# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Clara Vinas' _publ_contact_author_email CLARA@ICMAB.ES _publ_section_title ; A convenient synthetic route to useful monobranched polyethoxylated halogen terminated [3,3-Co(1,2-C2B9H11)2]- synthons ; _publ_requested_category ? loop_ _publ_author_name 'Clara Vinas' 'Pau Farras' 'Reijo Sillanpaa' 'Francesc Teixidor' # Attachment 'PF590-91.cif' data_pf590 _database_code_depnum_ccdc_archive 'CCDC 738981' #TrackingRef 'PF590-91.cif' _audit_creation_date 2008-09-11T10:13:42-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C8 H29 B18 Br Co O2, C4 H12 N' _chemical_formula_sum 'C12 H41 B18 Br Co N O2' _chemical_formula_weight 564.88 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 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 13.1888(3) _cell_length_b 13.6557(2) _cell_length_c 15.0632(3) _cell_angle_alpha 90 _cell_angle_beta 90.6620(10) _cell_angle_gamma 90 _cell_volume 2712.74(9) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 17475 _cell_measurement_theta_min 0.407 _cell_measurement_theta_max 28.283 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.3 _exptl_crystal_density_diffrn 1.383 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1152 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.12 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Sheldrick, 2002)' _exptl_absorpt_correction_T_min 0.449 _exptl_absorpt_correction_T_max 0.529 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0461 _diffrn_reflns_av_unetI/netI 0.0499 _diffrn_reflns_number 27406 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 27 _diffrn_reflns_theta_full 27 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _reflns_number_total 5890 _reflns_number_gt 4201 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0438P)^2^+5.1339P] 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_number_reflns 5890 _refine_ls_number_parameters 320 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0795 _refine_ls_R_factor_gt 0.0478 _refine_ls_wR_factor_ref 0.1198 _refine_ls_wR_factor_gt 0.107 _refine_ls_goodness_of_fit_ref 1.04 _refine_ls_restrained_S_all 1.04 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.245 _refine_diff_density_min -1.58 _refine_diff_density_rms 0.084 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Br Br 0.68925(4) -0.18062(4) 0.61479(3) 0.05924(17) Uani 1 1 d . . . Co3 Co 0.77505(3) 0.31095(3) 0.21025(3) 0.01655(12) Uani 1 1 d . . . O1 O 0.69727(18) 0.23915(16) 0.39193(14) 0.0254(5) Uani 1 1 d . . . O2 O 0.75255(18) 0.02035(16) 0.51611(14) 0.0269(5) Uani 1 1 d . . . N N 0.7372(2) 0.4765(2) 0.57117(18) 0.0248(6) Uani 1 1 d . . . C1' C 0.8888(2) 0.3516(2) 0.1251(2) 0.0229(7) Uani 1 1 d . . . H1' H 0.8514 0.3777 0.0623 0.028 Uiso 1 1 calc R . . C1 C 0.6586(2) 0.3915(2) 0.1575(2) 0.0212(7) Uani 1 1 d . . . H1 H 0.6936 0.4545 0.1214 0.025 Uiso 1 1 calc R . . C2' C 0.8859(2) 0.4160(2) 0.2141(2) 0.0226(7) Uani 1 1 d . . . H2' H 0.8465 0.4886 0.2151 0.027 Uiso 1 1 calc R . . C2 C 0.6644(2) 0.2808(2) 0.1193(2) 0.0211(7) Uani 1 1 d . . . H2 H 0.703 0.2643 0.0552 0.025 Uiso 1 1 calc R . . C13 C 0.6908(3) 0.1388(2) 0.4151(2) 0.0254(7) Uani 1 1 d . . . H13A H 0.7172 0.0977 0.3664 0.031 Uiso 1 1 calc R . . H13B H 0.6193 0.1204 0.4254 0.031 Uiso 1 1 calc R . . C14 C 0.7522(3) 0.1229(2) 0.4974(2) 0.0269(7) Uani 1 1 d . . . H14A H 0.8224 0.1465 0.4888 0.032 Uiso 1 1 calc R . . H14B H 0.7224 0.1594 0.5475 0.032 Uiso 1 1 calc R . . C15 C 0.7934(3) 0.0011(3) 0.6011(2) 0.0376(9) Uani 1 1 d . . . H15A H 0.7456 0.0245 0.6467 0.045 Uiso 1 1 calc R . . H15B H 0.8577 0.0376 0.6088 0.045 Uiso 1 1 calc R . . C16 C 0.8125(3) -0.1041(3) 0.6144(2) 0.0328(8) Uani 1 1 d . . . H16A H 0.8489 -0.1136 0.6716 0.039 Uiso 1 1 calc R . . H16B H 0.8569 -0.1282 0.5666 0.039 Uiso 1 1 calc R . . C17 C 0.8116(3) 0.5332(3) 0.5182(3) 0.0406(9) Uani 1 1 d . . . H17A H 0.7812 0.5956 0.5 0.061 Uiso 1 1 calc R . . H17B H 0.83 0.4955 0.4654 0.061 Uiso 1 1 calc R . . H17C H 0.8724 0.5457 0.5543 0.061 Uiso 1 1 calc R . . C18 C 0.7828(4) 0.3820(3) 0.5997(4) 0.0658(15) Uani 1 1 d . . . H18A H 0.8445 0.3947 0.6347 0.099 Uiso 1 1 calc R . . H18B H 0.7997 0.3431 0.5473 0.099 Uiso 1 1 calc R . . H18C H 0.7342 0.3459 0.636 0.099 Uiso 1 1 calc R . . C19 C 0.6452(4) 0.4552(4) 0.5171(3) 0.0681(16) Uani 1 1 d . . . H19A H 0.5964 0.4192 0.5532 0.102 Uiso 1 1 calc R . . H19B H 0.6638 0.4156 0.4656 0.102 Uiso 1 1 calc R . . H19C H 0.6148 0.5169 0.4969 0.102 Uiso 1 1 calc R . . C20 C 0.7093(3) 0.5339(3) 0.6505(3) 0.0491(11) Uani 1 1 d . . . H20A H 0.6594 0.4974 0.6851 0.074 Uiso 1 1 calc R . . H20B H 0.6801 0.5967 0.6319 0.074 Uiso 1 1 calc R . . H20C H 0.77 0.5457 0.6872 0.074 Uiso 1 1 calc R . . B4' B 0.8886(3) 0.2294(3) 0.1479(2) 0.0224(8) Uani 1 1 d . . . H4' H 0.855 0.1711 0.1043 0.027 Uiso 1 1 calc R . . B4 B 0.6603(3) 0.3945(3) 0.2700(2) 0.0215(8) Uani 1 1 d . . . H4 H 0.6924 0.4548 0.3121 0.026 Uiso 1 1 calc R . . B5 B 0.5456(3) 0.4140(3) 0.2065(2) 0.0226(8) Uani 1 1 d . . . H5 H 0.5056 0.4864 0.2065 0.027 Uiso 1 1 calc R . . B5' B 1.0015(3) 0.2920(3) 0.1145(3) 0.0254(8) Uani 1 1 d . . . H5' H 1.039 0.275 0.05 0.03 Uiso 1 1 calc R . . B6 B 0.5508(3) 0.3420(3) 0.1094(3) 0.0235(8) Uani 1 1 d . . . H6 H 0.515 0.3665 0.0454 0.028 Uiso 1 1 calc R . . B6' B 0.9983(3) 0.4135(3) 0.1558(3) 0.0285(9) Uani 1 1 d . . . H6' H 1.0331 0.4764 0.1193 0.034 Uiso 1 1 calc R . . B7' B 0.8831(3) 0.3447(3) 0.3076(2) 0.0220(8) Uani 1 1 d . . . H7' H 0.8464 0.3641 0.3719 