Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_1 _database_code_CSD 185897 _journal_coden_Cambridge 186 loop_ _publ_author_name _publ_author_address 'Angus, Patricia M.' ; Department of Chemistry Faculty of Science Australian National University Canberra ACT Australia 0200 ; 'Geue, Rodney J.' ; Research School of Chemistry Australian National University Canberra ACT Australia 0200 ; 'Jensen, Niels Kristian Bech' ; Department of Chemistry University of Aarhus Langelandsgade 140 DK-8000 \%Arhus C Denmark ; 'Larsen, Finn Krebs' ; Department of Chemistry University of Aarhus Langelandsgade 140 DK-8000 \%Arhus C Denmark ; 'Qin Chang Jin' ; Research School of Chemistry Australian National University Canberra ACT Australia 0200 ; 'Sargeson, Alan M.' ; Research School of Chemistry Australian National University Canberra ACT Australia 0200 ; _publ_contact_author_name 'Prof Alan Sargeson' _publ_contact_author_address ; Research School of Chemistry Australian National University Canberra ACT 0200 AUSTRALIA ; _publ_contact_author_email 'ALAN.SARGESON@ANU.EDU.AU' _publ_requested_journal 'Dalton Transactions' #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; An unusual pendant-arm macrocycle formed by condensation of a cobalt(III) tripodal complex with methanal. ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. #============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; 8-(4'-ammonio-2'-thiabutyl)-8-methyl-1-oxa-6,10-dithia-3,13-diazacyclo- tetradecane(chloro)cobalt(III) triperchlorate trihydrate ; _chemical_name_common ? _chemical_formula_sum 'C13 H36 Cl4 Co N3 O16 S3' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_moiety 'C13 H30 Cl Co N3 O S3, 3(Cl O4), 3(H2 O)' _chemical_formula_weight 787.46 _chemical_melting_point ? _chemical_compound_source 'Alan M. Sargeson' #================================== # 6. CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz '+x,+y,+z' '1/2-x,1/2+y,1/2-z' '-x,-y,-z' '1/2+x,1/2-y,1/2+z' _cell_length_a 8.0402(3) _cell_length_b 32.169(1) _cell_length_c 11.8590(4) _cell_angle_alpha 90 _cell_angle_beta 109.662(1) _cell_angle_gamma 90 _cell_volume 2888.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 6887 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 30.04 _exptl_crystal_description rod _exptl_crystal_colour 'Dark red-blue' _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.811 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1652 _exptl_absorpt_coefficient_mu 1.260 _exptl_absorpt_correction_type 'integration' _exptl_absorpt_process_details 'XPREP (Siemens, 1995)' _exptl_absorpt_correction_T_min 0.6344 _exptl_absorpt_correction_T_max 0.9055 #================================== # 7. EXPERIMENTAL