Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_section_title ;Chiral and achiral phosphine derivatives of alkylidyne tricobalt carbonyl clusters as catalyst precursors for (asymmetric) inter- and intramolecular Pauson-Khand reactions ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Ebbe Nordlander' ? ? 'Stephen Colbran' '' '' 'Donald C. Craig' '' '' 'Anthony Deeming' '' '' 'Viktor Moberg' '' '' 'M. Abdul Mottalib' '' '' 'Yulia Poplavskaya' '' '' 'Desiree Sauer' '' '' _publ_contact_author_address ? _publ_contact_author_email EBBE.NORDLANDER@INORG.LU.SE # SUBMISSION DETAILS _publ_contact_author_name 'Ebbe Nordlander' _publ_contact_letter ? _publ_requested_category ? # Attachment 'COBALTO.CIF' data_str0006 _database_code_depnum_ccdc_archive 'CCDC 668301' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H12 Co3 O8 P' _chemical_formula_weight 552.03 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 monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.7435(7) _cell_length_b 14.8061(12) _cell_length_c 9.0608(8) _cell_angle_alpha 90.00 _cell_angle_beta 116.1070(10) _cell_angle_gamma 90.00 _cell_volume 1053.31(15) _cell_formula_units_Z 2 _cell_measurement_temperature 566(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'dark purple' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.741 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 548 _exptl_absorpt_coefficient_mu 2.450 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4407 _exptl_absorpt_correction_T_max 0.7101 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 292(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 APEX' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6738 _diffrn_reflns_av_R_equivalents 0.0151 _diffrn_reflns_av_sigmaI/netI 0.0329 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 28.32 _reflns_number_total 4622 _reflns_number_gt 4337 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0531P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.282(13) _refine_ls_number_reflns 4622 _refine_ls_number_parameters 262 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0294 _refine_ls_R_factor_gt 0.0272 _refine_ls_wR_factor_ref 0.0709 _refine_ls_wR_factor_gt 0.0696 _refine_ls_goodness_of_fit_ref 0.872 _refine_ls_restrained_S_all 0.871 _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 0.72834(4) 0.32818(2) 0.71773(5) 0.04048(10) Uani 1 1 d . . . Co2 Co 0.85423(5) 0.28552(3) 0.53125(5) 0.04414(10) Uani 1 1 d . . . Co3 Co 0.98374(4) 0.40878(3) 0.73033(4) 0.04044(9) Uani 1 1 d . . . P1 P 1.04684(10) 0.49246(6) 0.94991(10) 0.04799(18) Uani 1 1 d . . . C41 C 0.8766(4) 0.5597(2) 0.9580(4) 0.0476(7) Uani 1 1 d . . . C42 C 0.8001(5) 0.6259(3) 0.8402(5) 0.0638(9) Uani 1 1 d . . . H42A H 0.8357 0.6346 0.7584 0.077 Uiso 1 1 calc R . . C43 C 0.6726(6) 0.6785(3) 0.8427(5) 0.0711(11) Uani 1 1 d . . . H43A H 0.6227 0.7227 0.7628 0.085 Uiso 1 1 calc R . . C44 C 0.6178(5) 0.6667(3) 0.9616(5) 0.0713(11) Uani 1 1 d . . . H44A H 0.5309 0.7027 0.9623 0.086 Uiso 1 1 calc R . . C45 C 0.6917(5) 0.6017(3) 1.0796(6) 0.0708(10) Uani 1 1 d . . . H45A H 0.6544 0.5933 1.1602 0.085 Uiso 1 1 calc R . . C46 C 0.8227(5) 0.5481(3) 1.0793(5) 0.0592(8) Uani 1 1 d . . . H46A H 0.8737 0.5046 1.1604 0.071 Uiso 1 1 calc R . . C47 C 1.1491(5) 0.4344(3) 1.1452(5) 0.0754(12) Uani 1 1 d . . . H47A H 1.1714 0.4765 1.2329 0.113 Uiso 1 1 calc R . . H47B H 1.2545 0.4085 1.1567 0.113 Uiso 1 1 calc R . . H47C H 1.0757 0.3873 1.1496 0.113 Uiso 1 1 calc R . . C48 C 1.2033(6) 0.5793(3) 0.9695(7) 0.0882(15) Uani 1 1 d . . . H48A H 1.2284 0.6147 1.0662 0.132 Uiso 1 1 calc R . . H48B H 1.1579 0.6177 0.8745 0.132 Uiso 1 1 calc R . . H48C H 1.3057 0.5511 0.9781 0.132 Uiso 1 1 calc R . . C1 C 0.9496(4) 0.2868(2) 0.7660(4) 0.0436(6) Uani 1 1 d . . . H1 H 1.0237 0.2435 0.8481 0.052 Uiso 1 1 calc R . . C11 C 0.5794(4) 0.2366(3) 0.6466(5) 0.0575(8) Uani 1 1 d . . . C12 C 0.7576(5) 0.3252(3) 0.9228(4) 0.0591(8) Uani 1 1 d . . . C13 C 0.5929(4) 0.4242(2) 0.6186(5) 0.0598(9) Uani 1 1 d . . . C21 C 1.0271(5) 0.2867(3) 0.4781(4) 0.0602(8) Uani 1 1 d . . . C22 C 0.8093(5) 0.1670(3) 0.5071(6) 0.0667(10) Uani 1 1 d . . . C23 C 0.6917(4) 0.3437(3) 0.3579(4) 0.0567(8) Uani 1 1 d . . . C31 C 1.2022(4) 0.3931(3) 0.7809(5) 0.0643(10) Uani 1 1 d . . . C32 C 0.9034(4) 0.4985(2) 0.5801(4) 0.0534(7) Uani 1 1 d . . . O11 O 0.4886(4) 0.1785(2) 0.6080(4) 0.0900(10) Uani 1 1 d . . . O12 O 0.7733(5) 0.3176(3) 1.0526(4) 0.0988(11) Uani 1 1 d . . . O13 O 0.5077(5) 0.4832(2) 0.5562(5) 0.1025(12) Uani 1 1 d . . . O21 O 1.1357(4) 0.2859(3) 0.4426(4) 0.0906(9) Uani 1 1 d . . . O22 O 0.7903(5) 0.0920(2) 0.4957(7) 0.1151(15) Uani 1 1 d . . . O23 O 0.5884(4) 0.3821(2) 0.2535(4) 0.0837(9) Uani 1 1 d . . . O31 O 1.3411(4) 0.3807(3) 0.8163(5) 0.1066(13) Uani 1 1 d . . . O32 O 0.8538(4) 0.5522(2) 0.4826(4) 0.0832(9) 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 0.03689(18) 0.04478(19) 0.0460(2) 0.00094(16) 0.02395(15) 0.00080(15) Co2 0.0442(2) 0.0480(2) 0.0455(2) -0.00584(17) 0.02462(17) 0.00088(16) Co3 0.03569(18) 0.04620(19) 0.0428(2) -0.00182(16) 0.02036(15) -0.00254(15) P1 0.0409(4) 0.0525(4) 0.0477(4) -0.0074(3) 0.0168(3) -0.0025(3) C41 0.0500(16) 0.0450(15) 0.0451(15) -0.0071(12) 0.0184(13) -0.0012(12) C42 0.083(3) 0.058(2) 0.0531(19) 0.0017(16) 0.0315(18) 0.0095(18) C43 0.082(3) 0.061(2) 0.062(2) 0.0053(17) 0.024(2) 0.0226(19) C44 0.053(2) 0.076(3) 0.080(3) -0.011(2) 0.0238(19) 0.0130(18) C45 0.063(2) 0.081(3) 0.078(3) -0.001(2) 0.040(2) 0.0087(19) C46 0.060(2) 0.061(2) 0.0577(19) 0.0062(16) 0.0277(16) 0.0090(16) C47 0.060(2) 0.096(3) 0.054(2) 0.0024(19) 0.0095(16) 0.025(2) C48 0.072(3) 0.085(3) 0.117(4) -0.042(3) 0.050(3) -0.036(2) C1 0.0400(13) 0.0470(14) 0.0460(14) 0.0052(13) 0.0209(12) 0.0057(12) C11 0.0461(17) 0.064(2) 0.064(2) -0.0046(17) 0.0259(15) -0.0029(15) C12 0.066(2) 0.0634(19) 0.060(2) -0.0094(17) 0.0388(16) -0.0123(18) C13 0.0513(17) 0.059(2) 0.077(2) 0.0094(17) 0.0356(17) 0.0120(16) C21 0.064(2) 0.0651(19) 0.0603(19) -0.0033(17) 0.0351(16) 0.0057(17) C22 0.062(2) 0.063(2) 0.090(3) -0.020(2) 0.047(2) -0.0117(18) C23 0.0493(16) 0.074(2) 0.0484(18) -0.0090(16) 0.0230(14) 0.0046(16) C31 0.0428(16) 0.084(3) 0.072(2) -0.0167(19) 0.0311(16) -0.0072(16) C32 0.0588(18) 0.0543(19) 0.0520(18) -0.0018(15) 0.0289(15) -0.0085(15) O11 0.0741(18) 0.088(2) 0.113(3) -0.0242(19) 0.0455(18) -0.0384(17) O12 0.138(3) 0.118(3) 0.0638(17) -0.0122(18) 0.0650(19) -0.025(2) O13 0.080(2) 0.081(2) 0.145(3) 0.029(2) 0.049(2) 0.0343(19) O21 0.0826(19) 0.119(2) 0.103(2) -0.005(2) 0.0702(18) 0.0051(18) O22 0.108(3) 0.063(2) 0.203(5) -0.039(2) 0.095(3) -0.0224(19) O23 0.0648(16) 0.113(3) 0.0589(15) 0.0078(16) 0.0142(13) 0.0155(16) O31 0.0469(16) 0.155(4) 0.122(3) -0.024(3) 0.0406(16) -0.0015(18) O32 0.101(2) 0.077(2) 0.0706(18) 0.0239(15) 0.0363(17) 0.0015(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 Co1 C12 1.761(3) . ? Co1 C11 1.792(4) . ? Co1 C13 1.814(3) . ? Co1 C1 1.888(3) . ? Co1 Co2 2.4703(5) . ? Co1 Co3 2.4899(5) . ? Co2 C21 1.777(4) . ? Co2 C22 1.791(4) . ? Co2 C23 1.807(4) . ? Co2 C1 1.913(3) . ? Co2 Co3 2.4636(6) . ? Co3 C31 1.773(3) . ? Co3 C32 1.808(4) . ? Co3 C1 1.881(3) . ? Co3 P1 2.1981(9) . ? P1 C47 1.810(4) . ? P1 C41 1.819(3) . ? P1 C48 1.828(4) . ? C41 C46 1.384(5) . ? C41 C42 1.385(5) . ? C42 C43 1.369(5) . ? C43 C44 1.369(6) . ? C44 C45 1.372(6) . ? C45 C46 1.394(6) . ? C11 O11 1.117(4) . ? C12 O12 1.128(4) . ? C13 O13 1.126(4) . ? C21 O21 1.129(4) . ? C22 O22 1.120(5) . ? C23 O23 1.132(4) . ? C31 O31 1.126(5) . ? C32 O32 1.124(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 C12 Co1 C11 96.07(17) . . ? C12 Co1 C13 107.55(18) . . ? C11 Co1 C13 101.65(16) . . ? C12 Co1 C1 95.12(16) . . ? C11 Co1 C1 110.27(15) . . ? C13 Co1 C1 138.40(15) . . ? C12 Co1 Co2 144.47(13) . . ? C11 Co1 Co2 91.88(12) . . ? C13 Co1 Co2 104.60(12) . . ? C1 Co1 Co2 49.91(9) . . ? C12 Co1 Co3 104.62(11) . . ? C11 Co1 Co3 150.98(12) . . ? C13 Co1 Co3 91.38(12) . . ? C1 Co1 Co3 48.54(10) . . ? Co2 Co1 Co3 59.559(16) . . ? C21 Co2 C22 98.25(18) . . ? C21 Co2 C23 101.37(16) . . ? C22 Co2 C23 108.33(19) . . ? C21 Co2 C1 107.14(15) . . ? C22 Co2 C1 96.36(18) . . ? C23 Co2 C1 138.87(14) . . ? C21 Co2 Co3 91.12(13) . . ? C22 Co2 Co3 145.18(16) . . ? C23 Co2 Co3 102.46(12) . . ? C1 Co2 Co3 48.95(10) . . ? C21 Co2 Co1 150.58(13) . . ? C22 Co2 Co1 101.20(13) . . ? C23 Co2 Co1 93.22(10) . . ? C1 Co2 Co1 49.02(9) . . ? Co3 Co2 Co1 60.616(15) . . ? C31 Co3 C32 107.94(18) . . ? C31 Co3 C1 93.71(16) . . ? C32 Co3 C1 142.74(14) . . ? C31 Co3 P1 91.56(12) . . ? C32 Co3 P1 97.30(11) . . ? C1 Co3 P1 112.40(10) . . ? C31 Co3 Co2 100.85(12) . . ? C32 Co3 Co2 95.27(11) . . ? C1 Co3 Co2 50.07(9) . . ? P1 Co3 Co2 158.70(3) . . ? C31 Co3 Co1 142.37(14) . . ? C32 Co3 Co1 105.90(11) . . ? C1 Co3 Co1 48.76(9) . . ? P1 Co3 Co1 100.05(3) . . ? Co2 Co3 Co1 59.825(16) . . ? C47 P1 C41 106.37(17) . . ? C47 P1 C48 102.3(3) . . ? C41 P1 C48 101.6(2) . . ? C47 P1 Co3 115.87(16) . . ? C41 P1 Co3 117.46(10) . . ? C48 P1 Co3 111.31(17) . . ? C46 C41 C42 118.9(3) . . ? C46 C41 P1 122.3(3) . . ? C42 C41 P1 118.8(3) . . ? C43 C42 C41 120.7(4) . . ? C42 C43 C44 120.7(4) . . ? C43 C44 C45 119.7(4) . . ? C44 C45 C46 120.2(4) . . ? C41 C46 C45 119.9(3) . . ? Co3 C1 Co1 82.70(12) . . ? Co3 C1 Co2 80.98(12) . . ? Co1 C1 Co2 81.08(11) . . ? O11 C11 Co1 177.5(4) . . ? O12 C12 Co1 175.5(4) . . ? O13 C13 Co1 179.4(4) . . ? O21 C21 Co2 178.6(4) . . ? O22 C22 Co2 176.3(4) . . ? O23 C23 Co2 177.3(3) . . ? O31 C31 Co3 177.6(4) . . ? O32 C32 Co3 177.5(3) . . ? 