# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Dr W Gregory Jackson' _publ_contact_author_address ; Dr W Gregory Jackson The University of New South Wales AUSTRALIA ; _publ_contact_author_email G-JACKSON@ADFA.EDU.AU _publ_section_title ; The first structurally characterised Perchlorato-cobalt(III) complexes, involving the C-bonded macrobicyclic ligand 1,4,8,11-tetraazabicyclo[9.5.2]octadecane ; loop_ _publ_author_name 'W Gregory Jackson' 'Anthony I. Day' 'Anthony C. Willis' 'Xiangting Zhou' data_wgj10 _database_code_CSD 210479 _chemical_name_common sym-syn-perchlorato _audit_creation_date 03-20-01 _audit_creation_method CRYSTALS_ver_12-03-99 # 1201144 wgj10 _audit_update_record ; 2003-01-20 - Report on C14 H29 Cl2 Co N4 O9 (S-D952-3) by Anthony C. Willis for W. Greg Jackson and Xiangting Zhou, ADFA 2003-01-21 - passes checkcif tests with minor warnings ; #============================================================================== # 4. TEXT _publ_section_abstract #Text of the abstract ; The crystal structure of [(C~14~H~29~N~4~)Co(OClO~3~)]^+^ (ClO~4~)^-^ is reported. ; _publ_section_comment #Text of the paper ; The crystallographic asymmetric unit consists of one [(C~14~H~29~N~4~)Co(OClO~3~)]^+^ cation and one (ClO~4~)^-^ anion. Hydrogen atoms attached to N atoms were refined positionally, and those bonded to C atoms were included at calculated positions and ride on the atoms to which they are bonded. The largest peaks in the final difference electron density map are close to atoms of the uncoordinated perchlorate. The space group is centrosymmetric. ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions #Captions to figures ; ? ; _publ_section_exptl_refinement # see also _refine_ls_hydrogen for refinement keywords. ; Hydrogen atoms attached to N atoms were refined positionally, and those bonded to C atoms were included at calculated positions and ride on the atoms to which they are bonded. ; _publ_section_exptl_prep ; The compound was prepared by XZ and recrystallized from water. The sample ID is S-D952-3. ; #========================================================================== _chemical_name_systematic # IUPAC name, in full ; sym-syn-perchlorato ; _chemical_melting_point 'not measured' # choose from 'full, fullcycle, atomblock, userblock, diagonal, sparse' _refine_ls_matrix_type full # choose from 'heavy, direct, difmap, geom' _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed' _refine_ls_hydrogen_treatment mixed #**************************************************************************** # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al 2001) ; _computing_publication_material ; CRYSTALS (Watkin et al 2001) ; _computing_molecular_graphics ; teXsan (MSC, 1992-1997) ; #============================================================= _cell_length_a 8.4196(1) _cell_angle_alpha 90.0 _cell_length_b 16.6021(2) _cell_angle_beta 92.6915(7) _cell_length_c 14.4434(2) _cell_angle_gamma 90.0 _cell_volume 2016.72(4) _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z+1/2 x,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 International_Tables_Vol_IV_Table_2.2B 'Cl ' 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 International_Tables_Vol_IV_Table_2.2B 'Co ' 0.2990 0.9730 12.2841 4.2791 7.3409 0.2784 4.0034 13.5359 2.3488 71.1692 1.0118 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B 'O ' 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 International_Tables_Vol_IV_Table_2.2B _chemical_formula_sum ' C14 H29 Cl2 Co1 N4 O8 ' _chemical_formula_moiety ' C14 H29 Cl Co1 N4 O4 +, Cl O4 -' _chemical_compound_source ; ? ; _chemical_formula_weight 511.24 _cell_measurement_reflns_used 42431 _cell_measurement_theta_min 3 _cell_measurement_theta_max 30 _cell_measurement_temperature 200 _cell_formula_units_Z 4 _exptl_crystal_description ' block ' _exptl_crystal_colour ' orange ' _exptl_crystal_size_min 0.23 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_max 0.47 _exptl_crystal_density_diffrn 1.684 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1066.823 _exptl_absorpt_coefficient_mu 1.167 # Sheldrick geometric definitions 0.66 0.76 _diffrn_measurement_device_type ; Enraf