# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Philip Power' _publ_contact_author_name 'Philip Power' _publ_contact_author_email PPPOWER@UCDAVIS.EDU _publ_section_title ; Unusual Magnetic Properties of a Two-coordinate Heteroleptic Linear Cobalt(II) Complex ; # Attachment 'CIF_Co100510.cif' data_cbn17fffmi _database_code_depnum_ccdc_archive 'CCDC 762897' #TrackingRef 'CIF_Co100510.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H55 Co N Si2' _chemical_formula_sum 'C36 H55 Co N Si2' _chemical_formula_weight 616.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P c a 21' _symmetry_space_group_name_Hall 'P 2c -2ac' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 18.2549(10) _cell_length_b 10.8473(6) _cell_length_c 18.5964(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3682.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 9514 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 27.50 _exptl_crystal_description Block _exptl_crystal_colour Orange _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.113 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1332 _exptl_absorpt_coefficient_mu 0.554 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8427 _exptl_absorpt_correction_T_max 0.9021 _exptl_absorpt_process_details 'SADABS 2008/2 (Sheldrick, 2008)' _exptl_special_details ; An orange block with approximate orthogonal dimensions 0.32 x 0.28 x 0.19mm3 was placed and optically centered on the Bruker SMART1000(1) CCD diffractometer at -183\%C. The initial unit cell was indexed using a least-squares analysis of a random set of reflections collected from three series of 0.3?wide omega-scans, 10 seconds per frame, and 25 frames per series that were well distributed in reciprocal space. Four omega-scan data frame series were collected [MoKa] with 0.3?wide scans, 35 seconds per frame and 606, 455, 606, 455 frames collected per series at varying phi angles (phi=0? 90? 90? 180?. The crystal to detector distance was 4.34cm, thus providing a complete sphere of data to 2ThetaMax=55.08? ; _diffrn_ambient_temperature 90(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 APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 30329 _diffrn_reflns_av_R_equivalents 0.0298 _diffrn_reflns_av_sigmaI/netI 0.0258 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8440 _reflns_number_gt 7413 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. Structural determination and Refinement: All crystallographic calculations were performed on a Personal computer (PC) with a Pentium 3.20GHz processor and 4GB of extended memory. A total of 41380 reflections were collected and corrected for Lorentz and polarization effects and absorption using Blessing's method as incorporated into the program SADABS(2,3,6) with 9179 unique for point group mm2. The SHELXTL(4,6) program package was implemented to determine the probable space group and set up the initial files. System symmetry, systematic absences, and intensity statistics indicated the non-centrosymmetric orthorhombic space group Pca21 (no. 29). The structure was determined by direct methods with the successful location of a majority of the molecule of interest using the program XS(5,6). The structure was refined with XL(5,6). The 41380 data collected were merged based upon identical indices to 31755 [R(int)=0.0195] that were truncated to 2ThetaMax=55.0?totaling 30329 and merged during least-squares refinement to 8440 unique data [R(int)=0.0298]. A series of least-squares difference-Fourier cycles were required to locate the remaining non-hydrogen atoms. All non-hydrogen atoms were refined anisotropically. Hydrogen atoms were placed in calculated positions throughout the final refinement stages. The final structure was refined to convergence with R(F)=4.44%, wR(F2)=8.30%, GOF=1.079 for all 8440 unique reflections [R(F)=3.08%, wR(F2)=7.47% for those 7413 data with Fo > 4sigma (Fo)]. The final difference-Fourier map was featureless indicating that the structure is both correct and complete. An empirical correction for extinction was also attempted but found to be negative and therefore not applied. The structure was found to be racemically twinned so Twin/BASF was employed to determine the relative amounts of the two domains and, Flack(x)7, was found to be -0.351(11). Platon Checkcif noted that the ADDSYM function found the structure could be in Pbcn so this alternative was checked but found to have over 300 systematic absence violations, a structure that was disordered and additionally convergence ceased at R(F)obsd=18% so this space group was abandoned. The structure can also be determined in Cmc21 with the same non-convergence as above, many systematic absence violations, and ceased at approximately R(F)obsd=18%. The structure was therefore completed in Pca21. ADDSYM Detects (Pseudo) Centre of Symmetry ..... 