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 C12 Co1 Co2 C21 -53.8(3) . . . . ? C11 Co1 Co2 C21 -156.9(3) . . . . ? C13 Co1 Co2 C21 100.5(3) . . . . ? C1 Co1 Co2 C21 -41.8(3) . . . . ? Co3 Co1 Co2 C21 17.6(3) . . . . ? C12 Co1 Co2 C22 76.7(3) . . . . ? C11 Co1 Co2 C22 -26.5(2) . . . . ? C13 Co1 Co2 C22 -129.0(2) . . . . ? C1 Co1 Co2 C22 88.7(2) . . . . ? Co3 Co1 Co2 C22 148.10(15) . . . . ? C12 Co1 Co2 C23 -173.9(2) . . . . ? C11 Co1 Co2 C23 82.93(17) . . . . ? C13 Co1 Co2 C23 -19.62(18) . . . . ? C1 Co1 Co2 C23 -161.88(18) . . . . ? Co3 Co1 Co2 C23 -102.49(12) . . . . ? C12 Co1 Co2 C1 -12.0(2) . . . . ? C11 Co1 Co2 C1 -115.19(18) . . . . ? C13 Co1 Co2 C1 142.26(18) . . . . ? Co3 Co1 Co2 C1 59.39(13) . . . . ? C12 Co1 Co2 Co3 -71.4(2) . . . . ? C11 Co1 Co2 Co3 -174.58(13) . . . . ? C13 Co1 Co2 Co3 82.87(13) . . . . ? C1 Co1 Co2 Co3 -59.39(13) . . . . ? C21 Co2 Co3 C31 -26.22(19) . . . . ? C22 Co2 Co3 C31 80.0(3) . . . . ? C23 Co2 Co3 C31 -128.13(18) . . . . ? C1 Co2 Co3 C31 85.73(18) . . . . ? Co1 Co2 Co3 C31 145.22(14) . . . . ? C21 Co2 Co3 C32 83.21(17) . . . . ? C22 Co2 Co3 C32 -170.6(2) . . . . ? C23 Co2 Co3 C32 -18.69(16) . . . . ? C1 Co2 Co3 C32 -164.83(15) . . . . ? Co1 Co2 Co3 C32 -105.34(11) . . . . ? C21 Co2 Co3 C1 -111.96(17) . . . . ? C22 Co2 Co3 C1 -5.7(2) . . . . ? C23 Co2 Co3 C1 146.14(16) . . . . ? Co1 Co2 Co3 C1 59.49(11) . . . . ? C21 Co2 Co3 P1 -150.80(15) . . . . ? C22 Co2 Co3 P1 -44.6(2) . . . . ? C23 Co2 Co3 P1 107.30(14) . . . . ? C1 Co2 Co3 P1 -38.84(14) . . . . ? Co1 Co2 Co3 P1 20.65(8) . . . . ? C21 Co2 Co3 Co1 -171.44(13) . . . . ? C22 Co2 Co3 Co1 -65.2(2) . . . . ? C23 Co2 Co3 Co1 86.65(11) . . . . ? C1 Co2 Co3 Co1 -59.49(11) . . . . ? C12 Co1 Co3 C31 78.7(2) . . . . ? C11 Co1 Co3 C31 -55.3(3) . . . . ? C13 Co1 Co3 C31 -172.7(2) . . . . ? C1 Co1 Co3 C31 -5.1(2) . . . . ? Co2 Co1 Co3 C31 -66.6(2) . . . . ? C12 Co1 Co3 C32 -127.86(18) . . . . ? C11 Co1 Co3 C32 98.1(3) . . . . ? C13 Co1 Co3 C32 -19.32(17) . . . . ? C1 Co1 Co3 C32 148.31(17) . . . . ? Co2 Co1 Co3 C32 86.84(11) . . . . ? C12 Co1 Co3 C1 83.83(19) . . . . ? C11 Co1 Co3 C1 -50.2(3) . . . . ? C13 Co1 Co3 C1 -167.62(17) . . . . ? Co2 Co1 Co3 C1 -61.47(12) . . . . ? C12 Co1 Co3 P1 -27.23(15) . . . . ? C11 Co1 Co3 P1 -161.3(3) . . . . ? C13 Co1 Co3 P1 81.32(13) . . . . ? C1 Co1 Co3 P1 -111.05(12) . . . . ? Co2 Co1 Co3 P1 -172.53(3) . . . . ? C12 Co1 Co3 Co2 145.30(14) . . . . ? C11 Co1 Co3 Co2 11.2(3) . . . . ? C13 Co1 Co3 Co2 -106.15(13) . . . . ? C1 Co1 Co3 Co2 61.47(12) . . . . ? C31 Co3 P1 C47 -67.9(2) . . . . ? C32 Co3 P1 C47 -176.17(19) . . . . ? C1 Co3 P1 C47 26.81(19) . . . . ? Co2 Co3 P1 C47 58.15(18) . . . . ? Co1 Co3 P1 C47 76.19(16) . . . . ? C31 Co3 P1 C41 164.92(19) . . . . ? C32 Co3 P1 C41 56.60(17) . . . . ? C1 Co3 P1 C41 -100.42(16) . . . . ? Co2 Co3 P1 C41 -69.08(15) . . . . ? Co1 Co3 P1 C41 -51.04(13) . . . . ? C31 Co3 P1 C48 48.4(3) . . . . ? C32 Co3 P1 C48 -59.9(2) . . . . ? C1 Co3 P1 C48 143.1(2) . . . . ? Co2 Co3 P1 C48 174.4(2) . . . . ? Co1 Co3 P1 C48 -167.6(2) . . . . ? C47 P1 C41 C46 -12.6(3) . . . . ? C48 P1 C41 C46 -119.3(3) . . . . ? Co3 P1 C41 C46 119.1(3) . . . . ? C47 P1 C41 C42 166.4(3) . . . . ? C48 P1 C41 C42 59.7(3) . . . . ? Co3 P1 C41 C42 -61.9(3) . . . . ? C46 C41 C42 C43 -0.4(6) . . . . ? P1 C41 C42 C43 -179.4(3) . . . . ? C41 C42 C43 C44 -0.2(6) . . . . ? C42 C43 C44 C45 0.2(7) . . . . ? C43 C44 C45 C46 0.4(7) . . . . ? C42 C41 C46 C45 0.9(6) . . . . ? P1 C41 C46 C45 179.9(3) . . . . ? C44 C45 C46 C41 -0.9(7) . . . . ? C31 Co3 C1 Co1 176.88(14) . . . . ? C32 Co3 C1 Co1 -56.6(3) . . . . ? P1 Co3 C1 Co1 83.67(10) . . . . ? Co2 Co3 C1 Co1 -82.07(10) . . . . ? C31 Co3 C1 Co2 -101.05(14) . . . . ? C32 Co3 C1 Co2 25.5(3) . . . . ? P1 Co3 C1 Co2 165.74(5) . . . . ? Co1 Co3 C1 Co2 82.07(10) . . . . ? C12 Co1 C1 Co3 -105.02(15) . . . . ? C11 Co1 C1 Co3 156.57(14) . . . . ? C13 Co1 C1 Co3 18.8(3) . . . . ? Co2 Co1 C1 Co3 81.96(11) . . . . ? C12 Co1 C1 Co2 173.03(14) . . . . ? C11 Co1 C1 Co2 74.62(17) . . . . ? C13 Co1 C1 Co2 -63.1(3) . . . . ? Co3 Co1 C1 Co2 -81.96(11) . . . . ? C21 Co2 C1 Co3 76.02(17) . . . . ? C22 Co2 C1 Co3 176.71(13) . . . . ? C23 Co2 C1 Co3 -55.8(2) . . . . ? Co1 Co2 C1 Co3 -83.96(11) . . . . ? C21 Co2 C1 Co1 159.98(16) . . . . ? C22 Co2 C1 Co1 -99.33(14) . . . . ? C23 Co2 C1 Co1 28.2(3) . . . . ? Co3 Co2 C1 Co1 83.96(11) . . . . ? C12 Co1 C11 O11 -20(8) . . . . ? C13 Co1 C11 O11 -130(8) . . . . ? C1 Co1 C11 O11 78(8) . . . . ? Co2 Co1 C11 O11 125(8) . . . . ? Co3 Co1 C11 O11 115(8) . . . . ? C11 Co1 C12 O12 25(5) . . . . ? C13 Co1 C12 O12 129(5) . . . . ? C1 Co1 C12 O12 -86(5) . . . . ? Co2 Co1 C12 O12 -77(5) . . . . ? Co3 Co1 C12 O12 -135(5) . . . . ? C12 Co1 C13 O13 -115(39) . . . . ? C11 Co1 C13 O13 -15(39) . . . . ? C1 Co1 C13 O13 125(39) . . . . ? Co2 Co1 C13 O13 80(39) . . . . ? Co3 Co1 C13 O13 139(39) . . . . ? C22 Co2 C21 O21 25(17) . . . . ? C23 Co2 C21 O21 -86(17) . . . . ? C1 Co2 C21 O21 124(17) . . . . ? Co3 Co2 C21 O21 171(17) . . . . ? Co1 Co2 C21 O21 156(17) . . . . ? C21 Co2 C22 O22 40(7) . . . . ? C23 Co2 C22 O22 145(7) . . . . ? C1 Co2 C22 O22 -68(7) . . . . ? Co3 Co2 C22 O22 -64(7) . . . . ? Co1 Co2 C22 O22 -118(7) . . . . ? C21 Co2 C23 O23 -135(8) . . . . ? C22 Co2 C23 O23 122(8) . . . . ? C1 Co2 C23 O23 -1(8) . . . . ? Co3 Co2 C23 O23 -41(8) . . . . ? Co1 Co2 C23 O23 19(8) . . . . ? C32 Co3 C31 O31 -175(9) . . . . ? C1 Co3 C31 O31 -26(9) . . . . ? P1 Co3 C31 O31 87(9) . . . . ? Co2 Co3 C31 O31 -76(9) . . . . ? Co1 Co3 C31 O31 -22(9) . . . . ? C31 Co3 C32 O32 71(8) . . . . ? C1 Co3 C32 O32 -51(8) . . . . ? P1 Co3 C32 O32 165(8) . . . . ? Co2 Co3 C32 O32 -32(8) . . . . ? Co1 Co3 C32 O32 -92(8) . . . . ? _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.345 _refine_diff_density_min -0.189 _refine_diff_density_rms 0.053 data_str0077a _database_code_depnum_ccdc_archive 'CCDC 668302' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H34 Co3 O6 P3' _chemical_formula_weight 772.28 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 P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 10.1219(18) _cell_length_b 10.4665(19) _cell_length_c 10.5068(19) _cell_angle_alpha 115.346(3) _cell_angle_beta 115.601(3) _cell_angle_gamma 94.383(3) _cell_volume 859.3(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour orange-red _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.492 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 394 _exptl_absorpt_coefficient_mu 1.610 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5865 _exptl_absorpt_correction_T_max 0.9110 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 APEX diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7355 _diffrn_reflns_av_R_equivalents 0.0168 _diffrn_reflns_av_sigmaI/netI 0.0783 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 28.30 _reflns_number_total 6667 _reflns_number_gt 5456 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0150P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.015(15) _refine_ls_number_reflns 6667 _refine_ls_number_parameters 394 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0572 _refine_ls_R_factor_gt 0.0440 _refine_ls_wR_factor_ref 0.0884 _refine_ls_wR_factor_gt 0.0802 _refine_ls_goodness_of_fit_ref 0.986 _refine_ls_restrained_S_all 0.985 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.36815(7) 0.70319(7) 0.68380(7) 0.03830(18) Uani 1 1 d . . . Co2 Co 0.21756(7) 0.85894(7) 0.76230(7) 0.03919(19) Uani 1 1 d . . . Co3 Co 0.31588(7) 0.88537(6) 0.59708(7) 0.03749(18) Uani 1 1 d . . . P1 P 0.29974(19) 0.46222(16) 0.54454(18) 0.0528(4) Uani 1 1 d . . . P2 P -0.01987(17) 0.79972(17) 0.70273(18) 0.0478(4) Uani 1 1 d . . . P3 P 0.20499(16) 0.84655(14) 0.34907(16) 0.0393(3) Uani 1 1 d . . . C1 C 0.2890(7) 0.7191(6) 0.8284(7) 0.0494(14) Uani 1 1 d . . . C2 C 0.2067(8) 1.0016(6) 0.6849(7) 0.0549(16) Uani 1 1 d . . . C3 C 0.4431(7) 0.7543(6) 0.5667(7) 0.0486(14) Uani 1 1 d . . . C4 C 0.5579(7) 0.7483(7) 0.8390(7) 0.0541(14) Uani 1 1 d . . . C5 C 0.3117(7) 1.0065(7) 0.9668(8) 0.0589(16) Uani 1 1 d . . . C6 C 0.4772(8) 1.0420(7) 0.6979(8) 0.0652(17) Uani 1 1 d . . . C7 C 0.1780(6) 0.7180(5) 0.5522(6) 0.0387(11) Uani 1 1 d . . . H7 H 0.0826 0.6422 0.4519 0.046 Uiso 1 1 calc R . . C8 C 0.3531(11) 0.3879(8) 0.3890(10) 0.101(3) Uani 1 1 d . . . H8A H 0.3281 0.2816 0.3406 0.152 Uiso 1 1 calc R . . H8B H 0.4622 0.4320 0.4389 0.152 Uiso 1 1 calc R . . H8C H 0.2973 0.4108 0.3054 0.152 Uiso 1 1 calc R . . C9 C 0.3951(9) 