Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global #Paper: B101119G _journal_coden_Cambridge 186 _audit_creation_method 'manual editing' # SUBMISSION DETAILS _publ_contact_author_name 'Marabello Domenica' _publ_contact_author_address ; Dipartimento di Chimica I.F.M. Via P. Giuria 7 10125 TORINO, Italy ; _publ_contact_author_mail 'marabello@ch.unito.it' _publ_contact_author_fax '39(11)6707855' _publ_contact_author_phone '39(11)3919719' _publ_contact_letter ; Please consider this CIF submission for pubblication in Journal of Chemical Society, Dalton Transactions ; _publ_requested_journal 'Journal of Chemical Society, Dalton Transactions' publ_requested_category FM # TITLE AND AUTHOR LIST _publ_section_title ;Activation of alkynols on transition metal carbonyl clusters. Reactions of ethynylcyclohexanol with Fe3(CO)12 and Co2(CO)8. Crystal structures of Co3(CO)9[mu3-CCH2(C6H10OH)], Fe3(CO)9(mu-CO)[mu3-eta2-C=C(C6H10)] and Co2Fe(CO)6(mu-CO)[mu3-eta7-(C6H9)CC(H)C(H)C(H)(C6H10)]. ; ; ; loop_ _publ_author_name 'Gatto, Elisabetta' 'Gervasio, Giuliana' 'Marabello, Domenica' 'Sappa, Enrico' data_Co3(CO)9(CCH2(C6H10OH))#,Complex 2 _database_code_CSD 159811 _chemical_formula_sum 'C17 H13 Co3 O10' _chemical_formula_structural 'Co3(CO)9(CCH2(C6H10OH))' _chemical_formula_weight 554.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.415(4) _cell_length_b 11.316(3) _cell_length_c 17.759(6) _cell_angle_alpha 90.00 _cell_angle_beta 92.76(3) _cell_angle_gamma 90.00 _cell_volume 2090.5(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 30 _cell_measurement_theta_min 9 _cell_measurement_theta_max 15 _exptl_crystal_description prismatic _exptl_crystal_colour black _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.760 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1104 _exptl_absorpt_coefficient_mu 2.403 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.140 _exptl_absorpt_correction_T_max 0.190 _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 'Siemens P4' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 50 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 8058 _diffrn_reflns_av_R_equivalents 0.0366 _diffrn_reflns_av_sigmaI/netI 0.0612 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 30.00 _reflns_number_total 6105 _reflns_number_gt 3446 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens XSCANS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL XP' _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^)+(0.0376P)^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 6105 _refine_ls_number_parameters 323 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1088 _refine_ls_R_factor_gt 0.0474 _refine_ls_wR_factor_ref 0.1004 _refine_ls_wR_factor_gt 0.0820 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicit _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.27894(4) 0.78323(4) 0.23787(2) 0.04131(12) Uani 1 1 d . . . Co2 Co 0.32814(4) 0.66606(4) 0.35245(2) 0.04053(12) Uani 1 1 d . . . Co3 Co 0.32915(4) 0.88465(4) 0.35845(2) 0.04006(12) Uani 1 1 d . . . C1 C 0.1940(3) 0.7786(3) 0.33244(16) 0.0382(6) Uani 1 1 d . . . C2 C 0.0503(3) 0.7812(4) 0.33764(19) 0.0431(7) Uani 1 1 d . . . H2A H 0.026(3) 0.847(3) 0.3087(19) 0.057(11) Uiso 1 1 d . . . H2B H 0.014(3) 0.716(3) 0.3111(18) 0.043(9) Uiso 1 1 d . . . C3 C -0.0117(3) 0.7922(3) 0.41398(18) 0.0408(7) Uani 1 1 d . . . C4 C -0.1575(3) 0.7990(4) 0.3981(2) 0.0536(10) Uani 1 1 d . . . H4A H -0.183(3) 0.728(3) 0.365(2) 0.063(12) Uiso 1 1 d . . . H4B H -0.173(3) 0.871(4) 0.3722(19) 0.065(12) Uiso 1 1 d . . . C5 C -0.2338(4) 0.7988(4) 0.4686(3) 0.0633(11) Uani 1 1 d . . . H5A H -0.222(4) 0.873(3) 0.490(2) 0.060(12) Uiso 1 1 d . . . H5B H -0.337(4) 0.795(4) 0.453(3) 0.093(15) Uiso 1 1 d . . . C6 C -0.2020(4) 0.6909(4) 0.5155(3) 0.0622(11) Uani 1 1 d . . . H6A H -0.249(4) 0.689(4) 0.564(3) 0.085(14) Uiso 1 1 d . . . H6B H -0.231(3) 0.617(3) 0.4820(18) 0.055(10) Uiso 1 1 d . . . C7 C -0.0587(4) 0.6871(5) 0.5358(2) 0.0660(12) Uani 1 1 d . . . H7A H -0.037(3) 