Nonius Kappa CCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; COLLECT (Nonius BV, 1997) ; _computing_data_reduction ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_structure_solution ; SIR92 (Altomare et al, 1994) ; _diffrn_measurement_method ' \f and \w scans with CCD ' _diffrn_special_details ; CCD data collecting conditions- phi and omega scans of width 1.8 deg at rate 27 sec/frame, crystal-detector distance 32mm, multiple scan sets so over 90 percent of data collected with 4-fold redundancy or more. ; # Absorption correction loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 0 0 0.180 -1 0 0 0.180 0 1 0 0.150 0 -1 0 0.080 0 0 -1 0.250 0 1 1 0.180 0 -1 1 0.170 -2 4 0 0.190 2 -4 0 0.120 -2 -4 0 0.110 2 4 0 0.180 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.652 _exptl_absorpt_correction_T_max 0.800 _exptl_absorpt_process_details ; via Gaussian method (Coppens, 1970) implemented in maXus (2000) ; #_diffrn_reflns_av_R_equivalents 0.036 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 200 _diffrn_reflns_number 47680 _reflns_number_total 5878 _diffrn_reflns_av_R_equivalents 0.05 # Number of reflections with Friedels Law is 5878 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 5899 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 0.997 _reflns_number_gt 4106 _diffrn_reflns_theta_min 4.39 _diffrn_reflns_theta_max 30.03 _diffrn_reflns_theta_full 30.03 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _reflns_limit_h_min -11 _reflns_limit_h_max 11 _reflns_limit_k_min 0 _reflns_limit_k_max 23 _reflns_limit_l_min 0 _reflns_limit_l_max 20 _refine_diff_density_min -0.55 _refine_diff_density_max 0.82 _reflns_threshold_expression >3.00\s(I) _refine_ls_number_reflns 4106 _refine_ls_number_parameters 268 _refine_ls_R_factor_gt 0.0314 _refine_ls_wR_factor_ref 0.0371 _refine_ls_goodness_of_fit_ref 1.0616 _refine_ls_shift/su_max 0.007474 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters, Carruthers & Watkin , 1979, 0.935 0.256 0.589 ; _refine_ls_extinction_method None _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 ## -------------------REFERENCES ----------------------## ## Insert your own references - in alphabetic order _publ_section_references ; Mackay, S., Gilmore, C. J.,Edwards, C., Stewart, N. & Shankland, K. (2000). maXus Computer Program for the Solution and Refinement of Crystal Structures. Nonius, The Netherlands, MacScience, Japan & The University of Glasgow. Coppens, P. (1970). The Evaluation of Absorption and Extinction in Single-Crystal Structure Analysis. Crystallographic Computing. F. R. Ahmed, S. R. Hall and C. P. Huber, eds., Munksgaard. Copenhagen. pp 255-270. Carruthers, J.R. & Watkin, D.J. (1979) Acta Cryst., A35, 698-699. Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. (27), 435-435 COLLECT Software, Nonius BV 1997-2001) Otwinowski, Z. & Minor, W. (1996), Processing of X-ray Diffraction Data Collected in Oscillation Mode. Methods Enzymol. 276, 1997, 307-326. Ed Carter, C.W. & Sweet, R.M., Academic Press. Watkin, D.J., Prout, C.K., Carruthers, J.R., Betteridge, P.W. & Cooper R.I. (2001) CRYSTALS Issue 11. Chemical Crystallography Laboratory, OXFORD, UK. Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.8. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. ; # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 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_occupancy _atom_site_adp_type Co1 co 0.22084(3) 0.583038(13) 0.234349(15) 0.0188 1.0000 Uani Cl1 cl -0.09358(5) 0.44518(3) 0.23567(3) 0.0303 1.0000 Uani Cl2 cl 0.67172(7) 0.72169(4) 0.49013(4) 0.0452 1.0000 Uani O1 o 0.00399(19) 0.5015(1) 0.18504(11) 0.0382 1.0000 Uani O2 o -0.1674(2) 0.48944(14) 0.30717(14) 0.0607 1.0000 Uani O3 o 0.0073(2) 0.38490(12) 0.2764(2) 0.0710 1.0000 Uani O4 o -0.2115(2) 0.41129(12) 0.17404(13) 0.0535 1.0000 Uani O5 o 0.7849(3) 0.78331(15) 0.47718(16) 0.0716 1.0000 Uani O6 o 0.7043(3) 0.65307(13) 0.43337(15) 0.0597 1.0000 Uani O7 o 0.5168(3) 0.7536(3) 0.4639(2) 0.1121 1.0000 Uani O8 o 0.6775(4) 0.70019(19) 0.58617(16) 0.0996 1.0000 Uani N1 n 0.13472(18) 0.6628(1) 0.1474(1) 0.0258 1.0000 Uani N4 n 0.08256(19) 0.6246(1) 0.3279(1) 0.0273 1.0000 Uani N8 n 