0.026 Uiso 1 1 calc R . . B7 B 0.6715(3) 0.1956(3) 0.2031(2) 0.0202(7) Uani 1 1 d . . . H7 H 0.7105 0.1228 0.2006 0.024 Uiso 1 1 calc R . . B8' B 0.8889(3) 0.2201(3) 0.2675(3) 0.0230(8) Uani 1 1 d . . . H8' H 0.8581 0.1556 0.3044 0.028 Uiso 1 1 calc R . . B8 B 0.6650(3) 0.2674(3) 0.3059(2) 0.0207(7) Uani 1 1 d . . . B9' B 1.0047(3) 0.2105(3) 0.2064(3) 0.0248(8) Uani 1 1 d . . . H9' H 1.046 0.139 0.203 0.03 Uiso 1 1 calc R . . B9 B 0.5461(3) 0.3337(3) 0.2989(2) 0.0236(8) Uani 1 1 d . . . H9 H 0.5046 0.3527 0.361 0.028 Uiso 1 1 calc R . . B10' B 1.0715(3) 0.3235(3) 0.2122(3) 0.0286(9) Uani 1 1 d . . . H10' H 1.1564 0.3261 0.2138 0.034 Uiso 1 1 calc R . . B10 B 0.4792(3) 0.3007(3) 0.2000(3) 0.0247(8) Uani 1 1 d . . . H10 H 0.3944 0.2969 0.1974 0.03 Uiso 1 1 calc R . . B11' B 0.9956(3) 0.4077(3) 0.2725(3) 0.0285(9) Uani 1 1 d . . . H11' H 1.0293 0.4684 0.3132 0.034 Uiso 1 1 calc R . . B11 B 0.5569(3) 0.2179(3) 0.1399(3) 0.0230(8) Uani 1 1 d . . . H11 H 0.5242 0.1598 0.0956 0.028 Uiso 1 1 calc R . . B12 B 0.5531(3) 0.2113(3) 0.2570(3) 0.0234(8) Uani 1 1 d . . . H12 H 0.5161 0.1481 0.2911 0.028 Uiso 1 1 calc R . . B12' B 1.0013(3) 0.2826(3) 0.3056(3) 0.0268(8) Uani 1 1 d . . . H12' H 1.0405 0.2597 0.3686 0.032 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 Br 0.0477(3) 0.0563(3) 0.0738(4) 0.0349(2) 0.0043(2) -0.0064(2) Co3 0.0159(2) 0.0144(2) 0.0194(2) 0.00134(16) 0.00018(15) 0.00078(17) O1 0.0336(13) 0.0181(11) 0.0247(12) 0.0019(9) 0.0005(10) -0.0017(10) O2 0.0357(14) 0.0215(12) 0.0234(12) 0.0031(9) -0.0076(10) 0.0021(10) N 0.0287(15) 0.0235(15) 0.0223(14) -0.0013(11) 0.0010(11) -0.0031(12) C1' 0.0203(16) 0.0238(17) 0.0247(17) 0.0030(13) 0.0026(13) -0.0009(13) C1 0.0159(15) 0.0188(16) 0.0289(17) 0.0029(13) -0.0005(13) 0.0021(12) C2' 0.0194(16) 0.0184(16) 0.0299(18) 0.0016(13) -0.0022(13) -0.0018(13) C2 0.0202(16) 0.0204(16) 0.0225(17) 0.0010(12) -0.0021(13) 0.0007(13) C13 0.0327(19) 0.0202(17) 0.0234(17) 0.0058(13) 0.0007(14) -0.0020(14) C14 0.0322(19) 0.0214(17) 0.0271(18) 0.0028(13) -0.0003(14) -0.0004(14) C15 0.050(2) 0.033(2) 0.030(2) -0.0012(15) -0.0152(17) 0.0057(18) C16 0.037(2) 0.033(2) 0.0283(19) 0.0016(15) -0.0059(15) 0.0043(16) C17 0.046(2) 0.041(2) 0.035(2) -0.0002(17) 0.0083(18) -0.0152(19) C18 0.059(3) 0.033(2) 0.106(4) 0.023(3) 0.021(3) 0.012(2) C19 0.063(3) 0.098(4) 0.043(3) 0.015(3) -0.021(2) -0.043(3) C20 0.051(3) 0.049(3) 0.048(3) -0.025(2) 0.020(2) -0.013(2) B4' 0.0200(18) 0.0216(18) 0.026(2) 0.0003(15) 0.0016(15) 0.0012(15) B4 0.0193(18) 0.0182(18) 0.027(2) 0.0013(14) 0.0010(15) 0.0020(14) B5 0.0179(18) 0.0210(19) 0.029(2) 0.0014(15) 0.0010(15) 0.0016(15) B5' 0.0175(18) 0.030(2) 0.028(2) 0.0016(16) 0.0025(15) 0.0016(16) B6 0.0168(18) 0.027(2) 0.027(2) 0.0034(15) -0.0023(15) 0.0017(15) B6' 0.0189(18) 0.027(2) 0.039(2) 0.0012(17) 0.0026(16) -0.0048(16) B7' 0.0201(18) 0.0232(19) 0.0227(19) -0.0021(14) -0.0027(14) 0.0022(15) B7 0.0202(17) 0.0166(17) 0.0239(19) 0.0010(14) 0.0001(14) -0.0011(14) B8' 0.0197(18) 0.0199(18) 0.029(2) 0.0018(15) -0.0004(15) 0.0059(15) B8 0.0220(18) 0.0176(18) 0.0225(19) 0.0019(14) 0.0027(14) 0.0015(15) B9' 0.0191(18) 0.023(2) 0.032(2) -0.0003(15) 0.0020(15) 0.0029(15) B9 0.0222(19) 0.024(2) 0.0245(19) -0.0009(14) 0.0022(15) 0.0032(15) B10' 0.0190(19) 0.031(2) 0.036(2) -0.0016(17) -0.0017(16) 0.0023(16) B10 0.0197(18) 0.024(2) 0.030(2) 0.0031(15) -0.0001(15) -0.0001(16) B11' 0.0207(19) 0.029(2) 0.036(2) -0.0042(17) -0.0076(16) -0.0001(16) B11 0.0198(18) 0.0226(19) 0.026(2) 0.0014(14) -0.0017(15) -0.0028(15) B12 0.0208(18) 0.0214(19) 0.028(2) 0.0029(15) 0.0027(15) -0.0001(15) B12' 0.0231(19) 0.029(2) 0.028(2) 0.0002(16) -0.0037(15) 0.0025(16) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Br C16 1.933(4) . ? Co3 C2 2.033(3) . ? Co3 C1 2.042(3) . ? Co3 C2' 2.049(3) . ? Co3 C1' 2.061(3) . ? Co3 B7' 2.084(4) . ? Co3 B7 2.086(4) . ? Co3 B4' 2.096(4) . ? Co3 B4 2.106(4) . ? Co3 B8' 2.123(4) . ? Co3 B8 2.142(4) . ? O1 B8 1.412(4) . ? O1 C13 1.417(4) . ? O2 C15 1.408(4) . ? O2 C14 1.428(4) . ? N C20 1.480(4) . ? N C19 1.481(5) . ? N C18 1.484(5) . ? N C17 1.489(4) . ? C1' C2' 1.605(5) . ? C1' B4' 1.703(5) . ? C1' B5' 1.704(5) . ? C1' B6' 1.732(5) . ? C1' H1' 1.12 . ? C1 C2 1.619(4) . ? C1 B4 1.695(5) . ? C1 B5 1.699(5) . ? C1 B6 1.725(5) . ? C1 H1 1.12 . ? C2' B11' 1.688(5) . ? C2' B7' 1.712(5) . ? C2' B6' 1.733(5) . ? C2' H2' 1.12 . ? C2 B11 1.689(5) . ? C2 B7 1.719(5) . ? C2 B6 1.719(5) . ? C2 H2 1.12 . ? C13 C14 1.489(5) . ? C13 H13A 0.99 . ? C13 H13B 0.99 . ? C14 H14A 0.99 . ? C14 H14B 0.99 . ? C15 C16 1.472(5) . ? C15 H15A 0.99 . ? C15 H15B 0.99 . ? C16 H16A 0.99 . ? C16 H16B 0.99 . ? C17 H17A 0.98 . ? C17 H17B 0.98 . ? C17 H17C 0.98 . ? C18 H18A 0.98 . ? C18 H18B 0.98 . ? C18 H18C 0.98 . ? C19 H19A 0.98 . ? C19 H19B 0.98 . ? C19 H19C 0.98 . ? C20 H20A 0.98 . ? C20 H20B 0.98 . ? C20 H20C 0.98 . ? B4' B9' 1.777(5) . ? B4' B5' 1.794(5) . ? B4' B8' 1.806(5) . ? B4' H4' 1.12 . ? B4 B9 1.778(5) . ? B4 B5 1.800(5) . ? B4 B8 1.819(5) . ? B4 H4 1.12 . ? B5 B6 1.764(5) . ? B5 B9 1.772(5) . ? B5 B10 1.781(5) . ? B5 H5 1.12 . ? B5' B6' 1.773(6) . ? B5' B9' 1.776(5) . ? B5' B10' 1.781(5) . ? B5' H5' 1.12 . ? B6 B11 1.758(5) . ? B6 B10 1.761(5) . ? B6 H6 1.12 . ? B6' B11' 1.761(6) . ? B6' B10' 1.774(6) . ? B6' H6' 1.12 . ? B7' B12' 1.776(5) . ? B7' B11' 1.800(5) . ? B7' B8' 1.808(5) . ? B7' H7' 1.12 . ? B7 B12 1.781(5) . ? B7 B11 1.803(5) . ? B7 B8 1.835(5) . ? B7 H7 1.12 . ? B8' B9' 1.797(5) . ? B8' B12' 1.799(5) . ? B8' H8' 1.12 . ? B8 B12 1.812(5) . ? B8 B9 1.813(5) . ? B9' B10' 1.778(5) . ? B9' B12' 1.790(6) . ? B9' H9' 1.12 . ? B9 B10 1.780(5) . ? B9 B12 1.789(5) . ? B9 H9 1.12 . ? B10' B11' 1.780(6) . ? B10' B12' 1.783(6) . ? B10' H10' 1.12 . ? B10 B12 1.777(5) . ? B10 B11 1.780(5) . ? B10 H10 1.12 . ? B11' B12' 1.781(6) . ? B11' H11' 1.12 . ? B11 B12 1.767(5) . ? B11 H11 1.12 . ? B12 H12 1.12 . ? B12' H12' 1.12 . ? 