0.614(3) 0.565(2) 0.068(12) Uiso 1 1 d . . . H7B H -0.033(4) 0.755(3) 0.570(2) 0.077(14) Uiso 1 1 d . . . C8 C 0.0197(4) 0.6888(4) 0.4658(2) 0.0522(9) Uani 1 1 d . . . H8A H 0.000(3) 0.616(3) 0.4359(19) 0.054(10) Uiso 1 1 d . . . H8B H 0.113(4) 0.693(3) 0.478(2) 0.065(11) Uiso 1 1 d . . . O1 O 0.0346(3) 0.8967(3) 0.4515(2) 0.0660(8) Uani 1 1 d . . . H H 0.003(5) 0.946(5) 0.439(3) 0.12(3) Uiso 1 1 d . . . C11 C 0.1991(4) 0.9057(3) 0.1938(2) 0.0515(9) Uani 1 1 d . . . O11 O 0.1443(3) 0.9820(3) 0.16620(17) 0.0845(9) Uani 1 1 d . . . C12 C 0.1904(4) 0.6718(3) 0.1867(2) 0.0532(9) Uani 1 1 d . . . O12 O 0.1305(3) 0.6026(3) 0.15510(17) 0.0819(9) Uani 1 1 d . . . C13 C 0.4333(4) 0.7849(4) 0.1917(2) 0.0670(11) Uani 1 1 d . . . O13 O 0.5261(3) 0.7853(4) 0.16204(19) 0.1163(14) Uani 1 1 d . . . C21 C 0.2370(3) 0.5362(3) 0.32578(19) 0.0512(9) Uani 1 1 d . . . O21 O 0.1786(3) 0.4565(3) 0.30892(16) 0.0771(9) Uani 1 1 d . . . C22 C 0.3477(4) 0.6342(3) 0.4513(2) 0.0574(10) Uani 1 1 d . . . O22 O 0.3651(3) 0.6115(3) 0.51304(16) 0.0918(10) Uani 1 1 d . . . C23 C 0.4924(4) 0.6349(3) 0.3269(2) 0.0567(9) Uani 1 1 d . . . O23 O 0.5934(3) 0.6166(3) 0.31070(19) 0.0868(10) Uani 1 1 d . . . C31 C 0.3383(4) 0.8921(3) 0.4596(2) 0.0588(10) Uani 1 1 d . . . O31 O 0.3465(4) 0.8975(3) 0.52311(15) 0.0957(11) Uani 1 1 d . . . C32 C 0.2417(3) 1.0189(4) 0.3413(2) 0.0530(9) Uani 1 1 d . . . O32 O 0.1848(3) 1.1022(3) 0.33027(18) 0.0834(9) Uani 1 1 d . . . C33 C 0.4926(3) 0.9241(3) 0.3359(2) 0.0525(9) Uani 1 1 d . . . O33 O 0.5911(2) 0.9511(3) 0.31930(17) 0.0775(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 0.0396(2) 0.0486(3) 0.0357(2) 0.0000(2) 0.00233(17) -0.0003(2) Co2 0.0382(2) 0.0404(2) 0.0429(2) 0.0011(2) 0.00120(18) 0.0050(2) Co3 0.0378(2) 0.0410(2) 0.0415(2) -0.0031(2) 0.00232(18) -0.0024(2) C1 0.0373(15) 0.0394(16) 0.0378(15) 0.0013(15) 0.0012(12) -0.0020(15) C2 0.0323(15) 0.051(2) 0.0462(17) 0.0061(19) 0.0011(13) 0.0013(18) C3 0.0363(15) 0.0356(17) 0.0510(18) -0.0012(15) 0.0063(14) 0.0022(15) C4 0.0391(18) 0.060(3) 0.063(2) 0.016(2) 0.0070(17) 0.0054(18) C5 0.045(2) 0.069(3) 0.078(3) 0.009(2) 0.0158(19) 0.007(2) C6 0.056(2) 0.068(3) 0.065(2) 0.012(2) 0.019(2) 0.000(2) C7 0.062(3) 0.081(3) 0.055(2) 0.019(2) 0.010(2) 0.014(2) C8 0.047(2) 0.057(3) 0.052(2) 0.0040(18) 0.0061(17) 0.0110(18) O1 0.0652(19) 0.0507(18) 0.084(2) -0.0212(16) 0.0181(16) -0.0102(16) C11 0.055(2) 0.050(2) 0.0493(19) 0.0062(17) -0.0057(17) -0.0110(18) O11 0.092(2) 0.0628(19) 0.095(2) 0.0223(17) -0.0333(18) -0.0057(17) C12 0.061(2) 0.052(2) 0.0456(19) -0.0010(18) -0.0050(17) 0.011(2) O12 0.101(2) 0.0614(19) 0.080(2) -0.0142(15) -0.0297(17) -0.0042(17) C13 0.051(2) 0.101(3) 0.050(2) 0.003(2) 0.0086(18) 0.005(2) O13 0.0593(19) 0.213(5) 0.079(2) 0.008(2) 0.0268(17) 0.007(2) C21 0.051(2) 0.054(2) 0.0491(19) 0.0028(17) 0.0033(16) -0.0012(18) O21 0.091(2) 0.0641(19) 0.0756(18) 0.0024(15) 0.0004(16) -0.0302(17) C22 0.066(2) 0.048(2) 0.058(2) -0.0018(19) -0.0056(19) 0.0092(19) O22 0.122(3) 0.095(2) 0.0557(17) 0.0128(17) -0.0141(18) 0.013(2) C23 0.050(2) 0.048(2) 0.071(2) -0.0066(19) -0.0021(19) 0.0073(19) O23 0.0416(16) 0.094(2) 0.126(3) -0.016(2) 0.0098(16) 0.0163(16) C31 0.071(3) 0.047(2) 0.058(2) -0.0107(18) -0.004(2) -0.0050(19) O31 0.150(3) 0.089(2) 0.0468(16) -0.0114(16) -0.0040(18) 0.004(2) C32 0.052(2) 0.052(2) 0.055(2) -0.0038(18) 0.0068(17) 0.0039(19) O32 0.094(2) 0.064(2) 0.092(2) -0.0028(17) 0.0058(18) 0.0254(18) C33 0.044(2) 0.055(2) 0.058(2) -0.0005(18) -0.0017(17) -0.0078(19) O33 0.0430(16) 0.095(2) 0.094(2) 0.0131(18) 0.0042(14) -0.0122(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 C11 1.778(4) . ? Co1 C12 1.785(4) . ? Co1 C13 1.840(4) . ? Co1 C1 1.936(3) . ? Co1 Co2 2.4619(9) . ? Co1 Co3 2.4634(9) . ? Co2 C22 1.793(4) . ? Co2 C21 1.800(4) . ? Co2 C23 1.825(4) . ? Co2 C1 1.911(3) . ? Co2 Co3 2.4759(9) . ? Co3 C32 1.790(4) . ? Co3 C31 1.796(4) . ? Co3 C33 1.823(4) . ? Co3 C1 1.890(3) . ? C1 C2 1.504(4) . ? C2 C3 1.535(5) . ? C3 O1 1.429(4) . ? C3 C8 1.514(5) . ? C3 