Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _publ_contact_author_email HERWIG.SCHOTTENBERGER@UIBK.AC.AT _publ_contact_author_name 'Prof Herwig Schottenberger' _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_address ; Institut fuer Allgemeine, Anorganische und Theoretische Chemie Leopold Franzens Universitaet Innrain 52a Innsbruck 6020 AUSTRIA ; _publ_section_title ; Synthesis and characterisation of organometallic imidazolium compounds that include a new organometallic ionic liquid ; loop_ _publ_author_name 'Herwig Schottenberger' 'Stephanie Cronje' 'Ulrike Erika Ida Horvath' 'Josef Lukasser' ; J.M.McKenzie ; 'Johann Polin' 'Helgard G. Raubenheimer' 'Klaus Wurst' data_3c _database_code_CSD 215682 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H9 Co2 F6 N2 O6 P' _chemical_formula_weight 564.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.089(2) _cell_length_b 9.378(2) _cell_length_c 14.739(4) _cell_angle_alpha 85.89(2) _cell_angle_beta 87.19(2) _cell_angle_gamma 66.28(2) _cell_volume 1020.7(4) _cell_formula_units_Z 2 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 22 _cell_measurement_theta_min 5.0 _cell_measurement_theta_max 12.0 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.7 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.835 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 556 _exptl_absorpt_coefficient_mu 1.791 _exptl_absorpt_correction_type PSI-scans _exptl_absorpt_correction_T_min 0.671 _exptl_absorpt_correction_T_max 0.842 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method omega-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 4392 _diffrn_reflns_av_R_equivalents 0.0191 _diffrn_reflns_av_sigmaI/netI 0.0253 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 4.09 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3578 _reflns_number_gt 3006 _reflns_threshold_expression >2sigma(I) _computing_data_collection XSCANS _computing_cell_refinement XSCANS _computing_data_reduction XSCANS _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; 3:1 disorder of the ethenyl group C7=C8 : C7A=C8A ; _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^)+(0.0435P)^2^+0.6396P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'mixed, refined at C1' _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0001(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3578 _refine_ls_number_parameters 303 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0432 _refine_ls_R_factor_gt 0.0331 _refine_ls_wR_factor_ref 0.0854 _refine_ls_wR_factor_gt 0.0815 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.002 _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 0.06983(5) 0.28395(4) 0.89332(3) 0.04054(14) Uani 1 1 d . . . Co2 Co 0.30249(5) 0.04917(4) 0.82918(3) 0.03529(14) Uani 1 1 d . . . P1 P 0.01984(11) 0.23588(9) 0.37971(6) 0.0407(2) Uani 1 1 d . . . F1 F 0.2183(3) 0.1872(3) 0.34047(18) 0.0873(8) Uani 1 1 d . . . F2 F -0.0064(3) 0.1116(2) 0.32247(15) 0.0675(6) Uani 1 1 d . . . F3 F -0.0577(5) 0.3660(3) 0.30139(17) 0.1052(10) Uani 1 1 d . . . F4 F -0.1785(3) 0.2837(3) 0.42337(15) 0.0741(7) Uani 1 1 d . . . F5 F 0.0472(4) 0.3595(3) 0.44002(17) 0.0844(8) Uani 1 1 d . . . F6 F 0.0956(3) 0.1087(2) 0.46265(13) 0.0544(5) Uani 1 1 d . . . O1 O -0.3074(4) 0.5052(4) 0.9047(2) 0.1068(13) Uani 1 1 d . . . O2 O 0.2621(5) 0.4937(3) 0.8672(2) 0.0802(9) Uani 1 1 d . . . O3 O 0.1279(5) 0.1710(4) 1.08578(18) 0.0879(10) Uani 1 1 d . . . O4 O 0.4131(4) -0.1724(4) 0.6860(2) 0.0925(11) Uani 1 1 d . . . O5 O 0.5928(3) 0.1626(3) 0.79768(17) 0.0645(7) Uani 1 1 d . . . O6 O 0.3950(5) -0.1711(3) 0.9905(2) 0.0902(10) Uani 1 1 d . . . N1 N -0.1473(3) 0.3265(2) 0.65731(15) 0.0316(5) Uani 1 1 d . A . N2 N -0.3996(3) 0.3352(3) 0.61064(16) 0.0433(6) Uani 1 1 d . . . C10 C -0.1607(6) 0.4210(5) 0.9001(3) 0.0695(11) Uani 1 1 d . . . C20 C 0.1864(5) 0.4151(4) 0.8771(2) 0.0548(9) Uani 1 1 d . . . C30 C 0.1035(5) 0.2173(4) 1.0123(2) 0.0557(9) Uani 1 1 d . . . C40 C 0.3706(4) -0.0884(4) 0.7422(3) 0.0550(9) Uani 1 1 d . . . C50 C 0.4835(4) 0.1171(4) 0.8104(2) 0.0452(7) Uani 1 1 d . . . C60 C 0.3632(5) -0.0858(4) 0.9292(2) 0.0560(9) Uani 1 1 d . . . C1 C 0.0415(4) 0.1143(4) 0.8342(2) 0.0378(6) Uani 1 1 d . . . H1 H -0.024(5) 0.063(4) 0.844(2) 0.047(10) Uiso 1 1 d . . . C2 C 0.0848(3) 0.2054(3) 0.77235(19) 0.0325(6) Uani 1 1 d . . . C3 C 0.0460(4) 0.2703(4) 0.6769(2) 0.0398(7) Uani 1 1 d . . . H3A H 0.0847 0.3567 0.6663 0.048 Uiso 1 1 calc . . . H3B H 0.1157 0.1893 0.6352 0.048 Uiso 1 1 calc . . . C4 C -0.2250(4) 0.2468(3) 