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 C2 Co3 C1 46.82(12) . . ? C2 Co3 C2' 131.89(13) . . ? C1 Co3 C2' 99.62(13) . . ? C2 Co3 C1' 99.06(13) . . ? C1 Co3 C1' 99.36(13) . . ? C2' Co3 C1' 45.97(13) . . ? C2 Co3 B7' 177.17(14) . . ? C1 Co3 B7' 131.25(14) . . ? C2' Co3 B7' 48.94(14) . . ? C1' Co3 B7' 83.20(14) . . ? C2 Co3 B7 49.31(13) . . ? C1 Co3 B7 84.13(13) . . ? C2' Co3 B7 175.19(14) . . ? C1' Co3 B7 130.68(14) . . ? B7' Co3 B7 130.15(14) . . ? C2 Co3 B4' 95.83(14) . . ? C1 Co3 B4' 130.50(14) . . ? C2' Co3 B4' 82.62(14) . . ? C1' Co3 B4' 48.35(13) . . ? B7' Co3 B4' 86.95(15) . . ? B7 Co3 B4' 92.66(14) . . ? C2 Co3 B4 83.30(14) . . ? C1 Co3 B4 48.19(13) . . ? C2' Co3 B4 97.16(14) . . ? C1' Co3 B4 130.70(13) . . ? B7' Co3 B4 93.93(14) . . ? B7 Co3 B4 87.58(14) . . ? B4' Co3 B4 178.64(14) . . ? C2 Co3 B8' 130.88(14) . . ? C1 Co3 B8' 176.18(14) . . ? C2' Co3 B8' 84.07(14) . . ? C1' Co3 B8' 83.89(14) . . ? B7' Co3 B8' 50.89(14) . . ? B7 Co3 B8' 92.23(14) . . ? B4' Co3 B8' 50.68(14) . . ? B4 Co3 B8' 130.66(14) . . ? C2 Co3 B8 84.86(13) . . ? C1 Co3 B8 84.20(13) . . ? C2' Co3 B8 131.63(14) . . ? C1' Co3 B8 175.90(14) . . ? B7' Co3 B8 92.93(14) . . ? B7 Co3 B8 51.44(14) . . ? B4' Co3 B8 130.31(14) . . ? B4 Co3 B8 50.72(14) . . ? B8' Co3 B8 92.62(14) . . ? B8 O1 C13 118.2(3) . . ? C15 O2 C14 111.3(3) . . ? C20 N C19 109.8(3) . . ? C20 N C18 109.3(3) . . ? C19 N C18 108.4(4) . . ? C20 N C17 109.2(3) . . ? C19 N C17 110.3(3) . . ? C18 N C17 109.9(3) . . ? C2' C1' B4' 111.6(2) . . ? C2' C1' B5' 111.7(3) . . ? B4' C1' B5' 63.5(2) . . ? C2' C1' B6' 62.4(2) . . ? B4' C1' B6' 115.3(3) . . ? B5' C1' B6' 62.1(2) . . ? C2' C1' Co3 66.64(16) . . ? B4' C1' Co3 66.92(16) . . ? B5' C1' Co3 124.9(2) . . ? B6' C1' Co3 125.2(2) . . ? C2' C1' H1' 121.1 . . ? B4' C1' H1' 118.7 . . ? B5' C1' H1' 116.6 . . ? B6' C1' H1' 115.3 . . ? Co3 C1' H1' 107.2 . . ? C2 C1 B4 112.2(2) . . ? C2 C1 B5 111.6(2) . . ? B4 C1 B5 64.1(2) . . ? C2 C1 B6 61.8(2) . . ? B4 C1 B6 115.5(3) . . ? B5 C1 B6 62.0(2) . . ? C2 C1 Co3 66.27(15) . . ? B4 C1 Co3 67.87(16) . . ? B5 C1 Co3 126.0(2) . . ? B6 C1 Co3 124.4(2) . . ? C2 C1 H1 121.5 . . ? B4 C1 H1 117.8 . . ? B5 C1 H1 116.1 . . ? B6 C1 H1 116 . . ? Co3 C1 H1 106.9 . . ? C1' C2' B11' 111.7(3) . . ? C1' C2' B7' 112.1(2) . . ? B11' C2' B7' 63.9(2) . . ? C1' C2' B6' 62.4(2) . . ? B11' C2' B6' 62.0(2) . . ? B7' C2' B6' 115.6(3) . . ? C1' C2' Co3 67.39(16) . . ? B11' C2' Co3 125.1(2) . . ? B7' C2' Co3 66.59(16) . . ? B6' C2' Co3 125.9(2) . . ? C1' C2' H2' 120.8 . . ? B11' C2' H2' 116.7 . . ? B7' C2' H2' 118.6 . . ? B6' C2' H2' 115.2 . . ? Co3 C2' H2' 106.8 . . ? C1 C2 B11 111.5(2) . . ? C1 C2 B7 111.9(2) . . ? B11 C2 B7 63.9(2) . . ? C1 C2 B6 62.1(2) . . ? B11 C2 B6 62.1(2) . . ? B7 C2 B6 115.7(2) . . ? C1 C2 Co3 66.90(15) . . ? B11 C2 Co3 125.2(2) . . ? B7 C2 Co3 66.96(16) . . ? B6 C2 Co3 125.3(2) . . ? C1 C2 H2 121.2 . . ? B11 C2 H2 116.5 . . ? B7 C2 H2 118.4 . . ? B6 C2 H2 115.3 . . ? Co3 C2 H2 106.9 . . ? O1 C13 C14 108.2(3) . . ? O1 C13 H13A 110.1 . . ? C14 C13 H13A 110.1 . . ? O1 C13 H13B 110.1 . . ? C14 C13 H13B 110.1 . . ? H13A C13 H13B 108.4 . . ? O2 C14 C13 107.9(3) . . ? O2 C14 H14A 110.1 . . ? C13 C14 H14A 110.1 . . ? O2 C14 H14B 110.1 . . ? C13 C14 H14B 110.1 . . ? H14A C14 H14B 108.4 . . ? O2 C15 C16 111.7(3) . . ? O2 C15 H15A 109.3 . . ? C16 C15 H15A 109.3 . . ? O2 C15 H15B 109.3 . . ? C16 C15 H15B 109.3 . . ? H15A C15 H15B 107.9 . . ? C15 C16 Br 112.6(3) . . ? C15 C16 H16A 109.1 . . ? Br C16 H16A 109.1 . . ? C15 C16 H16B 109.1 . . ? Br C16 H16B 109.1 . . ? H16A C16 H16B 107.8 . . ? N C17 H17A 109.5 . . ? N C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N C18 H18A 109.5 . . ? N C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N C19 H19A 109.5 . . ? N C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N C20 H20A 109.5 . . ? N C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C1' B4' B9' 103.8(3) . . ? C1' B4' B5' 58.3(2) . . ? B9' B4' B5' 59.6(2) . . ? C1' B4' B8' 105.7(3) . . ? B9' B4' B8' 60.2(2) . . ? B5' B4' B8' 108.7(3) . . ? C1' B4' Co3 64.73(16) . . ? B9' B4' Co3 118.1(2) . . ? B5' B4' Co3 118.2(2) . . ? B8' B4' Co3 65.43(16) . . ? C1' B4' H4' 125.5 . . ? B9' B4' H4' 121.3 . . ? B5' B4' H4' 119.8 . . ? B8' B4' H4' 122.1 . . ? Co3 B4' H4' 111.2 . . ? C1 B4 B9 103.4(3) . . ? C1 B4 B5 58.08(19) . . ? B9 B4 B5 59.4(2) . . ? C1 B4 B8 105.9(2) . . ? B9 B4 B8 60.5(2) . . ? B5 B4 B8 109.0(3) . . ? C1 B4 Co3 63.94(16) . . ? B9 B4 Co3 117.8(2) . . ? B5 B4 Co3 117.2(2) . . ? B8 B4 Co3 65.66(16) . . ? C1 B4 H4 125.8 . . ? B9 B4 H4 121.4 . . ? B5 B4 H4 120.1 . . ? B8 B4 H4 121.5 . . ? Co3 B4 H4 111.8 . . ? C1 B5 B6 59.7(2) . . ? C1 B5 B9 103.5(2) . . ? B6 B5 B9 107.8(3) . . ? C1 B5 B10 104.6(3) . . ? B6 B5 B10 59.6(2) . . ? B9 B5 B10 60.1(2) . . ? C1 B5 B4 57.85(19) . . ? B6 B5 B4 108.5(3) . . ? B9 B5 B4 59.7(2) . . ? B10 B5 B4 108.1(3) . . ? C1 B5 H5 125.2 . . ? B6 B5 H5 121 . . ? B9 B5 H5 122.9 . . ? B10 B5 H5 122.4 . . ? B4 B5 H5 121.6 . . ? C1' B5' B6' 59.7(2) . . ? C1' B5' B9' 103.8(3) . . ? B6' B5' B9' 108.3(3) . . ? C1' B5' B10' 