0.29642(19) 0.4934(1) 0.31197(11) 0.0284 1.0000 Uani N11 n 0.33500(19) 0.5388(1) 0.13252(11) 0.0283 1.0000 Uani C2 c -0.0191(2) 0.68849(13) 0.18553(14) 0.0316 1.0000 Uani C3 c 0.0036(2) 0.69920(13) 0.28919(15) 0.0345 1.0000 Uani C5 c 0.1514(3) 0.63255(16) 0.42390(13) 0.0411 1.0000 Uani C6 c 0.2156(3) 0.55169(18) 0.46022(15) 0.0479 1.0000 Uani C7 c 0.3493(3) 0.51340(16) 0.40890(15) 0.0417 1.0000 Uani C9 c 0.4118(3) 0.44606(14) 0.25920(17) 0.0397 1.0000 Uani C10 c 0.3618(3) 0.45229(12) 0.15697(16) 0.0369 1.0000 Uani C12 c 0.4914(3) 0.58265(15) 0.12335(17) 0.0408 1.0000 Uani C13 c 0.5446(3) 0.62149(16) 0.21440(19) 0.0431 1.0000 Uani C14 c 0.4030(2) 0.65653(13) 0.26120(15) 0.0328 1.0000 Uani C15 c 0.3529(3) 0.73969(13) 0.22759(19) 0.0435 1.0000 Uani C16 c 0.2469(3) 0.73347(13) 0.14084(17) 0.0400 1.0000 Uani C17 c 0.1137(3) 0.62087(16) 0.05562(14) 0.0407 1.0000 Uani C18 c 0.2286(3) 0.55017(16) 0.04719(14) 0.0431 1.0000 Uani H4 h 0.003(3) 0.5860(16) 0.3318(18) 0.0329 1.0000 Uiso H8 h 0.214(3) 0.4594(16) 0.3192(17) 0.0339 1.0000 Uiso H21 h -0.0540(2) 0.74064(13) 0.15649(14) 0.0380 1.0000 Uiso H22 h -0.1018(2) 0.64641(13) 0.17170(14) 0.0380 1.0000 Uiso H31 h 0.0723(2) 0.74720(13) 0.30326(15) 0.0417 1.0000 Uiso H32 h -0.1018(2) 0.70682(13) 0.31708(15) 0.0417 1.0000 Uiso H51 h 0.2403(3) 0.67254(16) 0.42452(13) 0.0494 1.0000 Uiso H52 h 0.0671(3) 0.65189(16) 0.46505(13) 0.0494 1.0000 Uiso H61 h 0.2551(3) 0.56001(18) 0.52591(15) 0.0574 1.0000 Uiso H62 h 0.1249(3) 0.51279(18) 0.45843(15) 0.0574 1.0000 Uiso H71 h 0.4406(3) 0.55188(16) 0.40802(15) 0.0495 1.0000 Uiso H72 h 0.3841(3) 0.46292(16) 0.44173(15) 0.0495 1.0000 Uiso H91 h 0.5213(3) 0.46854(14) 0.27021(17) 0.0477 1.0000 Uiso H92 h 0.4105(3) 0.38843(14) 0.27928(17) 0.0477 1.0000 Uiso H101 h 0.4474(3) 0.42971(12) 0.11887(16) 0.0445 1.0000 Uiso H102 h 0.2612(3) 0.42128(12) 0.14441(16) 0.0445 1.0000 Uiso H121 h 0.4776(3) 0.62527(15) 0.07471(17) 0.0496 1.0000 Uiso H122 h 0.5742(3) 0.54334(15) 0.10486(17) 0.0496 1.0000 Uiso H131 h 0.6222(3) 0.66548(16) 0.20248(19) 0.0518 1.0000 Uiso H132 h 0.5968(3) 0.58004(16) 0.25583(19) 0.0518 1.0000 Uiso H141 h 0.4346(2) 0.66195(13) 0.32852(15) 0.0393 1.0000 Uiso H151 h 0.4497(3) 0.77167(13) 0.21399(19) 0.0524 1.0000 Uiso H152 h 0.2939(3) 0.76735(13) 0.27698(19) 0.0524 1.0000 Uiso H161 h 0.1836(3) 0.78418(13) 0.13286(17) 0.0486 1.0000 Uiso H162 h 0.3140(3) 0.72587(13) 0.08621(17) 0.0486 1.0000 Uiso H171 h 0.1329(3) 0.66047(16) 0.00519(14) 0.0486 1.0000 Uiso H172 h 0.0022(3) 0.60019(16) 0.04845(14) 0.0486 1.0000 Uiso H181 h 0.2963(3) 0.56021(16) -0.00668(14) 0.0517 1.0000 Uiso H182 h 0.1653(3) 0.49984(16) 0.03606(14) 0.0517 1.0000 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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0196(1) 0.0186(1) 0.0181(1) -0.00006(8) 0.00090(7) -0.00021(8) Cl1 0.0286(2) 0.0262(2) 0.0355(2) 0.00446(17) -0.00395(16) -0.00618(16) Cl2 0.0383(3) 0.0642(4) 0.0336(2) -0.0142(2) 0.0056(2) -0.0153(2) O1 0.0417(8) 0.0366(8) 0.0364(8) 0.0038(6) 0.0023(6) -0.0138(6) O2 0.0553(11) 0.0755(14) 0.0532(11) -0.015(1) 0.0214(9) -0.018(1) O3 0.047(1) 0.036(1) 0.127(2) 0.0330(12) -0.0245(12) -0.0063(8) O4 0.053(1) 0.0590(11) 0.0471(9) 0.0015(8) -0.0138(8) -0.0272(9) O5 0.0843(16) 0.0663(14) 0.0640(13) 0.0013(11) 0.0010(11) -0.0299(12) O6 0.0639(12) 0.0608(13) 0.0547(11) -0.0163(9) 0.0079(9) -0.005(1) O7 0.0489(13) 0.167(3) 0.119(2) -0.089(2) -0.0113(14) 0.0153(17) O8 0.155(3) 0.106(2) 0.0388(11) -0.0021(12) 0.0145(14) -0.065(2) N1 0.0286(7) 0.0249(7) 0.0240(7) 0.0022(5) 0.0019(5) 0.0037(6) N4 0.0288(7) 0.0307(8) 0.0226(7) -0.0043(6) 0.0045(5) -0.0027(6) N8 0.0277(7) 0.0276(8) 0.0295(8) 0.0062(6) -0.0040(6) -0.0016(6) N11 0.0307(8) 0.0266(8) 0.0280(7) -0.0041(6) 0.0069(6) 0.0046(6) C2 0.0264(8) 0.0310(9) 0.037(1) 0.0023(8) 0.0023(7) 0.0074(7) C3 0.0318(9) 0.033(1) 0.039(1) -0.0060(8) 0.0097(8) 0.0056(8) C5 0.0471(12) 0.0551(14) 0.0214(8) -0.0099(9) 0.0044(8) -0.005(1) C6 0.0560(14) 0.0655(16) 0.0221(9) 0.009(1) -0.0011(9) -0.0083(12) C7 0.0445(12) 0.0477(13) 0.031(1) 0.0121(9) -0.0125(8) -0.003(1) C9 0.036(1) 0.030(1) 0.0532(13) 0.0086(9) 0.0023(9) 0.0108(8) C10 0.0409(11) 0.0248(9) 0.0457(11) -0.0060(8) 0.0076(9) 0.0069(8) C12 0.034(1) 0.0386(11) 0.0512(12) 0.001(1) 0.0196(9) 0.0041(9) C13 0.0241(9) 0.0428(12) 0.0627(14) 0.0010(11) 0.0059(9) -0.0016(8) C14 0.0263(8) 0.033(1) 0.039(1) -0.0029(8) -0.0001(7) -0.0099(7) C15 0.0381(11) 0.027(1) 0.0659(15) -0.006(1) 0.009(1) -0.0089(8) C16 0.0417(11) 0.026(1) 0.0537(13) 0.0123(9) 0.017(1) 0.0017(8) C17 0.0514(12) 0.0476(13) 0.0224(8) -0.0008(8) -0.0060(8) 0.011(1) C18 0.0549(13) 0.0510(13) 0.0233(8) -0.0100(9) -0.0007(8) 0.0132(11) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Co1 . O1 . 