3 Co C2 O2 174(6) . . . . ? C1 Co C2 O2 -23(6) . . . . ? P Co C2 O2 76(6) . . . . ? Co Co C2 O2 -106(6) 2_766 . . . ? C1 Co C3 O3 136(11) . . . . ? C2 Co C3 O3 -62(11) . . . . ? P Co C3 O3 37(11) . . . . ? Co Co C3 O3 -143(11) 2_766 . . . ? O12 P O11 C11 -173.75(12) . . . . ? O13 P O11 C11 85.46(13) . . . . ? Co P O11 C11 -43.81(13) . . . . ? O12 P O13 C31 81.38(13) . . . . ? O11 P O13 C31 -178.35(12) . . . . ? Co P O13 C31 -48.31(13) . . . . ? O11 P O12 C21 90.78(13) . . . . ? O13 P O12 C21 -168.58(12) . . . . ? Co P O12 C21 -39.41(14) . . . . ? P O11 C11 C12 -67.09(19) . . . . ? P O11 C11 C16 116.23(15) . . . . ? P O12 C21 C26 118.38(15) . . . . ? P O12 C21 C22 -66.07(19) . . . . ? P O13 C31 C32 -70.42(19) . . . . ? P O13 C31 C36 112.46(16) . . . . ? C12 C11 C16 C15 0.9(3) . . . . ? O11 C11 C16 C15 177.50(15) . . . . ? C26 C21 C22 C23 -1.2(3) . . . . ? O12 C21 C22 C23 -176.50(16) . . . . ? C16 C11 C12 C13 -1.4(3) . . . . ? O11 C11 C12 C13 -177.89(16) . . . . ? C22 C21 C26 C25 0.6(3) . . . . ? O12 C21 C26 C25 176.12(17) . . . . ? C36 C31 C32 C33 -0.5(3) . . . . ? O13 C31 C32 C33 -177.55(17) . . . . ? C32 C31 C36 C35 0.4(3) . . . . ? O13 C31 C36 C35 177.46(17) . . . . ? C31 C32 C33 C34 0.2(3) . . . . ? C32 C33 C34 C35 0.2(3) . . . . ? C33 C34 C35 C36 -0.4(3) . . . . ? C31 C36 C35 C34 0.1(3) . . . . ? C21 C22 C23 C24 0.9(3) . . . . ? C15 C14 C13 C12 0.1(3) . . . . ? C11 C12 C13 C14 0.8(3) . . . . ? C13 C14 C15 C16 -0.7(3) . . . . ? C11 C16 C15 C14 0.2(3) . . . . ? C22 C23 C24 C25 -0.2(3) . . . . ? C23 C24 C25 C26 -0.4(3) . . . . ? C21 C26 C25 C24 0.2(3) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.271 _refine_diff_density_min -0.285 #===END data_cohydride _database_code_depnum_ccdc_archive 'CCDC 232541' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H30 Co O8 P2' _chemical_formula_weight 735.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.8233(5) _cell_length_b 10.6474(6) _cell_length_c 18.5277(11) _cell_angle_alpha 80.813(4) _cell_angle_beta 81.284(4) _cell_angle_gamma 64.028(4) _cell_volume 1712.52(17) _cell_formula_units_Z 2 _cell_measurement_temperature 201(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Cuboidal _exptl_crystal_colour brown _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.426 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 758 _exptl_absorpt_coefficient_mu 0.648 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 201(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 'Siemens Smart CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean '512 x 512' _diffrn_standards_number 