104.6(3) . . ? B6' B5' B10' 59.9(2) . . ? B9' B5' B10' 60.0(2) . . ? C1' B5' B4' 58.19(19) . . ? B6' B5' B4' 108.9(3) . . ? B9' B5' B4' 59.7(2) . . ? B10' B5' B4' 107.9(3) . . ? C1' B5' H5' 125 . . ? B6' B5' H5' 120.6 . . ? B9' B5' H5' 122.8 . . ? B10' B5' H5' 122.5 . . ? B4' B5' H5' 121.4 . . ? C2 B6 C1 56.07(18) . . ? C2 B6 B11 58.1(2) . . ? C1 B6 B11 103.5(2) . . ? C2 B6 B10 104.6(3) . . ? C1 B6 B10 104.3(3) . . ? B11 B6 B10 60.8(2) . . ? C2 B6 B5 104.0(2) . . ? C1 B6 B5 58.3(2) . . ? B11 B6 B5 108.9(3) . . ? B10 B6 B5 60.7(2) . . ? C2 B6 H6 125.3 . . ? C1 B6 H6 125.6 . . ? B11 B6 H6 122 . . ? B10 B6 H6 122.5 . . ? B5 B6 H6 121.8 . . ? C1' B6' C2' 55.18(19) . . ? C1' B6' B11' 102.6(3) . . ? C2' B6' B11' 57.8(2) . . ? C1' B6' B5' 58.2(2) . . ? C2' B6' B5' 102.7(3) . . ? B11' B6' B5' 108.0(3) . . ? C1' B6' B10' 103.7(3) . . ? C2' B6' B10' 103.6(3) . . ? B11' B6' B10' 60.5(2) . . ? B5' B6' B10' 60.3(2) . . ? C1' B6' H6' 126 . . ? C2' B6' H6' 126.2 . . ? B11' B6' H6' 122.5 . . ? B5' B6' H6' 122.3 . . ? B10' B6' H6' 122.9 . . ? C2' B7' B12' 103.3(3) . . ? C2' B7' B11' 57.4(2) . . ? B12' B7' B11' 59.7(2) . . ? C2' B7' B8' 105.0(2) . . ? B12' B7' B8' 60.3(2) . . ? B11' B7' B8' 108.3(3) . . ? C2' B7' Co3 64.47(16) . . ? B12' B7' Co3 118.4(2) . . ? B11' B7' Co3 117.3(2) . . ? B8' B7' Co3 65.67(17) . . ? C2' B7' H7' 126.2 . . ? B12' B7' H7' 121.1 . . ? B11' B7' H7' 120.5 . . ? B8' B7' H7' 122.2 . . ? Co3 B7' H7' 111.2 . . ? C2 B7 B12 102.3(2) . . ? C2 B7 B11 57.27(19) . . ? B12 B7 B11 59.1(2) . . ? C2 B7 B8 104.8(2) . . ? B12 B7 B8 60.1(2) . . ? B11 B7 B8 108.0(2) . . ? C2 B7 Co3 63.73(15) . . ? B12 B7 Co3 117.6(2) . . ? B11 B7 Co3 116.4(2) . . ? B8 B7 Co3 65.84(16) . . ? C2 B7 H7 126.7 . . ? B12 B7 H7 121.8 . . ? B11 B7 H7 120.9 . . ? B8 B7 H7 122 . . ? Co3 B7 H7 111.9 . . ? B9' B8' B12' 59.7(2) . . ? B9' B8' B4' 59.1(2) . . ? B12' B8' B4' 106.1(3) . . ? B9' B8' B7' 106.2(3) . . ? B12' B8' B7' 59.0(2) . . ? B4' B8' B7' 105.5(3) . . ? B9' B8' Co3 115.8(2) . . ? B12' B8' Co3 115.4(2) . . ? B4' B8' Co3 63.90(16) . . ? B7' B8' Co3 63.44(16) . . ? B9' B8' H8' 120.8 . . ? B12' B8' H8' 121.1 . . ? B4' B8' H8' 123.7 . . ? B7' B8' H8' 123.8 . . ? Co3 B8' H8' 113.7 . . ? O1 B8 B12 119.5(3) . . ? O1 B8 B9 116.2(3) . . ? B12 B8 B9 59.2(2) . . ? O1 B8 B4 122.9(3) . . ? B12 B8 B4 104.9(2) . . ? B9 B8 B4 58.6(2) . . ? O1 B8 B7 127.7(3) . . ? B12 B8 B7 58.46(19) . . ? B9 B8 B7 105.4(2) . . ? B4 B8 B7 105.1(2) . . ? O1 B8 Co3 119.6(2) . . ? B12 B8 Co3 113.5(2) . . ? B9 B8 Co3 114.5(2) . . ? B4 B8 Co3 63.63(16) . . ? B7 B8 Co3 62.72(15) . . ? B5' B9' B4' 60.7(2) . . ? B5' B9' B10' 60.1(2) . . ? B4' B9' B10' 108.8(3) . . ? B5' B9' B12' 107.8(3) . . ? B4' B9' B12' 107.7(3) . . ? B10' B9' B12' 59.9(2) . . ? B5' B9' B8' 109.9(3) . . ? B4' B9' B8' 60.7(2) . . ? B10' B9' B8' 109.6(3) . . ? B12' B9' B8' 60.2(2) . . ? B5' B9' H9' 121.1 . . ? B4' B9' H9' 121.4 . . ? B10' B9' H9' 121.1 . . ? B12' B9' H9' 122.3 . . ? B8' B9' H9' 120.3 . . ? B5 B9 B4 60.9(2) . . ? B5 B9 B10 60.2(2) . . ? B4 B9 B10 109.1(3) . . ? B5 B9 B12 107.6(3) . . ? B4 B9 B12 107.6(3) . . ? B10 B9 B12 59.7(2) . . ? B5 B9 B8 110.6(3) . . ? B4 B9 B8 60.9(2) . . ? B10 B9 B8 110.1(3) . . ? B12 B9 B8 60.4(2) . . ? B5 B9 H9 121 . . ? B4 B9 H9 121.3 . . ? B10 B9 H9 121 . . ? B12 B9 H9 122.6 . . ? B8 B9 H9 119.8 . . ? B6' B10' B9' 108.1(3) . . ? B6' B10' B11' 59.4(2) . . ? B9' B10' B11' 107.7(3) . . ? B6' B10' B5' 59.8(2) . . ? B9' B10' B5' 59.9(2) . . ? B11' B10' B5' 106.8(3) . . ? B6' B10' B12' 108.1(3) . . ? B9' B10' B12' 60.3(2) . . ? B11' B10' B12' 60.0(2) . . ? B5' B10' B12' 107.9(3) . . ? B6' B10' H10' 121.8 . . ? B9' B10' H10' 121.6 . . ? B11' B10' H10' 122.5 . . ? B5' B10' H10' 122.3 . . ? B12' B10' H10' 121.4 . . ? B6 B10 B12 107.4(3) . . ? B6 B10 B11 59.5(2) . . ? B12 B10 B11 59.6(2) . . ? B6 B10 B9 107.5(3) . . ? B12 B10 B9 60.4(2) . . ? B11 B10 B9 107.7(3) . . ? B6 B10 B5 59.7(2) . . ? B12 B10 B5 107.7(3) . . ? B11 B10 B5 107.1(3) . . ? B9 B10 B5 59.7(2) . . ? B6 B10 H10 122.2 . . ? B12 B10 H10 121.8 . . ? B11 B10 H10 122.3 . . ? B9 B10 H10 121.7 . . ? B5 B10 H10 122.1 . . ? C2' B11' B6' 60.3(2) . . ? C2' B11' B10' 105.2(3) . . ? B6' B11' B10' 60.1(2) . . ? C2' B11' B12' 104.1(3) . . ? B6' B11' B12' 108.7(3) . . ? B10' B11' B12' 60.1(2) . . ? C2' B11' B7' 58.7(2) . . ? B6' B11' B7' 109.9(3) . . ? B10' B11' B7' 108.2(3) . . ? B12' B11' B7' 59.5(2) . . ? C2' B11' H11' 124.6 . . ? B6' B11' H11' 120 . . ? B10' B11' H11' 122.3 . . ? B12' B11' H11' 122.8 . . ? B7' B11' H11' 121.1 . . ? C2 B11 B6 59.8(2) . . ? C2 B11 B12 104.1(3) . . ? B6 B11 B12 107.9(3) . . ? C2 B11 B10 105.0(3) . . ? B6 B11 B10 59.7(2) . . ? B12 B11 B10 60.1(2) . . ? C2 B11 B7 58.85(19) . . ? B6 B11 B7 109.6(3) . . ? B12 B11 B7 59.8(2) . . ? B10 B11 B7 108.8(3) . . ? C2 B11 H11 124.7 . . ? B6 B11 H11 120.8 . . ? B12 B11 H11 122.9 . . ? B10 B11 H11 122.2 . . ? B7 B11 H11 120.7 . . ? B11 B12 B10 60.3(2) . . ? B11 B12 B7 61.1(2) . . ? B10 B12 B7 110.0(3) . . ? B11 B12 B9 107.8(3) . . ? B10 B12 B9 59.9(2) . . ? B7 B12 B9 108.8(3) . . ? B11 B12 B8 110.6(3) . . ? B10 B12 B8 110.2(3) . . ? B7 B12 B8 61.4(2) . . ? B9 B12 B8 60.4(2) . . ? B11 B12 H12 121 . . ? B10 B12 H12 120.7 . . ? B7 B12 H12 120.4 . . ? B9 B12 H12 122.2 . . ? B8 B12 H12 119.8 . . ? B7' B12' B11' 60.8(2) . . ? B7' B12' B10' 109.1(3) . . ? B11' B12' B10' 60.0(2) . . ? B7' B12' B9' 107.9(3) . . ? B11' B12' B9' 107.2(3) . . ? B10' B12' B9' 59.7(2) . . ? B7' B12' B8' 60.7(2) . . ? B11' B12' B8' 