0.3810(8) 0.6666(9) 0.095(3) Uani 1 1 d . . . H9A H 0.3718 0.4079 0.7522 0.142 Uiso 1 1 calc R . . H9B H 0.5049 0.4179 0.7145 0.142 Uiso 1 1 calc R . . H9C H 0.3591 0.2743 0.5976 0.142 Uiso 1 1 calc R . . C10 C 0.0999(8) 0.3547(6) 0.4394(7) 0.0567(16) Uani 1 1 d . . . C11 C -0.0001(10) 0.3010(8) 0.2756(9) 0.089(2) Uani 1 1 d . . . H11 H 0.0355 0.3220 0.2164 0.107 Uiso 1 1 calc R . . C12 C -0.1486(16) 0.2185(13) 0.1986(15) 0.143(5) Uani 1 1 d . . . H12 H -0.2120 0.1819 0.0867 0.171 Uiso 1 1 calc R . . C13 C -0.2073(14) 0.1878(12) 0.277(2) 0.149(6) Uani 1 1 d . . . H13 H -0.3103 0.1305 0.2205 0.179 Uiso 1 1 calc R . . C14 C -0.1141(12) 0.2417(10) 0.4428(16) 0.116(3) Uani 1 1 d . . . H14 H -0.1542 0.2235 0.5003 0.139 Uiso 1 1 calc R . . C15 C 0.0390(9) 0.3228(7) 0.5219(10) 0.077(2) Uani 1 1 d . . . H15 H 0.1030 0.3568 0.6330 0.092 Uiso 1 1 calc R . . C16 C -0.0771(8) 0.6629(8) 0.7487(8) 0.0727(19) Uani 1 1 d . . . H16A H -0.0162 0.7013 0.8648 0.109 Uiso 1 1 calc R . . H16B H -0.0606 0.5720 0.6907 0.109 Uiso 1 1 calc R . . H16C H -0.1846 0.6435 0.7149 0.109 Uiso 1 1 calc R . . C17 C -0.0668(9) 0.9553(9) 0.8178(10) 0.085(2) Uani 1 1 d . . . H17A H -0.0524 1.0322 0.7937 0.128 Uiso 1 1 calc R . . H17B H -0.0003 0.9939 0.9333 0.128 Uiso 1 1 calc R . . H17C H -0.1726 0.9224 0.7876 0.128 Uiso 1 1 calc R . . C18 C -0.1706(7) 0.7291(8) 0.4917(7) 0.0550(15) Uani 1 1 d . . . C19 C -0.2130(8) 0.8228(9) 0.4340(9) 0.0732(19) Uani 1 1 d . . . H19 H -0.1637 0.9252 0.5037 0.088 Uiso 1 1 calc R . . C20 C -0.3287(10) 0.7669(13) 0.2729(12) 0.097(3) Uani 1 1 d . . . H20 H -0.3582 0.8321 0.2357 0.116 Uiso 1 1 calc R . . C21 C -0.3997(10) 0.6173(14) 0.1688(11) 0.103(3) Uani 1 1 d . . . H21 H -0.4792 0.5806 0.0615 0.124 Uiso 1 1 calc R . . C22 C -0.3559(9) 0.5239(11) 0.2195(10) 0.102(3) Uani 1 1 d . . . H22 H -0.4019 0.4215 0.1463 0.122 Uiso 1 1 calc R . . C23 C -0.2413(8) 0.5776(9) 0.3818(8) 0.076(2) Uani 1 1 d . . . H23 H -0.2122 0.5108 0.4164 0.092 Uiso 1 1 calc R . . C24 C 0.0611(7) 0.9377(7) 0.2989(7) 0.0649(18) Uani 1 1 d . . . H24A H 0.0195 0.9135 0.1872 0.097 Uiso 1 1 calc R . . H24B H 0.1082 1.0438 0.3712 0.097 Uiso 1 1 calc R . . H24C H -0.0207 0.9039 0.3118 0.097 Uiso 1 1 calc R . . C25 C 0.3413(8) 0.9177(7) 0.3059(8) 0.0695(19) Uani 1 1 d . . . H25A H 0.4130 0.8626 0.3085 0.104 Uiso 1 1 calc R . . H25B H 0.3967 1.0214 0.3874 0.104 Uiso 1 1 calc R . . H25C H 0.2857 0.9066 0.1991 0.104 Uiso 1 1 calc R . . C26 C 0.1060(7) 0.6558(6) 0.1779(6) 0.0446(13) Uani 1 1 d . . . C27 C -0.0505(7) 0.5912(7) 0.1104(7) 0.0636(17) Uani 1 1 d . . . H27 H -0.1038 0.6461 0.1537 0.076 Uiso 1 1 calc R . . C28 C -0.1272(10) 0.4477(8) -0.0193(10) 0.089(3) Uani 1 1 d . . . H28 H -0.2322 0.4066 -0.0631 0.107 Uiso 1 1 calc R . . C29 C -0.0548(11) 0.3662(8) -0.0835(9) 0.088(3) Uani 1 1 d . . . H29 H -0.1098 0.2693 -0.1727 0.105 Uiso 1 1 calc R . . C30 C 0.1029(12) 0.4237(8) -0.0193(9) 0.089(3) Uani 1 1 d . . . H30 H 0.1536 0.3658 -0.0641 0.107 Uiso 1 1 calc R . . C31 C 0.1836(8) 0.5701(6) 0.1138(7) 0.0626(16) Uani 1 1 d . . . H31 H 0.2892 0.6098 0.1592 0.075 Uiso 1 1 calc R . . O1 O 0.2919(6) 0.6761(5) 0.9129(5) 0.0700(13) Uani 1 1 d . . . O2 O 0.1663(6) 1.1069(5) 0.7007(6) 0.0770(14) Uani 1 1 d . . . O3 O 0.5198(6) 0.7263(6) 0.5103(6) 0.0795(15) Uani 1 1 d . . . O4 O 0.6829(6) 0.7753(7) 0.9373(6) 0.0952(17) Uani 1 1 d . . . O5 O 0.3720(7) 1.1054(6) 1.0996(6) 0.107(2) Uani 1 1 d . . . O6 O 0.5833(6) 1.1417(6) 0.7637(7) 0.122(2) 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 0.0421(4) 0.0375(4) 0.0361(4) 0.0189(3) 0.0202(3) 0.0166(3) Co2 0.0481(5) 0.0379(4) 0.0339(4) 0.0165(3) 0.0244(4) 0.0164(4) Co3 0.0414(4) 0.0343(4) 0.0330(4) 0.0162(3) 0.0181(4) 0.0070(3) P1 0.0707(11) 0.0421(8) 0.0503(9) 0.0238(7) 0.0331(8) 0.0274(8) P2 0.0538(9) 0.0553(9) 0.0499(9) 0.0294(8) 0.0350(8) 0.0263(8) P3 0.0472(8) 0.0353(7) 0.0367(7) 0.0187(6) 0.0231(7) 0.0097(6) C1 0.053(4) 0.061(4) 0.040(3) 0.029(3) 0.024(3) 0.023(3) C2 0.083(5) 0.037(3) 0.054(4) 0.027(3) 0.038(3) 0.024(3) C3 0.052(4) 0.050(3) 0.056(4) 0.029(3) 0.034(3) 0.019(3) C4 0.053(4) 0.067(4) 0.050(3) 0.031(3) 0.032(3) 0.022(3) C5 0.071(4) 0.052(4) 0.056(4) 0.026(3) 0.038(3) 0.010(3) C6 0.055(4) 0.059(4) 0.049(4) 0.024(3) 0.009(3) 0.003(3) C7 0.045(3) 0.040(3) 0.040(3) 0.021(2) 0.027(2) 0.019(2) C8 0.143(8) 0.060(5) 0.101(6) 0.016(4) 0.087(6) 0.044(5) C9 0.101(6) 0.061(5) 0.107(6) 0.052(5) 0.030(5) 0.039(4) C10 0.079(4) 0.033(3) 0.045(3) 0.020(3) 0.023(3) 0.020(3) C11 0.102(6) 0.060(5) 0.059(5) 0.027(4) 0.012(4) 0.021(4) C12 0.119(11) 0.080(7) 0.096(8) 0.019(6) -0.018(7) 0.009(7) C13 0.072(7) 0.058(6) 0.195(16) 0.032(8) 0.011(9) -0.001(5) C14 0.096(7) 0.066(6) 0.178(11) 0.057(7) 0.071(8) 0.024(5) C15 0.085(6) 0.051(4) 0.082(5) 0.029(4) 0.039(5) 0.020(4) C16 0.071(5) 0.095(5) 0.075(4) 0.058(4) 0.042(4) 0.018(4) C17 0.096(6) 0.098(6) 0.099(6) 0.049(5) 0.074(5) 0.060(5) C18 0.044(3) 0.080(5) 0.062(4) 0.041(4) 0.037(3) 0.035(4) C19 0.053(4) 0.114(6) 0.081(5) 0.067(5) 0.038(4) 0.036(4) C20 0.086(6) 0.169(9) 0.109(7) 0.108(7) 0.065(6) 0.078(7) C21 0.059(6) 0.171(10) 0.075(6) 0.061(7) 0.030(5) 0.055(7) C22 0.063(5) 0.124(7) 0.074(6) 0.032(5) 0.022(5) 0.025(5) C23 0.059(4) 0.090(6) 0.067(5) 0.034(4) 0.027(4) 0.032(4) C24 0.075(4) 0.053(4) 0.045(3) 0.021(3) 0.017(3) 0.024(3) C25 0.096(5) 0.056(4) 0.062(4) 0.028(3) 0.050(4) 0.006(4) C26 0.059(4) 0.036(3) 0.036(3) 0.019(2) 0.023(3) 0.012(3) C27 0.061(4) 0.049(4) 0.060(4) 0.019(3) 0.025(3) 0.009(3) C28 0.087(6) 0.046(4) 0.076(5) 0.025(4) 0.008(5) -0.006(4) C29 0.108(7) 0.043(4) 0.056(5) 0.016(4) 0.014(5) -0.007(5) C30 0.165(9) 0.057(5) 0.071(5) 0.034(4) 0.078(6) 0.048(5) C31 0.082(5) 0.048(4) 0.063(4) 0.022(3) 0.047(4) 0.022(3) O1 0.103(4) 0.090(3) 0.072(3) 0.064(3) 0.062(3) 0.054(3) O2 0.132(4) 0.059(3) 0.095(4) 0.052(3) 0.083(3) 0.062(3) O3 0.094(4) 0.108(4) 0.109(4) 0.074(3) 0.085(3) 0.061(3) O4 0.049(3) 0.142(5) 0.078(3) 0.060(4) 0.017(3) 0.026(3) O5 0.137(5) 0.077(4) 0.047(3) -0.004(3) 0.041(3) 0.012(3) O6 0.077(4) 0.080(4) 0.117(5) 0.041(4) -0.004(3) -0.031(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 C4 1.751(6) . ? Co1 C7 1.889(5) . ? Co1 C3 1.920(6) . ? Co1 C1 1.958(6) . ? Co1 P1 2.1632(16) . ? Co1 Co3 2.4436(9) . ? Co1 Co2 2.4445(9) . ? Co2 C5 1.754(6) . ? Co2 C7 1.888(5) . ? Co2 C1 1.936(6) . ? Co2 C2 1.973(5) . ? Co2 P2 2.1660(17) . ? Co2 Co3 2.4377(9) . ? Co3 C6 1.756(7) . ? Co3 C7 1.895(5) . ? Co3 C2 1.918(6) . ? Co3 C3 1.972(6) . ? Co3 P3 2.1705(15) . ? P1 C10 1.798(7) . ? P1 C9 1.813(6) . ? P1 C8 1.819(7) . ? P2 C17 1.808(6) . ? P2 C18 1.814(6) . ? P2 C16 1.824(6) . ? P3 C26 1.813(5) . ? P3 C24 1.813(6) . ? P3 C25 1.826(6) . ? C1 O1 1.145(6) . ? C2 O2 1.174(6) . ? C3 O3 1.151(6) . ? C4 O4 1.146(6) . ? C5 O5 1.149(6) . ? C6 O6 1.136(7) . ? C10 C11 1.371(8) . ? C10 C15 1.387(9) . ? C11 C12 1.345(14) . ? C12 C13 1.323(17) . ? C13 C14 1.380(15) . ? C14 C15 1.377(11) . ? C18 C19 1.365(9) . ? C18 C23 1.380(9) . ? C19 C20 1.383(10) . ? C20 C21 1.359(11) . ? C21 C22 1.321(12) . ? C22 C23 1.393(10) . ? C26 C31 1.387(8) . ? C26 C27 1.387(8) . ? C27 C28 1.368(9) . ? C28 C29 1.323(11) . ? C29 C30 1.392(11) . ? C30 C31 1.399(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C4 Co1 C7 162.6(2) . . ? C4 Co1 C3 90.7(3) . . ? C7 Co1 C3 86.5(2) . . ? C4 Co1 C1 91.6(2) . . ? C7 Co1 C1 85.6(2) . . ? C3 Co1 C1 160.8(2) . . ? C4 Co1 P1 101.5(2) . . ? C7 Co1 P1 95.96(16) . . ? C3 Co1 P1 100.86(17) . . ? C1 Co1 P1 97.34(18) . . ? C4 Co1 Co3 116.1(2) . . ? C7 Co1 Co3 49.88(15) . . ? C3 Co1 Co3 52.08(17) . . ? C1 Co1 Co3 110.35(17) . . ? P1 Co1 Co3 131.57(5) . . ? C4 Co1 Co2 116.54(18) . . ? C7 Co1 Co2 49.66(14) . . ? C3 Co1 Co2 111.78(17) . . ? C1 Co1 Co2 50.70(16) . . ? P1 Co1 Co2 128.28(6) . . ? Co3 Co1 Co2 59.83(3) . . ? C5 Co2 C7 162.1(3) . . ? C5 Co2 C1 92.2(3) . . ? C7 Co2 C1 86.3(2) . . ? C5 Co2 C2 90.7(3) . . ? C7 Co2 C2 85.0(2) . . ? C1 Co2 C2 160.2(3) . . ? C5 Co2 P2 102.0(2) . . ? C7 Co2 P2 95.79(17) . . ? C1 Co2 P2 100.88(19) . . ? C2 Co2 P2 97.7(2) . . ? C5 Co2 Co3 115.05(19) . . ? C7 Co2 Co3 50.00(15) . . ? C1 Co2 Co3 111.40(17) . . ? C2 Co2 Co3 50.21(18) . . ? P2 Co2 Co3 128.66(5) . . ? C5 Co2 Co1 116.8(2) . . ? C7 Co2 Co1 49.69(15) . . ? C1 Co2 Co1 51.52(17) . . ? C2 Co2 Co1 110.17(18) . . ? P2 Co2 Co1 130.85(5) . . ? Co3 Co2 Co1 60.07(3) . . ? C6 Co3 C7 161.7(3) . . ? C6 Co3 C2 93.2(3) . . ? C7 Co3 C2 86.4(2) . . ? C6 Co3 C3 89.9(3) . . ? C7 Co3 C3 84.9(2) . . ? C2 Co3 C3 161.1(2) . . ? C6 Co3 P3 100.6(2) . . ? C7 Co3 P3 97.31(16) . . ? C2 Co3 P3 102.01(18) . . ? C3 Co3 P3 95.67(17) . . ? C6 Co3 Co2 117.0(2) . . ? C7 Co3 Co2 49.77(14) . . ? C2 Co3 Co2 52.22(17) . . ? C3 Co3 Co2 110.14(17) . . ? P3 Co3 Co2 133.38(5) . . ? C6 Co3 Co1 114.6(2) . . ? C7 Co3 Co1 49.68(15) . . ? C2 Co3 Co1 112.22(17) . . ? C3 Co3 Co1 50.16(17) . . ? P3 Co3 Co1 128.08(5) . . ? Co2 Co3 Co1 60.11(3) . . ? C10 P1 C9 101.8(3) . . ? C10 P1 C8 104.4(3) . . ? C9 P1 C8 100.6(4) . . ? C10 P1 Co1 119.21(18) . . ? C9 P1 Co1 113.9(2) . . ? C8 P1 Co1 114.7(3) . . ? C17 P2 C18 102.8(3) . . ? C17 P2 C16 101.3(4) . . ? C18 P2 C16 103.5(3) . . ? C17 P2 Co2 113.1(3) . . ? C18 P2 Co2 117.30(19) . . ? C16 P2 Co2 116.7(2) . . ? C26 P3 C24 102.7(3) . . ? C26 P3 C25 102.6(3) . . ? C24 P3 C25 102.1(3) . . ? C26 P3 Co3 118.52(17) . . ? C24 P3 Co3 116.1(2) . . ? C25 P3 Co3 112.6(2) . . ? O1 C1 Co2 141.2(5) . . ? O1 C1 Co1 140.9(5) . . ? Co2 C1 Co1 77.8(2) . . ? O2 C2 Co3 143.0(5) . . ? O2 C2 Co2 139.1(5) . . ? Co3 C2 Co2 77.6(2) . . ? O3 C3 Co1 141.8(5) . . ? O3 C3 Co3 140.5(5) . . ? Co1 C3 Co3 77.8(2) . . ? O4 C4 Co1 178.1(6) . . ? O5 C5 Co2 178.4(6) . . ? O6 C6 Co3 178.7(7) . . ? Co2 C7 Co1 80.6(2) . . ? Co2 C7 Co3 80.2(2) . . ? Co1 C7 Co3 80.4(2) . . ? C11 C10 C15 116.5(7) . . ? C11 C10 P1 122.5(6) . . ? C15 C10 P1 121.0(5) . . ? C12 C11 C10 121.6(9) . . ? C13 C12 C11 122.1(12) . . ? C12 C13 C14 119.4(12) . . ? C15 C14 C13 119.0(11) . . ? C14 C15 C10 121.4(8) . . ? C19 C18 C23 117.7(6) . . ? C19 C18 P2 121.5(5) . . ? C23 C18 P2 120.8(5) . . ? C18 C19 C20 120.6(8) . . ? C21 C20 C19 120.3(8) . . ? C22 C21 C20 120.2(8) . . ? C21 C22 C23 120.4(9) . . ? C18 C23 C22 120.6(7) . . ? C31 C26 C27 118.4(5) . . ? C31 C26 P3 121.7(5) . . ? C27 C26 P3 119.9(4) . . ? C28 C27 C26 120.7(7) . . ? C29 C28 C27 121.3(8) . . ? C28 C29 C30 120.8(7) . . ? C29 C30 C31 118.9(7) . . ? C26 C31 C30 119.9(7) . . ? 