0 _diffrn_standards_interval_count 'First 80 frames repeated after collection' _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 16026 _diffrn_reflns_av_R_equivalents 0.0557 _diffrn_reflns_av_sigmaI/netI 0.1135 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.12 _diffrn_reflns_theta_max 28.35 _reflns_number_total 8502 _reflns_number_gt 4758 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenberg & Berndt, 1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0370P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8502 _refine_ls_number_parameters 446 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1147 _refine_ls_R_factor_gt 0.0489 _refine_ls_wR_factor_ref 0.0983 _refine_ls_wR_factor_gt 0.0825 _refine_ls_goodness_of_fit_ref 0.908 _refine_ls_restrained_S_all 0.908 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co Co 0.44410(4) 0.23293(4) 0.26475(2) 0.02399(11) Uani 1 d . . . P1 P 0.36053(8) 0.19181(8) 0.37338(4) 0.02364(17) Uani 1 d . . . P2 P 0.31666(8) 0.24142(8) 0.18078(4) 0.02467(17) Uani 1 d . . . H1 H 0.313(4) 0.367(4) 0.2719(19) 0.075(11) Uiso 1 d . . . C1 C 0.6068(3) 0.0734(3) 0.25727(16) 0.0317(7) Uani 1 d . . . C2 C 0.5453(3) 0.3392(3) 0.25127(16) 0.0335(7) Uani 1 d . . . O1 O 0.7191(2) -0.0276(2) 0.25381(13) 0.0504(6) Uani 1 d . . . O2 O 0.6108(3) 0.4077(2) 0.24393(13) 0.0519(6) Uani 1 d . . . O11 O 0.1804(2) 0.26815(19) 0.39916(11) 0.0297(5) Uani 1 d . . . O12 O 0.3894(2) 0.03403(19) 0.40748(11) 0.0304(5) Uani 1 d . . . O13 O 0.42050(19) 0.22910(19) 0.44038(10) 0.0266(4) Uani 1 d . . . O21 O 0.3557(2) 0.1112(2) 0.13528(11) 0.0318(5) Uani 1 d . . . O22 O 0.13953(19) 0.2753(2) 0.20335(10) 0.0289(5) Uani 1 d . . . O23 O 0.3064(2) 0.35744(19) 0.10995(10) 0.0298(5) Uani 1 d . . . C11 C 0.0990(3) 0.4151(3) 0.38651(16) 0.0284(7) Uani 1 d . . . C12 C -0.0095(3) 0.4683(3) 0.33776(17) 0.0382(8) Uani 1 d . . . H12 H -0.0271 0.4087 0.3126 0.046 Uiso 1 calc R . . C13 C -0.0934(3) 0.6134(4) 0.32644(18) 0.0448(9) Uani 1 d . . . H13 H -0.1670 0.6510 0.2932 0.054 Uiso 1 calc R . . C14 C -0.0677(4) 0.7017(3) 0.3643(2) 0.0460(9) Uani 1 d . . . H14 H -0.1230 0.7985 0.3564 0.055 Uiso 1 calc R . . C15 C 0.0398(4) 0.6454(3) 0.4136(2) 0.0477(9) Uani 1 d . . . H15 H 0.0568 0.7045 0.4394 0.057 Uiso 1 calc R . . C16 C 0.1236(3) 0.5015(3) 0.42554(18) 0.0399(8) Uani 1 d . . . H16 H 0.1956 0.4638 0.4596 0.048 Uiso 1 calc R . . C21 C 0.3746(3) -0.0652(3) 0.37160(16) 0.0273(7) Uani 1 d . . . C22 C 0.4946(3) -0.1953(3) 0.37139(17) 0.0335(7) Uani 1 d . . . H22 H 0.5837 -0.2130 0.3911 0.040 Uiso 1 calc R . . C23 C 