109.5(3) . . ? B10' B12' B8' 109.3(3) . . ? B9' B12' B8' 60.1(2) . . ? B7' B12' H12' 121 . . ? B11' B12' H12' 121.5 . . ? B10' B12' H12' 121.2 . . ? B9' B12' H12' 122.6 . . ? B8' B12' H12' 120.6 . . ? #===END data_pf591 _database_code_depnum_ccdc_archive 'CCDC 738982' #TrackingRef 'PF590-91.cif' _audit_creation_date 2008-09-11T09:24:37-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C8 H29 B18 Co I O2, C4 H12 N' _chemical_formula_sum 'C12 H41 B18 Co I N O2' _chemical_formula_weight 611.87 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 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 13.3105(2) _cell_length_b 13.7168(3) _cell_length_c 15.1793(4) _cell_angle_alpha 90 _cell_angle_beta 90.290(2) _cell_angle_gamma 90 _cell_volume 2771.36(10) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 22982 _cell_measurement_theta_min 0.407 _cell_measurement_theta_max 28.283 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.466 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.747 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Sheldrick, 2002)' _exptl_absorpt_correction_T_min 0.597 _exptl_absorpt_correction_T_max 0.707 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0391 _diffrn_reflns_av_unetI/netI 0.0408 _diffrn_reflns_number 24021 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2 _diffrn_reflns_theta_max 27 _diffrn_reflns_theta_full 27 _diffrn_measured_fraction_theta_full 0.979 _diffrn_measured_fraction_theta_max 0.979 _reflns_number_total 5922 _reflns_number_gt 4813 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0362P)^2^+5.0746P] 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_number_reflns 5922 _refine_ls_number_parameters 320 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0539 _refine_ls_R_factor_gt 0.0394 _refine_ls_wR_factor_ref 0.0954 _refine_ls_wR_factor_gt 0.0896 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.604 _refine_diff_density_min -0.96 _refine_diff_density_rms 0.089 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 I I 0.690274(19) -0.172033(19) 0.629163(18) 0.04411(10) Uani 1 1 d . . . Co3 Co 0.78001(3) 0.31512(3) 0.21215(2) 0.01520(10) Uani 1 1 d . . . O1 O 0.70513(16) 0.24284(15) 0.39355(14) 0.0232(5) Uani 1 1 d . . . O2 O 0.76534(16) 0.02464(15) 0.51448(14) 0.0241(5) Uani 1 1 d . . . N N 0.7360(2) 0.4765(2) 0.57169(17) 0.0257(6) Uani 1 1 d . . . C1' C 0.8905(2) 0.3555(2) 0.1250(2) 0.0219(6) Uani 1 1 d . . . H1' H 0.852 0.3796 0.063 0.026 Uiso 1 1 calc R . . C1 C 0.6634(2) 0.3935(2) 0.1608(2) 0.0196(6) Uani 1 1 d . . . H1 H 0.6969 0.4563 0.124 0.023 Uiso 1 1 calc R . . C2' C 0.8881(2) 0.4213(2) 0.2124(2) 0.0203(6) Uani 1 1 d . . . H2' H 0.8477 0.493 0.2132 0.024 Uiso 1 1 calc R . . C2 C 0.6700(2) 0.2829(2) 0.12355(19) 0.0198(6) Uani 1 1 d . . . H2 H 0.7081 0.266 0.0597 0.024 Uiso 1 1 calc R . . C13 C 0.7005(2) 0.1424(2) 0.4160(2) 0.0250(7) Uani 1 1 d . . . H13A H 0.7259 0.1023 0.3668 0.03 Uiso 1 1 calc R . . H13B H 0.6301 0.1233 0.4277 0.03 Uiso 1 1 calc R . . C14 C 0.7631(3) 0.1265(2) 0.4959(2) 0.0262(7) Uani 1 1 d . . . H14A H 0.8321 0.1508 0.4858 0.031 Uiso 1 1 calc R . . H14B H 0.7344 0.1625 0.5464 0.031 Uiso 1 1 calc R . . C15 C 0.8170(3) 0.0070(3) 0.5948(2) 0.0348(8) Uani 1 1 d . . . H15A H 0.7789 0.0359 0.6442 0.042 Uiso 1 1 calc R . . H15B H 0.8839 0.0386 0.593 0.042 Uiso 1 1 calc R . . C16 C 0.8294(2) -0.0999(2) 0.6097(2) 0.0270(7) Uani 1 1 d . . . H16A H 0.8728 -0.1103 0.662 0.032 Uiso 1 1 calc R . . H16B H 0.8636 -0.1289 0.5582 0.032 Uiso 1 1 calc R . . C17 C 0.8073(3) 0.5390(3) 0.5203(3) 0.0413(9) Uani 1 1 d . . . H17A H 0.7765 0.6027 0.5093 0.062 Uiso 1 1 calc R . . H17B H 0.8224 0.5073 0.4641 0.062 Uiso 1 1 calc R . . H17C H 0.8696 0.5477 0.5541 0.062 Uiso 1 1 calc R . . C18 C 0.7832(4) 0.3813(3) 0.5898(4) 0.0597(13) Uani 1 1 d . . . H18A H 0.8433 0.3908 0.6264 0.09 Uiso 1 1 calc R . . H18B H 0.802 0.3503 0.5341 0.09 Uiso 1 1 calc R . . H18C H 0.7355 0.3394 0.6211 0.09 Uiso 1 1 calc R . . C19 C 0.6430(4) 0.4609(4) 0.5199(3) 0.0691(16) Uani 1 1 d . . . H19A H 0.597 0.4193 0.5533 0.104 Uiso 1 1 calc R . . H19B H 0.6596 0.4291 0.464 0.104 Uiso 1 1 calc R . . H19C H 0.6108 0.5238 0.5081 0.104 Uiso 1 1 calc R . . C20 C 0.7128(3) 0.5254(3) 0.6564(3) 0.0438(10) Uani 1 1 d . . . H20A H 0.666 0.485 0.6902 0.066 Uiso 1 1 calc R . . H20B H 0.6821 0.589 0.6447 0.066 Uiso 1 1 calc R . . H20C H 0.7749 0.5343 0.6904 0.066 Uiso 1 1 calc R . . B4' B 0.8929(3) 0.2341(3) 0.1496(2) 0.0224(7) Uani 1 1 d . . . H4' H 0.8602 0.1743 0.1081 0.027 Uiso 1 1 calc R . . B4 B 0.6661(3) 0.3973(2) 0.2728(2) 0.0200(7) Uani 1 1 d . . . H4 H 0.6977 0.4579 0.3138 0.024 Uiso 1 1 calc R . . B5 B 0.5514(3) 0.4147(3) 0.2115(2) 0.0227(7) Uani 1 1 d . . . H5 H 0.5108 0.4862 0.2122 0.027 Uiso 1 1 calc R . . B5' B 1.0025(3) 0.2977(3) 0.1132(3) 0.0257(8) Uani 1 1 d . . . H5' H 1.0386 0.2799 0.0486 0.031 Uiso 1 1 calc R . . B6 B 0.5568(3) 0.3433(3) 0.1146(2) 0.0218(7) Uani 1 1 d . . . H6 H 0.5207 0.3674 0.0515 0.026 Uiso 1 1 calc R . . B6' B 0.9982(3) 0.4196(3) 0.1519(3) 0.0272(8) Uani 1 1 d . . . H6' H 1.0305 0.4821 0.114 0.033 Uiso 1 1 calc R . . B7' B 0.8880(3) 0.3523(2) 0.3067(2) 0.0204(7) Uani 1 1 d . . . H7' H 0.8525 0.3722 0.371 0.024 Uiso 1 1 calc R . . B7 B 0.6784(3) 0.1992(2) 0.2064(2) 0.0198(7) Uani 1 1 d . . . H7 H 0.7177 0.127 0.2032 0.024 Uiso 1 1 calc R . . B8' B 0.8954(3) 0.2279(3) 0.2687(2) 0.0216(7) Uani 1 1 d . . . H8' H 0.8667 0.1642 0.3073 0.026 Uiso 1 1 calc R . . B8 B 0.6725(3) 0.2713(2) 0.3089(2) 0.0193(7) Uani 