C4 1.533(5) . ? C4 C5 1.515(5) . ? C5 C6 1.507(6) . ? C6 C7 1.519(6) . ? C7 C8 1.520(5) . ? C11 O11 1.133(4) . ? C12 O12 1.133(4) . ? C13 O13 1.122(5) . ? C21 O21 1.120(4) . ? C22 O22 1.133(4) . ? C23 O23 1.123(4) . ? C31 O31 1.128(4) . ? C32 O32 1.126(4) . ? C33 O33 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 C11 Co1 C12 96.16(16) . . ? C11 Co1 C13 101.31(18) . . ? C12 Co1 C13 102.78(18) . . ? C11 Co1 C1 100.35(15) . . ? C12 Co1 C1 100.15(16) . . ? C13 Co1 C1 146.34(15) . . ? C11 Co1 Co2 149.08(12) . . ? C12 Co1 Co2 97.03(12) . . ? C13 Co1 Co2 102.84(13) . . ? C1 Co1 Co2 49.75(9) . . ? C11 Co1 Co3 95.44(12) . . ? C12 Co1 Co3 148.73(13) . . ? C13 Co1 Co3 103.25(13) . . ? C1 Co1 Co3 49.11(9) . . ? Co2 Co1 Co3 60.36(3) . . ? C22 Co2 C21 97.31(16) . . ? C22 Co2 C23 98.11(18) . . ? C21 Co2 C23 105.38(16) . . ? C22 Co2 C1 111.30(15) . . ? C21 Co2 C1 97.10(15) . . ? C23 Co2 C1 140.18(15) . . ? C22 Co2 Co1 157.85(12) . . ? C21 Co2 Co1 97.82(11) . . ? C23 Co2 Co1 93.36(13) . . ? C1 Co2 Co1 50.67(9) . . ? C22 Co2 Co3 99.11(12) . . ? C21 Co2 Co3 145.89(11) . . ? C23 Co2 Co3 101.64(12) . . ? C1 Co2 Co3 49.00(10) . . ? Co1 Co2 Co3 59.85(2) . . ? C32 Co3 C31 97.61(17) . . ? C32 Co3 C33 103.18(17) . . ? C31 Co3 C33 101.73(17) . . ? C32 Co3 C1 97.50(15) . . ? C31 Co3 C1 106.08(16) . . ? C33 Co3 C1 142.56(15) . . ? C32 Co3 Co1 99.34(12) . . ? C31 Co3 Co1 152.87(12) . . ? C33 Co3 Co1 94.84(12) . . ? C1 Co3 Co1 50.75(9) . . ? C32 Co3 Co2 147.08(12) . . ? C31 Co3 Co2 95.16(12) . . ? C33 Co3 Co2 103.72(12) . . ? C1 Co3 Co2 49.71(10) . . ? Co1 Co3 Co2 59.79(2) . . ? C2 C1 Co3 134.7(3) . . ? C2 C1 Co2 136.3(3) . . ? Co3 C1 Co2 81.29(12) . . ? C2 C1 Co1 123.4(2) . . ? Co3 C1 Co1 80.14(12) . . ? Co2 C1 Co1 79.57(12) . . ? C1 C2 C3 121.2(3) . . ? O1 C3 C8 107.3(3) . . ? O1 C3 C4 110.7(3) . . ? C8 C3 C4 109.5(3) . . ? O1 C3 C2 109.4(3) . . ? C8 C3 C2 112.7(3) . . ? C4 C3 C2 107.3(3) . . ? C5 C4 C3 113.7(3) . . ? C6 C5 C4 110.4(4) . . ? C5 C6 C7 109.9(4) . . ? C6 C7 C8 111.5(3) . . ? C3 C8 C7 113.4(3) . . ? O11 C11 Co1 177.6(4) . . ? O12 C12 Co1 177.7(4) . . ? O13 C13 Co1 178.4(4) . . ? O21 C21 Co2 178.9(4) . . ? O22 C22 Co2 176.9(4) . . ? O23 C23 Co2 179.4(4) . . ? O31 C31 Co3 178.6(4) . . ? O32 C32 Co3 178.8(4) . . ? O33 C33 Co3 176.9(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.349 _refine_diff_density_min -0.367 _refine_diff_density_rms 0.081 #===END data_Fe3(CO)10(C2(C6H10))# Complex 5 _database_code_CSD 159812 _audit_creation_method 'manual editing' _chemical_formula_structural 'Fe3(CO)10(C2(C6H10))' 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' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.0953(16) _cell_length_b 10.366(2) _cell_length_c 12.665(2) _cell_angle_alpha 90.00 _cell_angle_beta 109.838(10) _cell_angle_gamma 90.00 _cell_volume 2111.1(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 30 _cell_measurement_theta_min 10 _cell_measurement_theta_max 17 _exptl_crystal_description prismatic _exptl_crystal_colour black _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.742 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1104 _exptl_absorpt_coefficient_mu 2.086 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.360 _exptl_absorpt_correction_T_max 0.439 _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 'Siemens P4' _diffrn_measurement_method \q--2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 50 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 8022 _diffrn_reflns_av_R_equivalents 0.0291 _diffrn_reflns_av_sigmaI/netI 0.0586 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 30.01 _reflns_number_total 6159 _reflns_number_gt 3822 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens XSCANS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELTL XP' _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^)+(0.0345P)^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 6159 _refine_ls_number_parameters 310 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0936 _refine_ls_R_factor_gt 0.0444 _refine_ls_wR_factor_ref 0.0918 _refine_ls_wR_factor_gt 0.0771 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.105 _refine_ls_shift/su_mean 0.013 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 Fe1 Fe 0.26716(2) 0.01935(4) 0.27966(3) 0.03741(11) Uani 1 1 d . . . Fe2 Fe 0.37378(2) -0.07565(4) 0.19425(3) 0.03776(11) Uani 1 1 d . . . Fe3 Fe 0.27117(2) 0.09633(4) 0.08592(3) 0.04069(11) Uani 1 1 d . . . C1 C 0.25482(16) -0.0723(3) 0.1357(2) 0.0364(6) Uani 1 1 d . . . C2 C 0.19467(17) -0.1248(3) 0.1687(2) 0.0392(6) Uani 1 1 d . . . C3 C 0.13254(16) -0.2055(3) 0.1586(2) 0.0397(6) Uani 1 1 d . . . C4 C 0.08625(19) -0.2176(3) 0.2403(3) 0.0450(7) Uani 1 1 d . . . H4A H 0.110(2) -0.157(3) 0.303(3) 0.060 Uiso 1 1 d . . . H4B H 0.027(2) -0.200(3) 0.201(3) 0.060 Uiso 1 1 d . . . C5 C 0.0929(2) -0.3544(4) 0.2859(3) 0.0574(9) Uani 1 1 d . . . H5A H 0.151(2) -0.367(3) 0.334(3) 0.070 Uiso 1 1 d . . . H5B H 0.065(2) -0.360(3) 0.334(3) 0.070 Uiso 1 1 d . . . C6 C 0.0671(3) -0.4538(4) 0.1929(4) 0.0665(10) Uani 1 1 d . . . H6A H 0.010(2) -0.440(4) 0.154(3) 0.080 Uiso 1 1 d . . . H6B H 0.076(2) -0.538(4) 0.223(3) 0.080 Uiso 1 1 d . . . C7 C 0.1141(2) -0.4387(3) 0.1127(3) 0.0580(9) Uani 1 1 d . . . H7A H 0.098(2) -0.504(3) 0.055(3) 0.070 Uiso 1 1 d . . . H7B H 0.167(2) -0.455(3) 0.148(3) 0.070 Uiso 1 1 d . . . C8 C 0.1063(2) -0.3023(3) 0.0644(3) 0.0510(8) Uani 1 1 d . . . H8A H 0.137(2) -0.295(3) 0.020(3) 0.060 Uiso 1 1 d . . . H8B H 0.045(2) -0.284(3) 0.018(3) 0.060 Uiso 1 1 d . . . C11 C 0.2801(2) -0.0848(3) 0.3981(3) 0.0523(8) Uani 1 1 d . . . O11 O 0.28583(18) -0.1499(3) 0.4721(2) 0.0848(8) Uani 1 1 d . . . C12 C 0.1802(2) 0.1089(3) 0.2872(3) 0.0570(8) Uani 1 1 d . . . O12 O 0.12606(17) 0.1677(3) 0.2947(3) 0.0991(10) Uani 1 1 d . . . C13 C 0.34390(19) 0.1360(3) 0.3521(3) 0.0494(7) Uani 1 1 d . . . O13 O 0.39162(15) 0.2093(2) 0.4001(2) 0.0737(7) Uani 1 1 d . . . C21 C 0.35897(19) -0.2372(3) 0.2391(3) 0.0512(8) Uani 1 1 d . . . O21 O 0.34802(17) -0.3383(2) 0.2639(3) 0.0805(8) Uani 1 1 d . . . C22 C 0.4172(2) -0.1381(4) 0.0923(3) 0.0584(8) Uani 1 1 d . . . O22 O 0.44246(17) -0.1750(3) 0.0266(2) 0.0968(10) Uani 1 1 d . . . C23 C 0.4678(2) -0.0465(3) 0.3154(3) 0.0522(8) Uani 1 1 d . . . O23 O 0.52545(16) -0.0273(3) 0.3894(2) 0.0823(8) Uani 1 1 d . . . C31 C 0.1602(2) 0.1087(4) 0.0385(3) 0.0684(10) Uani 1 1 d . . . O31 O 0.08984(16) 0.1154(4) 0.0069(3) 0.1104(12) Uani 1 1 d . . . C32 C 0.2725(2) 0.0801(3) -0.0560(3) 0.0520(8) Uani 1 1 d . . . O32 O 0.27187(19) 0.0678(3) -0.1444(2) 0.0816(8) Uani 1 1 d . . . C33 C 0.2854(2) 0.2685(3) 0.1093(3) 0.0563(8) Uani 1 1 d . . . O33 O 0.2936(2) 0.3769(2) 0.1221(3) 0.0886(9) Uani 1 1 d . . . C44 C 0.39677(19) 0.0988(3) 0.1499(3) 0.0484(7) Uani 1 1 d . . . O44 O 0.45057(14) 0.1672(2) 0.1540(2) 0.0763(8) 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 Fe1 0.0358(2) 0.0402(2) 0.0377(2) -0.00049(18) 0.01437(17) 0.00249(17) Fe2 0.03163(19) 0.0402(2) 0.0420(2) 0.00152(18) 0.01321(17) 0.00425(16) Fe3 0.0379(2) 0.0428(2) 0.0423(2) 0.00936(18) 0.01469(18) 0.00391(17) C1 0.0352(13) 0.0408(14) 0.0323(13) 0.0014(12) 0.0103(11) 0.0033(12) C2 0.0363(14) 0.0429(15) 0.0372(15) 0.0044(12) 0.0111(12) 0.0042(12) C3 0.0326(13) 0.0477(16) 0.0384(15) 0.0031(13) 0.0114(12) 0.0027(12) C4 0.0381(15) 0.0535(17) 0.0470(17) -0.0007(15) 0.0192(14) -0.0034(14) C5 0.062(2) 0.064(2) 0.055(2) 0.0086(18) 0.0304(18) -0.0056(18) C6 0.073(2) 0.054(2) 0.079(3) 0.0010(19) 0.034(2) -0.0112(19) C7 0.057(2) 0.053(2) 0.062(2) -0.0124(17) 0.0180(18) -0.0041(17) C8 0.0431(17) 0.067(2) 0.0430(17) -0.0036(16) 0.0145(14) -0.0057(16) C11 0.0549(18) 0.058(2) 0.0455(18) 0.0004(16) 0.0188(15) 0.0013(15) O11 0.102(2) 0.092(2) 0.0626(16) 0.0335(16) 0.0307(15) 0.0053(17) C12 0.0466(17) 0.0573(19) 0.071(2) -0.0090(17) 0.0258(17) -0.0029(16) O12 0.0629(17) 0.092(2) 0.156(3) -0.017(2) 0.0550(19) 0.0198(15) C13 0.0450(17) 0.0528(18) 0.0498(18) -0.0060(16) 0.0154(15) 0.0084(15) O13 0.0602(15) 0.0675(16) 0.0850(18) -0.0286(15) 