0.4814(4) -0.3000(3) 0.34142(19) 0.0426(8) Uani 1 d . . . H23 H 0.5624 -0.3885 0.3409 0.051 Uiso 1 calc R . . C24 C 0.3498(4) -0.2748(3) 0.31238(18) 0.0426(8) Uani 1 d . . . H24 H 0.3416 -0.3456 0.2923 0.051 Uiso 1 calc R . . C25 C 0.2300(4) -0.1432(3) 0.31329(18) 0.0417(8) Uani 1 d . . . H25 H 0.1403 -0.1263 0.2944 0.050 Uiso 1 calc R . . C26 C 0.2416(3) -0.0356(3) 0.34211(17) 0.0347(7) Uani 1 d . . . H26 H 0.1619 0.0538 0.3415 0.042 Uiso 1 calc R . . C31 C 0.5697(3) 0.2161(3) 0.43707(15) 0.0241(6) Uani 1 d . . . C32 C 0.5878(3) 0.3363(3) 0.44057(17) 0.0326(7) Uani 1 d . . . H32 H 0.5038 0.4226 0.4428 0.039 Uiso 1 calc R . . C33 C 0.7329(4) 0.3263(4) 0.44072(18) 0.0416(8) Uani 1 d . . . H33 H 0.7467 0.4065 0.4432 0.050 Uiso 1 calc R . . C34 C 0.8566(4) 0.1992(4) 0.43731(18) 0.0434(9) Uani 1 d . . . H34 H 0.9538 0.1934 0.4373 0.052 Uiso 1 calc R . . C35 C 0.8367(3) 0.0790(3) 0.43385(18) 0.0403(8) Uani 1 d . . . H35 H 0.9205 -0.0073 0.4315 0.048 Uiso 1 calc R . . C36 C 0.6917(3) 0.0882(3) 0.43398(16) 0.0323(7) Uani 1 d . . . H36 H 0.6774 0.0081 0.4320 0.039 Uiso 1 calc R . . C41 C 0.5037(3) 0.0137(3) 0.11477(16) 0.0258(6) Uani 1 d . . . C42 C 0.5924(3) 0.0506(3) 0.05950(17) 0.0375(8) Uani 1 d . . . H42 H 0.5578 0.1422 0.0368 0.045 Uiso 1 calc R . . C43 C 0.7343(4) -0.0498(4) 0.03776(19) 0.0489(9) Uani 1 d . . . H43 H 0.7966 -0.0258 0.0007 0.059 Uiso 1 calc R . . C44 C 0.7835(4) -0.1861(4) 0.0713(2) 0.0543(10) Uani 1 d . . . H44 H 0.8783 -0.2542 0.0562 0.065 Uiso 1 calc R . . C45 C 0.6924(4) -0.2207(3) 0.1267(2) 0.0513(10) Uani 1 d . . . H45 H 0.7262 -0.3123 0.1493 0.062 Uiso 1 calc R . . C46 C 0.5505(3) -0.1207(3) 0.14951(18) 0.0387(8) Uani 1 d . . . H46 H 0.4886 -0.1438 0.1872 0.046 Uiso 1 calc R . . C51 C 0.0425(3) 0.2714(3) 0.15588(16) 0.0297(7) Uani 1 d . . . C52 C 0.0133(3) 0.1539(3) 0.16415(19) 0.0411(8) Uani 1 d . . . H52 H 0.0595 0.0789 0.1989 0.049 Uiso 1 calc R . . C53 C -0.0862(4) 0.1496(4) 0.1196(2) 0.0489(9) Uani 1 d . . . H53 H -0.1065 0.0710 0.1244 0.059 Uiso 1 calc R . . C54 C -0.1549(3) 0.2613(4) 0.0685(2) 0.0468(9) Uani 1 d . . . H54 H -0.2206 0.2578 0.0384 0.056 Uiso 1 calc R . . C55 C -0.1260(3) 0.3780(4) 0.06208(19) 0.0464(9) Uani 1 d . . . H55 H -0.1738 0.4537 0.0280 0.056 Uiso 1 calc R . . C56 C -0.0268(3) 0.3844(3) 0.10567(18) 0.0389(8) Uani 1 d . . . H56 H -0.0074 0.4635 0.1011 0.047 Uiso 1 calc R . . C61 C 0.2956(3) 0.4908(3) 0.11829(15) 0.0279(7) Uani 1 d . . . C62 C 0.4167(4) 0.5213(3) 0.08988(17) 0.0370(8) Uani 1 d . . . H62 H 0.5049 0.4536 0.0687 0.044 Uiso 1 calc R . . C63 C 0.4050(4) 0.6542(4) 0.09334(18) 