0.61855(19) 0.0399(7) Uani 1 1 d . A . H4 H -0.1660 0.1444 0.5997 0.048 Uiso 1 1 calc . . . C5 C -0.4345(4) 0.4746(4) 0.6464(2) 0.0479(8) Uani 1 1 d . A . H5 H -0.5477 0.5588 0.6498 0.057 Uiso 1 1 calc . . . C6 C -0.2792(4) 0.4698(3) 0.6756(2) 0.0417(7) Uani 1 1 d . . . H6 H -0.2627 0.5499 0.7036 0.050 Uiso 1 1 calc . . . C7 C -0.5431(8) 0.3090(7) 0.5712(3) 0.0390(10) Uani 0.75 1 d P A 1 H7 H -0.6553 0.3933 0.5628 0.047 Uiso 0.75 1 calc P B 1 C8 C -0.5229(7) 0.1745(7) 0.5471(4) 0.0637(15) Uani 0.75 1 d P A 1 H8A H -0.4115 0.0890 0.5550 0.076 Uiso 0.75 1 calc P C 1 H8B H -0.6195 0.1611 0.5214 0.076 Uiso 0.75 1 calc P D 1 C7A C -0.469(2) 0.233(2) 0.5612(10) 0.039(3) Uani 0.25 1 d P A 2 H7A H -0.4021 0.1264 0.5519 0.047 Uiso 0.25 1 calc P E 2 C8A C -0.625(2) 0.307(2) 0.5353(11) 0.055(4) Uani 0.25 1 d P A 2 H8C H -0.6850 0.4132 0.5469 0.066 Uiso 0.25 1 calc P F 2 H8D H -0.6838 0.2575 0.5040 0.066 Uiso 0.25 1 calc P G 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0421(3) 0.0381(2) 0.0332(2) -0.00749(16) -0.00204(17) -0.00650(18) Co2 0.0296(2) 0.0338(2) 0.0368(2) -0.00369(16) -0.00756(15) -0.00576(16) P1 0.0416(4) 0.0290(4) 0.0464(4) 0.0006(3) -0.0037(3) -0.0089(3) F1 0.0653(15) 0.116(2) 0.0903(18) -0.0229(15) 0.0315(13) -0.0478(15) F2 0.0715(14) 0.0598(12) 0.0731(14) -0.0174(10) -0.0173(11) -0.0243(11) F3 0.164(3) 0.0588(14) 0.0631(15) 0.0248(12) -0.0192(16) -0.0163(16) F4 0.0355(11) 0.0875(16) 0.0710(14) -0.0066(12) -0.0024(9) 0.0053(10) F5 0.125(2) 0.0540(13) 0.0862(17) -0.0193(12) -0.0065(15) -0.0459(14) F6 0.0514(11) 0.0420(10) 0.0577(11) 0.0061(8) -0.0127(9) -0.0064(8) O1 0.062(2) 0.116(3) 0.092(2) -0.043(2) -0.0071(16) 0.0236(19) O2 0.105(2) 0.0632(18) 0.085(2) 0.0006(15) -0.0180(17) -0.0461(18) O3 0.128(3) 0.082(2) 0.0400(15) 0.0034(14) -0.0040(16) -0.0290(19) O4 0.0510(16) 0.100(2) 0.125(3) -0.078(2) 0.0059(16) -0.0168(15) O5 0.0515(15) 0.097(2) 0.0550(15) 0.0061(14) -0.0072(12) -0.0406(15) O6 0.114(3) 0.0655(18) 0.0675(19) 0.0220(15) -0.0227(17) -0.0130(17) N1 0.0308(12) 0.0286(11) 0.0323(12) 0.0007(9) -0.0059(9) -0.0086(10) N2 0.0413(14) 0.0580(16) 0.0380(13) 0.0103(12) -0.0103(11) -0.0287(13) C10 0.063(3) 0.068(2) 0.052(2) -0.0213(18) -0.0037(18) 0.003(2) C20 0.068(2) 0.0425(18) 0.0471(19) -0.0071(15) -0.0121(16) -0.0127(17) C30 0.067(2) 0.0507(19) 0.0417(19) -0.0094(15) 0.0006(16) -0.0153(17) C40 0.0302(16) 0.056(2) 0.072(2) -0.0224(18) -0.0090(15) -0.0060(15) C50 0.0391(17) 0.0574(19) 0.0340(16) -0.0019(14) -0.0094(13) -0.0131(15) C60 0.055(2) 0.0473(19) 0.053(2) 0.0035(16) -0.0136(17) -0.0072(16) C1 0.0319(15) 0.0444(17) 0.0358(15) -0.0032(13) -0.0044(12) -0.0134(13) C2 0.0249(13) 0.0301(13) 0.0357(14) -0.0067(11) -0.0040(11) -0.0029(11) C3 0.0253(14) 0.0477(17) 0.0382(15) -0.0021(13) -0.0030(11) -0.0059(12) C4 0.0539(19) 0.0367(15) 0.0314(14) 0.0003(12) -0.0019(13) -0.0207(14) C5 0.0330(16) 0.0420(17) 0.062(2) 0.0118(15) -0.0080(14) -0.0095(13) C6 0.0357(16) 0.0275(14) 0.0583(19) -0.0008(13) -0.0066(14) -0.0087(12) C7 0.027(3) 0.040(3) 0.045(3) 0.003(2) -0.008(2) -0.008(2) C8 0.036(3) 0.066(4) 0.089(4) -0.030(3) -0.018(2) -0.014(3) C7A 0.037(9) 0.028(8) 0.050(8) -0.019(6) -0.003(7) -0.006(7) C8A 0.051(9) 0.067(11) 0.044(8) -0.021(7) 0.007(7) -0.017(9) _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 C10 1.792(4) . ? Co1 C30 1.815(4) . ? Co1 C20 1.824(4) . ? Co1 C2 1.957(3) . ? Co1 C1 1.963(3) . ? Co1 Co2 2.4644(9) . ? Co2 C40 1.791(4) . ? Co2 C50 1.820(4) . ? Co2 C60 1.822(4) . ? Co2 C1 1.947(3) . ? Co2 C2 1.960(3) . ? P1 F3 1.571(2) . ? P1 F2 1.572(2) . ? P1 F1 1.574(2) . ? P1 F4 1.597(2) . ? P1 F5 1.599(2) . ? P1 F6 1.6030(19) . ? O1 C10 1.132(5) . ? O2 C20 1.131(4) . ? O3 C30 1.133(4) . ? O4 C40 1.128(4) . ? O5 C50 1.129(4) . ? O6 C60 1.130(4) . ? N1 C4 1.324(4) . ? N1 C6 1.374(4) . ? N1 C3 1.472(3) . ? N2 C4 1.325(4) . ? N2 C5 1.362(4) . ? N2 C7 1.435(6) . ? N2 C7A 1.534(18) . ? C1 H1 0.85(3) . ? C1 C2 1.334(4) . ? C2 C3 1.488(4) . ? C5 C6 1.331(4) . ? C7 C8 1.280(8) . ? C7A C8A 1.23(2) . ? 