0.0136(14) -0.0112(13) C21 0.0432(16) 0.0522(19) 0.058(2) 0.0057(16) 0.0176(15) 0.0063(14) O21 0.0780(17) 0.0485(14) 0.112(2) 0.0244(15) 0.0286(16) 0.0040(13) C22 0.0438(17) 0.072(2) 0.059(2) -0.0061(18) 0.0167(16) 0.0097(16) O22 0.0822(19) 0.141(3) 0.081(2) -0.0208(19) 0.0455(17) 0.0265(19) C23 0.0483(17) 0.0498(18) 0.0556(19) -0.0018(15) 0.0138(16) 0.0111(15) O23 0.0593(15) 0.0917(19) 0.0713(17) -0.0125(15) -0.0101(14) 0.0116(14) C31 0.053(2) 0.080(3) 0.072(2) 0.033(2) 0.0194(19) 0.0178(18) O31 0.0429(15) 0.153(3) 0.126(3) 0.061(2) 0.0156(17) 0.0283(17) C32 0.0572(19) 0.0463(17) 0.0500(19) 0.0037(15) 0.0152(16) -0.0095(15) O32 0.113(2) 0.0887(19) 0.0465(14) -0.0088(13) 0.0314(15) -0.0252(16) C33 0.063(2) 0.0499(19) 0.061(2) 0.0085(16) 0.0270(17) 0.0109(16) O33 0.122(2) 0.0468(15) 0.108(2) 0.0017(15) 0.054(2) 0.0097(16) C44 0.0429(16) 0.0537(18) 0.0485(17) 0.0050(15) 0.0155(14) 0.0004(15) O44 0.0473(13) 0.0690(16) 0.106(2) 0.0239(15) 0.0176(14) -0.0138(12) _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 Fe1 C12 1.782(3) . ? Fe1 C13 1.791(3) . ? Fe1 C11 1.800(3) . ? Fe1 C1 2.002(3) . ? Fe1 C2 2.135(3) . ? Fe1 Fe3 2.6031(7) . ? Fe1 Fe2 2.6077(6) . ? Fe2 C22 1.812(4) . ? Fe2 C21 1.814(3) . ? Fe2 C23 1.832(3) . ? Fe2 C1 1.914(3) . ? Fe2 C44 1.972(3) . ? Fe2 Fe3 2.5503(6) . ? Fe3 C31 1.790(4) . ? Fe3 C33 1.811(3) . ? Fe3 C32 1.813(3) . ? Fe3 C1 1.911(3) . ? Fe3 C44 2.021(3) . ? C1 C2 1.349(4) . ? C2 C3 1.324(4) . ? C3 C8 1.506(4) . ? C3 C4 1.506(4) . ? C4 C5 1.520(5) . ? C5 C6 1.514(5) . ? C6 C7 1.501(5) . ? C7 C8 1.529(5) . ? C11 O11 1.131(4) . ? C12 O12 1.139(4) . ? C13 O13 1.130(4) . ? C21 O21 1.127(4) . ? C22 O22 1.128(4) . ? C23 O23 1.123(4) . ? C31 O31 1.134(4) . ? C32 O32 1.124(4) . ? C33 O33 1.137(4) . ? C44 O44 1.149(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 Fe1 C13 95.77(14) . . ? C12 Fe1 C11 97.83(16) . . ? C13 Fe1 C11 96.72(15) . . ? C12 Fe1 C1 117.63(13) . . ? C13 Fe1 C1 128.24(13) . . ? C11 Fe1 C1 114.79(13) . . ? C12 Fe1 C2 95.23(13) . . ? C13 Fe1 C2 165.91(12) . . ? C11 Fe1 C2 90.47(13) . . ? C1 Fe1 C2 37.87(11) . . ? C12 Fe1 Fe3 100.38(12) . . ? C13 Fe1 Fe3 91.52(10) . . ? C11 Fe1 Fe3 159.13(10) . . ? C1 Fe1 Fe3 46.82(8) . . ? C2 Fe1 Fe3 77.83(8) . . ? C12 Fe1 Fe2 158.74(12) . . ? C13 Fe1 Fe2 88.49(9) . . ? C11 Fe1 Fe2 102.35(10) . . ? C1 Fe1 Fe2 46.82(7) . . ? C2 Fe1 Fe2 78.12(8) . . ? Fe3 Fe1 Fe2 58.604(17) . . ? C22 Fe2 C21 91.59(16) . . ? C22 Fe2 C23 101.57(14) . . ? C21 Fe2 C23 93.80(14) . . ? C22 Fe2 C1 111.62(13) . . ? C21 Fe2 C1 83.98(13) . . ? C23 Fe2 C1 146.77(13) . . ? C22 Fe2 C44 87.44(15) . . ? C21 Fe2 C44 176.73(13) . . ? C23 Fe2 C44 83.34(14) . . ? C1 Fe2 C44 99.29(12) . . ? C22 Fe2 Fe3 103.85(11) . . ? C21 Fe2 Fe3 132.10(10) . . ? C23 Fe2 Fe3 125.67(10) . . ? C1 Fe2 Fe3 48.13(8) . . ? C44 Fe2 Fe3 51.17(9) . . ? C22 Fe2 Fe1 160.53(10) . . ? C21 Fe2 Fe1 91.57(10) . . ? C23 Fe2 Fe1 97.38(10) . . ? C1 Fe2 Fe1 49.72(8) . . ? C44 Fe2 Fe1 90.38(9) . . ? Fe3 Fe2 Fe1 60.607(17) . . ? C31 Fe3 C33 93.01(17) . . ? C31 Fe3 C32 92.45(17) . . ? C33 Fe3 C32 101.95(14) . . ? C31 Fe3 C1 85.36(14) . . ? C33 Fe3 C1 150.89(13) . . ? C32 Fe3 C1 107.15(13) . . ? C31 Fe3 C44 173.90(17) . . ? C33 Fe3 C44 81.75(14) . . ? C32 Fe3 C44 91.70(14) . . ? C1 Fe3 C44 97.68(12) . . ? C31 Fe3 Fe2 133.46(12) . . ? C33 Fe3 Fe2 124.81(11) . . ? C32 Fe3 Fe2 103.34(11) . . ? C1 Fe3 Fe2 48.23(8) . . ? C44 Fe3 Fe2 49.46(9) . . ? C31 Fe3 Fe1 88.52(12) . . ? C33 Fe3 Fe1 101.13(11) . . ? C32 Fe3 Fe1 156.81(10) . . ? C1 Fe3 Fe1 49.82(8) . . ? C44 Fe3 Fe1 89.43(9) . . ? Fe2 Fe3 Fe1 60.788(16) . . ? C2 C1 Fe3 133.1(2) . . ? C2 C1 Fe2 134.0(2) . . ? Fe3 C1 Fe2 83.63(11) . . ? C2 C1 Fe1 76.41(17) . . ? Fe3 C1 Fe1 83.36(11) . . ? Fe2 C1 Fe1 83.47(10) . . ? C3 C2 C1 153.6(3) . . ? C3 C2 Fe1 140.7(2) . . ? C1 C2 Fe1 65.71(16) . . ? C2 C3 C8 120.7(3) . . ? C2 C3 C4 125.3(3) . . ? C8 C3 C4 113.9(3) . . ? C3 C4 C5 110.5(3) . . ? C6 C5 C4 112.0(3) . . ? C7 C6 C5 112.0(3) . . ? C6 C7 C8 112.0(3) . . ? C3 C8 C7 109.7(3) . . ? O11 C11 Fe1 