95 PerFi Flack test results are ambiguous. ADDSYM Suggests Possible Pseudo/New Space-group. Pbcn See above. References: 1. Bruker (2002) SMART (Version 5.054) and SAINT (Version 7.60A). Bruker AXS Inc., Madison, Wisconsin, USA. 2. An Empirical Correction for Absorption Anisotropy, Blessing, R. H. (1995). Acta Cryst., A51, 33-38. 3. Sheldrick, G.M., SADABS (2008) Version 2008/2, 'Siemens Area Detector Absorption Correction' Universit\"at G\"ottingen: G\"ottingen, Germany. 4. Sheldrick, G.M., (2002). SHELXTL. Version 6.1. Bruker AXS Inc., Madison, Wisconsin, USA. 5. Sheldrick, G. M., (1997). SHELXS97 and SHELXL97. Universit\"at G\"ottingen: G\"ottingen, Germany. 6. A short history of SHELX, George M. Sheldrick, Acta Cryst. (2008). A64, 112-122 7. On Enantiomorph-Polarity Estimation, Flack, H.D. (1983). Acta Cryst., A39, 876-881. PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.00 Ratio This is due to the large librational shifts of the isopropyl carbon atoms, which were not treated as positional disorder. These large librational shifts are frequently observed in complexes with similar ligands. ; _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^)+(0.0411P)^2^+1.1412P] 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 constr _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 0.351(11) _refine_ls_number_reflns 8440 _refine_ls_number_parameters 376 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0444 _refine_ls_R_factor_gt 0.0308 _refine_ls_wR_factor_ref 0.0830 _refine_ls_wR_factor_gt 0.0747 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _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 0.469028(12) 0.24394(2) 0.17351(2) 0.01993(6) Uani 1 1 d . . . Si1 Si 0.60501(3) 0.33992(5) 0.10344(3) 0.02302(12) Uani 1 1 d . . . Si2 Si 0.62406(3) 0.18328(6) 0.23847(3) 0.02515(13) Uani 1 1 d . . . N1 N 0.57161(7) 0.25188(14) 0.17281(15) 0.0190(3) Uani 1 1 d . . . C1 C 0.36100(9) 0.23766(16) 0.17289(15) 0.0155(3) Uani 1 1 d . . . C2 C 0.31888(10) 0.21751(17) 0.11034(11) 0.0154(4) Uani 1 1 d . . . C3 C 0.24238(11) 0.21153(18) 0.11340(11) 0.0192(4) Uani 1 1 d . . . H3 H 0.2149 0.1951 0.0711 0.023 Uiso 1 1 calc R . . C4 C 0.20653(10) 0.22976(17) 0.17883(14) 0.0218(4) Uani 1 1 d . . . H4 H 0.1546 0.2269 0.1809 0.026 Uiso 1 1 calc R . . C5 C 0.24662(12) 0.25206(16) 0.24066(11) 0.0197(4) Uani 1 1 d . . . H5 H 0.2219 0.2661 0.2849 0.024 Uiso 1 1 calc R . . C6 C 0.32313(12) 0.25405(16) 0.23848(12) 0.0165(4) Uani 1 1 d . . . C7 C 0.36800(11) 0.26843(19) 0.30586(11) 0.0173(4) Uani 1 1 d . . . C8 C 0.40993(11) 0.37643(19) 0.31758(11) 0.0196(4) Uani 1 1 d . . . C9 C 0.45242(11) 0.3845(2) 0.38005(12) 0.0239(4) Uani 1 1 d . . . H9 H 0.4806 0.4566 0.3886 0.029 Uiso 1 1 calc R . . C10 C 0.45401(12) 0.2893(2) 0.42948(12) 0.0255(4) Uani 1 1 d . . . H10 H 0.4834 0.2959 0.4715 0.031 Uiso 1 1 calc R . . C11 C 0.41257(12) 0.1841(2) 0.41756(11) 0.0242(4) Uani 1 1 d . . . H11 H 0.4136 0.1193 0.4520 0.029 Uiso 1 1 calc R . . C12 C 0.36942(11) 0.17135(18) 0.35610(11) 0.0196(4) Uani 1 1 d . . . C13 C 0.35842(11) 0.20584(19) 0.03967(11) 0.0172(4) Uani 1 1 d . . . C14 C 0.35521(11) 0.30338(18) -0.01098(10) 0.0181(4) Uani 1 1 d . . . C15 C 0.39574(11) 0.2937(2) -0.07404(11) 0.0222(4) Uani 1 1 d . . . H15 H 0.3938 0.3585 -0.1084 0.027 Uiso 1 1 calc R . . C16 C 0.43895(12) 0.1911(2) -0.08767(11) 0.0242(4) Uani 1 1 d . . . H16 H 0.4669 0.1867 -0.1307 0.029 Uiso 1 1 calc R . . C17 C 0.44142(12) 0.09535(19) -0.03876(11) 0.0225(4) Uani 1 1 d . . . H17 H 0.4707 0.0250 -0.0488 0.027 Uiso 1 1 calc R . . C18 C 0.40123(11) 0.10055(18) 0.02554(11) 0.0195(4) Uani 1 1 d . . . C19 C 0.40567(12) 0.48723(19) 0.26687(12) 0.0237(4) Uani 1 1 d . . . H19 H 0.3966 0.4543 0.2174 0.028 Uiso 1 1 calc R . . C20 C 0.34067(15) 0.5683(2) 0.28604(15) 0.0405(6) Uani 1 1 d . . . H20A H 0.3467 0.6001 0.3350 0.061 Uiso 1 1 calc R . . H20B H 0.2955 0.5197 0.2832 0.061 Uiso 1 1 calc R . . H20C H 0.3379 0.6375 0.2522 0.061 Uiso 1 1 calc R . . C21 C 0.47610(14) 0.5631(2) 0.26353(15) 0.0371(6) Uani 1 1 d . . . H21A H 0.4727 0.6230 0.2242 0.056 Uiso 1 1 calc R . . H21B H 0.5178 0.5082 0.2551 0.056 Uiso 1 1 calc R . . H21C H 0.4830 0.6068 0.3091 0.056 Uiso 1 1 calc R . . C22 C 0.32631(11) 0.05272(18) 0.34512(11) 0.0225(4) Uani 1 1 d . . . H22 H 0.2998 0.0598 0.2983 0.027 Uiso 1 1 calc R . . C23 C 0.37629(14) -0.0598(2) 0.34052(14) 0.0328(5) Uani 1 1 d . . . H23A H 0.4096 -0.0506 0.2995 0.049 Uiso 1 1 calc R . . H23B H 0.3465 -0.1341 0.3341 0.049 Uiso 1 1 calc R . . H23C H 0.4049 -0.0668 0.3849 0.049 Uiso 1 1 calc R . . C24 C 0.26855(13) 0.0361(2) 0.40443(13) 0.0330(5) Uani 1 1 d . . . H24A H 0.2931 0.0248 0.4508 0.050 Uiso 1 1 calc R . . H24B H 0.2385 -0.0365 0.3938 0.050 Uiso 1 1 calc R . . H24C H 0.2372 0.1094 0.4065 0.050 Uiso 1 1 calc R . . C25 C 0.30809(11) 0.41711(18) 0.00110(11) 0.0216(4) Uani 1 1 d . . . H25 H 0.2870 0.4113 0.0506 0.026 Uiso 1 1 calc R . . C26 C 0.35115(14) 0.5372(2) -0.00339(16) 0.0383(6) Uani 1 1 d . . . H26A H 0.3885 0.5387 0.0345 0.058 Uiso 1 1 calc R . . H26B H 0.3177 0.6071 0.0030 0.058 