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 C4 Co1 Co2 C5 1.3(3) . . . . ? C7 Co1 Co2 C5 -165.9(3) . . . . ? C3 Co1 Co2 C5 -101.1(3) . . . . ? C1 Co1 Co2 C5 69.7(3) . . . . ? P1 Co1 Co2 C5 133.9(2) . . . . ? Co3 Co1 Co2 C5 -104.9(2) . . . . ? C4 Co1 Co2 C7 167.2(3) . . . . ? C3 Co1 Co2 C7 64.8(3) . . . . ? C1 Co1 Co2 C7 -124.4(3) . . . . ? P1 Co1 Co2 C7 -60.2(2) . . . . ? Co3 Co1 Co2 C7 61.0(2) . . . . ? C4 Co1 Co2 C1 -68.4(3) . . . . ? C7 Co1 Co2 C1 124.4(3) . . . . ? C3 Co1 Co2 C1 -170.8(3) . . . . ? P1 Co1 Co2 C1 64.2(2) . . . . ? Co3 Co1 Co2 C1 -174.6(2) . . . . ? C4 Co1 Co2 C2 102.8(3) . . . . ? C7 Co1 Co2 C2 -64.4(3) . . . . ? C3 Co1 Co2 C2 0.4(3) . . . . ? C1 Co1 Co2 C2 171.2(3) . . . . ? P1 Co1 Co2 C2 -124.6(2) . . . . ? Co3 Co1 Co2 C2 -3.36(19) . . . . ? C4 Co1 Co2 P2 -136.8(2) . . . . ? C7 Co1 Co2 P2 56.0(2) . . . . ? C3 Co1 Co2 P2 120.8(2) . . . . ? C1 Co1 Co2 P2 -68.4(2) . . . . ? P1 Co1 Co2 P2 -4.19(10) . . . . ? Co3 Co1 Co2 P2 117.07(7) . . . . ? C4 Co1 Co2 Co3 106.1(2) . . . . ? C7 Co1 Co2 Co3 -61.04(19) . . . . ? C3 Co1 Co2 Co3 3.75(19) . . . . ? C1 Co1 Co2 Co3 174.6(2) . . . . ? P1 Co1 Co2 Co3 -121.26(7) . . . . ? C5 Co2 Co3 C6 3.5(3) . . . . ? C7 Co2 Co3 C6 -164.8(3) . . . . ? C1 Co2 Co3 C6 -99.6(3) . . . . ? C2 Co2 Co3 C6 71.7(3) . . . . ? P2 Co2 Co3 C6 135.4(2) . . . . ? Co1 Co2 Co3 C6 -104.2(2) . . . . ? C5 Co2 Co3 C7 168.3(3) . . . . ? C1 Co2 Co3 C7 65.1(3) . . . . ? C2 Co2 Co3 C7 -123.5(3) . . . . ? P2 Co2 Co3 C7 -59.8(2) . . . . ? Co1 Co2 Co3 C7 60.58(19) . . . . ? C5 Co2 Co3 C2 -68.2(3) . . . . ? C7 Co2 Co3 C2 123.5(3) . . . . ? C1 Co2 Co3 C2 -171.3(3) . . . . ? P2 Co2 Co3 C2 63.7(2) . . . . ? Co1 Co2 Co3 C2 -175.9(2) . . . . ? C5 Co2 Co3 C3 104.1(3) . . . . ? C7 Co2 Co3 C3 -64.2(3) . . . . ? C1 Co2 Co3 C3 1.0(3) . . . . ? C2 Co2 Co3 C3 172.3(3) . . . . ? P2 Co2 Co3 C3 -124.01(19) . . . . ? Co1 Co2 Co3 C3 -3.61(18) . . . . ? C5 Co2 Co3 P3 -136.5(2) . . . . ? C7 Co2 Co3 P3 55.25(19) . . . . ? C1 Co2 Co3 P3 120.4(2) . . . . ? C2 Co2 Co3 P3 -68.3(2) . . . . ? P2 Co2 Co3 P3 -4.57(10) . . . . ? Co1 Co2 Co3 P3 115.82(6) . . . . ? C5 Co2 Co3 Co1 107.7(2) . . . . ? C7 Co2 Co3 Co1 -60.58(19) . . . . ? C1 Co2 Co3 Co1 4.57(19) . . . . ? C2 Co2 Co3 Co1 175.9(2) . . . . ? P2 Co2 Co3 Co1 -120.40(7) . . . . ? C4 Co1 Co3 C6 1.3(3) . . . . ? C7 Co1 Co3 C6 168.9(3) . . . . ? C3 Co1 Co3 C6 -67.4(3) . . . . ? C1 Co1 Co3 C6 103.7(3) . . . . ? P1 Co1 Co3 C6 -135.6(3) . . . . ? Co2 Co1 Co3 C6 108.2(3) . . . . ? C4 Co1 Co3 C7 -167.6(3) . . . . ? C3 Co1 Co3 C7 123.7(3) . . . . ? C1 Co1 Co3 C7 -65.2(3) . . . . ? P1 Co1 Co3 C7 55.5(2) . . . . ? Co2 Co1 Co3 C7 -60.71(18) . . . . ? C4 Co1 Co3 C2 -103.4(3) . . . . ? C7 Co1 Co3 C2 64.2(3) . . . . ? C3 Co1 Co3 C2 -172.1(3) . . . . ? C1 Co1 Co3 C2 -1.0(3) . . . . ? P1 Co1 Co3 C2 119.7(2) . . . . ? Co2 Co1 Co3 C2 3.5(2) . . . . ? C4 Co1 Co3 C3 68.7(3) . . . . ? C7 Co1 Co3 C3 -123.7(3) . . . . ? C1 Co1 Co3 C3 171.1(3) . . . . ? P1 Co1 Co3 C3 -68.2(2) . . . . ? Co2 Co1 Co3 C3 175.6(2) . . . . ? C4 Co1 Co3 P3 129.3(2) . . . . ? C7 Co1 Co3 P3 -63.07(19) . . . . ? C3 Co1 Co3 P3 60.6(2) . . . . ? C1 Co1 Co3 P3 -128.26(19) . . . . ? P1 Co1 Co3 P3 -7.54(10) . . . . ? Co2 Co1 Co3 P3 -123.78(7) . . . . ? C4 Co1 Co3 Co2 -106.9(2) . . . . ? C7 Co1 Co3 Co2 60.71(18) . . . . ? C3 Co1 Co3 Co2 -175.6(2) . . . . ? C1 Co1 Co3 Co2 -4.48(18) . . . . ? P1 Co1 Co3 Co2 116.24(8) . . . . ? C4 Co1 P1 C10 149.6(3) . . . . ? C7 Co1 P1 C10 -29.9(3) . . . . ? C3 Co1 P1 C10 -117.4(3) . . . . ? C1 Co1 P1 C10 56.4(3) . . . . ? Co3 Co1 P1 C10 -69.2(2) . . . . ? Co2 Co1 P1 C10 11.8(2) . . . . ? C4 Co1 P1 C9 29.4(4) . . . . ? C7 Co1 P1 C9 -150.0(3) . . . . ? C3 Co1 P1 C9 122.4(4) . . . . ? C1 Co1 P1 C9 -63.7(4) . . . . ? Co3 Co1 P1 C9 170.6(3) . . . . ? Co2 Co1 P1 C9 -108.4(3) . . . . ? C4 Co1 P1 C8 -85.7(4) . . . . ? C7 Co1 P1 C8 94.8(4) . . . . ? C3 Co1 P1 C8 7.3(4) . . . . ? C1 Co1 P1 C8 -178.8(4) . . . . ? Co3 Co1 P1 C8 55.5(3) . . . . ? Co2 Co1 P1 C8 136.5(3) . . . . ? C5 Co2 P2 C17 28.7(4) . . . . ? C7 Co2 P2 C17 -149.5(3) . . . . ? C1 Co2 P2 C17 123.2(3) . . . . ? C2 Co2 P2 C17 -63.7(3) . . . . ? Co3 Co2 P2 C17 -107.7(3) . . . . ? Co1 Co2 P2 C17 171.1(3) . . . . ? C5 Co2 P2 C18 148.1(3) . . . . ? C7 Co2 P2 C18 -30.0(3) . . . . ? C1 Co2 P2 C18 -117.3(3) . . . . ? C2 Co2 P2 C18 55.7(3) . . . . ? Co3 Co2 P2 C18 11.7(3) . . . . ? Co1 Co2 P2 C18 -69.5(3) . . . . ? C5 Co2 P2 C16 -88.3(3) . . . . ? C7 Co2 P2 C16 93.6(3) . . . . ? C1 Co2 P2 C16 6.3(3) . . . . ? C2 Co2 P2 C16 179.4(3) . . . . ? Co3 Co2 P2 C16 135.3(3) . . . . ? Co1 Co2 P2 C16 54.1(3) . . . . ? C6 Co3 P3 C26 145.4(3) . . . . ? C7 Co3 P3 C26 -31.0(3) . . . . ? C2 Co3 P3 C26 -118.9(3) . . . . ? C3 Co3 P3 C26 54.5(3) . . . . ? Co2 Co3 P3 C26 -70.3(2) . . . . ? Co1 Co3 P3 C26 12.2(2) . . . . ? C6 Co3 P3 C24 -91.5(3) . . . . ? C7 Co3 P3 C24 92.0(3) . . . . ? C2 Co3 P3 C24 4.1(3) . . . . ? C3 Co3 P3 C24 177.5(3) . . . . ? Co2 Co3 P3 C24 52.8(3) . . . . ? Co1 Co3 P3 C24 135.3(2) . . . . ? C6 Co3 P3 C25 25.7(3) . . . . ? C7 Co3 P3 C25 -150.8(3) . . . . ? C2 Co3 P3 C25 121.4(3) . . . . ? C3 Co3 P3 C25 -65.3(3) . . . . ? Co2 Co3 P3 C25 170.0(2) . . . . ? Co1 Co3 P3 C25 -107.5(2) . . . . ? C5 Co2 C1 O1 52.6(9) . . . . ? C7 Co2 C1 O1 -145.2(9) . . . . ? C2 Co2 C1 O1 150.7(7) . . . . ? P2 Co2 C1 O1 -50.0(9) . . . . ? Co3 Co2 C1 O1 170.6(8) . . . . ? Co1 Co2 C1 O1 175.7(10) . . . . ? C5 Co2 C1 Co1 -123.1(2) . . . . ? C7 Co2 C1 Co1 39.1(2) . . . . ? C2 Co2 C1 Co1 -25.0(8) . . . . ? P2 Co2 C1 Co1 134.28(13) . . . . ? Co3 Co2 C1 Co1 -5.1(2) . . . . ? C4 Co1 C1 O1 -52.1(8) . . . . ? C7 Co1 C1 O1 145.2(9) . . . . ? C3 Co1 C1 O1 -148.9(8) . . . . ? P1 Co1 C1 O1 49.7(8) . . . . ? Co3 Co1 C1 O1 -170.7(8) . . . . ? Co2 Co1 C1 O1 -175.7(9) . . . . ? C4 Co1 C1 Co2 123.7(2) . . . . ? C7 Co1 C1 Co2 -39.1(2) . . . . ? C3 Co1 C1 Co2 26.8(8) . . . . ? P1 Co1 C1 Co2 -134.56(14) . . . . ? Co3 Co1 C1 Co2 5.0(2) . . . . ? C6 Co3 C2 O2 51.4(9) . . . . ? C7 Co3 C2 O2 -146.9(9) . . . . ? C3 Co3 C2 O2 150.5(8) . . . . ? P3 Co3 C2 O2 -50.2(9) . . . . ? Co2 Co3 C2 O2 173.4(10) . . . . ? Co1 Co3 C2 O2 169.6(8) . . . . ? C6 Co3 C2 Co2 -122.1(2) . . . . ? C7 Co3 C2 Co2 39.6(2) . . . . ? C3 Co3 C2 Co2 -22.9(9) . . . . ? P3 Co3 C2 Co2 136.34(13) . . . . ? Co1 Co3 C2 Co2 -3.8(2) . . . . ? C5 Co2 C2 O2 -51.2(8) . . . . ? C7 Co2 C2 O2 146.2(8) . . . . ? C1 Co2 C2 O2 -149.5(8) . . . . ? P2 Co2 C2 O2 51.0(8) . . . . ? Co3 Co2 C2 O2 -174.0(9) . . . . ? Co1 Co2 C2 O2 -170.2(8) . . . . ? C5 Co2 C2 Co3 122.7(3) . . . . ? C7 Co2 C2 Co3 -39.9(2) . . . . ? C1 Co2 C2 Co3 24.4(8) . . . . ? P2 Co2 C2 Co3 -135.05(15) . . . . ? Co1 Co2 C2 Co3 3.8(2) . . . . ? C4 Co1 C3 O3 56.4(9) . . . . ? C7 Co1 C3 O3 -140.9(9) . . . . ? C1 Co1 C3 O3 153.4(7) . . . . ? P1 Co1 C3 O3 -45.5(9) . . . . ? Co3 Co1 C3 O3 179.6(10) . . . . ? Co2 Co1 C3 O3 175.4(8) . . . . ? C4 Co1 C3 Co3 -123.2(2) . . . . ? C7 Co1 C3 Co3 39.59(19) . . . . ? C1 Co1 C3 Co3 -26.2(8) . . . . ? P1 Co1 C3 Co3 134.99(13) . . . . ? Co2 Co1 C3 Co3 -4.1(2) . . . . ? C6 Co3 C3 O3 -56.7(9) . . . . ? C7 Co3 C3 O3 140.9(9) . . . . ? C2 Co3 C3 O3 -156.3(8) . . . . ? P3 Co3 C3 O3 44.0(8) . . . . ? Co2 Co3 C3 O3 -175.5(8) . . . . ? Co1 Co3 C3 O3 -179.6(9) . . . . ? C6 Co3 C3 Co1 122.9(3) . . . . ? C7 Co3 C3 Co1 -39.6(2) . . . . ? C2 Co3 C3 Co1 23.2(9) . . . . ? P3 Co3 C3 Co1 -136.42(14) . . . . ? Co2 Co3 C3 Co1 4.1(2) . . . . ? C7 Co1 C4 O4 -132(18) . . . . ? C3 Co1 C4 O4 -52(18) . . . . ? C1 Co1 C4 O4 148(18) . . . . ? P1 Co1 C4 O4 50(18) . . . . ? Co3 Co1 C4 O4 -99(18) . . . . ? Co2 Co1 C4 O4 -166(18) . . . . ? C7 Co2 C5 O5 96(21) . . . . ? C1 Co2 C5 O5 -179(100) . . . . ? C2 Co2 C5 O5 20(21) . . . . ? P2 Co2 C5 O5 -78(21) . . . . ? Co3 Co2 