2.3557(15) yes Co1 . N1 . 1.9418(15) yes Co1 . N4 . 1.9503(15) yes Co1 . N8 . 1.9521(16) yes Co1 . N11 . 1.9389(15) yes Co1 . C14 . 1.9836(19) yes Cl1 . O1 . 1.4633(15) yes Cl1 . O2 . 1.433(2) yes Cl1 . O3 . 1.4220(19) yes Cl1 . O4 . 1.4184(17) yes Cl2 . O5 . 1.417(2) yes Cl2 . O6 . 1.438(2) yes Cl2 . O7 . 1.442(3) yes Cl2 . O8 . 1.431(2) yes N1 . C2 . 1.493(2) yes N1 . C16 . 1.512(3) yes N1 . C17 . 1.501(3) yes N4 . C3 . 1.501(3) yes N4 . C5 . 1.484(2) yes N4 . H4 . 0.93(3) no N8 . C7 . 1.487(3) yes N8 . C9 . 1.487(3) yes N8 . H8 . 0.90(3) no N11 . C10 . 1.493(3) yes N11 . C12 . 1.516(3) yes N11 . C18 . 1.501(3) yes C2 . C3 . 1.511(3) yes C2 . H21 . 1.000 no C2 . H22 . 1.000 no C3 . H31 . 1.000 no C3 . H32 . 1.000 no C5 . C6 . 1.531(4) yes C5 . H51 . 1.000 no C5 . H52 . 1.000 no C6 . C7 . 1.516(4) yes C6 . H61 . 1.000 no C6 . H62 . 1.000 no C7 . H71 . 1.000 no C7 . H72 . 1.000 no C9 . C10 . 1.520(3) yes C9 . H91 . 1.000 no C9 . H92 . 1.000 no C10 . H101 . 1.000 no C10 . H102 . 1.000 no C12 . C13 . 1.513(4) yes C12 . H121 . 1.000 no C12 . H122 . 1.000 no C13 . C14 . 1.514(3) yes C13 . H131 . 1.000 no C13 . H132 . 1.000 no C14 . C15 . 1.516(3) yes C14 . H141 . 1.000 no C15 . C16 . 1.508(4) yes C15 . H151 . 1.000 no C15 . H152 . 1.000 no C16 . H161 . 1.000 no C16 . H162 . 1.000 no C17 . C18 . 1.530(3) yes C17 . H171 . 1.000 no C17 . H172 . 1.000 no C18 . H181 . 1.000 no C18 . H182 . 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 . Co1 . N1 . 86.32(6) yes O1 . Co1 . N4 . 86.16(6) yes N1 . Co1 . N4 . 89.41(7) yes O1 . Co1 . N8 . 87.87(6) yes N1 . Co1 . N8 . 173.32(7) yes N4 . Co1 . N8 . 93.49(7) yes O1 . Co1 . N11 . 87.58(6) yes N1 . Co1 . N11 . 87.22(7) yes N4 . Co1 . N11 . 173.07(7) yes N8 . Co1 . N11 . 89.25(7) yes O1 . Co1 . C14 . 173.45(7) yes N1 . Co1 . C14 . 88.20(8) yes N4 . Co1 . C14 . 97.37(8) yes N8 . Co1 . C14 . 97.39(8) yes N11 . Co1 . C14 . 88.58(8) yes O1 . Cl1 . O2 . 107.76(11) yes O1 . Cl1 . O3 . 108.56(12) yes O2 . Cl1 . O3 . 109.48(16) yes O1 . Cl1 . O4 . 109.4(1) yes O2 . Cl1 . O4 . 109.96(13) yes O3 . Cl1 . O4 . 111.55(13) yes O5 . Cl2 . O6 . 110.45(14) yes O5 . Cl2 . O7 . 107.8(2) yes O6 . Cl2 . O7 . 109.63(14) yes O5 . Cl2 . O8 . 108.41(15) yes O6 . Cl2 . O8 . 110.88(18) yes O7 . Cl2 . O8 . 109.6(2) yes Co1 . O1 . Cl1 . 131.41(9) yes Co1 . N1 . C2 . 105.10(11) yes Co1 . N1 . C16 . 110.77(13) yes C2 . N1 . C16 . 110.92(16) yes Co1 . N1 . C17 . 106.24(12) yes C2 . N1 . C17 . 112.93(16) yes C16 . N1 . C17 . 110.64(17) yes Co1 . N4 . C3 . 107.58(11) yes Co1 . N4 . C5 . 117.34(13) yes C3 . N4 . C5 . 114.89(17) yes Co1 . N4 . H4 . 104.7(16) no C3 . N4 . H4 . 106.5(16) no C5 . N4 . H4 . 104.8(16) no Co1 . N8 . C7 . 116.45(14) yes Co1 . N8 . C9 . 108.16(13) yes C7 . N8 . C9 . 115.27(17) yes Co1 . N8 . H8 . 108.0(16) no C7 . N8 . H8 . 103.2(16) no C9 . N8 . H8 . 104.7(16) no Co1 . N11 . C10 . 105.06(12) yes Co1 . N11 . C12 . 110.35(12) yes C10 . N11 . C12 . 111.13(16) yes Co1 . N11 . C18 . 106.08(12) yes C10 . N11 . C18 . 113.13(17) yes C12 . N11 . C18 . 110.80(18) yes N1 . C2 . C3 . 109.09(15) yes N1 . C2 . H21 . 109.6 no C3 . C2 . H21 . 109.57 no N1 . C2 . H22 . 109.57 no C3 . C2 . H22 . 109.57 no H21 . C2 . H22 . 109.467 no N4 . C3 . C2 . 107.76(15) yes N4 . C3 . H31 . 109.9 no C2 . C3 . H31 . 109.90 no N4 . C3 . H32 . 109.9 no C2 . C3 . H32 . 109.9 no H31 . C3 . H32 . 109.467 no N4 . C5 . C6 . 110.99(19) yes N4 . C5 . H51 . 109.09 no C6 . C5 . H51 . 109.09 no N4 . C5 . H52 . 109.09 no C6 . C5 . H52 . 109.09 no H51 . C5 . H52 . 109.467 no C5 . C6 . C7 . 117.29(19) yes C5 . C6 . H61 . 107.48 no C7 . C6 . H61 . 107.48 no C5 . C6 . H62 . 107.48 no C7 . C6 . H62 . 107.48 no H61 . C6 . H62 . 