Uiso 1 1 calc R . . H26C H 0.3749 0.5431 -0.0505 0.058 Uiso 1 1 calc R . . C27 C 0.24419(14) 0.4201(2) -0.05195(14) 0.0384(6) Uani 1 1 d . . . H27A H 0.2632 0.4239 -0.1012 0.058 Uiso 1 1 calc R . . H27B H 0.2138 0.4928 -0.0425 0.058 Uiso 1 1 calc R . . H27C H 0.2145 0.3454 -0.0462 0.058 Uiso 1 1 calc R . . C28 C 0.40158(12) -0.01153(19) 0.07523(11) 0.0224(4) Uani 1 1 d . . . H28 H 0.3758 0.0121 0.1206 0.027 Uiso 1 1 calc R . . C29 C 0.35875(14) -0.1182(2) 0.04092(14) 0.0353(5) Uani 1 1 d . . . H29A H 0.3821 -0.1418 -0.0045 0.053 Uiso 1 1 calc R . . H29B H 0.3083 -0.0920 0.0316 0.053 Uiso 1 1 calc R . . H29C H 0.3586 -0.1890 0.0737 0.053 Uiso 1 1 calc R . . C30 C 0.47835(13) -0.0546(2) 0.09521(15) 0.0321(5) Uani 1 1 d . . . H30A H 0.5037 -0.0838 0.0520 0.048 Uiso 1 1 calc R . . H30B H 0.4750 -0.1219 0.1302 0.048 Uiso 1 1 calc R . . H30C H 0.5057 0.0142 0.1163 0.048 Uiso 1 1 calc R . . C31 C 0.67625(15) 0.4505(2) 0.13469(14) 0.0405(6) Uani 1 1 d . . . H31A H 0.6582 0.4951 0.1770 0.061 Uiso 1 1 calc R . . H31B H 0.6872 0.5093 0.0962 0.061 Uiso 1 1 calc R . . H31C H 0.7209 0.4052 0.1474 0.061 Uiso 1 1 calc R . . C32 C 0.64125(16) 0.2436(2) 0.02812(14) 0.0364(6) Uani 1 1 d . . . H32A H 0.6857 0.2007 0.0439 0.055 Uiso 1 1 calc R . . H32B H 0.6529 0.2966 -0.0130 0.055 Uiso 1 1 calc R . . H32C H 0.6042 0.1829 0.0139 0.055 Uiso 1 1 calc R . . C33 C 0.52655(14) 0.4315(2) 0.06650(14) 0.0378(6) Uani 1 1 d . . . H33A H 0.4880 0.3753 0.0502 0.057 Uiso 1 1 calc R . . H33B H 0.5436 0.4815 0.0259 0.057 Uiso 1 1 calc R . . H33C H 0.5071 0.4856 0.1041 0.057 Uiso 1 1 calc R . . C34 C 0.71142(14) 0.1218(3) 0.19967(15) 0.0414(6) Uani 1 1 d . . . H34A H 0.7001 0.0653 0.1600 0.062 Uiso 1 1 calc R . . H34B H 0.7386 0.0775 0.2370 0.062 Uiso 1 1 calc R . . H34C H 0.7412 0.1903 0.1816 0.062 Uiso 1 1 calc R . . C35 C 0.64756(14) 0.2941(3) 0.31176(14) 0.0363(6) Uani 1 1 d . . . H35A H 0.6740 0.3646 0.2914 0.054 Uiso 1 1 calc R . . H35B H 0.6785 0.2529 0.3475 0.054 Uiso 1 1 calc R . . H35C H 0.6025 0.3231 0.3349 0.054 Uiso 1 1 calc R . . C36 C 0.57123(17) 0.0562(3) 0.28011(15) 0.0462(7) Uani 1 1 d . . . H36A H 0.5256 0.0889 0.3003 0.069 Uiso 1 1 calc R . . H36B H 0.6004 0.0184 0.3185 0.069 Uiso 1 1 calc R . . H36C H 0.5598 -0.0060 0.2436 0.069 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 0.01508(11) 0.02460(12) 0.02011(11) 0.00443(11) -0.00044(13) -0.00112(10) Si1 0.0236(3) 0.0250(3) 0.0204(3) 0.0015(2) 0.0021(2) -0.0054(2) Si2 0.0235(3) 0.0277(3) 0.0242(3) 0.0044(2) -0.0048(2) -0.0012(2) N1 0.0185(7) 0.0191(7) 0.0195(6) 0.0013(6) -0.0002(10) -0.0012(6) C1 0.0159(7) 0.0152(7) 0.0154(7) 0.0015(7) 0.0029(10) 0.0007(6) C2 0.0187(9) 0.0149(8) 0.0126(9) 0.0006(8) 0.0024(8) 0.0013(7) C3 0.0180(9) 0.0213(9) 0.0182(10) -0.0015(8) -0.0026(8) -0.0009(8) C4 0.0155(8) 0.0258(9) 0.0242(10) -0.0004(9) 0.0014(9) 0.0013(7) C5 0.0208(10) 0.0214(9) 0.0168(9) -0.0007(8) 0.0044(8) 0.0015(7) C6 0.0199(10) 0.0147(9) 0.0148(9) -0.0003(7) 0.0000(8) -0.0004(7) C7 0.0140(9) 0.0235(10) 0.0143(9) -0.0039(8) -0.0006(7) 0.0024(7) C8 0.0212(10) 0.0212(9) 0.0164(9) -0.0003(8) 0.0035(8) 0.0016(8) C9 0.0213(10) 0.0256(10) 0.0248(11) -0.0059(9) -0.0017(8) -0.0034(8) C10 0.0261(11) 0.0310(11) 0.0193(10) -0.0019(9) -0.0057(8) 0.0003(9) C11 0.0289(11) 0.0249(11) 0.0188(10) 0.0010(8) -0.0030(8) 0.0024(8) C12 0.0205(9) 0.0198(9) 0.0185(10) -0.0014(8) 0.0022(7) 0.0006(7) C13 0.0183(10) 0.0184(9) 0.0148(9) -0.0009(8) -0.0010(7) -0.0026(8) C14 0.0201(9) 0.0192(9) 0.0150(9) -0.0011(8) -0.0017(7) -0.0009(8) C15 0.0273(11) 0.0224(10) 0.0169(10) 0.0024(8) -0.0006(8) 0.0012(8) C16 0.0254(11) 0.0302(11) 0.0172(10) -0.0025(9) 0.0042(8) 0.0003(9) C17 0.0262(11) 0.0228(10) 0.0186(10) -0.0027(8) 0.0033(8) 0.0040(8) C18 0.0211(10) 0.0198(9) 0.0176(10) -0.0019(8) 0.0009(8) -0.0007(7) C19 0.0298(11) 0.0200(10) 0.0213(10) -0.0002(8) 0.0015(9) -0.0032(8) C20 0.0431(15) 0.0333(13) 0.0449(15) 0.0142(11) 0.0071(12) 0.0111(11) C21 0.0389(14) 0.0319(13) 0.0406(15) 0.0079(11) -0.0022(11) -0.0122(10) C22 0.0263(11) 0.0224(10) 0.0189(10) 0.0009(8) -0.0014(8) -0.0035(8) C23 0.0361(13) 0.0229(11) 0.0394(13) -0.0028(10) -0.0011(10) -0.0010(9) C24 0.0321(13) 0.0340(12) 0.0329(12) -0.0013(10) 0.0048(9) -0.0096(9) C25 0.0273(11) 0.0208(9) 0.0167(9) -0.0004(8) -0.0007(8) 0.0045(8) C26 0.0353(13) 0.0212(11) 0.0585(17) 0.0021(11) -0.0003(12) 0.0044(10) C27 0.0364(13) 0.0383(13) 0.0406(14) -0.0113(11) -0.0151(11) 0.0130(11) C28 0.0301(11) 0.0174(9) 0.0196(10) 0.0015(8) 0.0034(8) 0.0044(8) C29 0.0381(13) 0.0269(11) 0.0408(13) 0.0092(10) -0.0082(11) -0.0080(10) C30 0.0357(12) 0.0277(11) 0.0328(12) 0.0049(10) -0.0081(10) 0.0021(9) C31 0.0429(15) 0.0422(15) 0.0365(13) 0.0044(11) 0.0027(11) -0.0231(12) C32 0.0349(14) 0.0467(15) 0.0277(13) -0.0064(11) 0.0079(10) 0.0006(11) C33 0.0433(15) 0.0366(13) 0.0336(13) 0.0111(11) -0.0034(11) 0.0060(11) C34 0.0368(14) 0.0420(14) 0.0455(14) 0.0005(11) -0.0077(11) 0.0138(11) C35 0.0314(13) 0.0500(15) 0.0275(12) -0.0017(12) -0.0051(10) -0.0037(12) C36 