C5 O5 66(21) . . . . ? Co1 Co2 C5 O5 133(21) . . . . ? C7 Co3 C6 O6 54(31) . . . . ? C2 Co3 C6 O6 143(31) . . . . ? C3 Co3 C6 O6 -19(31) . . . . ? P3 Co3 C6 O6 -115(31) . . . . ? Co2 Co3 C6 O6 94(31) . . . . ? Co1 Co3 C6 O6 26(31) . . . . ? C5 Co2 C7 Co1 45.1(9) . . . . ? C1 Co2 C7 Co1 -40.3(2) . . . . ? C2 Co2 C7 Co1 121.8(2) . . . . ? P2 Co2 C7 Co1 -140.91(13) . . . . ? Co3 Co2 C7 Co1 81.82(18) . . . . ? C5 Co2 C7 Co3 -36.7(9) . . . . ? C1 Co2 C7 Co3 -122.2(2) . . . . ? C2 Co2 C7 Co3 40.0(2) . . . . ? P2 Co2 C7 Co3 137.28(12) . . . . ? Co1 Co2 C7 Co3 -81.82(18) . . . . ? C4 Co1 C7 Co2 -41.6(8) . . . . ? C3 Co1 C7 Co2 -122.7(2) . . . . ? C1 Co1 C7 Co2 39.8(2) . . . . ? P1 Co1 C7 Co2 136.76(13) . . . . ? Co3 Co1 C7 Co2 -81.57(17) . . . . ? C4 Co1 C7 Co3 40.0(8) . . . . ? C3 Co1 C7 Co3 -41.1(2) . . . . ? C1 Co1 C7 Co3 121.4(2) . . . . ? P1 Co1 C7 Co3 -141.67(12) . . . . ? Co2 Co1 C7 Co3 81.57(17) . . . . ? C6 Co3 C7 Co2 48.2(9) . . . . ? C2 Co3 C7 Co2 -41.3(2) . . . . ? C3 Co3 C7 Co2 121.9(2) . . . . ? P3 Co3 C7 Co2 -142.98(12) . . . . ? Co1 Co3 C7 Co2 82.05(17) . . . . ? C6 Co3 C7 Co1 -33.9(9) . . . . ? C2 Co3 C7 Co1 -123.4(2) . . . . ? C3 Co3 C7 Co1 39.9(2) . . . . ? P3 Co3 C7 Co1 134.97(12) . . . . ? Co2 Co3 C7 Co1 -82.05(17) . . . . ? C9 P1 C10 C11 -136.8(6) . . . . ? C8 P1 C10 C11 -32.5(6) . . . . ? Co1 P1 C10 C11 97.1(5) . . . . ? C9 P1 C10 C15 43.6(6) . . . . ? C8 P1 C10 C15 147.9(5) . . . . ? Co1 P1 C10 C15 -82.5(5) . . . . ? C15 C10 C11 C12 -1.5(11) . . . . ? P1 C10 C11 C12 178.8(7) . . . . ? C10 C11 C12 C13 1.7(17) . . . . ? C11 C12 C13 C14 0(2) . . . . ? C12 C13 C14 C15 -1.8(17) . . . . ? C13 C14 C15 C10 1.9(12) . . . . ? C11 C10 C15 C14 -0.2(9) . . . . ? P1 C10 C15 C14 179.4(5) . . . . ? C17 P2 C18 C19 44.7(6) . . . . ? C16 P2 C18 C19 149.9(5) . . . . ? Co2 P2 C18 C19 -80.0(5) . . . . ? C17 P2 C18 C23 -138.3(6) . . . . ? C16 P2 C18 C23 -33.2(6) . . . . ? Co2 P2 C18 C23 96.9(5) . . . . ? C23 C18 C19 C20 3.3(9) . . . . ? P2 C18 C19 C20 -179.7(5) . . . . ? C18 C19 C20 C21 -1.4(11) . . . . ? C19 C20 C21 C22 -1.7(13) . . . . ? C20 C21 C22 C23 2.7(13) . . . . ? C19 C18 C23 C22 -2.3(10) . . . . ? P2 C18 C23 C22 -179.4(6) . . . . ? C21 C22 C23 C18 -0.7(12) . . . . ? C24 P3 C26 C31 143.8(5) . . . . ? C25 P3 C26 C31 38.0(5) . . . . ? Co3 P3 C26 C31 -86.7(5) . . . . ? C24 P3 C26 C27 -37.7(5) . . . . ? C25 P3 C26 C27 -143.4(5) . . . . ? Co3 P3 C26 C27 91.8(4) . . . . ? C31 C26 C27 C28 -1.7(9) . . . . ? P3 C26 C27 C28 179.7(5) . . . . ? C26 C27 C28 C29 0.3(11) . . . . ? C27 C28 C29 C30 0.9(12) . . . . ? C28 C29 C30 C31 -0.6(11) . . . . ? C27 C26 C31 C30 2.0(9) . . . . ? P3 C26 C31 C30 -179.4(5) . . . . ? C29 C30 C31 C26 -0.9(10) . . . . ? _diffrn_measured_fraction_theta_max 0.914 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.538 _refine_diff_density_min -0.357 _refine_diff_density_rms 0.065 data_dsc139 _database_code_depnum_ccdc_archive 'CCDC 668303' _audit_creation_method 'RAELSPUB and manual entry' _publ_section_title_footnote ? # TEXT _publ_section_abstract ? _publ_section_comment ? _publ_section_acknowledgements ? _publ_section_references ; Altomare, A., Burla, M.C., Camalli, M., Cascarano, G.,Giacovazzo, C., Guagliardi, A., Polidori, G., J. Appl. Cryst., 1994, 27, 435. De Meulenaer, J. and Tompa, H. Acta Cryst., 1965, 19, 1014. Ibers, J.A. and Hamilton, W.C., (Eds) International Tables for X-Ray Crystallography Vol. 4 , Kynoch Press, Birmingham, 1974. Johnson, C.K.,'ORTEP-II', Oak Ridge National Laboratory, Tennessee, U.S.A., 1976. Rae, A.D., RAELS. A comprehensive Constrained Least Squares Refinement Program, University of New South Wales, 1996. Schagen, J.D., Straver, L., van Meurs, F., Williams, G., CAD4 Version 5.0, Delft Instruments X-ray Diffraction, 1989. ; _publ_section_figure_captions ? _publ_section_exptl_prep ? _publ_section_exptl_refinement ? _computing_data_collection 'CAD4 Version 5.0, (Schagen et al, 1989)' _computing_cell_refinement 'CAD4 Version 5.0, (Schagen et al, 1989)' _computing_data_reduction 'Local program' _computing_structure_solution 'SIR92 (Altomare et al, 1994)' _computing_structure_refinement 'RAELS, (Rae, 1996)' _computing_molecular_graphics 'ORTEP-II, (Johnson, 1976)' _computing_publication_material 'Local programs' # CHEMICAL DATA _chemical_name_systematic ? _chemical_formula_moiety 'C36 H29 Co3 P2 O9' _chemical_formula_sum 'C36 H29 Co3 P2 O9' _chemical_formula_iupac ? _chemical_formula_weight 844.4 _chemical_absolute_configuration ad # CRYSTAL DATA _space_group_crystal_system orthorhombic _space_group_name_H-M_alt 'P 21 21 21' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 1/2-x,-y,1/2+z 3 1/2+x,1/2-y,-z 4 -x,1/2+y,1/2-z _cell_length_a 11.968(2) _cell_length_b 12.618(2) _cell_length_c 24.770(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3741(1) _cell_formula_units_Z 4 _cell_measurement_reflns_used 11 _cell_measurement_theta_min 10 _cell_measurement_theta_max 11 _cell_measurement_temperature 294 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.17 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.50 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1712.0 _exptl_absorpt_coefficient_mu 1.450 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details '(DeMeulenaer & Tompa, 1965)' _exptl_absorpt_correction_T_min 0.74 _exptl_absorpt_correction_T_max 0.81 # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Nonius CAD-4' _diffrn_measurement_method \w--2\q _diffrn_reflns_number 3673 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_theta_max 25 _diffrn_measured_fraction_theta_max 1.00 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 1.00 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 29 _diffrn_standards_number 1 _diffrn_standards_interval_time 30 _diffrn_standards_decay_% 0 # REFINEMENT DATA _refine_special_details ? _reflns_number_total 3673 _reflns_number_gt 2687 _reflns_threshold_expression I>2\s(I) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.050 _refine_ls_wR_factor_ref 0.066 _refine_ls_abs_structure_details ; Absolute structure determined by Flack parameter ; _refine_ls_abs_structure_Flack 0.00(4) _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 2687 _refine_ls_number_parameters 324 _refine_ls_goodness_of_fit_ref 1.24 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(F) + 0.0004F^2^]' _refine_ls_shift/su_max 0.004 _refine_diff_density_max 1.18 _refine_diff_density_min -0.69 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _atom_type_scat_source 'International Tables for X-ray Crystallography, Vol. IV' # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_type_symbol _atom_site_occupancy Co1 0.31024(11) 0.48191(10) 0.34787(5) 0.0611(4) Uani Co 1.0 Co2 0.35203(10) 0.29034(9) 0.36386(5) 0.0549(3) Uani Co 1.0 Co3 0.49550(12) 0.41360(14) 0.32528(7) 0.0849(5) Uani Co 1.0 P1 0.18523(20) 0.53100(18) 0.40623(9) 0.0527(6) Uani P 1.0 P2 0.21643(19) 0.23988(17) 0.41882(9) 0.0491(5) Uani P 1.0 O1 -0.0122(6) 0.5118(6) 0.3311(2) 0.074(2) Uani O 1.0 O2 0.2813(7) 0.0259(5) 0.3953(3) 0.084(2) Uani O 1.0 C1 0.2326(7) 0.5950(5) 0.4686(3) 0.079(4) Uani C 1.0 C2 0.3428(8) 0.6267(6) 0.4735(4) 0.101(4) Uani C 1.0 C3 0.3772(9) 0.6765(6) 0.5213(5) 0.138(5) Uani C 1.0 C4 0.3031(11) 0.6932(6) 0.5620(4) 0.157(8) Uani C 1.0 C5 0.1947(12) 0.6623(7) 0.5574(3) 0.156(8) Uani C 1.0 C6 0.1574(8) 0.6122(7) 0.5102(4) 0.113(4) Uani C 1.0 C7 0.0943(8) 0.6355(7) 0.3789(3) 0.058(2) Uani C 1.0 C8 0.1219(10) 0.7398(8) 0.3899(4) 0.075(2) Uani C 1.0 C9 0.0665(11) 0.8228(9) 0.3654(5) 0.093(3) Uani C 1.0 C10 -0.0160(11) 0.7997(10) 0.3290(4) 0.088(3) Uani C 1.0 C11 -0.0449(9) 0.6985(10) 0.3169(4) 0.078(2) Uani C 1.0 C12 0.0102(9) 0.6163(9) 0.3412(4) 0.065(2) Uani C 1.0 C13 -0.0939(10) 0.4855(11) 0.2918(5) 0.098(4) Uani C 1.0 C14 0.0935(8) 0.4285(7) 0.4316(4) 0.057(2) Uani C 1.0 C15 0.1585(9) 0.3432(7) 0.4632(3) 0.059(2) Uani C 1.0 C16 0.0846(6) 0.1830(5) 0.3934(2) 0.055(2) Uani C 1.0 C17 0.0490(6) 0.2037(6) 0.3413(3) 0.068(2) Uani C 1.0 C18 -0.0552(7) 0.1649(7) 0.3245(4) 0.085(3) Uani C 1.0 C19 -0.1198(7) 0.1080(6) 0.3591(3) 0.084(3) Uani C 1.0 C20 -0.0852(6) 0.0874(6) 0.4103(4) 0.084(2) Uani C 1.0 C21 0.0185(6) 0.1249(6) 0.4284(3) 0.073(2) Uani C 1.0 C22 0.2568(8) 0.1383(7) 0.4682(4) 0.061(2) Uani C 1.0 C23 0.2630(9) 0.1594(8) 0.5233(4) 0.071(2) Uani C 1.0 C24 0.2914(11) 0.0763(10) 0.5590(5) 0.089(3) Uani C 1.0 C25 0.3179(10) -0.0206(10) 0.5400(5) 0.094(3) Uani C 1.0 C26 0.3161(10) -0.0390(8) 0.4854(5) 0.088(2) Uani C 1.0 C27 0.2874(9) 0.0390(7) 0.4494(5) 0.073(1) Uani C 1.0 C28 0.3478(13) -0.0553(9) 0.3721(6) 0.110(4) Uani C 1.0 CC1 0.2246(9) 0.4481(10) 0.2909(5) 0.082(3) Uani C 1.0 OC1 0.1730(9) 0.4306(10) 0.2537(3) 0.133(4) Uani O 1.0 CC2 0.3506(10) 0.6125(10) 0.3327(5) 0.084(3) Uani C 1.0 OC2 0.3764(9) 0.6969(7) 0.3201(5) 0.134(4) Uani O 1.0 CC3 0.3149(9) 0.2177(10) 0.3043(5) 0.083(3) Uani C 1.0 OC3 0.3023(9) 0.1693(9) 0.2659(4) 0.133(4) Uani O 1.0 CC4 0.4546(9) 0.2099(9) 0.3953(4) 0.073(3) Uani C 1.0 OC4 0.5200(7) 0.1594(7) 0.4158(4) 