1 1 d . . . B9' B 1.0091(3) 0.2188(3) 0.2056(2) 0.0234(7) Uani 1 1 d . . . H9' H 1.0513 0.1483 0.2028 0.028 Uiso 1 1 calc R . . B9 B 0.5533(3) 0.3355(3) 0.3030(2) 0.0221(7) Uani 1 1 d . . . H9 H 0.5121 0.3542 0.3649 0.027 Uiso 1 1 calc R . . B10' B 1.0734(3) 0.3326(3) 0.2076(3) 0.0275(8) Uani 1 1 d . . . H10' H 1.1574 0.3368 0.2069 0.033 Uiso 1 1 calc R . . B10 B 0.4871(3) 0.3016(3) 0.2057(2) 0.0218(7) Uani 1 1 d . . . H10 H 0.4031 0.297 0.2038 0.026 Uiso 1 1 calc R . . B11' B 0.9984(3) 0.4159(3) 0.2680(3) 0.0255(8) Uani 1 1 d . . . H11' H 1.0318 0.4774 0.3067 0.031 Uiso 1 1 calc R . . B11 B 0.5641(3) 0.2193(3) 0.1454(2) 0.0244(8) Uani 1 1 d . . . H11 H 0.5317 0.1609 0.1022 0.029 Uiso 1 1 calc R . . B12 B 0.5616(3) 0.2132(3) 0.2624(2) 0.0227(7) Uani 1 1 d . . . H12 H 0.5262 0.1502 0.2974 0.027 Uiso 1 1 calc R . . B12' B 1.0067(3) 0.2927(3) 0.3022(3) 0.0249(8) Uani 1 1 d . . . H12' H 1.0476 0.2719 0.3641 0.03 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 I 0.03646(16) 0.04254(16) 0.05341(18) 0.02050(12) 0.00653(12) -0.00349(11) Co3 0.0148(2) 0.01344(19) 0.0174(2) 0.00153(15) -0.00013(15) 0.00065(15) O1 0.0304(12) 0.0179(11) 0.0212(11) 0.0031(9) -0.0016(9) 0.0007(9) O2 0.0329(12) 0.0179(11) 0.0213(11) 0.0056(9) -0.0065(9) 0.0011(9) N 0.0312(15) 0.0245(14) 0.0214(13) 0.0016(11) 0.0011(11) -0.0034(12) C1' 0.0189(15) 0.0258(16) 0.0212(15) 0.0016(13) 0.0007(12) -0.0016(12) C1 0.0186(15) 0.0172(15) 0.0229(15) 0.0018(12) -0.0009(12) 0.0028(12) C2' 0.0181(15) 0.0156(14) 0.0273(16) 0.0005(12) -0.0023(12) -0.0009(11) C2 0.0196(15) 0.0200(15) 0.0197(15) -0.0013(12) -0.0009(12) 0.0016(12) C13 0.0306(18) 0.0210(16) 0.0236(16) 0.0044(13) 0.0001(13) 0.0023(13) C14 0.0316(18) 0.0197(16) 0.0272(17) 0.0033(13) -0.0017(14) -0.0013(13) C15 0.049(2) 0.0283(19) 0.0273(18) 0.0051(15) -0.0166(16) -0.0014(16) C16 0.0283(17) 0.0285(18) 0.0242(17) 0.0066(14) -0.0053(13) 0.0004(14) C17 0.053(2) 0.035(2) 0.037(2) 0.0047(17) 0.0121(18) -0.0110(18) C18 0.070(3) 0.029(2) 0.080(3) 0.007(2) 0.023(3) 0.009(2) C19 0.060(3) 0.107(4) 0.040(2) 0.018(3) -0.022(2) -0.038(3) C20 0.053(2) 0.041(2) 0.038(2) -0.0120(18) 0.0166(18) -0.0117(19) B4' 0.0201(17) 0.0222(18) 0.0249(18) -0.0046(14) 0.0003(14) 0.0009(14) B4 0.0187(17) 0.0179(16) 0.0236(18) 0.0011(14) 0.0013(13) 0.0036(13) B5 0.0164(17) 0.0214(18) 0.0303(19) 0.0025(15) 0.0009(14) 0.0032(13) B5' 0.0179(17) 0.031(2) 0.0286(19) -0.0018(16) 0.0040(15) 0.0002(15) B6 0.0176(17) 0.0269(19) 0.0209(17) 0.0033(14) -0.0014(14) 0.0015(14) B6' 0.0180(17) 0.0258(19) 0.038(2) 0.0052(16) 0.0000(15) -0.0034(14) B7' 0.0206(17) 0.0194(17) 0.0211(17) 0.0012(14) -0.0026(14) 0.0041(13) B7 0.0197(17) 0.0161(16) 0.0236(17) 0.0025(13) -0.0008(14) 0.0005(13) B8' 0.0207(17) 0.0186(17) 0.0256(18) 0.0018(14) -0.0006(14) 0.0042(13) B8 0.0216(17) 0.0177(16) 0.0186(16) 0.0025(13) 0.0001(13) -0.0001(13) B9' 0.0189(17) 0.0220(18) 0.0291(19) -0.0003(15) -0.0003(14) 0.0031(14) B9 0.0194(17) 0.0223(17) 0.0247(18) 0.0000(14) 0.0041(14) 0.0014(14) B10' 0.0184(17) 0.031(2) 0.033(2) -0.0006(16) -0.0011(15) 0.0005(15) B10 0.0188(17) 0.0223(18) 0.0242(18) 0.0026(14) 0.0023(14) -0.0001(14) B11' 0.0216(18) 0.0206(18) 0.034(2) -0.0026(15) -0.0056(15) 0.0000(14) B11 0.0213(18) 0.0224(18) 0.0293(19) 0.0009(15) -0.0020(15) -0.0053(14) B12 0.0217(18) 0.0219(18) 0.0244(18) 0.0029(14) 0.0003(14) -0.0030(14) B12' 0.0233(18) 0.0233(18) 0.0280(19) -0.0006(15) -0.0046(15) 0.0046(15) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 I C16 2.122(3) . ? Co3 C2 2.032(3) . ? Co3 C1 2.040(3) . ? Co3 C2' 2.047(3) . ? Co3 C1' 2.059(3) . ? Co3 B7 2.089(3) . ? Co3 B7' 2.089(4) . ? Co3 B4' 2.100(3) . ? Co3 B4 2.105(3) . ? Co3 B8' 2.125(3) . ? Co3 B8 2.143(3) . ? O1 B8 1.409(4) . ? O1 C13 1.421(4) . ? O2 C15 1.417(4) . ? O2 C14 1.426(4) . ? N C18 1.475(5) . ? N C19 1.479(5) . ? N C20 1.484(4) . ? N C17 1.500(4) . ? C1' C2' 1.605(4) . ? C1' B5' 1.699(5) . ? C1' B4' 1.707(5) . ? C1' B6' 1.729(5) . ? C1' H1' 1.12 . ? C1 C2 1.622(4) . ? C1 B4 1.700(5) . ? C1 B5 1.706(4) . ? C1 B6 1.723(5) . ? C1 H1 1.12 . ? C2' B11' 1.692(5) . ? C2' B7' 1.716(5) . ? C2' B6' 1.733(5) . ? C2' H2' 1.12 . ? C2 B11 1.692(4) . ? C2 B7 1.706(4) . ? C2 B6 1.725(4) . ? C2 H2 1.12 . ? C13 C14 1.483(4) . ? C13 H13A 0.99 . ? C13 H13B 0.99 . ? C14 H14A 0.99 . ? C14 H14B 0.99 . ? C15 C16 1.493(5) . ? C15 H15A 0.99 . ? C15 H15B 0.99 . ? C16 H16A 0.99 . ? C16 H16B 0.99 . ? C17 H17A 0.98 . ? C17 H17B 0.98 . ? C17 H17C 0.98 . ? C18 H18A 0.98 . ? C18 H18B 0.98 . ? C18 H18C 0.98 . ? C19 H19A 0.98 . ? C19 H19B 0.98 . ? C19 H19C 0.98 . ? C20 H20A 0.98 . ? C20 H20B 0.98 . ? C20 H20C 0.98 . ? B4' B9' 1.774(5) . ? B4' B5' 1.790(5) . ? B4' B8' 1.810(5) . ? B4' H4' 1.12 . ? B4 B9 1.786(5) . ? B4 B5 1.800(5) . ? B4 B8 1.816(5) . ? B4 H4 1.12 . ? B5 B9 1.764(5) . ? B5 B6 1.768(5) . ? B5 B10 1.774(5) . ? B5 H5 1.12 . ? B5' B9' 1.773(5) . ? B5' B6' 1.774(5) . ? B5' B10' 1.776(5) . ? B5' H5' 1.12 . ? B6 B10 1.763(5) . ? B6 B11 1.766(5) . ? B6 H6 1.12 . ? B6' B11' 1.763(6) . ? B6' B10' 1.769(5) . ? B6' H6' 1.12 . ? B7' B12' 1.781(5) . ? B7' B8' 1.805(5) . ? B7' B11' 1.809(5) . ? B7' H7' 1.12 . ? B7 B12 1.787(5) . ? B7 B11 1.799(5) . ? B7 B8 1.846(5) . ? B7 H7 1.12 . ? B8' B9' 1.799(5) . ? B8' B12' 1.799(5) . ? B8' H8' 1.12 . ? B8 B9 1.817(5) . ? B8 B12 1.817(5) . ? B9' B10' 1.780(5) . ? B9' B12' 1.782(5) . ? B9' H9' 1.12 . ? B9 B10 1.778(5) . ? B9 B12 1.790(5) . ? B9 H9 1.12 . ? B10' B11' 1.776(5) . ? B10' B12' 1.779(5) . ? B10' H10' 1.12 . ? B10 B11 1.780(5) . ? B10 B12 1.784(5) . ? B10 H10 1.12 . ? B11' B12' 1.771(5) . ? B11' H11' 1.12 . ? B11 B12 1.779(5) . ? B11 H11 1.12 . ? B12 H12 1.12 . ? B12' H12' 1.12 . ? 