0.0561(17) 0.0456(15) 0.0369(14) 0.0193(12) -0.0079(12) -0.0164(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N1 1.8747(14) . ? Co1 C1 1.9732(16) . ? Si1 N1 1.717(2) . ? Si1 C31 1.862(2) . ? Si1 C32 1.869(3) . ? Si1 C33 1.873(2) . ? Si2 N1 1.721(2) . ? Si2 C36 1.852(3) . ? Si2 C35 1.868(3) . ? Si2 C34 1.873(3) . ? C1 C2 1.411(3) . ? C1 C6 1.413(3) . ? C2 C3 1.399(3) . ? C2 C13 1.505(3) . ? C3 C4 1.396(3) . ? C3 H3 0.9500 . ? C4 C5 1.384(3) . ? C4 H4 0.9500 . ? C5 C6 1.397(3) . ? C5 H5 0.9500 . ? C6 C7 1.505(3) . ? C7 C12 1.408(3) . ? C7 C8 1.416(3) . ? C8 C9 1.400(3) . ? C8 C19 1.530(3) . ? C9 C10 1.383(3) . ? C9 H9 0.9500 . ? C10 C11 1.387(3) . ? C10 H10 0.9500 . ? C11 C12 1.395(3) . ? C11 H11 0.9500 . ? C12 C22 1.522(3) . ? C13 C18 1.409(3) . ? C13 C14 1.418(3) . ? C14 C15 1.390(3) . ? C14 C25 1.521(3) . ? C15 C16 1.387(3) . ? C15 H15 0.9500 . ? C16 C17 1.382(3) . ? C16 H16 0.9500 . ? C17 C18 1.404(3) . ? C17 H17 0.9500 . ? C18 C28 1.527(3) . ? C19 C20 1.519(3) . ? C19 C21 1.528(3) . ? C19 H19 1.0000 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.526(3) . ? C22 C24 1.536(3) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.524(3) . ? C25 C27 1.528(3) . ? C25 H25 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C30 1.523(3) . ? C28 C29 1.536(3) . ? C28 H28 1.0000 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? 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 N1 Co1 C1 179.02(11) . . ? N1 Si1 C31 111.82(11) . . ? N1 Si1 C32 112.20(11) . . ? C31 Si1 C32 110.29(13) . . ? N1 Si1 C33 107.40(10) . . ? C31 Si1 C33 107.87(13) . . ? C32 Si1 C33 107.00(13) . . ? N1 Si2 C36 109.20(11) . . ? N1 Si2 C35 111.54(12) . . ? C36 Si2 C35 107.09(13) . . ? N1 Si2 C34 110.75(11) . . ? C36 Si2 C34 109.83(14) . . ? C35 Si2 C34 108.35(12) . . ? Si1 N1 Si2 125.18(9) . . ? Si1 N1 Co1 112.67(11) . . ? Si2 N1 Co1 122.07(13) . . ? C2 C1 C6 117.66(14) . . ? C2 C1 Co1 123.69(17) . . ? C6 C1 Co1 118.66(17) . . ? C3 C2 C1 121.16(18) . . ? C3 C2 C13 120.69(18) . . ? C1 C2 C13 118.13(17) . . ? C4 C3 C2 119.79(18) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C5 C4 C3 120.07(17) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 120.5(2) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C5 C6 C1 120.8(2) . . ? C5 C6 C7 121.42(19) . . ? C1 C6 C7 117.73(18) . . ? C12 C7 C8 120.44(18) . . ? C12 C7 C6 119.01(18) . . ? C8 C7 C6 120.53(18) . . ? C9 C8 C7 118.61(19) . . ? C9 C8 C19 119.39(18) . . ? C7 C8 C19 121.85(18) . . ? C10 C9 C8 121.1(2) . . ? C10 C9 H9 119.4 . . ? C8 C9 H9 119.4 . . ? C9 C10 C11 119.8(2) . . ? C9 C10 H10 120.1 . . ? C11 C10 H10 120.1 . . ? C10 C11 C12 121.4(2) . . ? C10 C11 H11 119.3 . . ? C12 C11 H11 119.3 . . ? C11 C12 C7 118.70(19) . . ? C11 C12 C22 119.04(18) . . ? C7 C12 C22 122.26(18) . . ? C18 C13 C14 120.28(18) . . ? C18 C13 C2 119.82(17) . . ? C14 C13 C2 119.84(18) . . ? C15 C14 C13 118.82(18) . . ? C15 C14 C25 119.12(18) . . ? C13 C14 C25 122.06(17) . . ? C16 C15 C14 121.1(2) . . ? C16 C15 H15 119.4 . . ? C14 C15 H15 119.4 . . ? C17 C16 C15 120.1(2) . . ? C17 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? C16 C17 C18 120.89(19) . . ? C16 C17 H17 119.6 . . ? C18 C17 H17 119.6 . . ? C17 C18 C13 118.77(18) . . ? C17 C18 C28 118.76(18) . . ? C13 C18 C28 122.35(18) . . ? C20 C19 C21 110.8(2) . . ? C20 C19 C8 110.48(18) . . ? C21 C19 C8 113.93(18) . . ? C20 C19 H19 107.1 . . ? C21 C19 H19 107.1 . . ? C8 C19 H19 107.1 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C12 C22 C23 111.99(18) . . ? C12 C22 C24 110.97(18) . . ? C23 C22 C24 110.90(19) . . ? C12 C22 H22 107.6 . . ? C23 C22 H22 107.6 . . ? C24 C22 H22 107.6 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C14 C25 C26 113.18(18) . . ? C14 C25 C27 110.71(17) . . ? C26 C25 C27 109.91(19) . . ? C14 C25 H25 107.6 . . ? C26 C25 H25 107.6 . . ? C27 C25 H25 107.6 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C30 C28 C18 113.31(18) . . ? C30 C28 C29 109.79(18) . . ? C18 C28 C29 110.28(17) . . ? C30 C28 H28 107.8 . . ? C18 C28 H28 107.8 . . ? C29 C28 H28 107.8 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? Si1 C31 H31A 109.5 . . ? Si1 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? Si1 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? Si1 C32 H32A 109.5 . . ? Si1 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? Si1 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? Si1 C33 H33A 109.5 . . ? Si1 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? Si1 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? Si2 C34 H34A 109.5 . . ? Si2 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? Si2 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? Si2 C35 H35A 109.5 . . ? Si2 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? Si2 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? Si2 C36 H36A 109.5 . . ? Si2 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? Si2 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? 