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 C10 Co1 C30 99.36(17) . . ? C10 Co1 C20 100.98(19) . . ? C30 Co1 C20 103.80(16) . . ? C10 Co1 C2 102.21(14) . . ? C30 Co1 C2 141.27(14) . . ? C20 Co1 C2 103.17(14) . . ? C10 Co1 C1 100.54(17) . . ? C30 Co1 C1 104.73(15) . . ? C20 Co1 C1 140.62(14) . . ? C2 Co1 C1 39.80(12) . . ? C10 Co1 Co2 149.80(13) . . ? C30 Co1 Co2 97.30(11) . . ? C20 Co1 Co2 99.25(11) . . ? C2 Co1 Co2 51.07(8) . . ? C1 Co1 Co2 50.63(9) . . ? C40 Co2 C50 97.25(15) . . ? C40 Co2 C60 99.38(17) . . ? C50 Co2 C60 106.20(15) . . ? C40 Co2 C1 102.29(13) . . ? C50 Co2 C1 144.34(14) . . ? C60 Co2 C1 99.71(15) . . ? C40 Co2 C2 98.47(13) . . ? C50 Co2 C2 108.03(13) . . ? C60 Co2 C2 138.73(15) . . ? C1 Co2 C2 39.94(12) . . ? C40 Co2 Co1 148.67(10) . . ? C50 Co2 Co1 99.08(11) . . ? C60 Co2 Co1 101.45(12) . . ? C1 Co2 Co1 51.23(9) . . ? C2 Co2 Co1 50.96(8) . . ? F3 P1 F2 91.50(14) . . ? F3 P1 F1 91.84(17) . . ? F2 P1 F1 90.43(14) . . ? F3 P1 F4 89.99(16) . . ? F2 P1 F4 90.74(13) . . ? F1 P1 F4 177.80(14) . . ? F3 P1 F5 89.82(15) . . ? F2 P1 F5 178.64(13) . . ? F1 P1 F5 89.87(15) . . ? F4 P1 F5 88.92(14) . . ? F3 P1 F6 177.59(13) . . ? F2 P1 F6 90.57(11) . . ? F1 P1 F6 89.38(13) . . ? F4 P1 F6 88.75(12) . . ? F5 P1 F6 88.10(12) . . ? C4 N1 C6 107.7(2) . . ? C4 N1 C3 125.7(2) . . ? C6 N1 C3 126.6(2) . . ? C4 N2 C5 108.4(2) . . ? C4 N2 C7 131.9(4) . . ? C5 N2 C7 119.6(3) . . ? C4 N2 C7A 103.2(7) . . ? C5 N2 C7A 148.4(7) . . ? C7 N2 C7A 28.8(5) . . ? O1 C10 Co1 178.6(5) . . ? O2 C20 Co1 178.5(3) . . ? O3 C30 Co1 177.8(3) . . ? O4 C40 Co2 178.4(4) . . ? O5 C50 Co2 178.3(3) . . ? O6 C60 Co2 177.2(4) . . ? H1 C1 C2 143(2) . . ? H1 C1 Co2 132(2) . . ? C2 C1 Co2 70.58(18) . . ? H1 C1 Co1 135(2) . . ? C2 C1 Co1 69.85(18) . . ? Co2 C1 Co1 78.14(12) . . ? C1 C2 C3 140.5(3) . . ? C1 C2 Co1 70.35(18) . . ? C3 C2 Co1 137.9(2) . . ? C1 C2 Co2 69.48(17) . . ? C3 C2 Co2 132.1(2) . . ? Co1 C2 Co2 77.97(10) . . ? N1 C3 C2 111.8(2) . . ? N1 C4 N2 108.8(3) . . ? C6 C5 N2 107.5(3) . . ? C5 C6 N1 107.6(3) . . ? C8 C7 N2 122.0(6) . . ? C8A C7A N2 111.5(18) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.459 _refine_diff_density_min -0.268 _refine_diff_density_rms 0.059 data_3b _database_code_CSD 215683 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H29 B Co2 N2 O6' _chemical_formula_weight 738.30 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' 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 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.4434(2) _cell_length_b 17.5931(5) _cell_length_c 21.6424(7) _cell_angle_alpha 99.918(2) _cell_angle_beta 98.869(2) _cell_angle_gamma 91.452(2) _cell_volume 3494.58(17) _cell_formula_units_Z 4 _cell_measurement_temperature 233(2) _cell_measurement_reflns_used 64696 _cell_measurement_theta_min 1.0 _cell_measurement_theta_max 25.0 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.403 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1512 _exptl_absorpt_coefficient_mu 0.998 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 233(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 'Kappa CCD' _diffrn_measurement_method 'phi- and omega-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 17646 _diffrn_reflns_av_R_equivalents 0.0252 _diffrn_reflns_av_sigmaI/netI 0.0399 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 23.00 _reflns_number_total 9694 _reflns_number_gt 7664 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa CCD' _computing_cell_refinement ? _computing_data_reduction 'DENZO and SCALEPACK' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0449P)^2^+3.1441P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'mixed, refined at C1 and C1b' _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0006(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9694 _refine_ls_number_parameters 892 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0588 _refine_ls_R_factor_gt 0.0419 _refine_ls_wR_factor_ref 0.1090 _refine_ls_wR_factor_gt 0.1016 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _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 0.39299(5) 0.50552(3) 0.11829(2) 0.04232(15) Uani 1 1 d . . . Co2 Co 0.38403(6) 0.36293(3) 0.09077(3) 0.05419(17) Uani 1 1 d . . . N1 N 0.5809(3) 0.49606(16) 0.27339(13) 0.0415(7) Uani 1 1 d . . . N2 N 0.5143(3) 0.57691(17) 0.34903(14) 0.0455(7) Uani 1 1 d . . . O1 O 0.3883(3) 0.64814(17) 0.20991(15) 0.0722(8) Uani 1 1 d . . . O2 O 0.6536(3) 0.5478(2) 0.07081(16) 0.0863(10) Uani 1 1 d . . . O3 O 0.1438(3) 0.5358(2) 0.02745(17) 0.0878(10) Uani 1 1 d . . . O4 O 0.3813(4) 0.2111(2) 0.12822(19) 0.1054(12) Uani 1 1 d . . . O5 O 0.6317(7) 0.3505(2) 0.0236(3) 0.178(3) Uani 1 1 d . . . O6 O 0.1265(6) 0.3392(2) -0.0057(3) 0.181(3) Uani 1 1 d . . . C1 C 0.3158(4) 0.4287(2) 0.16094(19) 0.0464(9) Uani 1 1 d . . . H1 H 0.235(4) 0.424(2) 0.1804(17) 0.056(11) Uiso 1 1 d . . . C2 C 0.4566(3) 0.42924(18) 0.17120(17) 0.0403(8) Uani 1 1 d . . . C3 C 0.5792(4) 0.4276(2) 0.22338(18) 0.0481(9) Uani 1 1 d . . . H3A H 0.5698 0.3806 0.2413 0.058 Uiso 1 1 calc . . . H3B H 0.6696 0.4270 