DATA _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'x-ray tube' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation scans with narrow frames' _diffrn_standards_decay_% 0 _diffrn_reflns_number 23467 _diffrn_reflns_av_R_equivalents 0.057 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 44 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 30.04 _diffrn_reflns_reduction_process 23467 _reflns_number_total 7461 _reflns_number_observed 5891 _reflns_observed_criterion I>4\s(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution ; SIR97 (Cascarano et al., 1996), KRYSTAL (Hazell, 1995) ; _computing_structure_refinement ; modified ORFLS (Busing, Martin & Levy, 1962), KRYSTAL ; _computing_molecular_graphics ; ORTEP-III (Burnett & Johnson, 1996), KRYSTAL ; _computing_publication_material KRYSTAL _atom_type_scat_source IntTabIV #================================== # 8. REFINEMENT DATA _refine_special_details ; sfls: F calc weight full matrix ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme ; 1/{[\s~cs~(F^2^)+1.03F^2^]^1/2^-|F|}^2^ ; _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method ; B-C type 1 Lorentzian isotropic (Becker & Coppens, 1974) ; _refine_ls_extinction_coef 30(13) _refine_ls_number_reflns 5891 _refine_ls_number_parameters 363 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_obs 0.064 _refine_ls_wR_factor_obs 0.064 _refine_ls_goodness_of_fit_obs 1.29 _refine_ls_shift/su_max 0.0521 _refine_ls_shift/su_mean 0.0085 _refine_diff_density_max 1.2(2) _refine_diff_density_min -0.7(2) #========================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type Co 0.25336(7) 0.11672(2) 0.49193(5) 0.0169(3) Uij Cl 0.5144(1) 0.11128(4) 0.4641(1) 0.0296(7) Uij Cl(2) -0.3656(2) 0.14067(5) 0.0819(1) 0.0413(8) Uij Cl(3) -0.1034(2) 0.21832(4) -0.2040(1) 0.0344(7) Uij Cl(4) 0.0344(2) 0.05101(4) -0.1774(1) 0.0356(8) Uij S(6) -0.0043(1) 0.12123(3) 0.5224(1) 0.0185(6) Uij S(2') 0.1210(1) 0.14766(3) 0.3139(1) 0.0192(6) Uij S(10) 0.3493(1) 0.17714(3) 0.5791(1) 0.0229(6) Uij N(3) 0.1732(5) 0.0614(1) 0.4126(3) 0.021(2) Uij N(13) 0.3575(5) 0.0892(1) 0.6533(3) 0.024(2) Uij N(Am) 0.0827(6) 0.1405(1) 0.0306(4) 0.035(3) Uij O(1) 0.3294(5) 0.0196(1) 0.5807(3) 0.036(2) Uij C(2) 0.2993(7) 0.0267(1) 0.4582(5) 0.034(3) Uij C(14) 0.4439(7) 0.0479(2) 0.6578(5) 0.034(3) Uij C(4) -0.0036(6) 0.0481(1) 0.4174(5) 0.027(3) Uij C(5) -0.1236(6) 0.0848(1) 0.4066(4) 0.025(3) Uij C(12) 0.4858(7) 0.1172(2) 0.7403(5) 0.034(3) Uij C(11) 0.4031(7) 0.1600(2) 0.7336(4) 0.032(3) Uij C(7) -0.1143(6) 0.1707(1) 0.4714(4) 0.021(2) Uij C(9) 0.1672(6) 0.2129(1) 0.5616(4) 0.026(3) Uij C(1') 0.0487(6) 0.1998(1) 0.3378(4) 0.026(3) Uij C(8) 0.0015(6) 0.2058(1) 0.4511(4) 