0.0450(9) Uani 1 d . . . H63 H 0.4863 0.6760 0.0745 0.054 Uiso 1 calc R . . C64 C 0.2755(4) 0.7542(4) 0.12414(19) 0.0498(9) Uani 1 d . . . H64 H 0.2686 0.8437 0.1256 0.060 Uiso 1 calc R . . C65 C 0.1558(4) 0.7227(3) 0.15286(19) 0.0449(9) Uani 1 d . . . H65 H 0.0677 0.7911 0.1737 0.054 Uiso 1 calc R . . C66 C 0.1653(3) 0.5893(3) 0.15096(17) 0.0363(7) Uani 1 d . . . H66 H 0.0852 0.5669 0.1714 0.044 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co 0.0236(2) 0.0224(2) 0.0254(2) -0.00289(17) -0.00458(17) -0.00841(18) P1 0.0229(4) 0.0228(4) 0.0268(4) -0.0048(3) -0.0025(3) -0.0105(3) P2 0.0223(4) 0.0239(4) 0.0261(4) -0.0065(3) -0.0033(3) -0.0067(3) C1 0.0348(17) 0.0335(19) 0.0284(17) -0.0053(14) -0.0070(14) -0.0141(16) C2 0.0394(18) 0.0349(19) 0.0276(17) -0.0031(14) -0.0034(14) -0.0172(16) O1 0.0381(13) 0.0375(14) 0.0593(17) -0.0106(12) -0.0124(12) 0.0031(12) O2 0.0667(17) 0.0513(16) 0.0558(16) -0.0038(13) -0.0057(13) -0.0422(14) O11 0.0250(10) 0.0270(12) 0.0389(12) -0.0074(9) 0.0024(9) -0.0132(9) O12 0.0383(11) 0.0237(11) 0.0321(12) -0.0008(9) -0.0057(9) -0.0156(10) O13 0.0245(10) 0.0315(12) 0.0257(11) -0.0074(9) -0.0006(8) -0.0127(9) O21 0.0228(10) 0.0312(12) 0.0423(13) -0.0165(10) -0.0044(9) -0.0076(9) O22 0.0224(10) 0.0356(12) 0.0276(11) -0.0098(9) -0.0047(8) -0.0084(9) O23 0.0365(11) 0.0277(11) 0.0250(11) -0.0036(9) -0.0063(9) -0.0121(10) C11 0.0210(15) 0.0289(17) 0.0336(18) -0.0058(14) 0.0040(13) -0.0103(13) C12 0.0280(16) 0.047(2) 0.0383(19) -0.0157(16) -0.0008(14) -0.0114(16) C13 0.0295(17) 0.050(2) 0.040(2) -0.0103(17) -0.0072(15) -0.0001(16) C14 0.0390(19) 0.031(2) 0.053(2) -0.0036(17) -0.0031(17) -0.0019(16) C15 0.044(2) 0.032(2) 0.067(3) -0.0126(18) -0.0126(19) -0.0109(17) C16 0.0329(17) 0.035(2) 0.050(2) -0.0100(16) -0.0076(16) -0.0092(15) C21 0.0340(16) 0.0254(16) 0.0259(16) -0.0027(13) 0.0017(13) -0.0170(14) C22 0.0342(17) 0.0249(17) 0.0392(19) 0.0005(14) -0.0059(14) -0.0109(14) C23 0.052(2) 0.0200(17) 0.050(2) -0.0024(15) -0.0037(17) -0.0112(16) C24 0.061(2) 0.0305(19) 0.043(2) -0.0042(16) -0.0040(18) -0.0250(18) C25 0.046(2) 0.040(2) 0.051(2) -0.0059(17) -0.0095(17) -0.0266(17) C26 0.0314(16) 0.0265(17) 0.045(2) -0.0055(15) -0.0039(15) -0.0102(14) C31 0.0244(15) 0.0284(17) 0.0215(15) -0.0034(12) -0.0033(12) -0.0123(13) C32 0.0337(17) 0.0259(17) 0.0388(19) -0.0042(14) -0.0066(14) -0.0119(14) C33 0.045(2) 0.044(2) 0.048(2) -0.0089(17) -0.0072(17) -0.0280(18) C34 0.0281(17) 0.060(2) 0.050(2) -0.0083(18) -0.0050(15) -0.0252(18) C35 0.0270(17) 0.041(2) 0.047(2) -0.0051(17) -0.0086(15) -0.0077(15) C36 0.0328(17) 0.0326(18) 