0.102(3) Uani O 1.0 CC5 0.6034(12) 0.3187(13) 0.3216(7) 0.119(5) Uani C 1.0 OC5 0.6725(10) 0.2574(12) 0.3196(7) 0.200(7) Uani O 1.0 CC6 0.5772(11) 0.5277(14) 0.3423(7) 0.121(5) Uani C 1.0 OC6 0.6305(11) 0.5973(10) 0.3558(5) 0.151(5) Uani O 1.0 CC7 0.4275(17) 0.4040(12) 0.2712(7) 0.151(8) Uani C 1.0 OC7 0.4372(10) 0.4259(14) 0.2164(6) 0.198(7) Uani O 1.0 CH 0.4133(8) 0.4185(8) 0.3925(4) 0.068(3) Uani C 1.0 HC2 0.3971 0.6142 0.4435 0.117 Uani H 1.0 HC3 0.4566 0.6998 0.5255 0.176 Uani H 1.0 HC4 0.3287 0.7288 0.5959 0.200 Uani H 1.0 HC5 0.1414 0.6752 0.5877 0.211 Uani H 1.0 HC6 0.0777 0.5893 0.5066 0.134 Uani H 1.0 HC8 0.1832 0.7554 0.4162 0.085 Uani H 1.0 HC9 0.0863 0.8979 0.3739 0.119 Uani H 1.0 HC10 -0.0563 0.8592 0.3108 0.105 Uani H 1.0 HC11 -0.1061 0.6841 0.2904 0.090 Uani H 1.0 H1C13 -0.1007 0.4067 0.2891 0.098 Uani H 1.0 H2C13 -0.1676 0.5164 0.3026 0.098 Uani H 1.0 H3C13 -0.0710 0.5150 0.2560 0.098 Uani H 1.0 H1C14 0.0545 0.3942 0.4005 0.057 Uani H 1.0 H2C14 0.0369 0.4615 0.4561 0.057 Uani H 1.0 H1C15 0.1068 0.3092 0.4897 0.059 Uani H 1.0 H2C15 0.2214 0.3781 0.4829 0.059 Uani H 1.0 HC17 0.0968 0.2457 0.3160 0.083 Uani H 1.0 HC18 -0.0821 0.1793 0.2870 0.116 Uani H 1.0 HC19 -0.1940 0.0808 0.3466 0.103 Uani H 1.0 HC20 -0.1339 0.0453 0.4351 0.112 Uani H 1.0 HC21 0.0443 0.1099 0.4660 0.096 Uani H 1.0 HC22 0.2476 0.2322 0.5374 0.075 Uani H 1.0 HC23 0.2918 0.0895 0.5988 0.108 Uani H 1.0 HC25 0.3388 -0.0787 0.5655 0.112 Uani H 1.0 HC26 0.3361 -0.1109 0.4716 0.105 Uani H 1.0 H1C28 0.3359 -0.0569 0.3322 0.110 Uani H 1.0 H2C28 0.4284 -0.0412 0.3800 0.110 Uani H 1.0 H3C28 0.3260 -0.1253 0.3879 0.110 Uani H 1.0 HCH 0.4380 0.4369 0.4299 0.068 Uani H 1.0 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol Co1 0.0563(7) 0.0594(8) 0.0674(8) 0.0004(6) 0.0059(6) 0.0021(6) Co Co2 0.0524(6) 0.0571(7) 0.0553(6) 0.0050(6) 0.0039(6) -0.0033(6) Co Co3 0.0534(8) 0.097(1) 0.104(1) 0.0020(8) 0.0072(8) 0.0105(9) Co P1 0.056(1) 0.051(1) 0.051(1) 0.009(1) -0.006(1) -0.002(1) P P2 0.052(1) 0.047(1) 0.049(1) 0.004(1) 0.001(1) 0.000(1) P O1 0.072(3) 0.089(3) 0.061(3) 0.013(3) -0.016(3) -0.008(3) O O2 0.092(4) 0.058(3) 0.101(3) 0.015(3) -0.004(4) -0.015(3) O C1 0.116(6) 0.046(4) 0.075(4) 0.021(4) -0.037(4) -0.014(3) C C2 0.130(6) 0.059(5) 0.116(5) 0.004(5) -0.070(5) -0.008(4) C C3 0.213(9) 0.059(5) 0.141(7) 0.003(6) -0.118(8) -0.010(5) C C4 0.295(9) 0.067(5) 0.110(5) 0.033(8) -0.111(8) -0.029(5) C C5 0.271(9) 0.115(7) 0.082(4) 0.049(9) -0.047(5) -0.044(4) C C6 0.171(7) 0.096(6) 0.073(4) 0.035(6) -0.020(5) -0.031(4) C C7 0.062(3) 0.062(2) 0.051(3) 0.009(2) 0.006(3) 0.006(2) C C8 0.081(4) 0.058(3) 0.086(4) 0.010(3) -0.001(3) 0.010(3) C C9 0.100(6) 0.067(2) 0.111(6) 0.020(3) 0.002(4) 0.023(3) C C10 0.091(5) 0.091(3) 0.084(5) 0.032(4) 0.012(3) 0.030(3) C C11 0.076(4) 0.101(3) 0.057(3) 0.030(3) 0.007(2) 0.017(3) C C12 0.065(3) 0.082(2) 0.048(3) 0.017(2) 0.002(2) 0.006(2) C C13 0.084(8) 0.119(9) 0.091(8) -0.016(8) -0.034(7) 0.021(8) C C14 0.060(5) 0.052(5) 0.057(5) 0.012(5) -0.001(4) -0.001(4) C C15 0.079(7) 0.058(5) 0.041(5) 0.004(5) 0.008(5) -0.008(4) C C16 0.054(3) 0.050(4) 0.061(3) 0.002(2) 0.005(2) -0.007(3) C C17 0.058(3) 0.081(4) 0.064(3) 0.002(2) -0.001(3) -0.006(3) C C18 0.060(3) 0.112(7) 0.083(4) 0.000(3) -0.008(3) -0.020(4) C C19 0.057(3) 0.077(5) 0.118(6) -0.003(3) -0.003(3) -0.023(5) C C20 0.057(3) 0.071(4) 0.125(6) -0.004(3) 0.007(3) 0.010(5) C C21 0.057(3) 0.076(5) 0.086(3) -0.001(3) 0.009(3) 0.012(4) C C22 0.062(4) 0.054(2) 0.066(3) -0.002(3) -0.001(3) 0.007(2) C C23 0.073(4) 0.077(3) 0.062(3) 0.000(3) -0.005(3) 0.015(2) C C24 0.083(5) 0.100(4) 0.084(2) 0.002(4) -0.008(4) 0.037(3) C C25 0.075(5) 0.086(4) 0.122(4) -0.002(4) -0.009(4) 0.047(4) C C26 0.074(4) 0.060(2) 0.130(4) 0.001(3) -0.008(4) 0.024(3) C C27 0.071(3) 0.053(2) 0.096(3) 0.003(2) -0.003(3) 0.005(2) C C28 0.123(9) 0.078(7) 0.130(9) 0.011(8) 0.011(9) -0.029(8) C CC1 0.072(7) 0.108(9) 0.068(7) 0.016(7) 0.004(6) -0.016(6) C OC1 0.117(8) 0.208(9) 0.073(5) 0.014(8) -0.036(5) -0.028(6) O CC2 0.071(7) 0.076(7) 0.104(9) -0.004(6) 0.031(7) 0.015(7) C OC2 0.133(8) 0.077(6) 0.194(9) -0.001(6) 0.047(8) 0.032(7) O CC3 0.056(6) 0.112(9) 0.083(7) 0.018(7) 0.006(6) -0.019(7) C OC3 0.115(7) 0.190(9) 0.094(6) 0.019(8) -0.013(6) -0.084(7) O CC4 0.062(6) 0.081(7) 0.077(6) 0.007(6) -0.015(6) -0.014(6) C OC4 0.070(5) 0.115(6) 0.121(7) 0.020(5) -0.025(5) 0.016(6) O CC5 0.066(8) 0.131(9) 0.160(9) 0.002(9) 0.028(9) -0.014(9) C OC5 0.105(9) 0.216(9) 0.280(9) 0.083(9) 0.059(9) 0.054(9) O CC6 0.064(8) 0.126(9) 0.174(9) -0.013(8) -0.016(9) 0.006(9) C OC6 0.131(9) 0.141(9) 0.181(9) -0.065(8) -0.021(8) 0.014(8) O CC7 0.219(9) 0.107(9) 0.128(9) 0.084(9) -0.127(9) -0.040(9) C OC7 0.104(8) 0.323(9) 0.167(9) -0.009(9) 0.041(8) 0.025(9) O CH 0.062(6) 0.062(6) 0.081(7) -0.001(5) -0.006(5) -0.004(5) C # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 Co2 2.500(2) 1_555 1_555 no Co1 Co3 2.444(2) 1_555 1_555 no Co1 P1 2.171(3) 1_555 1_555 no Co1 CC1 1.796(12) 1_555 1_555 no Co1 CC2 1.758(12) 1_555 1_555 no Co1 CH 1.839(10) 1_555 1_555 no Co2 Co3 2.506(2) 1_555 1_555 no Co2 P2 2.212(3) 1_555 1_555 no Co2 CC3 1.792(12) 1_555 1_555 no Co2 CC4 1.773(11) 1_555 1_555 no Co2 CH 1.912(10) 1_555 1_555 no Co3 CC5 1.764(16) 1_555 1_555 no Co3 CC6 1.791(17) 1_555 1_555 no Co3 CC7 1.572(12) 1_555 1_555 no Co3 CH 1.935(11) 1_555 1_555 no P1 C1 1.833(8) 1_555 1_555 no P1 C7 1.839(9) 1_555 1_555 no P1 C14 1.809(10) 1_555 1_555 no P2 C15 1.840(8) 1_555 1_555 no P2 C16 1.844(7) 1_555 1_555 no P2 C22 1.837(9) 1_555 1_555 no O1 C12 1.368(13) 1_555 1_555 no O1 C13 1.420(12) 1_555 1_555 no O2 C27 1.353(12) 1_555 1_555 no O2 C28 1.419(13) 1_555 1_555 no C1 C2 1.384(6) 1_555 1_555 no C1 C6 1.384(6) 1_555 1_555 no C2 C3 1.402(8) 1_555 1_555 no C3 C4 1.359(8) 1_555 1_555 no C4 C5 1.359(8) 1_555 1_555 no C5 C6 1.402(8) 1_555 1_555 no C7 C8 1.384(14) 1_555 1_555 no C7 C12 1.395(13) 1_555 1_555 no C8 C9 1.380(14) 1_555 1_555 no C9 C10 1.368(17) 1_555 1_555 no C10 C11 1.356(16) 1_555 1_555 no C11 C12 1.369(14) 1_555 1_555 no C14 C15 1.542(12) 1_555 1_555 no C16 C17 1.384(6) 1_555 1_555 no C16 C21 1.384(6) 1_555 1_555 no C17 C18 1.402(8) 1_555 1_555 no C18 C19 1.359(8) 1_555 1_555 no C19 C20 1.359(8) 1_555 1_555 no C20 C21 1.402(8) 1_555 1_555 no C22 C23 1.392(13) 1_555 1_555 no C22 C27 1.386(13) 1_555 1_555 no C23 C24 1.413(14) 1_555 1_555 no C24 C25 1.348(16) 1_555 1_555 no C25 C26 1.371(16) 1_555 1_555 no C26 C27 1.371(14) 1_555 1_555 no CC1 OC1 1.131(12) 1_555 1_555 no CC2 OC2 1.152(12) 1_555 1_555 no CC3 OC3 1.142(12) 1_555 1_555 no CC4 OC4 1.130(12) 1_555 1_555 no CC5 OC5 1.133(17) 1_555 1_555 no CC6 OC6 1.135(16) 1_555 1_555 no CC7 OC7 1.389(18) 1_555 1_555 no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Co2 Co1 Co3 60.90(6) 1_555 1_555 1_555 no Co2 Co1 P1 107.96(8) 1_555 1_555 1_555 no Co2 Co1 CC1 90.5(4) 1_555 1_555 1_555 no Co2 Co1 CC2 152.3(4) 1_555 1_555 1_555 no Co2 Co1 CH 49.5(3) 1_555 1_555 1_555 no Co3 Co1 P1 151.46(9) 1_555 1_555 1_555 no Co3 Co1 CC1 104.7(3) 1_555 1_555 1_555 no Co3 Co1 CC2 91.9(4) 1_555 1_555 1_555 no Co3 Co1 CH 51.4(3) 1_555 1_555 1_555 no P1 Co1 CC1 101.4(3) 1_555 1_555 1_555 no P1 Co1 CC2 93.7(4) 1_555 1_555 1_555 no P1 Co1 CH 100.7(3) 1_555 1_555 1_555 no CC1 Co1 CC2 102.2(6) 1_555 1_555 1_555 no CC1 Co1 CH 138.7(5) 1_555 1_555 1_555 no CC2 Co1 CH 110.6(5) 1_555 1_555 1_555 no Co1 Co2 Co3 58.44(6) 1_555 1_555 1_555 no Co1 Co2 P2 103.24(8) 1_555 1_555 1_555 no Co1 Co2 CC3 108.3(4) 1_555 1_555 1_555 no Co1 Co2 CC4 139.6(4) 1_555 1_555 1_555 no Co1 Co2 CH 47.0(3) 1_555 1_555 1_555 no Co3 Co2 P2 156.35(9) 1_555 1_555 1_555 no Co3 Co2 CC3 100.0(4) 1_555 1_555 1_555 no Co3 Co2 CC4 92.8(4) 1_555 1_555 1_555 no Co3 Co2 CH 49.7(3) 1_555 1_555 1_555 no P2 Co2 CC3 100.2(4) 1_555 1_555 1_555 no P2 Co2 CC4 94.2(4) 1_555 1_555 1_555 no P2 Co2 CH 107.2(3) 1_555 1_555 1_555 no CC3 Co2 CC4 103.9(5) 1_555 1_555 1_555 no CC3 Co2 CH 146.4(5) 1_555 1_555 1_555 no CC4 Co2 CH 93.2(5) 1_555 1_555 1_555 no Co1 Co3 Co2 60.66(5) 1_555 1_555 1_555 no Co1 Co3 CC5 156.3(5) 1_555 1_555 1_555 no Co1 Co3 CC6 99.1(5) 1_555 1_555 1_555 no Co1 Co3 CC7 75.7(7) 1_555 1_555 1_555 no Co1 Co3 CH 48.0(3) 1_555 1_555 1_555 no Co2 Co3 CC5 95.8(5) 1_555 1_555 1_555 no Co2 Co3 CC6 141.6(5) 1_555 1_555 1_555 no Co2 Co3 CC7 85.6(9) 1_555 1_555 1_555 no Co2 Co3 CH 48.9(3) 1_555 1_555 1_555 no CC5 Co3 CC6 99.1(6) 1_555 1_555 1_555 no CC5 Co3 CC7 106.4(8) 1_555 1_555 1_555 no CC5 Co3 CH 116.0(6) 1_555 1_555 1_555 no CC6 Co3 CC7 123.0(9) 1_555 1_555 1_555 no CC6 Co3 CH 92.8(6) 1_555 1_555 1_555 no CC7 Co3 CH 118.2(9) 1_555 1_555 1_555 no Co1 P1 C1 118.3(3) 1_555 1_555 1_555 no Co1 P1 C7 111.6(3) 1_555 1_555 1_555 no Co1 P1 C14 116.5(3) 1_555 1_555 1_555 no C1 P1 C7 100.2(4) 1_555 1_555 1_555 no C1 P1 C14 102.1(4) 1_555 1_555 1_555 no C7 P1 C14 106.3(4) 1_555 1_555 1_555 no Co2 P2 C15 116.1(3) 1_555 1_555 1_555 no Co2 P2 C16 121.9(2) 1_555 1_555 1_555 no Co2 P2 C22 114.7(3) 1_555 1_555 1_555 no C15 P2 C16 99.1(4) 1_555 1_555 1_555 no C15 