178.1(3) . . ? O12 C12 Fe1 178.1(3) . . ? O13 C13 Fe1 178.2(3) . . ? O21 C21 Fe2 177.9(3) . . ? O22 C22 Fe2 178.0(3) . . ? O23 C23 Fe2 179.3(3) . . ? O31 C31 Fe3 178.8(4) . . ? O32 C32 Fe3 178.3(3) . . ? O33 C33 Fe3 178.8(4) . . ? O44 C44 Fe2 141.9(3) . . ? O44 C44 Fe3 138.7(3) . . ? Fe2 C44 Fe3 79.36(12) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.356 _refine_diff_density_min -0.334 _refine_diff_density_rms 0.073 #===END data_Co2Fe(CO)7((C6H9)CCHCHCH(C6H10))# Complex 8 _database_code_CSD 159813 _audit_creation_method 'manual editing' _chemical_formula_structural 'Co2Fe(CO)7((C6H9)CCHCHCH(C6H10)' 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.717(3) _cell_length_b 13.524(5) _cell_length_c 20.427(7) _cell_angle_alpha 90.00 _cell_angle_beta 93.23(2) _cell_angle_gamma 90.00 _cell_volume 2404.4(15) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 35 _cell_measurement_theta_min 10 _cell_measurement_theta_max 17 _exptl_crystal_description lamina _exptl_crystal_colour black _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.614 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1184 _exptl_absorpt_coefficient_mu 1.999 _exptl_absorpt_correction_type integration numerical gaussian _exptl_absorpt_correction_T_min 0.620 _exptl_absorpt_correction_T_max 0.824 _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 'Siemens P4' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 50 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 5833 _diffrn_reflns_av_R_equivalents 0.0483 _diffrn_reflns_av_sigmaI/netI 0.0716 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 25.04 _reflns_number_total 4228 _reflns_number_gt 2789 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens XSCANS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL XP' _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^)+(0.0964P)^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 4228 _refine_ls_number_parameters 302 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0987 _refine_ls_R_factor_gt 0.0594 _refine_ls_wR_factor_ref 0.16709 _refine_ls_wR_factor_gt 0.1405 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _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_multiplicit _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.39419(8) 0.91359(6) 0.15447(4) 0.0369(2) Uani 1 1 d . . . Fe2 Fe 0.66373(9) 0.95487(7) 0.20102(4) 0.0476(3) Uani 1 1 d . . . Co3 Co 0.43099(9) 0.99171(6) 0.26611(4) 0.0454(3) Uani 1 1 d . . . C11 C 0.2023(8) 0.8696(5) 0.1523(3) 0.0541(17) Uani 1 1 d . . . O11 O 0.0803(6) 0.8401(4) 0.1476(3) 0.0810(16) Uani 1 1 d . . . C12 C 0.3642(8) 1.0177(5) 0.1000(3) 0.0515(16) Uani 1 1 d . . . O12 O 0.3447(7) 1.0832(4) 0.0660(3) 0.0827(16) Uani 1 1 d . . . C21 C 0.7727(8) 1.0121(6) 0.1411(4) 0.0634(19) Uani 1 1 d . . . O21 O 0.8459(7) 1.0483(5) 0.1032(3) 0.0936(18) Uani 1 1 d . . . C22 C 0.8125(8) 0.9646(6) 0.2643(4) 0.071(2) Uani 1 1 d . . . O22 O 0.9042(7) 0.9744(6) 0.3050(3) 0.117(2) Uani 1 1 d . . . C23 C 0.5641(8) 1.0765(5) 0.2179(4) 0.0594(18) Uani 1 1 d . . . O23 O 0.5686(6) 1.1620(4) 0.2087(3) 0.0831(16) Uani 1 1 d . . . C31 C 0.2593(9) 1.0562(5) 0.2420(3) 0.0559(17) Uani 1 1 d . . . O31 O 0.1521(6) 1.1007(4) 0.2276(3) 0.0770(15) Uani 1 1 d . . . C32 C 0.4941(9) 1.0493(6) 0.3420(4) 0.069(2) Uani 1 1 d . . . O32 O 0.5332(8) 1.0920(5) 0.3874(3) 0.112(2) Uani 1 1 d . . . C1 C 0.5673(6) 0.8449(4) 0.0989(3) 0.0427(14) Uani 1 1 d . . . H1 H 0.6120 0.8847 0.0606 0.045(15) Uiso 1 1 d . . . C2 C 0.6837(7) 0.8206(5) 0.1505(3) 0.0510(16) Uani 1 1 d . . . H2 H 0.7754 0.7971 0.1302 0.054(18) Uiso 1 1 d . . . C3 C 0.6409(6) 0.8033(5) 0.2134(3) 0.0443(15) Uani 1 1 d . . . H3 H 0.7097 0.7733 0.2502 0.048(16) Uiso 1 1 d . . . C4 C 0.4972(6) 0.8474(4) 0.2301(3) 0.0386(13) Uani 1 1 d . . . C5 C 0.4374(6) 0.8362(4) 0.2949(3) 0.0400(13) Uani 1 1 d . . . C6 C 0.2897(7) 0.8601(5) 0.3062(3) 0.0470(15) Uani 1 1 d . . . H6 H 0.2100 0.8645 0.2665 0.07(2) Uiso 1 1 d . . . C7 C 0.2213(8) 0.8534(6) 0.3716(3) 0.065(2) Uani 1 1 d . . . H7A