0.021(2) Uij C(Me) -0.1078(7) 0.2458(1) 0.4348(5) 0.032(3) Uij C(3') 0.2741(6) 0.1599(1) 0.2356(4) 0.025(3) Uij C(4') 0.1805(7) 0.1748(1) 0.1104(5) 0.032(3) Uij O(21) -0.2775(9) 0.1031(2) 0.0860(7) 0.126(6) Uij O(22) -0.5422(6) 0.1401(2) 0.0009(4) 0.063(3) Uij O(23) -0.3570(6) 0.1548(2) 0.1944(4) 0.071(4) Uij O(24) -0.2688(8) 0.1692(3) 0.0339(7) 0.109(6) Uij O(31) 0.0106(7) 0.1838(1) -0.1970(4) 0.063(4) Uij O(32) -0.0345(8) 0.2511(2) -0.2625(5) 0.074(4) Uij O(33) -0.0889(8) 0.2341(2) -0.0932(4) 0.091(5) Uij O(34) -0.2721(8) 0.2143(3) -0.2819(7) 0.118(6) Uij O(41) 0.1813(6) 0.0787(1) -0.1493(5) 0.064(4) Uij O(42) 0.0908(8) 0.0110(1) -0.1228(5) 0.075(4) Uij O(43) -0.0374(10) 0.0460(2) -0.3023(4) 0.092(5) Uij O(44) -0.0913(7) 0.0676(2) -0.1312(5) 0.068(4) Uij O(w1) -0.1601(8) -0.0605(2) -0.1634(4) 0.055(4) Uij O(w2) 0.450(1) 0.0301(3) 0.110(1) 0.176(11) Uij O(w3) 0.277(4) 0.0472(6) 0.155(2) 0.088(23) Uij H(3) 0.1504 0.0685 0.3346 0.0400 Uiso H(13) 0.2679 0.0861 0.6831 0.0400 Uiso H(Am)a 0.0235 0.1499 -0.0488 0.0418 Uiso H(Am)b -0.0018 0.1293 0.0621 0.0418 Uiso H(Am)c 0.1644 0.1194 0.0285 0.0418 Uiso H(2)a 0.4082 0.0335 0.4478 0.0405 Uiso H(2)b 0.2527 0.0021 0.4147 0.0405 Uiso H(14)a 0.4785 0.0373 0.7371 0.0411 Uiso H(14)b 0.5453 0.0512 0.6346 0.0411 Uiso H(4)a 0.0133 0.0347 0.4916 0.0324 Uiso H(4)b -0.0569 0.0294 0.3536 0.0324 Uiso H(5)a -0.1506 0.0973 0.3297 0.0305 Uiso H(5)b -0.2299 0.0764 0.4182 0.0305 Uiso H(12)a 0.5906 0.1192 0.7204 0.0410 Uiso H(12)b 0.5139 0.1065 0.8192 0.0410 Uiso H(11)a 0.2990 0.1584 0.7543 0.0386 Uiso H(11)b 0.4841 0.1787 0.7861 0.0386 Uiso H(7)a -0.1628 0.1799 0.5299 0.0255 Uiso H(7)b -0.2068 0.1659 0.3980 0.0255 Uiso H(9)a 0.2087 0.2402 0.5568 0.0311 Uiso H(9)b 0.1333 0.2106 0.6308 0.0311 Uiso H(1')a -0.0526 0.2064 0.2712 0.0314 Uiso H(1')b 0.1415 0.2186 0.3413 0.0314 Uiso H(Me)a -0.0361 0.2675 0.4223 0.0382 Uiso H(Me)b -0.1374 0.2512 0.5047 0.0382 Uiso H(Me)c -0.2129 0.2433 0.3677 0.0382 Uiso H(3')a 0.3396 0.1356 0.2322 0.0305 Uiso H(3')b 0.3524 0.1811 0.2783 0.0305 Uiso H(4')a 0.0989 0.1959 0.1125 0.0386 Uiso H(4')b 0.2652 0.1859 0.0789 0.0386 Uiso loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Co 0.0143(3) 0.0159(2) 0.0235(3) 0.0010(2) 0.0104(2) -0.0020(2) Cl 0.0179(5) 0.0347(6) 0.0418(7) 0.0013(4) 0.0176(5) -0.0040(5) Cl(2 0.0338(7) 0.0587(9) 0.0285(7) 0.0106(6) 0.0065(5) -0.0085(6) Cl(3) 0.0269(6) 0.0406(7) 0.0334(7) 0.0046(5) 0.0072(5) -0.0052(5) Cl(4) 0.0475(8) 0.0302(6) 0.0343(7) -0.0124(5) 0.0205(6) -0.0103(5) S(6) 0.0185(5) 0.0152(4) 0.0269(6) 0.0019(4) 0.0143(4) 0.0009(4) S(2') 0.0200(5) 0.0186(5) 0.0222(6) -0.0022(4) 0.0113(4) -0.0013(4) S(10) 0.0188(5) 0.0214(5) 0.0283(6) -0.0029(4) 0.0077(5) -0.0053(4) N(3) 0.023(2) 