109.467 no N8 . C7 . C6 . 110.97(18) yes N8 . C7 . H71 . 109.10 no C6 . C7 . H71 . 109.10 no N8 . C7 . H72 . 109.10 no C6 . C7 . H72 . 109.10 no H71 . C7 . H72 . 109.467 no N8 . C9 . C10 . 107.70(16) yes N8 . C9 . H91 . 109.92 no C10 . C9 . H91 . 109.91 no N8 . C9 . H92 . 109.91 no C10 . C9 . H92 . 109.91 no H91 . C9 . H92 . 109.467 no N11 . C10 . C9 . 109.09(17) yes N11 . C10 . H101 . 109.6 no C9 . C10 . H101 . 109.57 no N11 . C10 . H102 . 109.57 no C9 . C10 . H102 . 109.57 no H101 . C10 . H102 . 109.467 no N11 . C12 . C13 . 110.58(17) yes N11 . C12 . H121 . 109.19 no C13 . C12 . H121 . 109.19 no N11 . C12 . H122 . 109.2 no C13 . C12 . H122 . 109.19 no H121 . C12 . H122 . 109.467 no C12 . C13 . C14 . 110.15(18) yes C12 . C13 . H131 . 109.30 no C14 . C13 . H131 . 109.30 no C12 . C13 . H132 . 109.30 no C14 . C13 . H132 . 109.30 no H131 . C13 . H132 . 109.467 no Co1 . C14 . C13 . 107.11(15) yes Co1 . C14 . C15 . 107.27(14) yes C13 . C14 . C15 . 114.81(19) yes Co1 . C14 . H141 . 114.42 no C13 . C14 . H141 . 106.82 no C15 . C14 . H141 . 106.65 no C14 . C15 . C16 . 110.39(18) yes C14 . C15 . H151 . 109.24 no C16 . C15 . H151 . 109.24 no C14 . C15 . H152 . 109.24 no C16 . C15 . H152 . 109.24 no H151 . C15 . H152 . 109.467 no N1 . C16 . C15 . 110.37(17) yes N1 . C16 . H161 . 109.2 no C15 . C16 . H161 . 109.25 no N1 . C16 . H162 . 109.25 no C15 . C16 . H162 . 109.25 no H161 . C16 . H162 . 109.467 no N1 . C17 . C18 . 112.18(16) yes N1 . C17 . H171 . 108.79 no C18 . C17 . H171 . 108.79 no N1 . C17 . H172 . 108.79 no C18 . C17 . H172 . 108.79 no H171 . C17 . H172 . 109.467 no N11 . C18 . C17 . 112.74(17) yes N11 . C18 . H181 . 108.65 no C17 . C18 . H181 . 108.65 no N11 . C18 . H182 . 108.65 no C17 . C18 . H182 . 108.65 no H181 . C18 . H182 . 109.467 no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O2 C6 3.471(3) . 2_566 no O2 O6 3.472(3) . 1_455 no O2 C13 3.490(3) . 1_455 no O3 C3 3.225(3) . 3_545 no O3 C2 3.308(3) . 3_545 no O3 O8 3.533(4) . 2_666 no O3 C16 3.546(3) . 3_545 no O4 C18 3.255(3) . 2_565 no O4 C15 3.422(3) . 3_545 no O4 C17 3.496(3) . 2_565 no O4 C9 3.503(3) . 1_455 no O5 C17 3.344(4) . 4_665 no O5 C2 3.396(3) . 4_665 no O5 C10 3.595(3) . 3_655 no O6 C13 3.418(3) . . no O6 C3 3.430(3) . 1_655 no O6 C14 3.468(3) . . no O7 C14 3.438(4) . . no O7 C16 3.505(4) . 4_565 no O7 C12 3.576(5) . 4_565 no O8 C9 3.407(4) . 2_666 no O8 C2 3.414(4) . 4_665 no O8 N8 3.537(3) . 2_666 no O8 C7 3.554(4) . 2_666 no C7 C7 3.597(5) . 2_666 no #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Co1 O1 Cl1 O2 . . . . 59.9(1) no Co1 O1 Cl1 O3 . . . . -58.6(2) no Co1 O1 Cl1 O4 . . . . 179.4(1) no Co1 N1 C2 C3 . . . . 42.6(2) no Co1 N1 C16 C15 . . . . -23.7(2) no Co1 N1 C17 C18 . . . . -26.5(2) no Co1 N4 C3 C2 . . . . 32.2(2) no Co1 N4 C5 C6 . . . . -57.1(2) no Co1 N8 C7 C6 . . . . 59.2(2) no Co1 N8 C9 C10 . . . . -31.4(2) no Co1 N11 C10 C9 . . . . -42.6(2) no Co1 N11 C12 C13 . . . . 23.3(2) no Co1 N11 C18 C17 . . . . 26.1(2) no Co1 C14 C13 C12 . . . . 35.8(2) no Co1 C14 C15 C16 . . . . -35.3(2) no Cl1 O1 Co1 N1 . . . . -143.3(1) no Cl1 O1 Co1 N4 . . . . -53.7(1) no Cl1 O1 Co1 N8 . . . . 40.0(1) no Cl1 O1 Co1 N11 . . . . 129.3(1) no Cl1 O1 Co1 C14 . . . . -176.7(6) no O1 Co1 N1 C2 . . . . 66.7(1) no O1 Co1 N1 C16 . . . . -173.5(1) no O1 Co1 N1 C17 . . . . -53.2(1) no O1 Co1 N4 C3 . . . . -93.5(1) no O1 Co1 N4 C5 . . . . 135.1(2) no O1 Co1 N8 C7 . . . . -134.2(1) no O1 Co1 N8 C9 . . . . 94.1(1) no O1 Co1 N11 C10 . . . . -67.9(1) no O1 Co1 N11 C12 . . . . 172.3(1) no O1 Co1 N11 C18 . . . . 52.2(1) no O1 Co1 C14 C13 . . . . -72.5(7) no O1 Co1 C14 C15 . . . . 51.2(7) no N1 Co1 N4 C3 . . . . -7.2(1) no N1 Co1 N4 C5 . . . . -138.6(2) no N1 Co1 N8 C7 . . . . -163.8(5) no N1 Co1 N8 C9 . . . . 64.5(6) no N1 Co1 N11 C10 . . . . -154.3(1) no N1 Co1 N11 C12 . . . . 85.9(1) no N1 Co1 N11 C18 . . . . -34.2(1) no N1 Co1 C14 C13 . . . . -105.8(2) no N1 Co1 C14 C15 . . . . 17.9(2) no N1 C2 C3 N4 . . . . -50.3(2) no N1 C16 C15 C14 . . . . 39.0(3) no N1 C17 C18 N11 . . . . 0.3(3) no N4 Co1 N1 C2 . . . . -19.5(1) no N4 Co1 N1 C16 . . . . 100.3(1) no N4 Co1 N1 C17 . . . . -139.5(1) no N4 Co1 N8 C7 . . . . -48.1(2) no N4 Co1 N8 C9 . . . . -179.8(1) no N4 Co1 N11 C10 . . . . -93.5(6) no N4 Co1 N11 C12 . . . . 