H 0.1513 0.7977 0.3714 0.078 Uiso 1 1 calc R . . H7B H 0.1621 0.9128 0.3787 0.078 Uiso 1 1 calc R . . C8 C 0.3405(9) 0.8414(7) 0.4275(3) 0.080(2) Uani 1 1 d . . . H8A H 0.3876 0.9049 0.4377 0.096 Uiso 1 1 calc R . . H8B H 0.2911 0.8185 0.4661 0.096 Uiso 1 1 calc R . . C9 C 0.4589(9) 0.7709(7) 0.4110(3) 0.081(2) Uani 1 1 d . . . H9A H 0.4116 0.7065 0.4042 0.097 Uiso 1 1 calc R . . H9B H 0.5331 0.7654 0.4480 0.097 Uiso 1 1 calc R . . C10 C 0.5429(7) 0.7976(5) 0.3509(3) 0.0572(18) Uani 1 1 d . . . H10A H 0.5964 0.7396 0.3360 0.069 Uiso 1 1 calc R . . H10B H 0.6194 0.8476 0.3626 0.069 Uiso 1 1 calc R . . C13 C 0.4285(6) 0.7957(4) 0.0852(3) 0.0405(14) Uani 1 1 d . . . C14 C 0.4001(8) 0.6933(4) 0.1117(3) 0.0512(16) Uani 1 1 d . . . H14A H 0.2921 0.6854 0.1196 0.061 Uiso 1 1 calc R . . H14B H 0.4593 0.6839 0.1529 0.061 Uiso 1 1 calc R . . C15 C 0.4483(10) 0.6168(5) 0.0612(4) 0.077(2) Uani 1 1 d . . . H15A H 0.5583 0.6213 0.0568 0.092 Uiso 1 1 calc R . . H15B H 0.4258 0.5509 0.0769 0.092 Uiso 1 1 calc R . . C16 C 0.3661(11) 0.6321(5) -0.0053(4) 0.079(2) Uani 1 1 d . . . H16A H 0.2567 0.6212 -0.0022 0.095 Uiso 1 1 calc R . . H16B H 0.4035 0.5847 -0.0363 0.095 Uiso 1 1 calc R . . C17 C 0.3937(8) 0.7370(5) -0.0297(3) 0.0616(19) Uani 1 1 d . . . H17A H 0.5017 0.7451 -0.0375 0.074 Uiso 1 1 calc R . . H17B H 0.3354 0.7472 -0.0710 0.074 Uiso 1 1 calc R . . C18 C 0.3471(7) 0.8133(5) 0.0191(3) 0.0474(15) Uani 1 1 d . . . H18A H 0.2369 0.8102 0.0233 0.057 Uiso 1 1 calc R . . H18B H 0.3721 0.8787 0.0035 0.057 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0332(4) 0.0358(5) 0.0411(5) 0.0025(4) -0.0022(3) 0.0021(3) Fe2 0.0358(5) 0.0524(6) 0.0538(6) 0.0047(5) -0.0064(4) -0.0057(4) Co3 0.0483(5) 0.0407(5) 0.0464(5) -0.0032(4) -0.0051(4) 0.0029(4) C11 0.046(4) 0.073(5) 0.043(4) -0.001(3) 0.001(3) 0.003(4) O11 0.041(3) 0.104(4) 0.098(4) -0.012(3) 0.004(3) -0.014(3) C12 0.058(4) 0.051(4) 0.045(4) -0.003(3) 0.002(3) -0.005(3) O12 0.115(5) 0.064(3) 0.070(3) 0.026(3) 0.006(3) 0.009(3) C21 0.058(4) 0.065(5) 0.066(5) 0.003(4) -0.010(4) -0.009(4) O21 0.094(4) 0.097(4) 0.091(4) 0.017(4) 0.020(4) -0.031(4) C22 0.051(4) 0.082(6) 0.077(5) 0.008(4) -0.009(4) -0.001(4) O22 0.078(4) 0.160(7) 0.108(5) 0.004(5) -0.051(4) -0.026(4) C23 0.054(4) 0.048(5) 0.075(5) 0.000(4) -0.006(3) -0.005(3) O23 0.091(4) 0.045(3) 0.112(4) 0.003(3) 0.001(3) -0.013(3) C31 0.072(5) 0.041(4) 0.055(4) 0.005(3) 0.007(3) 0.008(4) O31 0.076(4) 0.074(4) 0.081(4) 0.005(3) 0.003(3) 0.034(3) C32 0.086(6) 0.063(5) 0.057(5) -0.010(4) -0.009(4) -0.002(4) O32 0.148(6) 0.104(5) 0.079(4) -0.042(4) -0.027(4) -0.006(4) C1 0.042(3) 0.042(4) 0.045(3) -0.001(3) 0.008(3) -0.001(3) C2 0.031(3) 0.062(4) 0.059(4) 0.003(3) 0.001(3) 0.009(3) C3 0.031(3) 0.052(4) 0.049(4) 0.005(3) -0.007(3) 0.003(3) C4 0.039(3) 0.034(3) 0.041(3) -0.001(3) -0.008(3) 0.003(3) C5 0.038(3) 0.037(3) 0.045(3) 0.005(3) -0.003(3) -0.002(3) C6 0.045(3) 0.049(4) 0.047(4) 0.003(3) 0.005(3) 0.008(3) C7 0.070(5) 0.072(5) 0.055(4) 0.012(4) 0.019(4) 0.020(4) C8 0.085(6) 0.103(7) 0.051(4) 0.006(4) 0.013(4) 0.010(5) C9 0.077(5) 0.116(7) 0.050(4) 0.025(5) -0.002(4) 0.020(5) C10 0.053(4) 0.063(5) 0.053(4) 0.015(3) -0.009(3) 0.010(3) C13 0.037(3) 0.041(4) 0.043(3) -0.001(3) 0.004(3) 0.003(3) C14 0.053(4) 0.039(4) 0.061(4) 0.007(3) 0.004(3) 0.001(3) C15 0.104(6) 0.048(4) 0.080(5) -0.009(4) 0.014(5) 0.013(4) C16 0.108(6) 0.055(5) 0.075(5) -0.027(4) 0.009(5) -0.005(4) C17 0.068(5) 0.065(5) 0.053(4) -0.014(4) 0.006(3) -0.003(4) C18 0.049(4) 0.052(4) 0.041(3) -0.004(3) -0.003(3) 0.001(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 C11 1.774(7) . ? Co1 C12 1.804(7) . ? Co1 C4 1.960(5) . ? Co1 C1 2.150(6) . ? Co1 C13 2.164(6) . ? Co1 Co3 2.5176(13) . ? Co1 Fe2 2.5466(13) . ? Fe2 C21 1.769(8) . ? Fe2 C22 1.784(8) . ? Fe2 C23 1.901(7) . ? Fe2 C3 2.076(6) . ? Fe2 C2 2.100(7) . ? Fe2 C4 2.162(6) . ? Fe2 Co3 2.5369(14) . ? Co3 C31 1.778(8) . ? Co3 C32 1.793(8) . ? Co3 C23 1.939(7) . ? Co3 C4 2.175(6) . ? Co3 C5 2.184(6) . ? Co3 C6 2.339(6) . ? C11 