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 C31 Si1 N1 Si2 -44.01(19) . . . . ? C32 Si1 N1 Si2 80.52(18) . . . . ? C33 Si1 N1 Si2 -162.17(15) . . . . ? C31 Si1 N1 Co1 132.79(14) . . . . ? C32 Si1 N1 Co1 -102.68(13) . . . . ? C33 Si1 N1 Co1 14.63(15) . . . . ? C36 Si2 N1 Si1 -159.62(16) . . . . ? C35 Si2 N1 Si1 82.22(18) . . . . ? C34 Si2 N1 Si1 -38.55(18) . . . . ? C36 Si2 N1 Co1 23.86(18) . . . . ? C35 Si2 N1 Co1 -94.30(14) . . . . ? C34 Si2 N1 Co1 144.94(14) . . . . ? C6 C1 C2 C3 -1.2(3) . . . . ? Co1 C1 C2 C3 178.71(14) . . . . ? C6 C1 C2 C13 177.20(16) . . . . ? Co1 C1 C2 C13 -2.8(2) . . . . ? C1 C2 C3 C4 2.2(3) . . . . ? C13 C2 C3 C4 -176.25(18) . . . . ? C2 C3 C4 C5 -0.9(3) . . . . ? C3 C4 C5 C6 -1.3(3) . . . . ? C4 C5 C6 C1 2.2(3) . . . . ? C4 C5 C6 C7 -175.27(17) . . . . ? C2 C1 C6 C5 -0.9(3) . . . . ? Co1 C1 C6 C5 179.12(13) . . . . ? C2 C1 C6 C7 176.65(17) . . . . ? Co1 C1 C6 C7 -3.3(2) . . . . ? C5 C6 C7 C12 69.2(2) . . . . ? C1 C6 C7 C12 -108.4(2) . . . . ? C5 C6 C7 C8 -112.7(2) . . . . ? C1 C6 C7 C8 69.7(2) . . . . ? C12 C7 C8 C9 -0.2(3) . . . . ? C6 C7 C8 C9 -178.28(19) . . . . ? C12 C7 C8 C19 -175.71(18) . . . . ? C6 C7 C8 C19 6.2(3) . . . . ? C7 C8 C9 C10 0.3(3) . . . . ? C19 C8 C9 C10 175.90(19) . . . . ? C8 C9 C10 C11 -0.4(3) . . . . ? C9 C10 C11 C12 0.6(3) . . . . ? C10 C11 C12 C7 -0.5(3) . . . . ? C10 C11 C12 C22 178.8(2) . . . . ? C8 C7 C12 C11 0.3(3) . . . . ? C6 C7 C12 C11 178.41(18) . . . . ? C8 C7 C12 C22 -178.92(19) . . . . ? C6 C7 C12 C22 -0.8(3) . . . . ? C3 C2 C13 C18 -111.2(2) . . . . ? C1 C2 C13 C18 70.3(2) . . . . ? C3 C2 C13 C14 71.7(3) . . . . ? C1 C2 C13 C14 -106.7(2) . . . . ? C18 C13 C14 C15 -0.9(3) . . . . ? C2 C13 C14 C15 176.16(18) . . . . ? C18 C13 C14 C25 178.28(18) . . . . ? C2 C13 C14 C25 -4.7(3) . . . . ? C13 C14 C15 C16 -0.2(3) . . . . ? C25 C14 C15 C16 -179.38(19) . . . . ? C14 C15 C16 C17 1.0(3) . . . . ? C15 C16 C17 C18 -0.7(3) . . . . ? C16 C17 C18 C13 -0.4(3) . . . . ? C16 C17 C18 C28 175.70(19) . . . . ? C14 C13 C18 C17 1.1(3) . . . . ? C2 C13 C18 C17 -175.89(18) . . . . ? C14 C13 C18 C28 -174.77(18) . . . . ? C2 C13 C18 C28 8.2(3) . . . . ? C9 C8 C19 C20 -92.1(2) . . . . ? C7 C8 C19 C20 83.4(3) . . . . ? C9 C8 C19 C21 33.4(3) . . . . ? C7 C8 C19 C21 -151.2(2) . . . . ? C11 C12 C22 C23 -60.9(3) . . . . ? C7 C12 C22 C23 118.3(2) . . . . ? C11 C12 C22 C24 63.6(2) . . . . ? C7 C12 C22 C24 -117.2(2) . . . . ? C15 C14 C25 C26 -56.1(3) . . . . ? C13 C14 C25 C26 124.7(2) . . . . ? C15 C14 C25 C27 67.8(3) . . . . ? C13 C14 C25 C27 -111.3(2) . . . . ? C17 C18 C28 C30 53.8(3) . . . . ? C13 C18 C28 C30 -130.3(2) . . . . ? C17 C18 C28 C29 -69.7(3) . . . . ? C13 C18 C28 C29 106.2(2) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.412 _refine_diff_density_min -0.230 _refine_diff_density_rms 0.053 #===end data_cbn264fmi _database_code_depnum_ccdc_archive 'CCDC 762898' #TrackingRef 'CIF_Co100510.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H74 Co' _chemical_formula_sum 'C60 H74 Co' _chemical_formula_weight 854.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 15.6649(6) _cell_length_b 15.9068(6) _cell_length_c 19.7416(8) _cell_angle_alpha 90.00 _cell_angle_beta 93.6750(10) _cell_angle_gamma 90.00 _cell_volume 4909.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 9993 _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 27.50 _exptl_crystal_description plate _exptl_crystal_colour dark_green _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.156 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1844 _exptl_absorpt_coefficient_mu 0.387 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8272 _exptl_absorpt_correction_T_max 0.9551 _exptl_absorpt_process_details 'SADABS, 2008' _exptl_special_details ; An dark green plate with approximate orthogonal dimensions 0.51 x 0.24 x 0.12mm3 was placed and optically centered on the Bruker SMART1000(1) CCD diffractometer at -183\%C. The initial unit cell was indexed using a least-squares analysis of a random set of reflections collected from three series of 0.3?wide omega-scans, 10 seconds per frame, and 35 frames per series that were well distributed in reciprocal space. Four omega-scan data frame series were collected [MoKa] with 0.3?wide scans, 35 seconds per frame and 606, 455, 606, 455 frames collected per series at varying phi angles (phi=0? 90? 90? 