P2 C22 101.3(4) 1_555 1_555 1_555 no C16 P2 C22 100.4(4) 1_555 1_555 1_555 no C12 O1 C13 118.9(9) 1_555 1_555 1_555 no C27 O2 C28 117.3(10) 1_555 1_555 1_555 no P1 C1 C2 119.8(6) 1_555 1_555 1_555 no P1 C1 C6 119.7(6) 1_555 1_555 1_555 no C2 C1 C6 120.6(7) 1_555 1_555 1_555 no C1 C2 C3 118.9(6) 1_555 1_555 1_555 no C2 C3 C4 120.3(7) 1_555 1_555 1_555 no C3 C4 C5 121.0(8) 1_555 1_555 1_555 no C4 C5 C6 120.3(7) 1_555 1_555 1_555 no C1 C6 C5 118.9(6) 1_555 1_555 1_555 no P1 C7 C8 117.9(8) 1_555 1_555 1_555 no P1 C7 C12 123.3(7) 1_555 1_555 1_555 no C8 C7 C12 118.0(9) 1_555 1_555 1_555 no C7 C8 C9 121.3(10) 1_555 1_555 1_555 no C8 C9 C10 118.3(11) 1_555 1_555 1_555 no C9 C10 C11 122.1(10) 1_555 1_555 1_555 no C10 C11 C12 119.6(11) 1_555 1_555 1_555 no O1 C12 C7 115.5(8) 1_555 1_555 1_555 no O1 C12 C11 123.8(10) 1_555 1_555 1_555 no C7 C12 C11 120.7(10) 1_555 1_555 1_555 no P1 C14 C15 111.6(6) 1_555 1_555 1_555 no P2 C15 C14 112.5(5) 1_555 1_555 1_555 no P2 C16 C17 120.6(5) 1_555 1_555 1_555 no P2 C16 C21 118.7(5) 1_555 1_555 1_555 no C17 C16 C21 120.6(7) 1_555 1_555 1_555 no C16 C17 C18 118.9(6) 1_555 1_555 1_555 no C17 C18 C19 120.3(7) 1_555 1_555 1_555 no C18 C19 C20 121.0(8) 1_555 1_555 1_555 no C19 C20 C21 120.3(7) 1_555 1_555 1_555 no C16 C21 C20 118.9(6) 1_555 1_555 1_555 no P2 C22 C23 122.2(8) 1_555 1_555 1_555 no P2 C22 C27 118.5(8) 1_555 1_555 1_555 no C23 C22 C27 119.2(9) 1_555 1_555 1_555 no C22 C23 C24 119.0(10) 1_555 1_555 1_555 no C23 C24 C25 120.7(11) 1_555 1_555 1_555 no C24 C25 C26 119.6(11) 1_555 1_555 1_555 no C25 C26 C27 121.6(11) 1_555 1_555 1_555 no O2 C27 C22 115.4(9) 1_555 1_555 1_555 no O2 C27 C26 124.8(10) 1_555 1_555 1_555 no C22 C27 C26 119.7(11) 1_555 1_555 1_555 no Co1 CC1 OC1 176.7(12) 1_555 1_555 1_555 no Co1 CC2 OC2 176.6(13) 1_555 1_555 1_555 no Co2 CC3 OC3 173.2(10) 1_555 1_555 1_555 no Co2 CC4 OC4 179.2(7) 1_555 1_555 1_555 no Co3 CC5 OC5 179.4(13) 1_555 1_555 1_555 no Co3 CC6 OC6 176.1(16) 1_555 1_555 1_555 no Co3 CC7 OC7 140.7(18) 1_555 1_555 1_555 no Co1 CH Co2 83.6(4) 1_555 1_555 1_555 no Co1 CH Co3 80.7(4) 1_555 1_555 1_555 no Co2 CH Co3 81.3(4) 1_555 1_555 1_555 no data_dsc138 _database_code_depnum_ccdc_archive 'CCDC 668304' _audit_creation_method 'RAELSPUB and manual entry' _publ_section_title_footnote ? # TEXT _publ_section_abstract ? _publ_section_comment ? _publ_section_acknowledgements ? _publ_section_references ; Altomare, A., Burla, M.C., Camalli, M., Cascarano, G.,Giacovazzo, C., Guagliardi, A., Polidori, G., J. Appl. Cryst., 1994, 27, 435. De Meulenaer, J. and Tompa, H. Acta Cryst., 1965, 19, 1014. Ibers, J.A. and Hamilton, W.C., (Eds) International Tables for X-Ray Crystallography Vol. 4 , Kynoch Press, Birmingham, 1974. Johnson, C.K.,'ORTEP-II', Oak Ridge National Laboratory, Tennessee, U.S.A., 1976. Rae, A.D., RAELS. A comprehensive Constrained Least Squares Refinement Program, University of New South Wales, 1996. Schagen, J.D., Straver, L., van Meurs, F., Williams, G., CAD4 Version 5.0, Delft Instruments X-ray Diffraction, 1989. ; _publ_section_figure_captions ? _publ_section_exptl_prep ? _publ_section_exptl_refinement ? _computing_data_collection 'CAD4 Version 5.0, (Schagen et al, 1989)' _computing_cell_refinement 'CAD4 Version 5.0, (Schagen et al, 1989)' _computing_data_reduction 'Local program' _computing_structure_solution 'SIR92 (Altomare et al, 1994)' _computing_structure_refinement 'RAELS, (Rae, 1996)' _computing_molecular_graphics 'ORTEP-II, (Johnson, 1976)' _computing_publication_material 'Local programs' # CHEMICAL DATA _chemical_name_systematic ? _chemical_formula_moiety 'C26 H29 Co3 O7 P2' _chemical_formula_sum 'C26 H29 Co3 O7 P2' _chemical_formula_iupac ? _chemical_formula_weight 692.3 _chemical_absolute_configuration ad # CRYSTAL DATA _space_group_crystal_system orthorhombic _space_group_name_H-M_alt 'P 21 21 21' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 1/2-x,-y,1/2+z 3 1/2+x,1/2-y,-z 4 -x,1/2+y,1/2-z _cell_length_a 9.803(1) _cell_length_b 16.155(2) _cell_length_c 18.477(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2926.2(6) _cell_formula_units_Z 4 _cell_measurement_reflns_used 11 _cell_measurement_theta_min 11 _cell_measurement_theta_max 12 _cell_measurement_temperature 294 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.57 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408.0 _exptl_absorpt_coefficient_mu 1.829 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details '(DeMeulenaer & Tompa, 1965)' _exptl_absorpt_correction_T_min 0.68 _exptl_absorpt_correction_T_max 0.77 # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Nonius CAD-4' _diffrn_measurement_method \w--2\q _diffrn_reflns_number 2908 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_theta_max 25 _diffrn_measured_fraction_theta_max 1.00 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 1.00 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 22 _diffrn_standards_number 1 _diffrn_standards_interval_time 30 _diffrn_standards_decay_% 0 # REFINEMENT DATA _refine_special_details ? _reflns_number_total 2907 _reflns_number_gt 2520 _reflns_threshold_expression I>2\s(I) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.028 _refine_ls_wR_factor_ref 0.033 _refine_ls_abs_structure_details ; Absolute structure determined by Flack parameter ; _refine_ls_abs_structure_Flack 0.00(2) _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 2520 _refine_ls_number_parameters 343 _refine_ls_goodness_of_fit_ref 1.09 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(F) + 0.0004F^2^]' _refine_ls_shift/su_max 0.007 _refine_diff_density_max 0.35 _refine_diff_density_min -0.41 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _atom_type_scat_source 'International Tables for X-ray Crystallography, Vol. IV' # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_type_symbol _atom_site_occupancy Co1 0.45895(7) 0.52294(4) 0.45327(3) 0.0357(2) Uani Co 1.0 Co2 0.69422(7) 0.55554(4) 0.40498(4) 0.0428(2) Uani Co 1.0 Co3 0.49465(7) 0.61029(4) 0.34313(3) 0.0443(2) Uani Co 1.0 P1 0.34460(13) 0.40561(8) 0.46767(7) 0.0401(3) Uani P 1.0 P2 0.44269(14) 0.54433(7) 0.56892(6) 0.0375(3) Uani P 1.0 C1 0.3783(8) 0.3089(3) 0.4152(3) 0.068(2) Uani C 1.0 C2 0.2396(12) 0.2793(6) 0.3893(5) 0.141(4) Uani C 1.0 C3 0.1292(9) 0.3110(6) 0.4351(5) 0.105(3) Uani C 1.0 C4 0.1561(6) 0.4023(4) 0.4542(4) 0.070(2) Uani C 1.0 C5 0.4766(10) 0.3178(5) 0.3540(4) 0.104(3) Uani C 1.0 C6 0.0702(7) 0.4324(6) 0.5153(5) 0.097(3) Uani C 1.0 C7 0.3616(5) 0.3798(3) 0.5639(2) 0.038(1) Uani C 1.0 C8 0.3295(5) 0.3031(3) 0.5930(3) 0.046(1) Uani C 1.0 C9 0.3355(6) 0.2895(3) 0.6671(3) 0.056(2) Uani C 1.0 C10 0.3718(7) 0.3536(3) 0.7125(3) 0.058(2) Uani C 1.0 C11 0.4024(6) 0.4294(3) 0.6849(3) 0.050(1) Uani C 1.0 C12 0.3985(5) 0.4445(3) 0.6102(2) 0.037(1) Uani C 1.0 C13 0.3276(6) 0.6218(3) 0.6112(3) 0.061(2) Uani C 1.0 C14 0.4249(9) 0.6861(4) 0.6452(4) 0.087(2) Uani C 1.0 C15 0.5449(8) 0.6413(4) 0.6758(3) 0.072(2) Uani C 1.0 C16 0.5978(6) 0.5828(3) 0.6170(3) 0.053(1) Uani C 1.0 C17 0.2252(7) 0.6627(4) 0.5605(4) 0.088(2) Uani C 1.0 C18 0.7032(7) 0.5195(4) 0.6422(3) 0.073(2) Uani C 1.0 CC1 0.6180(5) 0.4582(3) 0.4640(3) 0.047(1) Uani C 1.0 OC1 0.6682(4) 0.3989(2) 0.4877(2) 0.067(1) Uani O 1.0 CC2 0.3162(6) 0.5645(4) 0.4006(3) 0.061(2) Uani C 1.0 OC2 0.2032(5) 0.5763(3) 0.3857(3) 0.090(2) Uani O 1.0 CC3 0.8164(6) 0.6061(4) 0.4602(3) 0.058(1) Uani C 1.0 OC3 0.8955(5) 0.6401(3) 0.4942(3) 0.089(2) Uani O 1.0 CC4 0.7981(7) 0.4809(4) 0.3599(3) 0.068(2) Uani C 1.0 OC4 0.8710(6) 0.4340(4) 0.3348(3) 0.115(2) Uani O 1.0 CC5 0.4273(7) 0.7111(4) 0.3322(3) 0.060(2) Uani C 1.0 OC5 0.3895(6) 0.7760(3) 0.3261(3) 0.101(2) Uani O 1.0 CC6 0.4501(7) 0.5536(4) 0.2628(3) 0.071(2) Uani C 1.0 OC6 0.4256(6) 0.5157(4) 0.2135(3) 0.126(2) Uani O 1.0 CC7 0.6795(6) 0.6224(3) 0.3137(3) 0.054(1) Uani C 1.0 OC7 0.7511(5) 0.6487(3) 0.2705(2) 0.073(1) Uani O 1.0 CH 0.5518(5) 0.6244(3) 0.4409(2) 0.037(1) Uani C 1.0 HC1 0.4155 0.2665 0.4493 0.068 Uani H 1.0 H1C2 0.2378 0.2174 0.3904 0.141 Uani H 1.0 H2C2 0.2249 0.2989 0.3385 0.141 Uani H 1.0 H1C3 0.1245 0.2777 0.4806 0.105 Uani H 1.0 H2C3 0.0407 0.3065 0.4086 0.105 Uani H 1.0 HC4 0.1340 0.4364 0.4106 0.070 Uani H 1.0 H1C5 0.4880 0.2631 0.3293 0.104 Uani H 1.0 H2C5 0.4409 0.3593 0.3186 0.104 Uani H 1.0 H3C5 0.5668 0.3368 0.3730 0.104 Uani H 1.0 H1C6 -0.0284 0.4277 0.5019 0.097 Uani H 1.0 H2C6 0.0885 0.3982 0.5593 0.097 Uani H 1.0 H3C6 0.0926 0.4916 0.5257 0.097 Uani H 1.0 HC8 0.3016 0.2569 0.5602 0.046 Uani H 1.0 HC9 0.3137 0.2337 0.6874 0.056 Uani H 1.0 HC10 0.3756 0.3443 0.7660 0.058 Uani H 1.0 HC11 0.4283 0.4753 0.7185 0.050 Uani H 1.0 HC13 0.2760 0.5940 0.6511 0.061 Uani H 1.0 H1C14 0.3767 0.7169 0.6846 0.087 Uani H 1.0 H2C14 0.4561 0.7261 0.6073 0.087 Uani H 1.0 H1C15 0.5167 0.6088 0.7194 0.072 Uani H 1.0 H2C15 0.6176 0.6817 0.6897 0.072 Uani H 1.0 HC16 0.6465 0.6189 0.5814 0.053 Uani H 1.0 H1C17 0.1685 0.7031 0.5884 0.088 Uani H 1.0 H2C17 0.2751 0.6924 0.5211 0.088 Uani H 1.0 H3C17 0.1648 0.6194 