0.016(2) 0.029(2) 0.000(1) 0.015(2) -0.004(1) N(13) 0.024(2) 0.026(2) 0.024(2) 0.009(2) 0.009(2) 0.001(2) N(Am) 0.041(3) 0.038(2) 0.027(2) 0.002(2) 0.014(2) 0.000(2) O(1) 0.039(2) 0.022(2) 0.047(2) 0.009(1) 0.015(2) 0.005(2) C(2) 0.032(3) 0.019(2) 0.052(3) 0.009(2) 0.018(2) -0.001(2) C(14) 0.033(3) 0.025(2) 0.044(3) 0.011(2) 0.012(2) 0.004(2) C(4) 0.024(2) 0.018(2) 0.042(3) -0.005(2) 0.016(2) -0.004(2) C(5) 0.020(2) 0.020(2) 0.042(3) -0.002(2) 0.017(2) -0.002(2) C(12) 0.034(3) 0.035(3) 0.030(3) 0.010(2) 0.006(2) -0.004(2) C(11) 0.031(3) 0.036(3) 0.024(3) 0.005(2) 0.003(2) -0.011(2) C(7) 0.019(2) 0.018(2) 0.029(2) 0.004(2) 0.010(2) 0.002(2) C(9) 0.029(2) 0.016(2) 0.033(3) 0.001(2) 0.010(2) -0.009(2) C(1') 0.032(3) 0.017(2) 0.034(3) 0.001(2) 0.017(2) 0.004(2) C(8) 0.023(2) 0.015(2) 0.027(2) 0.002(2) 0.011(2) -0.001(2) C(Me) 0.035(3) 0.021(2) 0.041(3) 0.009(2) 0.015(2) 0.003(2) C(3') 0.026(2) 0.028(2) 0.027(3) -0.004(2) 0.016(2) -0.001(2) C(4') 0.048(3) 0.027(2) 0.031(3) 0.000(2) 0.026(2) 0.003(2) O(21) 0.090(5) 0.105(5) 0.133(6) 0.053(4) -0.027(4) -0.077(5) O(22) 0.034(2) 0.104(4) 0.040(2) 0.008(2) -0.002(2) -0.031(3) O(23) 0.045(3) 0.124(5) 0.039(3) 0.012(3) 0.007(2) -0.024(3) O(24) 0.048(3) 0.158(7) 0.125(6) 0.011(4) 0.034(4) 0.049(5) O(31) 0.107(4) 0.039(2) 0.056(3) 0.032(2) 0.046(3) 0.010(2) O(32) 0.094(4) 0.049(3) 0.090(4) 0.012(3) 0.044(3) 0.014(3) O(33) 0.101(4) 0.134(5) 0.035(3) 0.076(4) 0.021(3) -0.006(3) O(34) 0.048(3) 0.158(7) 0.118(6) -0.012(4) -0.014(3) -0.040(5) O(41) 0.051(3) 0.053(3) 0.097(4) -0.024(2) 0.039(3) -0.020(3) O(42) 0.095(4) 0.037(2) 0.090(4) -0.004(3) 0.026(3) 0.014(3) O(43) 0.190(7) 0.050(3) 0.033(3) -0.044(4) 0.035(3) -0.015(2) O(44) 0.054(3) 0.079(4) 0.082(4) -0.006(3) 0.039(3) -0.021(3) O(w1) 0.090(4) 0.038(3) 0.033(3) -0.003(3) 0.014(3) -0.005(2) O(w2) 0.202(11) 0.139(8) 0.185(9) 0.108(8) 0.062(8) 0.040(7) O(w3) 0.174(32) 0.033(11) 0.046(12) -0.030(14) 0.024(15) 0.000(8) #================================= # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co Cl 2.239(1) . . yes Co N(3) 2.016(4) . . yes Co N(13) 2.016(4) . . yes Co S(6) 2.224(1) . . yes Co S(10) 2.214(1) . . yes Co S(2') 2.251(1) . . yes S(6) C(5) 1.814(5) . . yes S(6) C(7) 1.823(4) . . yes S(10) C(9) 1.818(5) . . yes S(10) C(11) 1.821(5) . . yes S(2') C(1') 1.828(5) . . yes S(2') C(3') 1.817(4) . . yes N(3) C(2) 1.481(6) . . yes N(3) C(4) 1.503(6) . . yes N(13) C(12) 1.491(6) . . yes N(13) C(14) 1.494(6) . . yes N(Am) C(4') 1.494(7) . . yes O(1) C(2) 1.408(7) . . yes O(1) C(14) 1.393(6) . . yes C(4) C(5) 1.503(6) . . yes C(7) C(8) 1.533(6) . . yes C(8) C(Me) 1.534(6) . . yes C(9) C(8) 1.540(7) . . yes C(12) C(11) 1.519(7) . . yes C(1') C(8) 1.526(6) . . yes C(3') C(4') 