180?. The crystal to detector distance was 4.34cm, thus providing a complete sphere of data to 2ThetaMax=55.08? ; _diffrn_ambient_temperature 90(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 APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 18454 _diffrn_reflns_av_R_equivalents 0.0160 _diffrn_reflns_av_sigmaI/netI 0.0146 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5641 _reflns_number_gt 5184 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. Structural determination and Refinement: All crystallographic calculations were performed on a Personal computer (PC) with a Pentium 3.20GHz processor and 4GB of extended memory. A total of 41380 reflections were collected and corrected for Lorentz and polarization effects and absorption using Blessing's method as incorporated into the program SADABS(2,3,6) with 9179 unique for point group mm2. The SHELXTL(4,6) program package was implemented to determine the probable space group and set up the initial files. System symmetry, systematic absences, and intensity statistics indicated the non-centrosymmetric orthorhombic space group Pca21 (no. 29). The structure was determined by direct methods with the successful location of a majority of the molecule of interest using the program XS(5,6). The structure was refined with XL(5,6). The 41380 data collected were merged based upon identical indices to 31755 [R(int)=0.0195] that were truncated to 2ThetaMax=55.0?totaling 30329 and merged during least-squares refinement to 8440 unique data [R(int)=0.0298]. A series of least-squares difference-Fourier cycles were required to locate the remaining non-hydrogen atoms. All non-hydrogen atoms were refined anisotropically. Hydrogen atoms were placed in calculated positions throughout the final refinement stages. Due to the dark color and the quality of the crystals, there are 58 systemic absence violation, which may attribute to the maximum/minimum residual density as follow: PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.72 References: 1. Bruker (2002) SMART (Version 5.054) and SAINT (Version 7.60A). Bruker AXS Inc., Madison, Wisconsin, USA. 2. An Empirical Correction for Absorption Anisotropy, Blessing, R. H. (1995). Acta Cryst., A51, 33-38. 3. Sheldrick, G.M., SADABS (2008) Version 2008/2, 'Siemens Area Detector Absorption Correction' Universit\"at G\"ottingen: G\"ottingen, Germany. 4. Sheldrick, G.M., (2002). SHELXTL. Version 6.1. Bruker AXS Inc., Madison, Wisconsin, USA. 5. Sheldrick, G. M., (1997). SHELXS97 and SHELXL97. Universit\"at G\"ottingen: G\"ottingen, Germany. 6. A short history of SHELX, George M. Sheldrick, Acta Cryst. (2008). A64, 112-122 7. On Enantiomorph-Polarity Estimation, Flack, H.D. (1983). Acta Cryst., A39, 876-881. PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.12 Ratio PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.04 Ratio These are due to the large librational shifts of the isopropyl carbon atoms, which were not treated as positional disorder. These large librational shifts are frequently observed in complexes with similar ligands. ; _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^)+(0.0536P)^2^+6.4491P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5641 _refine_ls_number_parameters 284 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0442 _refine_ls_R_factor_gt 0.0408 _refine_ls_wR_factor_ref 0.1099 _refine_ls_wR_factor_gt 0.1079 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _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 0.5000 0.751141(17) 0.7500 0.02042(9) Uani 1 2 d S . . C1 C 0.42575(9) 0.72843(9) 0.66488(7) 0.0182(3) Uani 1 1 d . . . C2 C 0.43959(9) 0.67451(9) 0.60939(7) 0.0184(3) Uani 1 1 d . . . C3 C 0.37095(9) 0.64679(10) 0.56605(7) 0.0232(3) Uani 1 1 d . . . H3A H 0.3811 0.6078 0.5310 0.028 Uiso 1 1 calc R . . C4 C 0.28826(10) 0.67538(11) 0.57347(8) 0.0266(3) Uani 1 1 d . . . H4A H 0.2418 0.6542 0.5452 0.032 Uiso 1 1 calc R . . C5 C 0.27447(10) 0.73476(10) 0.62238(8) 0.0247(3) Uani 1 1 d . . . H5A H 0.2190 0.7582 0.6253 0.030 Uiso 1 1 calc R . . C6 C 0.34177(9) 0.76090(9) 0.66782(7) 0.0202(3) Uani 1 1 d . . . C7 C 0.52622(9) 0.65234(9) 0.58510(7) 0.0197(3) Uani 1 1 d . . . C8 C 0.56078(9) 0.70696(10) 0.53738(7) 0.0226(3) Uani 1 1 d . . . C9 C 0.63324(10) 0.68118(12) 0.50495(8) 0.0293(3) Uani 1 1 d . . . H9A H 0.6580 0.7182 0.4739 0.035 Uiso 1 1 calc R . . C10 C 0.66951(10) 0.60273(12) 0.51725(8) 0.0320(4) Uani 1 1 d . . . H10A H 0.7169 0.5851 0.4931 0.038 Uiso 1 1 calc R . . C11 C 0.63635(10) 0.55030(11) 0.56475(8) 0.0285(3) Uani 1 1 d . . . H11A H 0.6621 0.4970 0.5738 0.034 Uiso 1 1 calc R . . C12 C 0.56543(9) 0.57445(10) 0.59981(7) 0.0223(3) Uani 1 1 d . . . C13 C 0.51914(10) 0.79076(10) 0.51821(8) 0.0249(3) Uani 1 1 d . . . H13A H 0.4735 0.8012 0.5503 0.030 Uiso 1 1 calc R . . C14 C 0.47594(11) 0.78789(11) 0.44635(9) 0.0327(4) Uani 1 1 d . . . H14A H 0.4338 0.7423 0.4434 0.049 Uiso 1 1 calc R . . H14B H 0.5192 0.7780 0.4135 0.049 Uiso 1 1 calc R . . H14C H 0.4472 0.8415 0.4362 0.049 Uiso 1 1 calc R . . C15 C 0.58241(13) 0.86379(12) 0.52545(10) 0.0379(4) Uani 1 1 d . . . H15A H 0.6090 0.8647 0.5717 0.057 Uiso 1 1 calc R . . H15B H 0.5521 0.9168 0.5162 0.057 Uiso 1 1 calc R . . H15C H 0.6267 0.8566 0.4931 0.057 Uiso 1 1 calc R . . C16 C 0.53272(10) 0.51522(10) 0.65236(8) 0.0252(3) Uani 1 1 d . . . H16A H 0.4856 0.5442 0.6750 0.030 Uiso 1 1 calc R . . C17 C 0.49645(19) 0.43573(14) 0.61918(12) 0.0568(6) Uani 1 1 d . . . H17A H 0.4769 0.3979 0.6541 0.085 Uiso 1 1 calc R . . H17B H 0.5409 0.4078 0.5947 0.085 