0.0333(18) -0.0027(14) -0.0054(14) -0.0152(15) C41 0.0230(14) 0.0259(16) 0.0289(16) -0.0111(13) -0.0041(13) -0.0075(13) C42 0.0380(18) 0.041(2) 0.0322(18) -0.0034(15) -0.0013(15) -0.0161(16) C43 0.037(2) 0.065(3) 0.045(2) -0.016(2) 0.0125(17) -0.024(2) C44 0.0290(18) 0.058(3) 0.065(3) -0.032(2) -0.0032(19) -0.0006(18) C45 0.050(2) 0.0235(19) 0.070(3) -0.0106(18) -0.016(2) -0.0010(17) C46 0.0397(19) 0.0322(19) 0.047(2) -0.0072(16) -0.0015(16) -0.0178(16) C51 0.0212(15) 0.0356(18) 0.0320(17) -0.0141(15) -0.0011(13) -0.0087(14) C52 0.0350(18) 0.039(2) 0.049(2) -0.0005(16) -0.0135(16) -0.0133(16) C53 0.041(2) 0.055(2) 0.063(3) -0.014(2) -0.0068(18) -0.0280(19) C54 0.0268(17) 0.060(2) 0.056(2) -0.025(2) -0.0083(16) -0.0126(17) C55 0.0338(18) 0.050(2) 0.051(2) -0.0059(18) -0.0149(16) -0.0100(17) C56 0.0342(17) 0.0359(19) 0.045(2) -0.0056(16) -0.0138(15) -0.0097(15) C61 0.0318(16) 0.0275(17) 0.0217(15) 0.0011(13) -0.0085(13) -0.0094(14) C62 0.0401(19) 0.038(2) 0.0287(18) 0.0057(15) -0.0063(15) -0.0150(16) C63 0.057(2) 0.054(2) 0.035(2) 0.0082(17) -0.0096(17) -0.035(2) C64 0.075(3) 0.037(2) 0.046(2) 0.0039(17) -0.024(2) -0.028(2) C65 0.047(2) 0.034(2) 0.047(2) -0.0103(17) -0.0139(17) -0.0062(17) C66 0.0380(18) 0.0376(19) 0.0359(19) -0.0049(15) -0.0044(15) -0.0178(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co C1 1.758(3) . ? Co C2 1.775(3) . ? Co P2 2.1076(8) . ? Co P1 2.1093(8) . ? Co H1 1.45(3) . ? P1 O12 1.6124(19) . ? P1 O11 1.6210(18) . ? P1 O13 1.6215(18) . ? P2 O21 1.6094(18) . ? P2 O22 1.6156(18) . ? P2 O23 1.635(2) . ? C1 O1 1.157(3) . ? C2 O2 1.147(3) . ? O11 C11 1.410(3) . ? O12 C21 1.402(3) . ? O13 C31 1.403(3) . ? O21 C41 1.404(3) . ? O22 C51 1.408(3) . ? O23 C61 1.408(3) . ? C11 C12 1.369(4) . ? C11 C16 1.374(4) . ? C12 C13 1.394(4) . ? C12 H12 0.9300 . ? C13 C14 1.383(4) . ? C13 H13 0.9300 . ? C14 C15 1.368(4) . ? C14 H14 0.9300 . ? C15 C16 1.383(4) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C21 C22 1.371(4) . ? C21 C26 1.381(4) . ? C22 C23 1.384(4) . ? C22 H22 0.9300 . ? C23 C24 1.376(4) . ? C23 H23 0.9300 . ? C24 C25 1.380(4) . ? C24 H24 0.9300 . ? C25 C26 1.393(4) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C31 C36 1.367(4) . ? C31 C32 1.379(4) . ? C32 C33 1.383(4) . ? C32 H32 0.9300 . ? C33 C34 1.369(4) . ? C33 H33 0.9300 . ? C34 C35 1.388(4) . ? C34 H34 0.9300 . ? C35 C36 1.384(4) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C41 C42 1.365(4) . ? C41 C46 1.376(4) . ? C42 C43 1.382(4) . ? C42 H42 0.9300 . ? C43 C44 1.384(5) . ? C43 H43 0.9300 . ? C44 C45 1.372(5) . ? C44 H44 0.9300 . ? C45 C46 1.386(4) . ? C45 H45 0.9300 . ? C46 H46 0.9300 . ? C51 C56 1.376(4) . ? C51 C52 1.382(4) . ? C52 C53 1.391(4) . ? C52 H52 0.9300 . ? C53 C54 1.378(5) . ? C53 H53 0.9300 . ? C54 C55 1.374(5) . ? C54 H54 0.9300 . ? C55 C56 1.386(4) . ? C55 H55 0.9300 . ? C56 H56 0.9300 . ? C61 C62 1.375(4) . ? C61 C66 1.378(4) . ? C62 C63 1.380(4) . ? C62 H62 0.9300 . ? C63 C64 1.366(5) . ? C63 H63 0.9300 . ? C64 C65 1.370(5) . ? C64 H64 0.9300 . ? C65 C66 1.388(4) . ? C65 H65 0.9300 . ? C66 H66 0.9300 . ? 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 Co C2 95.25(13) . . ? C1 Co P2 103.66(9) . . ? C2 Co P2 118.87(10) . . ? C1 Co P1 98.91(10) . . ? C2 Co P1 116.94(10) . . ? P2 Co P1 116.54(3) . . ? C1 Co H1 177.9(13) . . ? C2 Co H1 82.9(13) . . ? P2 Co H1 78.2(13) . . ? P1 Co H1 81.1(14) . . ? O12 P1 O11 97.86(10) . . ? O12 P1 O13 96.22(10) . . ? O11 P1 O13 97.07(9) . . ? O12 P1 Co 120.93(8) . . ? O11 P1 Co 120.46(8) . . ? O13 P1 Co 118.86(7) . . ? O21 P2 O22 96.58(9) . . ? O21 P2 O23 96.89(11) . . ? O22 P2 O23 101.76(10) . . ? O21 P2 Co 123.72(8) . . ? O22 P2 Co 116.90(8) . . ? O23 P2 Co 116.65(7) . . ? O1 C1 Co 175.6(2) . . ? O2 C2 Co 178.7(3) . . ? C11 O11 P1 120.85(16) . . ? C21 O12 P1 125.67(18) . . ? C31 O13 P1 121.55(15) . . ? C41 O21 P2 124.38(15) . . ? C51 O22 P2 124.05(16) . . ? C61 O23 P2 121.22(17) . . ? C12 C11 C16 121.3(3) . . ? C12 C11 O11 118.5(2) . . ? C16 C11 O11 120.1(3) . . ? C11 C12 C13 118.9(3) . . ? C11 C12 H12 120.6 . . ? C13 C12 H12 120.6 . . ? C14 C13 C12 120.4(3) . . ? C14 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C15 C14 C13 119.4(3) . . ? C15 C14 H14 120.3 . . ? C13 C14 H14 120.3 . . ? C14 C15 C16 120.8(3) . . ? C14 C15 H15 119.6 . . ? C16 C15 H15 119.6 . . ? C11 C16 C15 119.2(3) . . ? C11 C16 H16 120.4 . . ? C15 C16 H16 120.4 . . ? C22 C21 C26 121.8(3) . . ? C22 C21 O12 116.8(3) . . ? C26 C21 O12 121.3(3) . . ? C21 C22 C23 119.1(3) . . ? C21 C22 H22 120.5 . . ? C23 C22 H22 120.5 . . ? C24 C23 C22 120.8(3) . . ? C24 C23 H23 119.6 . . ? C22 C23 H23 119.6 . . ? C23 C24 C25 119.3(3) . . ? C23 C24 H24 120.3 . . ? C25 C24 H24 120.3 . . ? C24 C25 C26 120.9(3) . . ? C24 C25 H25 119.6 . . ? C26 C25 H25 119.6 . . ? C21 C26 C25 118.2(3) . . ? C21 C26 H26 120.9 . . ? C25 C26 H26 120.9 . . ? C36 C31 C32 121.4(3) . . ? C36 C31 O13 121.1(2) . . ? C32 C31 O13 117.4(2) . . ? C31 C32 C33 118.9(3) . . ? C31 C32 H32 120.5 . . ? C33 C32 H32 120.5 . . ? C34 C33 C32 120.5(3) . . ? C34 C33 H33 119.8 . . ? C32 C33 H33 119.8 . . ? C33 C34 C35 120.0(3) . . ? C33 C34 H34 120.0 . . ? C35 C34 H34 120.0 . . ? C36 C35 C34 