1.499(7) . . yes Cl(2) O(21) 1.393(6) . . yes Cl(2) O(22) 1.422(4) . . yes Cl(2) O(23) 1.390(5) . . yes Cl(2) O(24) 1.439(7) . . yes Cl(3) O(31) 1.424(4) . . yes Cl(3) O(32) 1.469(5) . . yes Cl(3) O(33) 1.375(5) . . yes Cl(3) O(34) 1.366(6) . . yes Cl(4) O(41) 1.426(4) . . yes Cl(4) O(42) 1.443(5) . . yes Cl(4) O(43) 1.406(5) . . yes Cl(4) O(44) 1.408(5) . . yes loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl Co N(3) 91.7(1) . . . yes Cl Co N(13) 89.7(1) . . . yes Cl Co S(6) 178.89(8) . . . yes Cl Co S(10) 86.62(5) . . . yes Cl Co S(2') 93.85(5) . . . yes N(3) Co N(13) 91.2(2) . . . yes S(6) Co N(3) 88.0(1) . . . yes S(6) Co N(13) 89.2(1) . . . yes S(6) Co S(10) 93.66(4) . . . yes S(6) Co S(2') 87.22(4) . . . yes S(10) Co N(3) 178.3(1) . . . yes S(10) Co N(13) 88.5(1) . . . yes S(2') Co N(3) 88.7(1) . . . yes S(2') Co N(13) 176.4(1) . . . yes S(2') Co S(10) 91.72(5) . . . yes Co N(3) C(2) 115.0(3) . . . yes Co N(3) C(4) 113.0(3) . . . yes C(2) N(3) C(4) 108.2(3) . . . yes Co N(13) C(12) 111.2(3) . . . yes Co N(13) C(14) 117.7(3) . . . yes C(14) N(13) C(12) 107.9(4) . . . yes Co S(6) C(5) 96.8(1) . . . yes Co S(6) C(7) 112.2(1) . . . yes C(5) S(6) C(7) 103.8(2) . . . yes Co S(10) C(9) 111.2(2) . . . yes Co S(10) C(11) 97.5(2) . . . yes C(11) S(10) C(9) 102.5(2) . . . yes Co S(2') C(1') 109.6(2) . . . yes Co S(2') C(3') 112.8(2) . . . yes C(1') S(2') C(3') 100.7(2) . . . yes C(2) O(1) C(14) 114.7(4) . . . yes N(3) C(2) O(1) 111.0(4) . . . yes N(3) C(4) C(5) 111.3(3) . . . yes S(6) C(5) C(4) 106.4(3) . . . yes S(6) C(7) C(8) 116.3(3) . . . yes C(7) C(8) C(9) 111.9(4) . . . yes C(7) C(8) C(Me) 106.5(3) . . . yes C(7) C(8) C(1') 113.0(4) . . . yes C(9) C(8) C(Me) 106.1(4) . . . yes C(9) C(8) C(1') 111.6(4) . . . yes C(1') C(8) C(Me) 107.3(4) . . . yes S(10) C(9) C(8) 115.8(3) . . . yes S(10) C(11) C(12) 106.2(3) . . . yes N(13) C(12) C(11) 108.8(4) . . . yes N(13) C(14) O(1) 111.2(4) . . . yes S(2') C(1') C(8) 116.0(3) . . . yes S(2') C(3') C(4') 112.0(3) . . . yes N(Am) C(4') C(3') 112.0(4) . . . yes O(21) Cl(2) O(22) 113.2(3) . . . yes O(21) Cl(2) O(23) 113.0(4) . . . yes O(21) Cl(2) O(24) 103.3(5) . . . yes O(22) Cl(2) O(23) 111.6(3) . . . yes O(22) Cl(2) O(24) 106.9(4) . . . yes O(23) Cl(2) O(24) 108.2(4) . . . yes O(31) Cl(3) O(32) 104.4(3) . . . yes O(31) Cl(3) O(34) 116.0(4) . . . yes O(31) Cl(3) O(33) 112.7(3) . . . yes O(32) Cl(3) O(33) 105.2(4) . . . yes O(32) Cl(3) O(34) 101.3(4) . . . yes O(33) Cl(3) O(34) 115.3(4) . . . yes O(41) Cl(4) O(42) 110.0(3) . . . yes O(41) Cl(4) O(43) 109.4(3) . . . yes O(41) Cl(4) O(44) 108.6(3) . . . yes O(42) Cl(4) O(43) 109.1(3) . . . yes O(42) Cl(4) O(44) 108.8(3) . . . yes O(43) Cl(4) O(44) 111.0(4) . . . yes