Uiso 1 1 calc R . . H17C H 0.4482 0.4502 0.5873 0.085 Uiso 1 1 calc R . . C18 C 0.60341(12) 0.49386(14) 0.70685(10) 0.0417(5) Uani 1 1 d . . . H18A H 0.5799 0.4584 0.7417 0.062 Uiso 1 1 calc R . . H18B H 0.6261 0.5459 0.7277 0.062 Uiso 1 1 calc R . . H18C H 0.6495 0.4636 0.6860 0.062 Uiso 1 1 calc R . . C19 C 0.32395(9) 0.82929(9) 0.71751(7) 0.0217(3) Uani 1 1 d . . . C20 C 0.26785(10) 0.81429(10) 0.76935(8) 0.0268(3) Uani 1 1 d . . . C21 C 0.25191(11) 0.87945(11) 0.81435(8) 0.0305(3) Uani 1 1 d . . . H21A H 0.2165 0.8692 0.8508 0.037 Uiso 1 1 calc R . . C22 C 0.28692(11) 0.95877(11) 0.80677(9) 0.0311(3) Uani 1 1 d . . . H22A H 0.2759 1.0022 0.8381 0.037 Uiso 1 1 calc R . . C23 C 0.33816(11) 0.97449(10) 0.75316(9) 0.0294(3) Uani 1 1 d . . . H23A H 0.3601 1.0295 0.7473 0.035 Uiso 1 1 calc R . . C24 C 0.35790(10) 0.91121(10) 0.70796(8) 0.0240(3) Uani 1 1 d . . . C25 C 0.22109(11) 0.73040(11) 0.77567(8) 0.0284(3) Uani 1 1 d . . . H25 H 0.2441 0.6905 0.7422 0.034 Uiso 1 1 calc R . . C26 C 0.12427(11) 0.73927(12) 0.75841(10) 0.0348(4) Uani 1 1 d . . . H26A H 0.0972 0.6838 0.7598 0.052 Uiso 1 1 calc R . . H26B H 0.1145 0.7633 0.7129 0.052 Uiso 1 1 calc R . . H26C H 0.0995 0.7764 0.7916 0.052 Uiso 1 1 calc R . . C27 C 0.23840(12) 0.69295(12) 0.84606(9) 0.0364(4) Uani 1 1 d . . . H27A H 0.3003 0.6893 0.8566 0.055 Uiso 1 1 calc R . . H27B H 0.2133 0.6366 0.8473 0.055 Uiso 1 1 calc R . . H27C H 0.2128 0.7288 0.8796 0.055 Uiso 1 1 calc R . . C28 C 0.40847(10) 0.93134(10) 0.64606(8) 0.0266(3) Uani 1 1 d . . . H28A H 0.4479 0.8831 0.6393 0.032 Uiso 1 1 calc R . . C29 C 0.46276(12) 1.01069(11) 0.65234(10) 0.0353(4) Uani 1 1 d . . . H29A H 0.4988 1.0144 0.6137 0.053 Uiso 1 1 calc R . . H29B H 0.4991 1.0087 0.6946 0.053 Uiso 1 1 calc R . . H29C H 0.4253 1.0600 0.6528 0.053 Uiso 1 1 calc R . . C30 C 0.34801(12) 0.93825(12) 0.58217(9) 0.0345(4) Uani 1 1 d . . . H30A H 0.3142 0.8866 0.5766 0.052 Uiso 1 1 calc R . . H30B H 0.3816 0.9463 0.5424 0.052 Uiso 1 1 calc R . . H30C H 0.3096 0.9863 0.5866 0.052 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 0.02318(15) 0.02320(15) 0.01476(14) 0.000 0.00031(10) 0.000 C1 0.0209(6) 0.0180(6) 0.0159(6) 0.0034(5) 0.0023(5) 0.0002(5) C2 0.0200(6) 0.0183(6) 0.0172(6) 0.0029(5) 0.0036(5) -0.0001(5) C3 0.0243(7) 0.0255(7) 0.0201(7) -0.0030(5) 0.0044(5) -0.0023(6) C4 0.0199(7) 0.0353(8) 0.0244(7) -0.0010(6) 0.0001(5) -0.0039(6) C5 0.0184(7) 0.0311(8) 0.0249(7) 0.0023(6) 0.0038(5) 0.0025(6) C6 0.0232(7) 0.0205(7) 0.0175(6) 0.0031(5) 0.0049(5) 0.0017(5) C7 0.0188(6) 0.0243(7) 0.0161(6) -0.0014(5) 0.0018(5) -0.0008(5) C8 0.0215(7) 0.0287(8) 0.0175(6) 0.0010(6) 0.0017(5) -0.0010(6) C9 0.0234(7) 0.0426(9) 0.0225(7) 0.0053(7) 0.0070(6) -0.0017(6) C10 0.0228(7) 0.0473(10) 0.0267(8) -0.0006(7) 0.0080(6) 0.0054(7) C11 0.0236(7) 0.0332(8) 0.0287(8) -0.0011(6) 0.0032(6) 0.0068(6) C12 0.0205(7) 0.0262(7) 0.0203(7) -0.0007(5) 0.0019(5) 0.0014(5) C13 0.0279(7) 0.0254(7) 0.0217(7) 0.0046(6) 0.0049(6) -0.0025(6) C14 0.0360(9) 0.0322(9) 0.0293(8) 0.0052(7) -0.0036(7) 0.0003(7) C15 0.0436(10) 0.0335(9) 0.0363(9) 0.0020(7) 0.0007(8) -0.0115(8) C16 0.0272(7) 0.0228(7) 0.0261(7) 0.0024(6) 0.0058(6) 0.0040(6) C17 0.0914(18) 0.0364(11) 0.0438(11) -0.0054(9) 0.0137(11) -0.0268(11) C18 0.0357(9) 0.0580(12) 0.0320(9) 0.0156(8) 0.0076(7) 0.0160(9) C19 0.0224(7) 0.0232(7) 0.0195(7) 0.0018(5) 0.0020(5) 0.0055(5) C20 0.0303(8) 0.0275(8) 0.0234(7) 0.0024(6) 0.0067(6) 0.0071(6) C21 0.0361(8) 0.0339(9) 0.0222(7) 0.0000(6) 0.0076(6) 0.0098(7) C22 0.0359(9) 0.0307(8) 0.0265(8) -0.0064(6) 0.0014(6) 0.0093(7) C23 0.0320(8) 0.0246(8) 0.0314(8) -0.0016(6) 0.0007(6) 0.0026(6) C24 0.0246(7) 0.0248(7) 0.0225(7) 0.0023(6) 0.0001(5) 0.0040(6) C25 0.0291(8) 0.0303(8) 0.0263(8) 0.0026(6) 0.0071(6) 0.0043(6) C26 0.0264(8) 0.0383(9) 0.0400(10) 0.0052(7) 0.0028(7) 0.0037(7) C27 0.0400(9) 0.0403(10) 0.0296(9) 0.0075(7) 0.0074(7) 0.0036(8) C28 0.0287(8) 0.0240(7) 0.0276(8) 0.0043(6) 0.0039(6) 0.0020(6) C29 0.0356(9) 0.0325(9) 0.0382(9) 0.0056(7) 0.0043(7) -0.0040(7) C30 0.0389(9) 0.0360(9) 0.0282(8) 0.0077(7) -0.0001(7) -0.0033(7) _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 C1 2.0141(14) . ? Co1 C1 2.0141(14) 2_656 ? C1 C6 1.418(2) . ? C1 C2 1.4188(19) . ? C2 C3 1.402(2) . ? C2 C7 1.5097(19) . ? C3 C4 1.389(2) . ? C3 H3A 0.9500 . ? C4 C5 1.378(2) . ? C4 H4A 0.9500 . ? C5 C6 1.403(2) . ? C5 H5A 0.9500 . ? C6 C19 1.503(2) . ? C7 C12 1.405(2) . ? C7 C8 1.415(2) . ? C8 C9 1.400(2) . ? C8 C13 1.521(2) . ? C9 C10 1.386(3) . ? C9 H9A 0.9500 . ? C10 C11 1.381(2) . ? C10 H10A 0.9500 . ? C11 C12 1.400(2) . ? C11 H11A 0.9500 . ? C12 C16 1.515(2) . ? C13 C15 1.528(2) . ? C13 C14 1.533(2) . ? C13 H13A 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.518(3) . ? C16 C18 1.532(2) . ? C16 H16A 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.411(2) . ? C19 C24 1.425(2) . ? C20 C21 1.398(2) . ? C20 C25 1.531(2) . ? C21 C22 1.388(3) . ? C21 H21A 0.9500 . ? C22 C23 1.391(2) . ? C22 H22A 0.9500 . ? C23 C24 1.393(2) . ? C23 H23A 0.9500 . ? C24 C28 1.532(2) . ? C25 C27 1.520(2) . ? C25 C26 1.539(2) . ? C25 H25 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.523(2) . ? C28 C30 1.532(2) . ? C28 H28A 1.0000 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Co1 C1 159.34(8) . 