119.8(3) . . ? C36 C35 H35 120.1 . . ? C34 C35 H35 120.1 . . ? C31 C36 C35 119.4(3) . . ? C31 C36 H36 120.3 . . ? C35 C36 H36 120.3 . . ? C42 C41 C46 122.2(3) . . ? C42 C41 O21 120.5(3) . . ? C46 C41 O21 117.2(3) . . ? C41 C42 C43 119.2(3) . . ? C41 C42 H42 120.4 . . ? C43 C42 H42 120.4 . . ? C42 C43 C44 119.8(3) . . ? C42 C43 H43 120.1 . . ? C44 C43 H43 120.1 . . ? C45 C44 C43 119.9(3) . . ? C45 C44 H44 120.0 . . ? C43 C44 H44 120.0 . . ? C44 C45 C46 120.8(3) . . ? C44 C45 H45 119.6 . . ? C46 C45 H45 119.6 . . ? C41 C46 C45 118.1(3) . . ? C41 C46 H46 121.0 . . ? C45 C46 H46 121.0 . . ? C56 C51 C52 121.4(3) . . ? C56 C51 O22 120.7(3) . . ? C52 C51 O22 117.8(3) . . ? C51 C52 C53 118.9(3) . . ? C51 C52 H52 120.5 . . ? C53 C52 H52 120.5 . . ? C54 C53 C52 120.3(3) . . ? C54 C53 H53 119.9 . . ? C52 C53 H53 119.9 . . ? C55 C54 C53 119.7(3) . . ? C55 C54 H54 120.1 . . ? C53 C54 H54 120.1 . . ? C54 C55 C56 121.0(3) . . ? C54 C55 H55 119.5 . . ? C56 C55 H55 119.5 . . ? C51 C56 C55 118.7(3) . . ? C51 C56 H56 120.7 . . ? C55 C56 H56 120.7 . . ? C62 C61 C66 121.2(3) . . ? C62 C61 O23 117.8(2) . . ? C66 C61 O23 120.9(3) . . ? C61 C62 C63 118.9(3) . . ? C61 C62 H62 120.6 . . ? C63 C62 H62 120.6 . . ? C64 C63 C62 120.7(3) . . ? C64 C63 H63 119.6 . . ? C62 C63 H63 119.6 . . ? C63 C64 C65 120.1(3) . . ? C63 C64 H64 120.0 . . ? C65 C64 H64 120.0 . . ? C64 C65 C66 120.3(3) . . ? C64 C65 H65 119.8 . . ? C66 C65 H65 119.8 . . ? C61 C66 C65 118.7(3) . . ? C61 C66 H66 120.6 . . ? C65 C66 H66 120.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Co P1 O12 -30.43(12) . . . . ? C2 Co P1 O12 -131.01(14) . . . . ? P2 Co P1 O12 79.78(9) . . . . ? C1 Co P1 O11 -152.94(12) . . . . ? C2 Co P1 O11 106.48(14) . . . . ? P2 Co P1 O11 -42.73(9) . . . . ? C1 Co P1 O13 87.90(12) . . . . ? C2 Co P1 O13 -12.68(14) . . . . ? P2 Co P1 O13 -161.89(8) . . . . ? C1 Co P2 O21 10.55(14) . . . . ? C2 Co P2 O21 114.52(14) . . . . ? P1 Co P2 O21 -96.88(10) . . . . ? C1 Co P2 O22 130.11(13) . . . . ? C2 Co P2 O22 -125.92(14) . . . . ? P1 Co P2 O22 22.68(9) . . . . ? C1 Co P2 O23 -109.21(13) . . . . ? C2 Co P2 O23 -5.24(14) . . . . ? P1 Co P2 O23 143.36(8) . . . . ? C2 Co C1 O1 26(4) . . . . ? P2 Co C1 O1 147(4) . . . . ? P1 Co C1 O1 -93(4) . . . . ? C1 Co C2 O2 -92(13) . . . . ? P2 Co C2 O2 160(13) . . . . ? P1 Co C2 O2 11(13) . . . . ? O12 P1 O11 C11 175.69(19) . . . . ? O13 P1 O11 C11 78.4(2) . . . . ? Co P1 O11 C11 -51.2(2) . . . . ? O11 P1 O12 C21 89.1(2) . . . . ? O13 P1 O12 C21 -172.9(2) . . . . ? Co P1 O12 C21 -43.7(2) . . . . ? O12 P1 O13 C31 96.5(2) . . . . ? O11 P1 O13 