146.7(5) no N4 Co1 N11 C18 . . . . 26.6(6) no N4 Co1 C14 C13 . . . . 165.0(2) no N4 Co1 C14 C15 . . . . -71.3(2) no N4 C5 C6 C7 . . . . 61.8(3) no N8 Co1 N1 C2 . . . . 96.4(6) no N8 Co1 N1 C16 . . . . -143.8(5) no N8 Co1 N1 C17 . . . . -23.6(6) no N8 Co1 N4 C3 . . . . 178.9(1) no N8 Co1 N4 C5 . . . . 47.5(2) no N8 Co1 N11 C10 . . . . 20.0(1) no N8 Co1 N11 C12 . . . . -99.8(1) no N8 Co1 N11 C18 . . . . 140.1(1) no N8 Co1 C14 C13 . . . . 70.5(2) no N8 Co1 C14 C15 . . . . -165.8(2) no N8 C7 C6 C5 . . . . -63.0(3) no N8 C9 C10 N11 . . . . 49.8(2) no N11 Co1 N1 C2 . . . . 154.5(1) no N11 Co1 N1 C16 . . . . -85.7(1) no N11 Co1 N1 C17 . . . . 34.5(1) no N11 Co1 N4 C3 . . . . -67.9(6) no N11 Co1 N4 C5 . . . . 160.7(5) no N11 Co1 N8 C7 . . . . 138.2(2) no N11 Co1 N8 C9 . . . . 6.5(1) no N11 Co1 C14 C13 . . . . -18.6(2) no N11 Co1 C14 C15 . . . . 105.2(2) no N11 C12 C13 C14 . . . . -39.2(3) no C2 N1 Co1 C14 . . . . -116.9(1) no C2 N1 C16 C15 . . . . 92.6(2) no C2 N1 C17 C18 . . . . -141.2(2) no C2 C3 N4 C5 . . . . 164.9(2) no C3 N4 Co1 C14 . . . . 81.0(1) no C3 N4 C5 C6 . . . . 174.9(2) no C3 C2 N1 C16 . . . . -77.1(2) no C3 C2 N1 C17 . . . . 158.0(2) no C5 N4 Co1 C14 . . . . -50.5(2) no C6 C7 N8 C9 . . . . -172.5(2) no C7 N8 Co1 C14 . . . . 49.8(2) no C7 N8 C9 C10 . . . . -163.7(2) no C9 N8 Co1 C14 . . . . -81.9(1) no C9 C10 N11 C12 . . . . 76.7(2) no C9 C10 N11 C18 . . . . -157.9(2) no C10 N11 Co1 C14 . . . . 117.4(1) no C10 N11 C12 C13 . . . . -92.8(2) no C10 N11 C18 C17 . . . . 140.7(2) no C12 N11 Co1 C14 . . . . -2.4(1) no C12 N11 C18 C17 . . . . -93.8(2) no C12 C13 C14 C15 . . . . -83.2(2) no C13 C12 N11 C18 . . . . 140.6(2) no C13 C14 C15 C16 . . . . 83.5(2) no C14 Co1 N1 C16 . . . . 2.9(1) no C14 Co1 N1 C17 . . . . 123.2(1) no C14 Co1 N11 C18 . . . . -122.5(1) no C15 C16 N1 C17 . . . . -141.2(2) no C16 N1 C17 C18 . . . . 93.8(2) no #------------------------------------------------------------------------------ #===END data_wgj11 _database_code_CSD 210480 _chemical_name_common 'Sym-anti perchlorato' _audit_creation_date 03-13-01 _audit_creation_method CRYSTALS_ver_12-03-99 # 1131415 wgj11 _audit_update_record ; 2003-01-14 - Report on C14 H29 Cl2 Co N4 O9 (S-D952-2) by Anthony C. Willis for W. Greg Jackson and Xiangting Zhou, ADFA 2003-01-14 - passes checkcif tests with minor warnings ; #============================================================================== # 4. TEXT _publ_section_abstract #Text of the abstract ; The crystal structure of [(C~14~H~29~N~4~)Co(OClO~3~)]^+^ (ClO~4~)^-^ is reported. ; _publ_section_comment #Text of the paper ; The crystallographic asymmetric unit consists of one [(C~14~H~29~N~4~)Co(OClO~3~)]^+^ cation and one (ClO~4~)^-^ anion. When C(12) was refined with anisotropic displacement factors the thermal ellipsoid was severely elongated. Consequently this atom was split over two sites, C(120) and C(121), with a common isotropic displacement factor, and the relative occupancies were refined. This corresponds to there being two conformations of the N(11)---C(12)---C(13)---C(14) linkage, with the two sites for C(12) being separated but the two sites for C(13) being sufficiently close together that they can be considered as one atom of full occupancy. Restraints were imposed on N(11)--C and C(13)--C distances and N(11)--C--C(13) angles so they tended to their respective means. In the final structure the C(13)--C(120) and C(13)--C(121) distances differ by a small amount (1.447(8)\%A cf. 1.487(7)\%A) even though there was a restraint that they should tend to be equal. This difference most likely arises from treating C(13) as a single site only. Atoms C(10), N(11) and C(18) are also each probably averages of two sites arising from the two conformations of the linkage, so distances and angles in this part of the cation are unreliable. An alternative, less plausible, interpretation is that the structure is a co-crystallization of two species, one with C(12)-[single bond]-C(13) and the other C(12)-[double bond]-C(13). This is unlikely as the N(11)--C distances are equal, even when no restraints are imposed. Hydrogen atoms attached to N atoms were refined positionally, and those bonded to C atoms were included at calculated positions and ride on the atoms to which they are bonded. The largest peaks in the final difference electron density map are close to atoms of the coordinated perchlorate. The space group is noncentrosymmetric. Refinement of a Flack parameter established the absolute structure. ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions #Captions to figures ; ? ; _publ_section_exptl_refinement # see also _refine_ls_hydrogen for refinement keywords. ; Hydrogen atoms attached to N atoms were refined positionally, and those bonded to C atoms were included at calculated positions and ride on the atoms to which they are bonded. ; _publ_section_exptl_prep ; The compound was prepared by XZ and recrystallized from water. The sample ID is S-D952-3. ; #========================================================================== _chemical_name_systematic # IUPAC name, in full ; Sym-anti perchlorato ; _chemical_melting_point 'not measured' # choose from 'full, fullcycle, atomblock, userblock, diagonal, sparse' _refine_ls_matrix_type full # choose from 'heavy, direct, difmap, geom' _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed' _refine_ls_hydrogen_treatment mixed #**************************************************************************** # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al 2001) ; _computing_publication_material ; CRYSTALS (Watkin et al 2001) ; _computing_molecular_graphics ; teXsan (MSC, 1992-1997) ; #============================================================= _cell_length_a 8.1097(1) _cell_angle_alpha 90.0 _cell_length_b 14.6807(3) _cell_angle_beta 108.442(1) _cell_length_c 8.7957(2) _cell_angle_gamma 90.0 _cell_volume 993.40(3) _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21 1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,y+1/2,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 International_Tables_Vol_IV_Table_2.2B 'Cl ' 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 International_Tables_Vol_IV_Table_2.2B 'Co ' 0.2990 0.9730 12.2841 4.2791 7.3409 0.2784 4.0034 13.5359 2.3488 71.1692 1.0118 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B 'O ' 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 International_Tables_Vol_IV_Table_2.2B _chemical_formula_sum ' C14 H29 Cl2 Co1 N4 O8 ' _chemical_formula_moiety ' C14 H29 Cl Co1 N4 O4 +, Cl O4 -' _chemical_compound_source ; ? ; _chemical_formula_weight 511.24 _cell_measurement_reflns_used 21669 _cell_measurement_theta_min 3 _cell_measurement_theta_max 30 _cell_measurement_temperature 200 _cell_formula_units_Z 2 _exptl_crystal_description ' plate ' _exptl_crystal_colour ' purple ' _exptl_crystal_size_min 0.13 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_max 0.32 _exptl_crystal_density_diffrn 1.709 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 533.411 _exptl_absorpt_coefficient_mu 1.185 # Sheldrick geometric definitions 0.68 0.86 _diffrn_measurement_device_type ; Enraf Nonius Kappa CCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; COLLECT (Nonius BV, 1997) ; _computing_data_reduction ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_structure_solution ; SIR92 (Altomare et al, 1994) ; _diffrn_measurement_method ' \f and \w scans with CCD ' _diffrn_special_details ; CCD data collecting conditions- phi and omega scans of width 2 deg at rate 20 sec/frame, crystal-detector distance 28mm, multiple scan sets so over 90 percent of data collected with 4-fold redundancy or more (assuming Friedel's Law). ; # Absorption correction loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 -1 0 0.130 -1 6 0 0.150 6 5 -1 0.150 -6 -5 1 0.170 0 0 1 0.010 -3 -1 -13 0.100 4 3 19 0.010 1 1 -14 0.120 -3 -8 1 0.140 4 -12 11 0.030 -1 -11 -18 0.110 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.704 _exptl_absorpt_correction_T_max 0.898 _exptl_absorpt_process_details ; via Gaussian method (Coppens, 1970) implemented in maXus (2000) ; #_diffrn_reflns_av_R_equivalents 0.047 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 200 _diffrn_reflns_number 24988 _reflns_number_total 5778 _diffrn_reflns_av_R_equivalents 