O11 1.135(7) . ? C12 O12 1.132(7) . ? C21 O21 1.142(8) . ? C22 O22 1.128(9) . ? C23 O23 1.172(8) . ? C31 O31 1.136(8) . ? C32 O32 1.129(8) . ? C1 C13 1.396(8) . ? C1 C2 1.459(8) . ? C2 C3 1.376(8) . ? C3 C4 1.446(8) . ? C4 C5 1.457(8) . ? C5 C6 1.360(8) . ? C5 C10 1.518(8) . ? C6 C7 1.495(8) . ? C7 C8 1.509(10) . ? C8 C9 1.458(10) . ? C9 C10 1.509(9) . ? C13 C18 1.508(8) . ? C13 C14 1.512(8) . ? C14 C15 1.537(9) . ? C15 C16 1.515(11) . ? C16 C17 1.527(10) . ? C17 C18 1.507(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 Co1 C12 98.2(3) . . ? C11 Co1 C4 104.8(3) . . ? C12 Co1 C4 152.5(3) . . ? C11 Co1 C1 122.1(3) . . ? C12 Co1 C1 95.3(3) . . ? C4 Co1 C1 85.1(2) . . ? C11 Co1 C13 84.4(3) . . ? C12 Co1 C13 101.1(3) . . ? C4 Co1 C13 96.0(2) . . ? C1 Co1 C13 37.8(2) . . ? C11 Co1 Co3 103.6(2) . . ? C12 Co1 Co3 103.8(2) . . ? C4 Co1 Co3 56.49(16) . . ? C1 Co1 Co3 127.02(16) . . ? C13 Co1 Co3 152.42(16) . . ? C11 Co1 Fe2 158.7(2) . . ? C12 Co1 Fe2 99.1(2) . . ? C4 Co1 Fe2 55.50(17) . . ? C1 Co1 Fe2 68.37(16) . . ? C13 Co1 Fe2 104.30(15) . . ? Co3 Co1 Fe2 60.12(4) . . ? C21 Fe2 C22 94.1(3) . . ? C21 Fe2 C23 90.9(3) . . ? C22 Fe2 C23 97.2(3) . . ? C21 Fe2 C3 125.1(3) . . ? C22 Fe2 C3 93.2(3) . . ? C23 Fe2 C3 141.7(3) . . ? C21 Fe2 C2 88.6(3) . . ? C22 Fe2 C2 110.0(3) . . ? C23 Fe2 C2 152.7(3) . . ? C3 Fe2 C2 38.5(2) . . ? C21 Fe2 C4 151.6(3) . . ? C22 Fe2 C4 108.8(3) . . ? C23 Fe2 C4 102.2(3) . . ? C3 Fe2 C4 39.8(2) . . ? C2 Fe2 C4 68.2(2) . . ? C21 Fe2 Co3 138.9(2) . . ? C22 Fe2 Co3 100.1(3) . . ? C23 Fe2 Co3 49.3(2) . . ? C3 Fe2 Co3 92.61(17) . . ? C2 Fe2 Co3 121.19(17) . . ? C4 Fe2 Co3 54.45(15) . . ? C21 Fe2 Co1 111.0(2) . . ? C22 Fe2 Co1 154.8(3) . . ? C23 Fe2 Co1 80.6(2) . . ? C3 Fe2 Co1 74.71(15) . . ? C2 Fe2 Co1 74.18(16) . . ? C4 Fe2 Co1 48.35(14) . . ? Co3 Fe2 Co1 59.37(4) . . ? C31 Co3 C32 103.8(3) . . ? C31 Co3 C23 95.0(3) . . ? C32 Co3 C23 91.0(3) . . ? C31 Co3 C4 125.6(3) . . ? C32 Co3 C4 127.4(3) . . ? C23 Co3 C4 100.5(3) . . ? C31 Co3 C5 123.7(3) . . ? C32 Co3 C5 100.6(3) . . ? C23 Co3 C5 134.4(3) . . ? C4 Co3 C5 39.1(2) . . ? C31 Co3 C6 91.1(3) . . ? C32 Co3 C6 99.8(3) . . ? C23 Co3 C6 166.0(3) . . ? C4 Co3 C6 65.8(2) . . ? C5 Co3 C6 34.8(2) . . ? C31 Co3 Co1 83.8(2) . . ? C32 Co3 Co1 169.3(3) . . ? C23 Co3 Co1 80.7(2) . . ? C4 Co3 Co1 48.71(14) . . ? C5 Co3 Co1 80.80(16) . . ? C6 Co3 Co1 87.45(15) . . ? C31 Co3 Fe2 129.6(2) . . ? C32 Co3 Fe2 108.8(3) . . ? C23 Co3 Fe2 48.0(2) . . ? C4 Co3 Fe2 53.95(15) . . ? C5 Co3 Fe2 86.73(15) . . ? C6 Co3 Fe2 119.13(15) . . ? Co1 Co3 Fe2 60.51(4) . . ? O11 C11 Co1 176.4(6) . . ? O12 C12 Co1 179.6(7) . . ? O21 C21 Fe2 178.6(7) . . ? O22 C22 Fe2 177.2(8) . . ? O23 C23 Fe2 143.5(6) . . ? O23 C23 Co3 133.8(6) . . ? Fe2 C23 Co3 82.7(3) . . ? O31 C31 Co3 177.3(7) . . ? O32 C32 Co3 175.0(7) . . ? C13 C1 C2 126.7(6) . . ? C13 C1 Co1 71.7(3) . . ? C2 C1 Co1 101.3(4) . . ? C3 C2 C1 119.9(5) . . ? C3 C2 Fe2 69.8(4) . . ? C1 C2 Fe2 95.0(4) . . ? C2 C3 C4 115.8(5) . . ? C2 C3 Fe2 71.7(4) . . ? C4 C3 Fe2 73.3(3) . . ? C3 C4 C5 122.1(5) . . ? C3 C4 Co1 111.5(4) . . ? C5 C4 Co1 126.3(4) . . ? C3 C4 Fe2 66.9(3) . . ? C5 C4 Fe2 126.8(4) . . ? Co1 C4 Fe2 76.1(2) . . ? C3 C4 Co3 134.4(4) . . ? C5 C4 Co3 70.8(3) . . ? Co1 C4 Co3 74.80(19) . . ? Fe2 C4 Co3 71.60(18) . . ? C6 C5 C4 121.3(5) . . ? C6 C5 C10 119.5(5) . . ? C4 C5 C10 119.1(5) . . ? C6 C5 Co3 78.9(4) . . ? C4 C5 Co3 70.2(3) . . ? C10 C5 Co3 122.6(4) . . ? C5 C6 C7 124.5(6) . . ? C5 C6 Co3 66.4(3) . . ? C7 C6 Co3 127.1(5) . . ? C6 C7 C8 113.0(6) . . ? C9 C8 C7 111.2(6) . . ? C8 C9 C10 114.4(7) . . ? C9 C10 C5 113.2(6) . . ? C1 C13 C18 117.6(5) . . ? C1 C13 C14 121.5(5) . . ? C18 C13 C14 112.7(5) . . ? C1 C13 Co1 70.6(3) . . ? C18 C13 Co1 113.2(4) . . ? C14 C13 Co1 114.1(4) . . ? C13 C14 C15 108.6(5) . . ? C16 C15 C14 112.1(6) . . ? C15 C16 C17 110.2(6) . . ? C18 C17 C16 111.5(6) . . ? C17 C18 C13 110.7(5) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.908 _refine_diff_density_min -0.585 _refine_diff_density_rms 0.098 #===END