C31 -164.71(19) . . . . ? Co P1 O13 C31 -34.0(2) . . . . ? O22 P2 O21 C41 -164.7(2) . . . . ? O23 P2 O21 C41 92.5(2) . . . . ? Co P2 O21 C41 -36.1(3) . . . . ? O21 P2 O22 C51 -40.3(2) . . . . ? O23 P2 O22 C51 58.1(2) . . . . ? Co P2 O22 C51 -173.58(19) . . . . ? O21 P2 O23 C61 -170.55(19) . . . . ? O22 P2 O23 C61 91.2(2) . . . . ? Co P2 O23 C61 -37.2(2) . . . . ? P1 O11 C11 C12 112.7(2) . . . . ? P1 O11 C11 C16 -70.7(3) . . . . ? C16 C11 C12 C13 1.7(4) . . . . ? O11 C11 C12 C13 178.3(3) . . . . ? C11 C12 C13 C14 -0.5(5) . . . . ? C12 C13 C14 C15 -0.6(5) . . . . ? C13 C14 C15 C16 0.4(5) . . . . ? C12 C11 C16 C15 -1.9(5) . . . . ? O11 C11 C16 C15 -178.4(3) . . . . ? C14 C15 C16 C11 0.8(5) . . . . ? P1 O12 C21 C22 129.2(2) . . . . ? P1 O12 C21 C26 -54.8(3) . . . . ? C26 C21 C22 C23 -0.6(5) . . . . ? O12 C21 C22 C23 175.3(3) . . . . ? C21 C22 C23 C24 -0.2(5) . . . . ? C22 C23 C24 C25 0.0(5) . . . . ? C23 C24 C25 C26 1.0(5) . . . . ? C22 C21 C26 C25 1.6(5) . . . . ? O12 C21 C26 C25 -174.2(3) . . . . ? C24 C25 C26 C21 -1.8(5) . . . . ? P1 O13 C31 C36 -64.3(3) . . . . ? P1 O13 C31 C32 118.7(2) . . . . ? C36 C31 C32 C33 0.2(5) . . . . ? O13 C31 C32 C33 177.2(3) . . . . ? C31 C32 C33 C34 0.1(5) . . . . ? C32 C33 C34 C35 -0.2(5) . . . . ? C33 C34 C35 C36 -0.1(5) . . . . ? C32 C31 C36 C35 -0.4(4) . . . . ? O13 C31 C36 C35 -177.3(3) . . . . ? C34 C35 C36 C31 0.4(5) . . . . ? P2 O21 C41 C42 -73.8(3) . . . . ? P2 O21 C41 C46 110.0(3) . . . . ? C46 C41 C42 C43 -0.3(4) . . . . ? O21 C41 C42 C43 -176.4(2) . . . . ? C41 C42 C43 C44 1.0(5) . . . . ? C42 C43 C44 C45 -1.0(5) . . . . ? C43 C44 C45 C46 0.4(5) . . . . ? C42 C41 C46 C45 -0.3(4) . . . . ? O21 C41 C46 C45 175.9(3) . . . . ? C44 C45 C46 C41 0.3(5) . . . . ? P2 O22 C51 C56 -82.7(3) . . . . ? P2 O22 C51 C52 100.6(3) . . . . ? C56 C51 C52 C53 1.2(5) . . . . ? O22 C51 C52 C53 177.8(3) . . . . ? C51 C52 C53 C54 -0.3(5) . . . . ? C52 C53 C54 C55 -0.7(5) . . . . ? C53 C54 C55 C56 0.9(5) . . . . ? C52 C51 C56 C55 -0.9(5) . . . . ? O22 C51 C56 C55 -177.5(3) . . . . ? C54 C55 C56 C51 -0.1(5) . . . . ? P2 O23 C61 C62 112.8(3) . . . . ? P2 O23 C61 C66 -70.1(3) . . . . ? C66 C61 C62 C63 -1.1(4) . . . . ? O23 C61 C62 C63 176.0(3) . . . . ? C61 C62 C63 C64 -0.3(5) . . . . ? C62 C63 C64 C65 0.8(5) . . . . ? C63 C64 C65 C66 0.1(5) . . . . ? C62 C61 C66 C65 2.0(4) . . . . ? O23 C61 C66 C65 -175.1(3) . . . . ? C64 C65 C66 C61 -1.4(5) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 28.35 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.507 _refine_diff_density_min -0.535 _refine_diff_density_rms 0.070