2_656 ? C6 C1 C2 116.10(13) . . ? C6 C1 Co1 112.84(10) . . ? C2 C1 Co1 130.09(10) . . ? C3 C2 C1 120.81(13) . . ? C3 C2 C7 113.74(12) . . ? C1 C2 C7 124.85(12) . . ? C4 C3 C2 121.10(14) . . ? C4 C3 H3A 119.5 . . ? C2 C3 H3A 119.5 . . ? C5 C4 C3 119.17(14) . . ? C5 C4 H4A 120.4 . . ? C3 C4 H4A 120.4 . . ? C4 C5 C6 120.42(14) . . ? C4 C5 H5A 119.8 . . ? C6 C5 H5A 119.8 . . ? C5 C6 C1 121.81(13) . . ? C5 C6 C19 117.94(13) . . ? C1 C6 C19 120.13(13) . . ? C12 C7 C8 119.89(13) . . ? C12 C7 C2 122.03(13) . . ? C8 C7 C2 117.28(13) . . ? C9 C8 C7 118.74(14) . . ? C9 C8 C13 119.36(13) . . ? C7 C8 C13 121.84(13) . . ? C10 C9 C8 121.25(15) . . ? C10 C9 H9A 119.4 . . ? C8 C9 H9A 119.4 . . ? C11 C10 C9 119.66(14) . . ? C11 C10 H10A 120.2 . . ? C9 C10 H10A 120.2 . . ? C10 C11 C12 121.00(15) . . ? C10 C11 H11A 119.5 . . ? C12 C11 H11A 119.5 . . ? C11 C12 C7 119.35(14) . . ? C11 C12 C16 118.82(14) . . ? C7 C12 C16 121.83(13) . . ? C8 C13 C15 112.20(14) . . ? C8 C13 C14 111.15(13) . . ? C15 C13 C14 110.76(13) . . ? C8 C13 H13A 107.5 . . ? C15 C13 H13A 107.5 . . ? C14 C13 H13A 107.5 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C12 C16 C17 110.87(14) . . ? C12 C16 C18 110.97(14) . . ? C17 C16 C18 110.62(17) . . ? C12 C16 H16A 108.1 . . ? C17 C16 H16A 108.1 . . ? C18 C16 H16A 108.1 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C24 120.38(14) . . ? C20 C19 C6 120.08(14) . . ? C24 C19 C6 119.29(13) . . ? C21 C20 C19 118.71(15) . . ? C21 C20 C25 119.24(14) . . ? C19 C20 C25 122.00(14) . . ? C22 C21 C20 121.18(15) . . ? C22 C21 H21A 119.4 . . ? C20 C21 H21A 119.4 . . ? C21 C22 C23 119.78(15) . . ? C21 C22 H22A 120.1 . . ? C23 C22 H22A 120.1 . . ? C22 C23 C24 121.34(16) . . ? C22 C23 H23A 119.3 . . ? C24 C23 H23A 119.3 . . ? C23 C24 C19 118.43(14) . . ? C23 C24 C28 120.48(14) . . ? C19 C24 C28 120.88(13) . . ? C27 C25 C20 110.97(15) . . ? C27 C25 C26 110.72(14) . . ? C20 C25 C26 111.82(14) . . ? C27 C25 H25 107.7 . . ? C20 C25 H25 107.7 . . ? C26 C25 H25 107.7 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 C30 108.68(14) . . ? C29 C28 C24 115.02(14) . . ? C30 C28 C24 110.34(13) . . ? C29 C28 H28A 107.5 . . ? C30 C28 H28A 107.5 . . ? C24 C28 H28A 107.5 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Co1 C1 C6 118.59(10) 2_656 . . . ? C1 Co1 C1 C2 -49.48(12) 2_656 . . . ? C6 C1 C2 C3 -8.3(2) . . . . ? Co1 C1 C2 C3 159.44(11) . . . . ? C6 C1 C2 C7 162.25(13) . . . . ? Co1 C1 C2 C7 -30.0(2) . . . . ? C1 C2 C3 C4 4.1(2) . . . . ? C7 C2 C3 C4 -167.44(14) . . . . ? C2 C3 C4 C5 2.9(2) . . . . ? C3 C4 C5 C6 -5.3(2) . . . . ? C4 C5 C6 C1 0.7(2) . . . . ? C4 C5 C6 C19 176.68(14) . . . . ? C2 C1 C6 C5 6.0(2) . . . . ? Co1 C1 C6 C5 -163.84(12) . . . . ? C2 C1 C6 C19 -169.90(12) . . . . ? Co1 C1 C6 C19 20.25(16) . . . . ? C3 C2 C7 C12 -85.82(17) . . . . ? C1 C2 C7 C12 103.03(17) . . . . ? C3 C2 C7 C8 83.90(16) . . . . ? C1 C2 C7 C8 -87.25(17) . . . . ? C12 C7 C8 C9 0.9(2) . . . . ? C2 C7 C8 C9 -169.02(13) . . . . ? C12 C7 C8 C13 178.17(13) . . . . ? C2 C7 C8 C13 8.2(2) . . . . ? C7 C8 C9 C10 2.0(2) . . . . ? C13 C8 C9 C10 -175.28(15) . . . . ? C8 C9 C10 C11 -3.2(3) . . . . ? C9 C10 C11 C12 1.3(3) . . . . ? C10 C11 C12 C7 1.6(2) . . . . ? C10 C11 C12 C16 -178.82(15) . . . . ? C8 C7 C12 C11 -2.7(2) . . . . ? C2 C7 C12 C11 166.74(14) . . . . ? C8 C7 C12 C16 177.74(13) . . . . ? C2 C7 C12 C16 -12.8(2) . . . . ? C9 C8 C13 C15 -55.25(19) . . . . ? C7 C8 C13 C15 127.53(15) . . . . ? C9 C8 C13 C14 69.39(19) . . . . ? C7 C8 C13 C14 -107.83(16) . . . . ? C11 C12 C16 C17 -66.5(2) . . . . ? C7 C12 C16 C17 113.06(19) . . . . ? C11 C12 C16 C18 56.9(2) . . . . ? C7 C12 C16 C18 -123.59(16) . . . . ? C5 C6 C19 C20 67.00(19) . . . . ? C1 C6 C19 C20 -116.93(16) . . . . ? C5 C6 C19 C24 -107.28(16) . . . . ? C1 C6 C19 C24 68.79(18) . . . . ? C24 C19 C20 C21 -5.1(2) . . . . ? C6 C19 C20 C21 -179.35(14) . . . . ? C24 C19 C20 C25 172.06(14) . . . . ? C6 C19 C20 C25 -2.2(2) . . . . ? C19 C20 C21 C22 3.1(2) . . . . ? C25 C20 C21 C22 -174.21(15) . . . . ? C20 C21 C22 C23 0.7(3) . . . . ? C21 C22 C23 C24 -2.4(3) . . . . ? C22 C23 C24 C19 0.3(2) . . . . ? C22 C23 C24 C28 175.14(15) . . . . ? C20 C19 C24 C23 3.5(2) . . . . ? C6 C19 C24 C23 177.75(14) . . . . ? C20 C19 C24 C28 -171.32(14) . . . . ? C6 C19 C24 C28 2.9(2) . . . . ? C21 C20 C25 C27 -57.6(2) . . . . ? C19 C20 C25 C27 125.21(16) . . . . ? C21 C20 C25 C26 66.6(2) . . . . ? C19 C20 C25 C26 -110.63(17) . . . . ? C23 C24 C28 C29 22.8(2) . . . . ? C19 C24 C28 C29 -162.51(14) . . . . ? C23 C24 C28 C30 -100.58(17) . . . . ? C19 C24 C28 C30 74.12(18) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.812 _refine_diff_density_min -0.298 _refine_diff_density_rms 0.054