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 C2 Co3 C1 46.95(12) . . ? C2 Co3 C2' 131.29(12) . . ? C1 Co3 C2' 99.14(12) . . ? C2 Co3 C1' 98.50(12) . . ? C1 Co3 C1' 99.06(12) . . ? C2' Co3 C1' 46.03(12) . . ? C2 Co3 B7 48.90(13) . . ? C1 Co3 B7 83.93(13) . . ? C2' Co3 B7 175.15(13) . . ? C1' Co3 B7 129.95(13) . . ? C2 Co3 B7' 177.18(13) . . ? C1 Co3 B7' 130.78(13) . . ? C2' Co3 B7' 49.02(13) . . ? C1' Co3 B7' 83.38(13) . . ? B7 Co3 B7' 131.11(13) . . ? C2 Co3 B4' 95.75(13) . . ? C1 Co3 B4' 130.63(13) . . ? C2' Co3 B4' 82.72(13) . . ? C1' Co3 B4' 48.45(13) . . ? B7 Co3 B4' 92.43(14) . . ? B7' Co3 B4' 87.07(14) . . ? C2 Co3 B4 83.55(13) . . ? C1 Co3 B4 48.41(12) . . ? C2' Co3 B4 97.22(13) . . ? C1' Co3 B4 130.94(13) . . ? B7 Co3 B4 87.62(13) . . ? B7' Co3 B4 93.62(14) . . ? B4' Co3 B4 179.03(14) . . ? C2 Co3 B8' 131.43(13) . . ? C1 Co3 B8' 176.73(13) . . ? C2' Co3 B8' 83.90(13) . . ? C1' Co3 B8' 83.90(13) . . ? B7 Co3 B8' 93.11(13) . . ? B7' Co3 B8' 50.73(13) . . ? B4' Co3 B8' 50.73(14) . . ? B4 Co3 B8' 130.24(14) . . ? C2 Co3 B8 84.91(13) . . ? C1 Co3 B8 84.27(12) . . ? C2' Co3 B8 132.09(13) . . ? C1' Co3 B8 176.32(13) . . ? B7 Co3 B8 51.72(13) . . ? B7' Co3 B8 93.27(13) . . ? B4' Co3 B8 130.05(14) . . ? B4 Co3 B8 50.61(13) . . ? B8' Co3 B8 92.81(13) . . ? B8 O1 C13 118.3(2) . . ? C15 O2 C14 110.3(2) . . ? C18 N C19 109.0(4) . . ? C18 N C20 109.2(3) . . ? C19 N C20 110.4(3) . . ? C18 N C17 109.5(3) . . ? C19 N C17 109.7(3) . . ? C20 N C17 109.1(3) . . ? C2' C1' B5' 111.8(2) . . ? C2' C1' B4' 111.6(2) . . ? B5' C1' B4' 63.4(2) . . ? C2' C1' B6' 62.5(2) . . ? B5' C1' B6' 62.3(2) . . ? B4' C1' B6' 115.5(2) . . ? C2' C1' Co3 66.60(15) . . ? B5' C1' Co3 124.9(2) . . ? B4' C1' Co3 67.03(15) . . ? B6' C1' Co3 125.4(2) . . ? C2' C1' H1' 121.1 . . ? B5' C1' H1' 116.6 . . ? B4' C1' H1' 118.7 . . ? B6' C1' H1' 115.1 . . ? Co3 C1' H1' 107.1 . . ? C2 C1 B4 112.1(2) . . ? C2 C1 B5 111.5(2) . . ? B4 C1 B5 63.8(2) . . ? C2 C1 B6 62.00(19) . . ? B4 C1 B6 115.6(2) . . ? B5 C1 B6 62.1(2) . . ? C2 C1 Co3 66.26(14) . . ? B4 C1 Co3 67.81(15) . . ? B5 C1 Co3 125.7(2) . . ? B6 C1 Co3 124.6(2) . . ? C2 C1 H1 121.5 . . ? B4 C1 H1 117.9 . . ? B5 C1 H1 116.4 . . ? B6 C1 H1 115.7 . . ? Co3 C1 H1 106.9 . . ? C1' C2' B11' 111.5(2) . . ? C1' C2' B7' 112.3(2) . . ? B11' C2' B7' 64.1(2) . . ? C1' C2' B6' 62.2(2) . . ? B11' C2' B6' 61.9(2) . . ? B7' C2' B6' 116.0(2) . . ? C1' C2' Co3 67.37(15) . . ? B11' C2' Co3 125.3(2) . . ? B7' C2' Co3 66.76(15) . . ? B6' C2' Co3 125.8(2) . . ? C1' C2' H2' 121 . . ? B11' C2' H2' 116.7 . . ? B7' C2' H2' 118.2 . . ? B6' C2' H2' 115.2 . . ? Co3 C2' H2' 106.7 . . ? C1 C2 B11 111.5(2) . . ? C1 C2 B7 112.1(2) . . ? B11 C2 B7 63.9(2) . . ? C1 C2 B6 61.88(19) . . ? B11 C2 B6 62.2(2) . . ? B7 C2 B6 115.8(2) . . ? C1 C2 Co3 66.79(15) . . ? B11 C2 Co3 125.5(2) . . ? B7 C2 Co3 67.31(15) . . ? B6 C2 Co3 125.0(2) . . ? C1 C2 H2 121.4 . . ? B11 C2 H2 116.4 . . ? B7 C2 H2 118.1 . . ? B6 C2 H2 115.5 . . ? Co3 C2 H2 106.9 . . ? O1 C13 C14 108.3(3) . . ? O1 C13 H13A 110 . . ? C14 C13 H13A 110 . . ? O1 C13 H13B 110 . . ? C14 C13 H13B 110 . . ? H13A C13 H13B 108.4 . . ? O2 C14 C13 108.5(3) . . ? O2 C14 H14A 110 . . ? C13 C14 H14A 110 . . ? O2 C14 H14B 110 . . ? C13 C14 H14B 110 . . ? H14A C14 H14B 108.4 . . ? O2 C15 C16 110.5(3) . . ? O2 C15 H15A 109.5 . . ? C16 C15 H15A 109.5 . . ? O2 C15 H15B 109.5 . . ? C16 C15 H15B 109.5 . . ? H15A C15 H15B 108.1 . . ? C15 C16 I 112.6(2) . . ? C15 C16 H16A 109.1 . . ? I C16 H16A 109.1 . . ? C15 C16 H16B 109.1 . . ? I C16 H16B 109.1 . . ? H16A C16 H16B 107.8 . . ? N C17 H17A 109.5 . . ? N C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N C18 H18A 109.5 . . ? N C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N C19 H19A 109.5 . . ? N C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N C20 H20A 109.5 . . ? N C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C1' B4' B9' 103.6(2) . . ? C1' B4' B5' 58.09(19) . . ? B9' B4' B5' 59.7(2) . . ? C1' B4' B8' 105.3(2) . . ? B9' B4' B8' 60.25(19) . . ? B5' B4' B8' 108.7(3) . . ? C1' B4' Co3 64.52(15) . . ? B9' B4' Co3 118.0(2) . . ? B5' B4' Co3 117.9(2) . . ? B8' B4' Co3 65.34(15) . . ? C1' B4' H4' 125.7 . . ? B9' B4' H4' 121.3 . . ? B5' B4' H4' 119.9 . . ? B8' B4' H4' 122.1 . . ? Co3 B4' H4' 111.4 . . ? C1 B4 B9 103.2(2) . . ? C1 B4 B5 58.25(18) . . ? B9 B4 B5 58.92(19) . . ? C1 B4 B8 105.9(2) . . ? B9 B4 B8 60.57(19) . . ? B5 B4 B8 108.7(2) . . ? C1 B4 Co3 63.78(15) . . ? B9 B4 Co3 117.8(2) . . ? B5 B4 Co3 117.1(2) . . ? B8 B4 Co3 65.76(15) . . ? C1 B4 H4 125.8 . . ? B9 B4 H4 121.6 . . ? B5 B4 H4 120.3 . . ? B8 B4 H4 121.4 . . ? Co3 B4 H4 111.8 . . ? C1 B5 B9 103.9(2) . . ? C1 B5 B6 59.42(19) . . ? B9 B5 B6 108.2(2) . . ? C1 B5 B10 104.5(2) . . ? B9 B5 B10 60.3(2) . . ? B6 B5 B10 59.7(2) . . ? C1 B5 B4 57.95(18) . . ? B9 B5 B4 60.15(19) . . ? B6 B5 B4 108.5(2) . . ? B10 B5 B4 108.5(2) . . ? C1 B5 H5 125.3 . . ? B9 B5 H5 122.5 . . ? B6 B5 H5 121 . . ? B10 B5 H5 122.3 . . ? B4 B5 H5 121.3 . . ? C1' B5' B9' 104.0(2) . . ? C1' B5' B6' 59.7(2) . . ? B9' B5' B6' 108.3(3) . . ? C1' B5' B10' 104.6(3) . . ? B9' B5' B10' 60.2(2) . . ? B6' B5' B10' 59.8(2) . . ? C1' B5' B4' 58.51(19) . . ? B9' B5' B4' 59.7(2) . . ? B6' B5' B4' 109.2(2) . . ? B10' B5' B4' 108.2(3) . . ? C1' B5' H5' 125 . . ? B9' B5' H5' 122.7 . . ? B6' B5' H5' 120.7 . . ? B10' B5' H5' 122.4 . . ? B4' B5' H5' 121.1 . . ? C1 B6 C2 56.13(17) . . ? C1 B6 B10 104.3(2) . . ? C2 B6 B10 104.2(2) . . ? C1 B6 B11 103.5(2) . . ? C2 B6 B11 57.98(19) . . ? B10 B6 B11 60.6(2) . . ? C1 B6 B5 58.49(18) . . ? C2 B6 B5 103.9(2) . . ? B10 B6 B5 60.3(2) . . ? B11 B6 B5 108.5(3) . . ? C1 B6 H6 125.4 . . ? C2 B6 H6 125.4 . . ? B10 B6 H6 122.8 . . ? B11 B6 H6 122.2 . . ? B5 B6 H6 121.9 . . ? C1' B6' C2' 55.25(18) . . ? C1' B6' B11' 102.6(2) . . ? C2' B6' B11' 57.87(19) . . ? C1' B6' B10' 103.7(3) . . ? C2' B6' B10' 103.6(3) . . ? B11' B6' B10' 60.4(2) . . ? C1' B6' B5' 58.04(19) . . ? C2' B6' B5' 102.6(2) . . ? B11' B6' B5' 107.7(3) . . ? B10' B6' B5' 60.2(2) . . ? C1' B6' H6' 126 . . ? C2' B6' H6' 126.1 . . ? B11' B6' H6' 122.5 . . ? B10' B6' H6' 122.9 . . ? B5' B6' H6' 122.6 . . ? C2' B7' B12' 102.5(2) . . ? C2' B7' B8' 104.7(2) . . ? B12' B7' B8' 60.19(19) . . ? C2' B7' B11' 57.28(18) . . ? B12' B7' B11' 59.1(2) . . ? B8' B7' B11' 107.8(2) . . ? C2' B7' Co3 64.22(15) . . ? B12' B7' Co3 117.9(2) . . ? B8' B7' Co3 65.65(16) . . ? B11' B7' Co3 116.8(2) . . ? C2' B7' H7' 126.5 . . ? B12' B7' H7' 121.6 . . ? B8' B7' H7' 122.2 . . ? B11' B7' H7' 120.8 . . ? Co3 B7' H7' 111.5 . . ? C2 B7 B12 102.9(2) . . ? C2 B7 B11 57.66(18) . . ? B12 B7 B11 59.5(2) . . ? C2 B7 B8 104.9(2) . . ? B12 B7 B8 59.99(19) . . ? B11 B7 B8 108.2(2) . . ? C2 B7 Co3 63.79(15) . . ? B12 B7 Co3 117.6(2) . . ? B11 B7 Co3 116.8(2) . . ? B8 B7 Co3 65.63(15) . . ? C2 B7 H7 126.3 . . ? B12 B7 H7 121.5 . . ? B11 B7 H7 120.5 . . ? B8 B7 H7 122.1 . . ? Co3 B7 H7 111.9 . . ? B9' B8' B12' 59.4(2) . . ? B9' B8' B7' 106.4(2) . . ? B12' B8' B7' 59.24(19) . . ? B9' B8' B4' 58.89(19) . . ? B12' B8' B4' 105.7(2) . . ? B7' B8' B4' 105.9(2) . . ? B9' B8' Co3 115.6(2) . . ? B12' B8' Co3 115.4(2) . . ? B7' B8' Co3 63.62(15) . . ? B4' B8' Co3 63.93(16) . . ? B9' B8' H8' 121 . . ? B12' B8' H8' 121.3 . . ? B7' B8' H8' 123.4 . . ? B4' B8' H8' 123.7 . . ? Co3 B8' H8' 113.7 . . ? O1 B8 B4 123.6(3) . . ? O1 B8 B9 116.4(3) . . ? B4 B8 B9 58.90(18) . . ? O1 B8 B12 118.6(3) . . ? B4 B8 B12 105.2(2) . . ? B9 B8 B12 59.03(19) . . ? O1 B8 B7 127.3(3) . . ? B4 B8 B7 104.9(2) . . ? B9 B8 B7 105.0(2) . . ? B12 B8 B7 58.39(18) . . ? O1 B8 Co3 119.9(2) . . ? B4 B8 Co3 63.63(15) . . ? B9 B8 Co3 114.6(2) . . ? B12 B8 Co3 113.6(2) . . ? B7 B8 Co3 62.65(14) . . ? B5' B9' B4' 60.6(2) . . ? B5' B9' B10' 60.0(2) . . ? B4' B9' B10' 108.8(3) . . ? B5' B9' B12' 107.7(3) . . ? B4' B9' B12' 107.9(2) . . ? B10' B9' B12' 59.9(2) . . ? B5' B9' B8' 109.9(2) . . ? B4' B9' B8' 60.86(19) . . ? B10' B9' B8' 109.7(3) . . ? B12' B9' B8' 60.3(2) . . ? B5' B9' H9' 121.3 . . ? B4' B9' H9' 121.3 . . ? B10' B9' H9' 121.2 . . ? B12' B9' H9' 122.3 . . ? B8' B9' H9' 120.2 . . ? B5 B9 B10 60.1(2) . . ? B5 B9 B4 60.93(19) . . ? B10 B9 B4 108.9(2) . . ? B5 B9 B12 107.9(3) . . ? B10 B9 B12 60.0(2) . . ? B4 B9 B12 107.6(2) . . ? B5 B9 B8 110.3(2) . . ? B10 B9 B8 110.1(2) . . ? B4 B9 B8 60.53(19) . . ? B12 B9 B8 60.49(19) . . ? B5 B9 H9 120.9 . . ? B10 B9 H9 121 . . ? B4 B9 H9 121.5 . . ? B12 B9 H9 122.3 . . ? B8 B9 H9 120 . . ? B6' B10' B11' 59.6(2) . . ? B6' B10' B5' 60.0(2) . . ? B11' B10' B5' 107.0(3) . . ? B6' B10' B9' 108.2(3) . . ? B11' B10' B9' 107.5(3) . . ? B5' B10' B9' 59.8(2) . . ? B6' B10' B12' 108.0(3) . . ? B11' B10' B12' 59.8(2) . . ? B5' B10' B12' 107.6(3) . . ? B9' B10' B12' 60.1(2) . . ? B6' B10' H10' 121.6 . . ? B11' B10' H10' 122.4 . . ? B5' B10' H10' 122.2 . . ? B9' B10' H10' 121.7 . . ? B12' B10' H10' 121.7 . . ? B6 B10 B5 60.0(2) . . ? B6 B10 B9 107.8(2) . . ? B5 B10 B9 59.5(2) . . ? B6 B10 B11 59.80(19) . . ? B5 B10 B11 107.6(2) . . ? B9 B10 B11 108.0(2) . . ? B6 B10 B12 107.8(2) . . ? B5 B10 B12 107.7(2) . . ? B9 B10 B12 60.3(2) . . ? B11 B10 B12 59.9(2) . . ? B6 B10 H10 121.8 . . ? B5 B10 H10 122.1 . . ? B9 B10 H10 121.7 . . ? B11 B10 H10 121.9 . . ? B12 B10 H10 121.7 . . ? C2' B11' B6' 60.2(2) . . ? C2' B11' B12' 104.0(2) . . ? B6' B11' B12' 108.7(3) . . ? C2' B11' B10' 105.0(3) . . ? B6' B11' B10' 60.0(2) . . ? B12' B11' B10' 60.2(2) . . ? C2' B11' B7' 58.60(19) . . ? B6' B11' B7' 110.0(2) . . ? B12' B11' B7' 59.7(2) . . ? B10' B11' B7' 108.5(3) . . ? C2' B11' H11' 124.8 . . ? B6' B11' H11' 120.1 . . ? B12' B11' H11' 122.8 . . ? B10' B11' H11' 122.2 . . ? B7' B11' H11' 120.9 . . ? C2 B11 B6 59.77(19) . . ? C2 B11 B12 103.9(2) . . ? B6 B11 B12 107.9(3) . . ? C2 B11 B10 104.8(2) . . ? B6 B11 B10 59.6(2) . . ? B12 B11 B10 60.2(2) . . ? C2 B11 B7 58.42(18) . . ? B6 B11 B7 109.2(2) . . ? B12 B11 B7 59.9(2) . . ? B10 B11 B7 108.7(3) . . ? C2 B11 H11 124.9 . . ? B6 B11 H11 120.9 . . ? B12 B11 H11 122.9 . . ? B10 B11 H11 122.2 . . ? B7 B11 H11 120.9 . . ? B11 B12 B10 60.0(2) . . ? B11 B12 B7 60.6(2) . . ? B10 B12 B7 109.0(2) . . ? B11 B12 B9 107.5(2) . . ? B10 B12 B9 59.7(2) . . ? B7 B12 B9 108.7(2) . . ? B11 B12 B8 110.4(2) . . ? B10 B12 B8 109.8(2) . . ? B7 B12 B8 61.62(19) . . ? B9 B12 B8 60.47(19) . . ? B11 B12 H12 121.3 . . ? B10 B12 H12 121.3 . . ? B7 B12 H12 120.8 . . ? B9 B12 H12 122.2 . . ? B8 B12 H12 119.8 . . ? B11' B12' B10' 60.0(2) . . ? B11' B12' B7' 61.2(2) . . ? B10' B12' B7' 109.6(3) . . ? B11' B12' B9' 107.6(3) . . ? B10' B12' B9' 60.0(2) . . ? B7' B12' B9' 108.2(3) . . ? B11' B12' B8' 109.8(2) . . ? B10' B12' B8' 109.7(3) . . ? B7' B12' B8' 60.56(19) . . ? B9' B12' B8' 60.3(2) . . ? B11' B12' H12' 121.2 . . ? B10' B12' H12' 120.9 . . ? B7' B12' H12' 120.8 . . ? B9' B12' H12' 122.3 . . ? B8' B12' H12' 120.5 . . ? #===END