0.2064 0.058 Uiso 1 1 calc . . . C4 C 0.4934(4) 0.5053(2) 0.31577(18) 0.0474(9) Uani 1 1 d . . . H4 H 0.4270 0.4675 0.3216 0.057 Uiso 1 1 calc . . . C5 C 0.6198(4) 0.6145(2) 0.32626(19) 0.0506(9) Uani 1 1 d . . . H5 H 0.6561 0.6657 0.3409 0.061 Uiso 1 1 calc . . . C6 C 0.6604(4) 0.5646(2) 0.27970(19) 0.0520(10) Uani 1 1 d . . . H6 H 0.7309 0.5742 0.2553 0.062 Uiso 1 1 calc . . . C7 C 0.4404(5) 0.6070(3) 0.3996(2) 0.0623(11) Uani 1 1 d . . . H7 H 0.3905 0.5715 0.4173 0.075 Uiso 1 1 calc . . . C8 C 0.4367(5) 0.6790(3) 0.4228(2) 0.0722(12) Uani 1 1 d . . . H8A H 0.4853 0.7163 0.4062 0.087 Uiso 1 1 calc . . . H8B H 0.3853 0.6946 0.4563 0.087 Uiso 1 1 calc . . . C01 C 0.3898(4) 0.5923(2) 0.1749(2) 0.0508(9) Uani 1 1 d . . . C02 C 0.5518(4) 0.5306(2) 0.08759(19) 0.0551(10) Uani 1 1 d . . . C03 C 0.2391(4) 0.5240(2) 0.0617(2) 0.0561(10) Uani 1 1 d . . . C04 C 0.3827(5) 0.2696(3) 0.1138(2) 0.0652(11) Uani 1 1 d . . . C05 C 0.5344(7) 0.3540(3) 0.0483(3) 0.100(2) Uani 1 1 d . . . C06 C 0.2282(7) 0.3486(3) 0.0305(3) 0.105(2) Uani 1 1 d . . . Co1B Co 0.15181(5) 0.85673(3) 0.08889(2) 0.04834(16) Uani 1 1 d . . . Co2B Co 0.19739(5) 0.99700(3) 0.12225(2) 0.04181(15) Uani 1 1 d . . . N1B N 0.0733(3) 0.99442(17) 0.26768(14) 0.0435(7) Uani 1 1 d . . . N2B N 0.1872(3) 1.07801(18) 0.34487(14) 0.0480(7) Uani 1 1 d . . . O1B O 0.1528(6) 0.7038(2) 0.1209(2) 0.1465(19) Uani 1 1 d . . . O2B O -0.1324(3) 0.85044(18) 0.00922(16) 0.0777(9) Uani 1 1 d . . . O3B O 0.3544(4) 0.8339(2) -0.00331(16) 0.0934(11) Uani 1 1 d . . . O4B O 0.3288(4) 1.11742(19) 0.22728(16) 0.0899(11) Uani 1 1 d . . . O5B O -0.0870(3) 1.03994(17) 0.06767(14) 0.0725(8) Uani 1 1 d . . . O6B O 0.3896(4) 1.0306(2) 0.03400(18) 0.1007(12) Uani 1 1 d . . . C1B C 0.2747(4) 0.9139(2) 0.16422(18) 0.0444(9) Uani 1 1 d . . . H1B H 0.362(4) 0.909(2) 0.1864(18) 0.054(11) Uiso 1 1 d . . . C2B C 0.1386(4) 0.92124(19) 0.17072(16) 0.0406(8) Uani 1 1 d . . . C3B C 0.0420(4) 0.9236(2) 0.21961(18) 0.0491(9) Uani 1 1 d . . . H3BA H -0.0583 0.9217 0.1989 0.059 Uiso 1 1 calc . . . H3BB H 0.0555 0.8783 0.2403 0.059 Uiso 1 1 calc . . . C4B C 0.1818(4) 1.0057(2) 0.31559(17) 0.0449(9) Uani 1 1 d . . . H4B H 0.2449 0.9681 0.3269 0.054 Uiso 1 1 calc . . . C5B C 0.0779(4) 1.1149(2) 0.3146(2) 0.0576(10) Uani 1 1 d . . . H5B H 0.0570 1.1670 0.3255 0.069 Uiso 1 1 calc . . . C6B C 0.0070(4) 1.0631(2) 0.2667(2) 0.0545(10) Uani 1 1 d . . . H6B H -0.0732 1.0719 0.2377 0.065 Uiso 1 1 calc . . . C7B C 0.2941(5) 1.1088(3) 0.3994(2) 0.0650(11) Uani 1 1 d . . . H7B H 0.3504 1.0742 0.4197 0.078 Uiso 1 1 calc . . . C8B C 0.3150(5) 1.1798(3) 0.4208(2) 0.0799(14) Uani 1 1 d . . . H8BA H 0.2599 1.2155 0.4013 0.096 Uiso 1 1 calc . . . H8BB H 0.3857 1.1973 0.4564 0.096 Uiso 1 1 calc . . . C01B C 0.1515(6) 0.7642(3) 0.1080(3) 0.0848(15) Uani 1 1 d . . . C02B C -0.0240(5) 0.8529(2) 0.0406(2) 0.0543(10) Uani 1 1 d . . . C03B C 0.2740(5) 0.8420(3) 0.0317(2) 0.0647(11) Uani 1 1 d . . . C04B C 0.2731(5) 1.0732(2) 0.1855(2) 0.0573(10) Uani 1 1 d . . . C05B C 0.0243(5) 1.0266(2) 0.08918(18) 0.0504(9) Uani 1 1 d . . . C06B C 0.3156(5) 1.0163(2) 0.0674(2) 0.0621(11) Uani 1 1 d . . . B1 B 0.0177(4) 0.3683(2) 0.30477(18) 0.0355(9) Uani 1 1 d . . . B2 B 0.6629(4) 0.8977(2) 0.33143(18) 0.0353(9) Uani 1 1 d . . . C9 C 0.0264(3) 0.44155(19) 0.26673(16) 0.0391(8) Uani 1 1 d . . . C10 C 0.1107(4) 0.5086(2) 0.29577(19) 0.0494(9) Uani 1 1 d . . . H10 H 0.1619 0.5101 0.3368 0.059 Uiso 1 1 calc . . . C11 C 0.1230(5) 0.5724(2) 0.2678(2) 0.0657(12) Uani 1 1 d . . . H11 H 0.1820 0.6157 0.2894 0.079 Uiso 1 1 calc . . . C12 C 0.0492(5) 0.5724(3) 0.2085(3) 0.0773(15) Uani 1 1 d . . . H12 H 0.0566 0.6160 0.1892 0.093 Uiso 1 1 calc . . . C13 C -0.0361(5) 0.5087(3) 0.1770(2) 0.0721(14) Uani 1 1 d . . . H13 H -0.0867 0.5085 0.1360 0.087 Uiso 1 1 calc . . . C14 C -0.0474(4) 0.4442(2) 0.20608(18) 0.0497(10) Uani 1 1 d . . . H14 H -0.1067 0.4012 0.1841 0.060 Uiso 1 1 calc . . . C15 C -0.0694(3) 0.29417(19) 0.25582(16) 0.0381(8) Uani 1 1 d . . . C16 C -0.0318(4) 0.2674(2) 0.19547(17) 0.0468(9) Uani 1 1 d . . . H16 H 0.0510 0.2898 0.1852 0.056 Uiso 1 1 calc . . . C17 C -0.1091(4) 0.2104(2) 0.15098(18) 0.0586(10) Uani 1 1 d . . . H17 H -0.0788 0.1951 0.1115 0.070 Uiso 1 1 calc . . . C18 C -0.2310(4) 0.1753(2) 0.1636(2) 0.0619(11) Uani 1 1 d . . . H18 H -0.2858 0.1370 0.1330 0.074 Uiso 1 1 calc . . . C19 C -0.2702(4) 0.1979(2) 0.2226(2) 0.0548(10) Uani 1 1 d . . . H19 H -0.3509 0.1735 0.2329 0.066 Uiso 1 1 calc . . . C20 C -0.1926(3) 0.2560(2) 0.26667(17) 0.0435(8) Uani 1 1 d . . . H20 H -0.2240 0.2707 0.3059 0.052 Uiso 1 1 calc . . . C21 C 0.1863(3) 0.35124(17) 0.33123(15) 0.0332(7) Uani 1 1 d . . . C22 C 0.2557(4) 0.3866(2) 0.39158(17) 0.0437(8) Uani 1 1 d . . . H22 H 0.2018 0.4165 0.4189 0.052 Uiso 1 1 calc . . . C23 C 0.4006(4) 0.3794(2) 0.41316(18) 0.0498(9) Uani 1 1 d . . . H23 H 0.4424 0.4051 0.4539 0.060 Uiso 1 1 calc . . . C24 C 0.4827(4) 0.3354(2) 0.3756(2) 0.0544(10) Uani 1 1 d . . . H24 H 0.5808 0.3310 0.3898 0.065 Uiso 1 1 calc . . . C25 C 0.4184(4) 0.2978(2) 0.3166(2) 0.0492(9) Uani 1 1 d . . . H25 H 0.4728 0.2664 0.2905 0.059 Uiso 1 1 calc . . . C26 C 0.2742(3) 0.30549(19) 0.29488(17) 0.0413(8) Uani 1 1 d . . . H26 H 0.2338 0.2790 0.2542 0.050 Uiso 1 1 calc . . . C27 C -0.0628(3) 0.39381(18) 0.36680(15) 0.0346(8) Uani 1 1 d . . . C28 C -0.1213(3) 0.4649(2) 0.38272(16) 0.0416(8) Uani 1 1 d . . . H28 H -0.1191 0.5009 0.3554 0.050 Uiso 1 1 calc . . . C29 C -0.1828(4) 0.4851(2) 0.43715(19) 0.0516(10) Uani 1 1 d . . . H29 H -0.2204 0.5340 0.4461 0.062 Uiso 1 1 calc . . . C30 C -0.1888(4) 0.4338(2) 0.47782(18) 0.0553(10) Uani 1 1 d . . . H30 H -0.2294 0.4474 0.5150 0.066 Uiso 1 1 calc . . . C31 C -0.1345(4) 0.3621(2) 0.46363(17) 0.0513(10) Uani 1 1 d . . . H31 H -0.1402 0.3259 0.4906 0.062 Uiso 1 1 calc . . . C32 C -0.0718(3) 0.3433(2) 0.40987(17) 0.0449(9) Uani 1 1 d . . . H32 H -0.0333 0.2945 0.4017 0.054 Uiso 1 1 calc . . . C33 C 0.7610(3) 0.82796(18) 0.35471(16) 0.0373(8) Uani 1 1 d . . . C34 C 0.7644(4) 0.8099(2) 0.41505(18) 0.0467(9) Uani 1 1 d . . . H34 H 0.7087 0.8379 0.4426 0.056 Uiso 1 1 calc . . . C35 C 0.8465(4) 0.7521(2) 0.43650(19) 0.0546(10) Uani 1 1 d . . . H35 H 0.8466 0.7426 0.4779 0.066 Uiso 1 1 calc . . . C36 C 0.9274(4) 0.7089(2) 0.3971(2) 0.0597(12) Uani 1 1 d . . . H36 H 0.9809 0.6688 0.4108 0.072 Uiso 1 1 calc . . . C37 C 0.9285(4) 0.7257(2) 0.3372(2) 0.0558(11) Uani 1 1 d . . . H37 H 0.9838 0.6969 0.3099 0.067 Uiso 1 1 calc . . . C38 C 0.8492(3) 0.7842(2) 0.31710(18) 0.0453(9) Uani 1 1 d . . . H38 H 0.8544 0.7952 0.2765 0.054 Uiso 1 1 calc . . . C39 C 0.6471(3) 0.8928(2) 0.25374(16) 0.0401(8) Uani 1 1 d . . . C40 C 0.6190(4) 0.8225(2) 0.21095(19) 0.0529(10) Uani 1 1 d . . . H40 H 0.6064 0.7771 0.2273 0.064 Uiso 1 1 calc . . . C41 C 0.6089(4) 0.8169(3) 0.1450(2) 0.0721(13) Uani 1 1 d . . . H41 H 0.5905 0.7685 0.1182 0.087 Uiso 1 1 calc . . . C42 C 0.6258(4) 0.8822(4) 0.1196(2) 0.0752(14) Uani 1 1 d . . . H42 H 0.6198 0.8791 0.0754 0.090 Uiso 1 1 calc . . . C43 C 0.6514(4) 0.9517(3) 0.1595(2) 0.0691(13) Uani 1 1 d . . . H43 H 0.6627 0.9967 0.1426 0.083 Uiso 1 1 calc . . . C44 C 0.6612(3) 0.9572(2) 0.22501(18) 0.0503(10) Uani 1 1 d . . . H44 H 0.6780 1.0063 0.2509 0.060 Uiso 1 1 calc . . . C45 C 0.5039(3) 0.88475(18) 0.35275(16) 0.0344(7) Uani 1 1 d . . . C46 C 0.4741(3) 0.9177(2) 0.41257(16) 0.0416(8) Uani 1 1 d . . . H46 H 0.5432 0.9525 0.4397 0.050 Uiso 1 1 calc . . . C47 C 0.3465(4) 0.9012(2) 0.43393(17) 0.0461(9) Uani 1 1 d . . . H47 H 0.3317 0.9245 0.4747 0.055 Uiso 1 1 calc . . . C48 C 0.2427(4) 0.8511(2) 0.39544(19) 0.0487(9) Uani 1 1 d . . . H48 H 0.1568 0.8396 0.4096 0.058 Uiso 1 1 calc . . . C49 C 0.2665(3) 0.8179(2) 0.33588(18) 0.0452(9) Uani 1 1 d . . . H49 H 0.1962 0.7835 0.3091 0.054 Uiso 1 1 calc . . . C50 C 0.3940(3) 0.83484(18) 0.31495(16) 0.0384(8) Uani 1 1 d . . . H50 H 0.4069 0.8118 0.2738 0.046 Uiso 1 1 calc . . . C51 C 0.7366(3) 0.98176(18) 0.36938(16) 0.0365(8) Uani 1 1 d . . . C52 C 0.8736(4) 0.9916(2) 0.40559(17) 0.0435(8) Uani 1 1 d . . . H52 H 0.9283 0.9480 0.4080 0.052 Uiso 1 1 calc . . . C53 C 0.9326(4) 1.0633(2) 0.43826(18) 0.0538(10) Uani 1 1 d . . . H53 H 1.0246 1.0670 0.4628 0.065 Uiso 1 1 calc . . . C54 C 0.8578(5) 1.1282(2) 0.43487(19) 0.0582(11) Uani 1 1 d . . . H54 H 0.8982 1.1766 0.4567 0.070 Uiso 1 1 calc . . . C55 C 0.7234(5) 1.1221(2) 0.3994(2) 0.0572(11) Uani 1 1 d . . . H55 H 0.6711 1.1664 0.3964 0.069 Uiso 1 1 calc . . . C56 C 0.6645(4) 1.0498(2) 0.36778(18) 0.0474(9) Uani 1 1 d . . . H56 H 0.5716 1.0468 0.3442 0.057 Uiso 1 1 calc . . . 