0.5388 0.088 Uani H 1.0 H1C18 0.7801 0.5487 0.6669 0.073 Uani H 1.0 H2C18 0.6594 0.4799 0.6768 0.073 Uani H 1.0 H3C18 0.7389 0.4883 0.5995 0.073 Uani H 1.0 HCH 0.5551 0.6750 0.4721 0.037 Uani H 1.0 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol Co1 0.0366(3) 0.0364(3) 0.0341(3) -0.0021(3) -0.0042(3) 0.0071(3) Co Co2 0.0398(4) 0.0452(4) 0.0433(4) 0.0005(3) 0.0006(3) 0.0029(3) Co Co3 0.0512(4) 0.0449(4) 0.0369(3) -0.0004(3) -0.0059(3) 0.0093(3) Co P1 0.0445(7) 0.0366(7) 0.0391(7) -0.0054(6) -0.0061(6) 0.0028(6) P P2 0.0419(7) 0.0329(6) 0.0378(6) 0.0028(6) -0.0020(6) 0.0023(5) P C1 0.106(5) 0.046(3) 0.052(3) -0.007(4) -0.001(4) -0.011(3) C C2 0.155(9) 0.138(8) 0.130(8) -0.073(8) -0.001(8) -0.068(7) C C3 0.090(6) 0.117(6) 0.107(6) -0.054(6) -0.022(5) -0.013(5) C C4 0.057(4) 0.068(4) 0.085(4) -0.024(3) -0.033(4) 0.025(4) C C5 0.137(8) 0.088(5) 0.086(5) -0.017(6) 0.030(6) -0.042(4) C C6 0.042(4) 0.123(7) 0.127(6) 0.006(4) -0.004(4) -0.006(5) C C7 0.039(3) 0.036(2) 0.039(2) 0.002(2) -0.002(2) 0.005(2) C C8 0.048(3) 0.032(2) 0.058(3) 0.002(2) 0.004(3) 0.009(2) C C9 0.066(4) 0.045(3) 0.056(3) 0.004(3) 0.008(3) 0.015(3) C C10 0.077(4) 0.055(3) 0.041(3) 0.013(3) 0.012(3) 0.014(3) C C11 0.063(3) 0.049(3) 0.037(3) 0.008(3) 0.006(3) 0.004(2) C C12 0.040(3) 0.035(2) 0.037(3) 0.006(2) 0.003(2) 0.007(2) C C13 0.070(4) 0.044(3) 0.070(4) 0.017(3) 0.012(3) 0.001(3) C C14 0.123(6) 0.050(4) 0.089(5) 0.023(4) -0.025(5) -0.036(4) C C15 0.105(5) 0.056(4) 0.056(3) -0.002(4) -0.022(4) -0.019(3) C C16 0.063(4) 0.050(3) 0.046(3) -0.006(3) -0.009(3) -0.001(3) C C17 0.069(5) 0.069(4) 0.127(6) 0.033(4) -0.010(5) -0.018(4) C C18 0.067(4) 0.086(5) 0.066(4) 0.005(4) -0.019(3) -0.004(4) C CC1 0.045(3) 0.050(3) 0.048(3) 0.002(3) 0.006(3) 0.008(3) C OC1 0.056(2) 0.054(2) 0.091(3) 0.013(2) 0.000(2) 0.026(2) O CC2 0.054(4) 0.063(4) 0.068(4) -0.012(3) -0.016(3) 0.029(3) C OC2 0.046(3) 0.120(4) 0.105(4) -0.006(3) -0.021(3) 0.060(3) O CC3 0.047(3) 0.060(3) 0.066(4) 0.001(3) -0.001(3) 0.011(3) C OC3 0.060(3) 0.100(4) 0.106(4) -0.019(3) -0.032(3) -0.005(3) O CC4 0.079(4) 0.070(4) 0.054(3) 0.017(4) 0.013(3) 0.014(3) C OC4 0.140(5) 0.123(4) 0.083(3) 0.068(4) 0.036(4) -0.005(3) O CC5 0.067(4) 0.059(4) 0.055(3) 0.003(3) -0.007(3) 0.018(3) C OC5 0.125(5) 0.058(3) 0.119(4) 0.030(3) -0.007(4) 0.024(3) O CC6 0.070(4) 0.086(4) 0.056(3) 0.008(4) -0.011(3) -0.013(3) C OC6 0.112(5) 0.173(6) 0.093(4) 0.018(4) -0.040(4) -0.067(4) O CC7 0.068(4) 0.049(3) 0.043(3) -0.010(3) 0.002(3) 0.005(3) C OC7 0.086(3) 0.075(3) 0.058(2) -0.015(3) 0.017(2) 0.018(2) O CH 0.037(2) 0.040(3) 0.034(2) -0.002(2) -0.003(2) 0.009(2) C # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 Co2 2.528(1) 1_555 1_555 no Co1 Co3 2.501(1) 1_555 1_555 no Co1 P1 2.218(1) 1_555 1_555 no Co1 P2 2.171(1) 1_555 1_555 no Co1 CC1 1.888(5) 1_555 1_555 no Co1 CC2 1.832(6) 1_555 1_555 no Co1 CH 1.889(5) 1_555 1_555 no Co2 Co3 2.432(1) 1_555 1_555 no Co2 CC1 2.054(5) 1_555 1_555 no Co2 CC3 1.773(6) 1_555 1_555 no Co2 CC4 1.785(6) 1_555 1_555 no Co2 CC7 2.008(5) 1_555 1_555 no Co2 CH 1.905(5) 1_555 1_555 no Co3 CC2 2.175(6) 1_555 1_555 no Co3 CC5 1.769(6) 1_555 1_555 no Co3 CC6 1.797(6) 1_555 1_555 no Co3 CC7 1.902(6) 1_555 1_555 no Co3 CH 1.905(4) 1_555 1_555 no P1 C1 1.869(6) 1_555 1_555 no P1 C4 1.865(6) 1_555 1_555 no P1 C7 1.834(4) 1_555 1_555 no P2 C12 1.836(4) 1_555 1_555 no P2 C13 1.857(5) 1_555 1_555 no P2 C16 1.868(6) 1_555 1_555 no C1 C2 1.519(12) 1_555 1_555 no C1 C5 1.492(10) 1_555 1_555 no C2 C3 1.467(13) 1_555 1_555 no C3 C4 1.539(10) 1_555 1_555 no C4 C6 1.491(10) 1_555 1_555 no C7 C8 1.388(6) 1_555 1_555 no C7 C12 1.397(6) 1_555 1_555 no C8 C9 1.387(7) 1_555 1_555 no C9 C10 1.379(8) 1_555 1_555 no C10 C11 1.360(7) 1_555 1_555 no C11 C12 1.402(6) 1_555 1_555 no C13 C14 1.545(9) 1_555 1_555 no C13 C17 1.523(9) 1_555 1_555 no C14 C15 1.492(10) 1_555 1_555 no C15 C16 1.531(8) 1_555 1_555 no C16 C18 1.527(8) 1_555 1_555 no CC1 OC1 1.162(6) 1_555 1_555 no CC2 OC2 1.157(7) 1_555 1_555 no CC3 OC3 1.139(7) 1_555 1_555 no CC4 OC4 1.140(7) 1_555 1_555 no CC5 OC5 1.117(6) 1_555 1_555 no CC6 OC6 1.125(7) 1_555 1_555 no CC7 OC7 1.145(6) 1_555 1_555 no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Co2 Co1 Co3 57.84(3) 1_555 1_555 1_555 no Co2 Co1 P1 132.95(5) 1_555 1_555 1_555 no Co2 Co1 P2 112.41(5) 1_555 1_555 1_555 no Co2 Co1 CC1 53.0(2) 1_555 1_555 1_555 no Co2 Co1 CC2 115.6(2) 1_555 1_555 1_555 no Co2 Co1 CH 48.5(2) 1_555 1_555 1_555 no Co3 Co1 P1 130.58(4) 1_555 1_555 1_555 no Co3 Co1 P2 136.18(4) 1_555 1_555 1_555 no Co3 Co1 CC1 106.4(2) 1_555 1_555 1_555 no Co3 Co1 CC2 57.8(2) 1_555 1_555 1_555 no Co3 Co1 CH 49.0(1) 1_555 1_555 1_555 no P1 Co1 P2 88.90(5) 1_555 1_555 1_555 no P1 Co1 CC1 86.1(2) 1_555 1_555 1_555 no P1 Co1 CC2 89.5(2) 1_555 1_555 1_555 no P1 Co1 CH 178.4(2) 1_555 1_555 1_555 no P2 Co1 CC1 92.6(2) 1_555 1_555 1_555 no P2 Co1 CC2 114.1(2) 1_555 1_555 1_555 no P2 Co1 CH 90.9(1) 1_555 1_555 1_555 no CC1 Co1 CC2 152.8(3) 1_555 1_555 1_555 no CC1 Co1 CH 95.5(2) 1_555 1_555 1_555 no CC2 Co1 CH 89.1(2) 1_555 1_555 1_555 no Co1 Co2 Co3 60.52(3) 1_555 1_555 1_555 no Co1 Co2 CC1 47.3(2) 1_555 1_555 1_555 no Co1 Co2 CC3 120.6(2) 1_555 1_555 1_555 no Co1 Co2 CC4 123.0(2) 1_555 1_555 1_555 no Co1 Co2 CC7 110.1(2) 1_555 1_555 1_555 no Co1 Co2 CH 48.0(1) 1_555 1_555 1_555 no Co3 Co2 CC1 103.6(2) 1_555 1_555 1_555 no Co3 Co2 CC3 130.3(2) 1_555 1_555 1_555 no Co3 Co2 CC4 119.0(2) 1_555 1_555 1_555 no Co3 Co2 CC7 49.6(2) 1_555 1_555 1_555 no Co3 Co2 CH 50.3(1) 1_555 1_555 1_555 no CC1 Co2 CC3 107.0(2) 1_555 1_555 1_555 no CC1 Co2 CC4 86.5(2) 1_555 1_555 1_555 no CC1 Co2 CC7 146.2(2) 1_555 1_555 1_555 no CC1 Co2 CH 89.8(2) 1_555 1_555 1_555 no CC3 Co2 CC4 101.2(3) 1_555 1_555 1_555 no CC3 Co2 CC7 106.5(2) 1_555 1_555 1_555 no CC3 Co2 CH 91.5(2) 1_555 1_555 1_555 no CC4 Co2 CC7 90.7(2) 1_555 1_555 1_555 no CC4 Co2 CH 167.3(3) 1_555 1_555 1_555 no CC7 Co2 CH 85.7(2) 1_555 1_555 1_555 no Co1 Co3 Co2 61.64(3) 1_555 1_555 1_555 no Co1 Co3 CC2 45.5(2) 1_555 1_555 1_555 no Co1 Co3 CC5 124.1(2) 1_555 1_555 1_555 no Co1 Co3 CC6 110.5(2) 1_555 1_555 1_555 no Co1 Co3 CC7 115.1(2) 1_555 1_555 1_555 no Co1 Co3 CH 48.5(1) 1_555 1_555 1_555 no Co2 Co3 CC2 107.1(2) 1_555 1_555 1_555 no Co2 Co3 CC5 133.5(2) 1_555 1_555 1_555 no Co2 Co3 CC6 113.4(2) 1_555 1_555 1_555 no Co2 Co3 CC7 53.5(2) 1_555 1_555 1_555 no Co2 Co3 CH 50.3(1) 1_555 1_555 1_555 no CC2 Co3 CC5 93.9(3) 1_555 1_555 1_555 no CC2 Co3 CC6 92.0(3) 1_555 1_555 1_555 no CC2 Co3 CC7 160.1(2) 1_555 1_555 1_555 no CC2 Co3 CH 79.3(2) 1_555 1_555 1_555 no CC5 Co3 CC6 106.5(3) 1_555 1_555 1_555 no CC5 Co3 CC7 103.2(3) 1_555 1_555 1_555 no CC5 Co3 CH 96.2(2) 1_555 1_555 1_555 no CC6 Co3 CC7 92.7(3) 1_555 1_555 1_555 no CC6 Co3 CH 156.3(3) 1_555 1_555 1_555 no CC7 Co3 CH 88.8(2) 1_555 1_555 1_555 no Co1 P1 C1 124.3(2) 1_555 1_555 1_555 no Co1 P1 C4 120.6(2) 1_555 1_555 1_555 no Co1 P1 C7 105.3(2) 1_555 1_555 1_555 no C1 P1 C4 94.7(3) 1_555 1_555 1_555 no C1 P1 C7 107.3(2) 1_555 1_555 1_555 no C4 P1 C7 102.3(3) 1_555 1_555 1_555 no Co1 P2 C12 106.6(2) 1_555 1_555 1_555 no Co1 P2 C13 124.5(2) 1_555 1_555 1_555 no Co1 P2 C16 117.5(2) 1_555 1_555 1_555 no C12 P2 C13 105.9(2) 1_555 1_555 1_555 no C12 P2 C16 106.7(2) 1_555 1_555 1_555 no C13 P2 C16 94.0(3) 1_555 1_555 1_555 no P1 C1 C2 105.6(6) 1_555 1_555 1_555 no P1 C1 C5 115.3(5) 1_555 1_555 1_555 no C2 C1 C5 111.7(6) 1_555 1_555 1_555 no C1 C2 C3 111.6(6) 1_555 1_555 1_555 no C2 C3 C4 109.9(7) 1_555 1_555 1_555 no P1 C4 C3 103.2(5) 1_555 1_555 1_555 no P1 C4 C6 116.7(5) 1_555 1_555 1_555 no C3 C4 C6 112.9(6) 1_555 1_555 1_555 no P1 C7 C8 124.0(4) 1_555 1_555 1_555 no P1 C7 C12 116.6(3) 1_555 1_555 1_555 no C8 C7 C12 119.3(4) 1_555 1_555 1_555 no C7 C8 C9 121.0(5) 1_555 1_555 1_555 no C8 C9 C10 119.5(5) 1_555 1_555 1_555 no C9 C10 C11 120.3(5) 1_555 1_555 1_555 no C10 C11 C12 121.3(5) 1_555 1_555 1_555 no P2 C12 C7 117.6(3) 1_555 1_555 1_555 no P2 C12 C11 123.7(4) 1_555 1_555 1_555 no C7 C12 C11 118.6(4) 1_555 1_555 1_555 no P2 C13 C14 104.4(4) 1_555 1_555 1_555 no P2 C13 C17 115.7(4) 1_555 1_555 1_555 no C14 C13 C17 111.4(5) 1_555 1_555 1_555 no C13 C14 C15 108.3(5) 1_555 1_555 1_555 no C14 C15 C16 107.3(5) 1_555 1_555 1_555 no P2 C16 C15 105.5(4) 1_555 1_555 1_555 no P2 C16 C18 118.2(4) 1_555 1_555 1_555 no C15 C16 C18 115.2(5) 1_555 1_555 1_555 no Co1 CC1 Co2 79.7(2) 1_555 1_555 1_555 no Co1 CC1 OC1 147.7(4) 1_555 1_555 1_555 no Co2 CC1 OC1 132.6(4) 1_555 1_555 1_555 no Co1 CC2 Co3 76.7(2) 1_555 1_555 1_555 no Co1 CC2 OC2 156.5(5) 1_555 1_555 1_555 no Co3 CC2 OC2 126.8(4) 1_555 1_555 1_555 no Co2 CC3 OC3 178.1(5) 1_555 1_555 1_555 no Co2 CC4 OC4 175.2(6) 1_555 1_555 1_555 no Co3 CC5 OC5 177.2(6) 1_555 1_555 1_555 no Co3 CC6 OC6 177.3(6) 1_555 1_555 1_555 no Co2 CC7 Co3 76.9(2) 1_555 1_555 1_555 no Co2 CC7 OC7 137.9(5) 1_555 1_555 1_555 no Co3 CC7 OC7 145.3(5) 1_555 1_555 1_555 no Co1 CH Co2 83.6(2) 1_555 1_555 1_555 no Co1 CH Co3 82.5(2) 1_555 1_555 1_555 no Co2 CH Co3 79.3(2) 1_555 1_555 1_555 no