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 0.0422(3) 0.0367(3) 0.0472(3) 0.0073(2) 0.0052(2) 0.0005(2) Co2 0.0731(4) 0.0359(3) 0.0513(3) 0.0037(2) 0.0083(3) -0.0017(2) N1 0.0313(15) 0.0506(18) 0.0423(18) 0.0118(14) 0.0024(13) -0.0031(13) N2 0.0394(16) 0.053(2) 0.0422(18) 0.0078(15) 0.0043(14) -0.0100(14) O1 0.074(2) 0.0477(18) 0.084(2) -0.0088(17) 0.0046(16) 0.0018(14) O2 0.066(2) 0.113(3) 0.091(3) 0.037(2) 0.0270(18) -0.0077(18) O3 0.066(2) 0.091(2) 0.098(3) 0.021(2) -0.0208(19) 0.0084(17) O4 0.150(3) 0.054(2) 0.115(3) 0.037(2) 0.009(3) -0.010(2) O5 0.254(6) 0.090(3) 0.244(6) 0.038(3) 0.200(6) 0.041(3) O6 0.219(6) 0.077(3) 0.189(5) 0.009(3) -0.127(5) -0.030(3) C1 0.042(2) 0.040(2) 0.058(3) 0.0113(18) 0.0095(19) -0.0037(16) C2 0.041(2) 0.0341(19) 0.047(2) 0.0053(16) 0.0132(16) 0.0005(15) C3 0.042(2) 0.050(2) 0.053(2) 0.0107(19) 0.0097(18) 0.0072(16) C4 0.042(2) 0.051(2) 0.050(2) 0.0152(19) 0.0034(18) -0.0101(17) C5 0.043(2) 0.054(2) 0.052(2) 0.012(2) -0.0010(18) -0.0157(17) C6 0.040(2) 0.063(3) 0.053(3) 0.015(2) 0.0046(18) -0.0136(18) C7 0.071(3) 0.060(3) 0.056(3) 0.004(2) 0.020(2) -0.016(2) C8 0.075(3) 0.073(3) 0.069(3) 0.007(3) 0.024(2) -0.004(2) C01 0.045(2) 0.041(2) 0.066(3) 0.013(2) 0.0019(19) 0.0013(17) C02 0.058(3) 0.057(3) 0.052(3) 0.017(2) 0.007(2) 0.0033(19) C03 0.052(2) 0.049(2) 0.063(3) 0.009(2) -0.001(2) 0.0011(18) C04 0.088(3) 0.046(3) 0.061(3) 0.009(2) 0.010(2) -0.003(2) C05 0.161(5) 0.048(3) 0.113(5) 0.013(3) 0.089(4) 0.018(3) C06 0.144(5) 0.048(3) 0.097(4) 0.004(3) -0.047(4) -0.019(3) Co1B 0.0564(3) 0.0348(3) 0.0490(3) 0.0059(2) -0.0052(2) 0.0046(2) Co2B 0.0500(3) 0.0375(3) 0.0394(3) 0.0075(2) 0.0112(2) 0.0015(2) N1B 0.0365(16) 0.057(2) 0.0424(18) 0.0190(15) 0.0108(14) 0.0045(14) N2B 0.0505(18) 0.055(2) 0.0412(19) 0.0088(16) 0.0139(15) 0.0078(15) O1B 0.198(5) 0.070(3) 0.168(5) 0.061(3) -0.024(4) -0.008(3) O2B 0.0637(19) 0.079(2) 0.078(2) 0.0090(17) -0.0191(17) -0.0044(16) O3B 0.087(2) 0.113(3) 0.069(2) -0.018(2) 0.015(2) 0.015(2) O4B 0.119(3) 0.072(2) 0.070(2) -0.0106(19) 0.024(2) -0.046(2) O5B 0.073(2) 0.072(2) 0.070(2) 0.0124(16) 0.0035(17) 0.0294(16) O6B 0.106(3) 0.112(3) 0.112(3) 0.045(2) 0.073(2) 0.023(2) C1B 0.044(2) 0.043(2) 0.042(2) 0.0058(17) -0.0025(18) 0.0031(17) C2B 0.043(2) 0.038(2) 0.041(2) 0.0132(16) -0.0013(16) -0.0018(15) C3B 0.041(2) 0.055(2) 0.052(2) 0.019(2) 0.0011(17) -0.0094(17) C4B 0.043(2) 0.054(2) 0.042(2) 0.0165(19) 0.0095(18) 0.0070(17) C5B 0.063(3) 0.057(3) 0.061(3) 0.016(2) 0.025(2) 0.019(2) C6B 0.045(2) 0.070(3) 0.056(3) 0.024(2) 0.0131(19) 0.019(2) C7B 0.081(3) 0.057(3) 0.057(3) 0.004(2) 0.019(2) 0.008(2) C8B 0.092(3) 0.073(4) 0.079(3) 0.016(3) 0.026(3) 0.001(3) C01B 0.109(4) 0.048(3) 0.090(4) 0.025(3) -0.021(3) -0.003(2) C02B 0.063(3) 0.040(2) 0.054(3) 0.0043(18) -0.003(2) -0.0028(18) C03B 0.064(3) 0.069(3) 0.052(3) -0.007(2) -0.003(2) 0.013(2) C04B 0.076(3) 0.045(2) 0.054(3) 0.007(2) 0.023(2) -0.014(2) C05B 0.067(3) 0.040(2) 0.046(2) 0.0063(18) 0.017(2) 0.0102(19) C06B 0.068(3) 0.060(3) 0.065(3) 0.015(2) 0.027(2) 0.012(2) B1 0.0327(19) 0.036(2) 0.039(2) 0.0077(18) 0.0087(17) 0.0085(16) B2 0.0314(19) 0.037(2) 0.037(2) 0.0070(17) 0.0052(16) -0.0012(16) C9 0.0328(17) 0.043(2) 0.046(2) 0.0101(17) 0.0155(16) 0.0135(15) C10 0.052(2) 0.041(2) 0.062(3) 0.0142(19) 0.0219(19) 0.0127(17) C11 0.067(3) 0.047(2) 0.096(4) 0.024(2) 0.037(3) 0.018(2) C12 0.076(3) 0.067(3) 0.116(5) 0.054(3) 0.051(3) 0.034(3) C13 0.056(3) 0.105(4) 0.075(3) 0.050(3) 0.029(2) 0.041(3) C14 0.0375(19) 0.066(3) 0.056(3) 0.029(2) 0.0193(18) 0.0174(17) C15 0.0326(17) 0.041(2) 0.041(2) 0.0096(16) 0.0050(15) 0.0074(14) C16 0.042(2) 0.055(2) 0.041(2) 0.0009(18) 0.0064(17) -0.0002(17) C17 0.065(3) 0.061(3) 0.043(2) -0.007(2) 0.006(2) 0.005(2) C18 0.062(3) 0.053(3) 0.059(3) -0.007(2) -0.008(2) 0.000(2) C19 0.044(2) 0.048(2) 0.069(3) 0.005(2) 0.0042(19) -0.0027(17) C20 0.0382(19) 0.042(2) 0.048(2) 0.0039(17) 0.0061(16) 0.0040(16) C21 0.0347(17) 0.0290(17) 0.037(2) 0.0076(15) 0.0067(15) 0.0003(14) C22 0.042(2) 0.043(2) 0.045(2) 0.0043(17) 0.0082(17) 0.0051(16) C23 0.041(2) 0.056(2) 0.048(2) 0.0091(19) -0.0043(17) -0.0034(17) C24 0.0328(19) 0.054(2) 0.077(3) 0.021(2) -0.001(2) 0.0046(17) C25 0.036(2) 0.044(2) 0.070(3) 0.010(2) 0.0156(19) 0.0100(16) C26 0.0370(19) 0.040(2) 0.046(2) 0.0012(16) 0.0085(16) 0.0041(15) C27 0.0286(16) 0.0398(19) 0.0351(19) 0.0056(16) 0.0048(14) 0.0052(14) C28 0.0348(18) 0.047(2) 0.041(2) 0.0038(17) 0.0057(16) 0.0045(15) C29 0.046(2) 0.051(2) 0.054(2) -0.008(2) 0.0180(18) 0.0038(17) C30 0.048(2) 0.074(3) 0.041(2) -0.007(2) 0.0173(18) -0.007(2) C31 0.048(2) 0.069(3) 0.039(2) 0.0114(19) 0.0086(17) -0.0048(19) C32 0.0379(19) 0.052(2) 0.045(2) 0.0065(18) 0.0085(16) 0.0065(16) C33 0.0261(16) 0.0357(19) 0.047(2) 0.0046(16) -0.0009(15) -0.0036(14) C34 0.046(2) 0.041(2) 0.048(2) 0.0037(18) -0.0031(17) 0.0012(16) C35 0.056(2) 0.047(2) 0.054(3) 0.0118(19) -0.0153(19) 0.0015(19) C36 0.038(2) 0.039(2) 0.091(4) 0.008(2) -0.020(2) 0.0034(17) C37 0.0287(19) 0.043(2) 0.092(3) 0.005(2) 0.0046(19) 0.0005(16) C38 0.0319(18) 0.041(2) 0.063(3) 0.0072(18) 0.0082(17) -0.0025(15) C39 0.0237(16) 0.052(2) 0.046(2) 0.0107(18) 0.0057(15) 0.0015(14) C40 0.044(2) 0.065(3) 0.050(3) 0.006(2) 0.0096(18) 0.0043(18) C41 0.058(3) 0.108(4) 0.042(3) -0.008(3) 0.007(2) 0.005(2) C42 0.053(3) 0.134(5) 0.044(3) 0.029(3) 0.010(2) -0.006(3) C43 0.043(2) 0.110(4) 0.061(3) 0.041(3) 0.005(2) -0.009(2) C44 0.0321(19) 0.068(3) 0.053(3) 0.022(2) 0.0028(17) -0.0061(17) C45 0.0312(17) 0.0307(18) 0.042(2) 0.0111(15) 0.0012(15) 0.0009(14) C46 0.0380(19) 0.043(2) 0.042(2) 0.0070(17) 0.0030(16) -0.0046(15) C47 0.046(2) 0.051(2) 0.045(2) 0.0115(18) 0.0153(17) 0.0033(17) C48 0.0371(19) 0.050(2) 0.065(3) 0.020(2) 0.0172(19) 0.0000(17) C49 0.0357(19) 0.041(2) 0.059(3) 0.0126(18) 0.0036(17) -0.0077(15) C50 0.0384(19) 0.0340(19) 0.043(2) 0.0085(16) 0.0044(16) 0.0013(15) C51 0.0338(18) 0.0381(19) 0.040(2) 0.0097(15) 0.0102(15) -0.0038(14) C52 0.044(2) 0.042(2) 0.045(2) 0.0118(17) 0.0067(17) -0.0065(16) C53 0.055(2) 0.059(3) 0.045(2) 0.0091(19) 0.0014(18) -0.023(2) C54 0.076(3) 0.044(2) 0.053(3) 0.0016(19) 0.020(2) -0.024(2) C55 0.071(3) 0.034(2) 0.071(3) 0.008(2) 0.027(2) 0.0005(19) C56 0.043(2) 0.044(2) 0.056(2) 0.0096(18) 0.0096(17) -0.0010(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 C01 1.789(4) . ? Co1 C02 1.806(4) . ? Co1 C03 1.824(4) . ? Co1 C1 1.949(4) . ? Co1 C2 1.957(3) . ? Co1 Co2 2.4726(7) . ? Co2 C06 1.790(6) . ? Co2 C04 1.796(4) . ? Co2 C05 1.803(5) . ? Co2 C2 1.937(3) . ? Co2 C1 1.948(4) . ? N1 C4 1.319(4) . ? N1 C6 1.378(4) . ? N1 C3 1.472(5) . ? N2 C4 1.332(5) . ? N2 C5 1.380(4) . ? N2 C7 1.420(5) . ? O1 C01 1.135(4) . ? O2 C02 1.131(4) . ? O3 C03 1.122(5) . ? O4 C04 1.126(5) . ? O5 C05 1.129(6) . ? O6 C06 1.131(6) . ? C1 H1 0.94(4) . ? C1 C2 1.313(5) . ? C2 C3 1.492(5) . ? C5 C6 1.328(5) . ? C7 C8 1.284(6) . ? Co1B C01B 1.747(5) . ? Co1B C03B 1.809(5) . ? Co1B C02B 1.813(4) . ? Co1B C1B 1.952(4) . ? Co1B C2B 1.955(4) . ? Co1B Co2B 2.4562(7) . ? Co2B C04B 1.790(4) . ? Co2B C05B 1.807(4) . ? Co2B C06B 1.817(4) . ? Co2B C1B 1.950(4) . ? Co2B C2B 1.951(3) . ? N1B C4B 1.325(4) . ? N1B C6B 1.377(5) . ? N1B C3B 1.471(5) . ? N2B C4B 1.315(5) . ? N2B C5B 1.374(5) . ? N2B C7B 1.446(5) . ? O1B C01B 1.145(5) . ? O2B C02B 1.133(4) . ? O3B C03B 1.147(5) . ? O4B C04B 1.135(5) . ? O5B C05B 1.130(4) . ? O6B C06B 1.133(5) . ? C1B H1B 0.90(4) . ? C1B C2B 1.321(5) . ? C2B C3B 1.496(5) . ? C5B C6B 1.335(6) . ? C7B C8B 1.254(6) . ? B1 C15 1.643(5) . ? B1 C27 1.645(5) . ? B1 C9 1.652(5) . ? B1 C21 1.661(5) . ? B2 C51 1.643(5) . ? B2 C39 1.652(5) . ? B2 C33 1.656(5) . ? B2 C45 1.659(5) . ? C9 C14 1.397(5) . ? C9 C10 1.401(5) . ? C10 C11 1.374(5) . ? C11 C12 1.362(7) . ? C12 C13 1.376(7) . ? C13 C14 1.400(6) . ? C15 C20 1.400(5) . ? C15 C16 1.412(5) . ? C16 C17 1.370(5) . ? C17 C18 1.379(6) . ? C18 C19 1.380(6) . ? C19 C20 1.379(5) . ? C21 C22 1.399(5) . ? C21 C26 1.405(4) . ? C22 C23 1.393(5) . ? C23 C24 1.368(5) . ? C24 C25 1.374(5) . ? C25 C26 1.388(5) . ? C27 C28 1.390(4) . ? C27 C32 1.404(5) . ? C28 C29 1.389(5) . ? C29 C30 1.370(6) . ? C30 C31 1.378(5) . ? C31 C32 1.380(5) . ? C33 C34 1.392(5) . ? C33 C38 1.406(5) . ? C34 C35 1.394(5) . ? C35 C36 1.376(6) . ? C36 C37 1.379(6) . ? C37 C38 1.379(5) . ? C39 C44 1.397(5) . ? C39 C40 1.403(5) . ? C40 C41 1.402(6) . ? C41 C42 1.372(7) . ? C42 C43 1.362(7) . ? C43 C44 1.392(6) . ? C45 C46 1.397(5) . ? C45 C50 1.400(4) . ? C46 C47 1.396(5) . ? C47 C48 1.373(5) . ? C48 C49 1.374(5) . ? C49 C50 1.393(5) . ? C51 C56 1.395(5) . ? C51 C52 1.396(5) . ? C52 C53 1.391(5) . ? C53 C54 1.365(6) . ? C54 C55 1.370(6) . ? C55 C56 1.393(5) . ? 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 C01 Co1 C02 97.97(17) . . ? C01 Co1 C03 96.67(17) . . ? C02 Co1 C03 106.82(18) . . ? C01 Co1 C1 101.58(16) . . ? C02 Co1 C1 141.56(17) . . ? C03 Co1 C1 103.39(17) . . ? C01 Co1 C2 103.47(16) . . ? C02 Co1 C2 103.95(15) . . ? C03 Co1 C2 140.20(16) . . ? C1 Co1 C2 39.28(14) . . ? C01 Co1 Co2 150.66(12) . . ? C02 Co1 Co2 101.03(13) . . ? C03 Co1 Co2 98.96(12) . . ? C1 Co1 Co2 50.59(11) . . ? C2 Co1 Co2 50.22(10) . . ? C06 Co2 C04 99.2(2) . . ? C06 Co2 C05 105.2(3) . . ? C04 Co2 C05 99.2(2) . . ? C06 Co2 C2 139.9(2) . . ? C04 Co2 C2 101.35(17) . . ? C05 Co2 C2 105.0(2) . . ? C06 Co2 C1 102.3(2) . . ? C04 Co2 C1 102.87(18) . . ? C05 Co2 C1 141.2(2) . . ? C2 Co2 C1 39.50(14) . . ? C06 Co2 Co1 99.04(16) . . ? C04 Co2 Co1 150.64(14) . . ? C05 Co2 Co1 97.94(15) . . ? C2 Co2 Co1 50.95(10) . . ? C1 Co2 Co1 50.62(10) . . ? C4 N1 C6 107.9(3) . . ? C4 N1 C3 125.1(3) . . ? C6 N1 C3 126.6(3) . . ? C4 N2 C5 108.0(3) . . ? C4 N2 C7 124.7(3) . . ? C5 N2 C7 127.3(3) . . ? H1 C1 C2 143(2) . . ? H1 C1 Co2 132(2) . . ? C2 C1 Co2 69.8(2) . . ? H1 C1 Co1 135(2) . . ? C2 C1 Co1 70.7(2) . . ? Co2 C1 Co1 78.78(15) . . ? C1 C2 C3 140.8(3) . . ? C1 C2 Co2 70.7(2) . . ? C3 C2 Co2 135.0(2) . . ? C1 C2 Co1 70.0(2) . . ? C3 C2 Co1 133.9(2) . . ? Co2 C2 Co1 78.83(13) . . ? N1 C3 C2 109.9(3) . . ? N1 C4 N2 109.0(3) . . ? C6 C5 N2 107.1(3) . . ? C5 C6 N1 108.0(3) . . ? C8 C7 N2 124.9(4) . . ? O1 C01 Co1 178.7(4) . . ? O2 C02 Co1 177.2(4) . . ? O3 C03 Co1 179.3(4) . . ? O4 C04 Co2 179.7(5) . . ? O5 C05 Co2 177.2(6) . . ? O6 C06 Co2 177.3(7) . . ? C01B Co1B C03B 98.2(2) . . ? C01B Co1B C02B 100.3(2) . . ? C03B Co1B C02B 104.23(18) . . ? C01B Co1B C1B 100.25(19) . . ? C03B Co1B C1B 102.12(17) . . ? C02B Co1B C1B 143.65(17) . . ? C01B Co1B C2B 101.8(2) . . ? C03B Co1B C2B 139.25(17) . . ? C02B Co1B C2B 106.63(16) . . ? C1B Co1B C2B 39.54(14) . . ? C01B Co1B Co2B 149.63(17) . . ? C03B Co1B Co2B 97.66(14) . . ? C02B Co1B Co2B 100.68(12) . . ? C1B Co1B Co2B 50.96(11) . . ? C2B Co1B Co2B 50.98(9) . . ? C04B Co2B C05B 106.89(18) . . ? C04B Co2B C06B 95.79(18) . . ? C05B Co2B C06B 104.57(18) . . ? C04B Co2B C1B 95.13(17) . . ? C05B Co2B C1B 138.19(16) . . ? C06B Co2B C1B 108.09(17) . . ? C04B Co2B C2B 100.41(16) . . ? C05B Co2B C2B 100.46(15) . . ? C06B Co2B C2B 144.65(17) . . ? C1B Co2B C2B 39.59(15) . . ? C04B Co2B Co1B 145.61(13) . . ? C05B Co2B Co1B 98.14(12) . . ? C06B Co2B Co1B 100.38(13) . . ? C1B Co2B Co1B 51.01(11) . . ? C2B Co2B Co1B 51.11(10) . . ? C4B N1B C6B 107.9(3) . . ? C4B N1B C3B 125.3(3) . . ? C6B N1B C3B 126.3(3) . . ? C4B N2B C5B 108.3(3) . . ? C4B N2B C7B 122.8(3) . . ? C5B N2B C7B 128.9(4) . . ? H1B C1B C2B 142(2) . . ? H1B C1B Co2B 132(2) . . ? C2B C1B Co2B 70.3(2) . . ? H1B C1B Co1B 136(2) . . ? C2B C1B Co1B 70.4(2) . . ? Co2B C1B Co1B 78.02(14) . . ? C1B C2B C3B 141.0(3) . . ? C1B C2B Co2B 70.2(2) . . ? C3B C2B Co2B 133.4(3) . . ? C1B C2B Co1B 70.1(2) . . ? C3B C2B Co1B 136.2(2) . . ? Co2B C2B Co1B 77.91(13) . . ? N1B C3B C2B 110.6(3) . . ? N2B C4B N1B 109.2(3) . . ? C6B C5B N2B 107.3(3) . . ? C5B C6B N1B 107.2(3) . . ? C8B C7B N2B 122.8(4) . . ? O1B C01B Co1B 179.2(5) . . ? O2B C02B Co1B 178.4(4) . . ? O3B C03B Co1B 178.1(4) . . ? O4B C04B Co2B 174.4(4) . . ? O5B C05B Co2B 175.4(3) . . ? O6B C06B Co2B 177.9(4) . . ? C15 B1 C27 111.0(3) . . ? C15 B1 C9 109.1(3) . . ? C27 B1 C9 109.6(3) . . ? C15 B1 C21 113.1(3) . . ? C27 B1 C21 107.9(3) . . ? C9 B1 C21 105.9(2) . . ? C51 B2 C39 110.8(3) . . ? C51 B2 C33 109.2(3) . . ? C39 B2 C33 110.9(3) . . ? C51 B2 C45 109.0(3) . . ? C39 B2 C45 110.8(3) . . ? C33 B2 C45 105.9(3) . . ? C14 C9 C10 114.6(3) . . ? C14 C9 B1 125.2(3) . . ? C10 C9 B1 120.1(3) . . ? C11 C10 C9 123.9(4) . . ? C12 C11 C10 119.5(4) . . ? C11 C12 C13 120.0(4) . . ? C12 C13 C14 119.8(4) . . ? C9 C14 C13 122.1(4) . . ? C20 C15 C16 113.6(3) . . ? C20 C15 B1 124.4(3) . . ? C16 C15 B1 121.8(3) . . ? C17 C16 C15 123.7(3) . . ? C16 C17 C18 120.6(4) . . ? C17 C18 C19 118.0(4) . . ? C20 C19 C18 120.8(3) . . ? C19 C20 C15 123.3(3) . . ? C22 C21 C26 114.2(3) . . ? C22 C21 B1 121.4(3) . . ? C26 C21 B1 124.2(3) . . ? C23 C22 C21 123.1(3) . . ? C24 C23 C22 120.5(3) . . ? C23 C24 C25 118.5(3) . . ? C24 C25 C26 120.9(3) . . ? C25 C26 C21 122.7(3) . . ? C28 C27 C32 114.7(3) . . ? C28 C27 B1 125.0(3) . . ? C32 C27 B1 120.2(3) . . ? C29 C28 C27 123.0(3) . . ? C30 C29 C28 120.1(3) . . ? C29 C30 C31 119.2(3) . . ? C30 C31 C32 120.0(3) . . ? C31 C32 C27 123.0(3) . . ? C34 C33 C38 114.7(3) . . ? C34 C33 B2 121.4(3) . . ? C38 C33 B2 123.9(3) . . ? C33 C34 C35 123.0(3) . . ? C36 C35 C34 120.1(4) . . ? C35 C36 C37 118.7(3) . . ? C36 C37 C38 120.6(4) . . ? C37 C38 C33 122.8(4) . . ? C44 C39 C40 114.3(3) . . ? C44 C39 B2 123.4(3) . . ? C40 C39 B2 122.2(3) . . ? C41 C40 C39 123.1(4) . . ? C42 C41 C40 120.0(4) . . ? C43 C42 C41 118.7(4) . . ? C42 C43 C44 121.3(4) . . ? C43 C44 C39 122.6(4) . . ? C46 C45 C50 114.7(3) . . ? C46 C45 B2 122.1(3) . . ? C50 C45 B2 122.9(3) . . ? C47 C46 C45 123.1(3) . . ? C48 C47 C46 120.1(3) . . ? C47 C48 C49 119.0(3) . . ? C48 C49 C50 120.5(3) . . ? C49 C50 C45 122.7(3) . . ? C56 C51 C52 114.5(3) . . ? C56 C51 B2 121.6(3) . . ? C52 C51 B2 123.8(3) . . ? C53 C52 C51 122.7(3) . . ? C54 C53 C52 120.4(4) . . ? C53 C54 C55 119.3(3) . . ? C54 C55 C56 119.7(4) . . ? C55 C56 C51 123.3(3) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 23.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.267 _refine_diff_density_min -0.813 _refine_diff_density_rms 0.051