0.07 # Number of reflections with Friedels Law is 24988 # Number of reflections without Friedels Law is 5778 # Theoretical number of reflections is about 2768 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measured_fraction_theta_full 1.000 _reflns_number_gt 3703 _diffrn_reflns_theta_min 4.13 _diffrn_reflns_theta_max 30.01 _diffrn_reflns_theta_full 30.01 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _reflns_limit_h_min -11 _reflns_limit_h_max 10 _reflns_limit_k_min -20 _reflns_limit_k_max 20 _reflns_limit_l_min 0 _reflns_limit_l_max 12 _refine_diff_density_min -0.50 _refine_diff_density_max 1.32 _reflns_threshold_expression >3.00\s(I) _refine_ls_number_reflns 3703 _refine_ls_number_parameters 268 _refine_ls_R_factor_gt 0.0368 _refine_ls_wR_factor_ref 0.0416 _refine_ls_goodness_of_fit_ref 1.0641 _refine_ls_shift/su_max 0.016625 _refine_ls_abs_structure_Flack 0.004(16) _chemical_absolute_configuration ad _refine_ls_abs_structure_details 'Flack, 2768 Friedel-pairs' _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters, Carruthers & Watkin , 1979, 0.635 0.226 0.338 ; _refine_ls_extinction_method None _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 ## -------------------REFERENCES ----------------------## ## Insert your own references - in alphabetic order _publ_section_references ; Mackay, S., Gilmore, C. J.,Edwards, C., Stewart, N. & Shankland, K. (2000). maXus Computer Program for the Solution and Refinement of Crystal Structures. Nonius, The Netherlands, MacScience, Japan & The University of Glasgow. Coppens, P. (1970). The Evaluation of Absorption and Extinction in Single-Crystal Structure Analysis. Crystallographic Computing. F. R. Ahmed, S. R. Hall and C. P. Huber, eds., Munksgaard. Copenhagen. pp 255-270. Carruthers, J.R. & Watkin, D.J. (1979) Acta Cryst., A35, 698-699. Flack, H.D. (1983) Acta Cryst., A39, 876-881. Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. (27), 435-435 COLLECT Software, Nonius BV 1997-2001) Otwinowski, Z. & Minor, W. (1996), Processing of X-ray Diffraction Data Collected in Oscillation Mode. Methods Enzymol. 276, 1997, 307-326. Ed Carter, C.W. & Sweet, R.M., Academic Press. Watkin, D.J., Prout, C.K., Carruthers, J.R., Betteridge, P.W. & Cooper R.I. (2001) CRYSTALS Issue 11. Chemical Crystallography Laboratory, OXFORD, UK. Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.8. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. ; # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 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_occupancy _atom_site_adp_type Co1 co 0.65671(5) 0.66584(7) 0.33903(5) 0.0256 1.0000 Uani Cl1 cl 0.35291(14) 0.71789(9) 0.58870(12) 0.0446 1.0000 Uani Cl2 cl 0.95225(13) 0.88683(9) 0.04728(11) 0.0422 1.0000 Uani O1 o 0.4464(5) 0.7093(2) 0.4742(4) 0.0541 1.0000 Uani O2 o 0.3371(5) 0.6327(3) 0.6567(5) 0.0664 1.0000 Uani O3 o 0.1948(6) 0.7629(4) 0.5181(7) 0.1121 1.0000 Uani O4 o 0.4635(7) 0.7752(3) 0.7166(5) 0.0826 1.0000 Uani O5 o 0.7875(6) 0.8429(4) -0.0048(6) 0.1027 1.0000 Uani O6 o 1.0374(7) 0.8746(5) -0.0697(5) 0.1116 1.0000 Uani O7 o 0.9207(9) 0.9802(3) 0.0578(8) 0.1250 1.0000 Uani O8 o 1.0561(6) 0.8548(4) 0.1980(5) 0.0879 1.0000 Uani N1 n 0.4761(5) 0.5928(2) 0.1915(4) 0.0399 1.0000 Uani N4 n 0.5682(5) 0.7696(2) 0.1953(4) 0.0388 1.0000 Uani N8 n 0.8245(5) 0.7333(3) 0.5139(4) 0.0488 1.0000 Uani N11 n 0.7306(4) 0.5597(3) 0.4717(4) 0.0425 1.0000 Uani C2 c 0.3293(5) 0.6565(4) 0.1227(5) 0.0486 1.0000 Uani C3 c 0.3993(6) 0.7418(3) 0.0699(5) 0.0512 1.0000 Uani C5 c 0.5536(6) 0.8579(3) 0.2726(6) 0.0499 1.0000 Uani C6 c 0.7257(7) 0.8843(3) 0.3913(6) 0.0578 1.0000 Uani C7 c 0.7811(6) 0.8295(3) 0.5410(6) 0.0520 1.0000 Uani C9 c 0.8558(8) 0.6804(4) 0.6662(6) 0.0763 1.0000 Uani C10 c 0.7615(9) 0.5899(4) 0.6382(6) 0.0717 1.0000 Uani C13 c 0.9275(8) 0.5504(5) 0.3114(7) 0.0760 1.0000 Uani C14 c 0.8174(6) 0.6289(3) 0.2206(5) 0.0439 1.0000 Uani C15 c 0.6976(7) 0.6031(3) 0.0534(5) 0.0519 1.0000 Uani C16 c 0.5411(7) 0.5515(3) 0.0648(6) 0.0561 1.0000 Uani C17 c 0.4309(7) 0.5214(3) 0.2976(6) 0.0564 1.0000 Uani C18 c 0.5891(11) 0.4918(4) 0.4250(9) 0.0994 1.0000 Uani C120 c 0.8490(14) 0.5012(6) 0.4134(13) 0.0479(15) 0.42(1) Uiso C121 c 0.9088(9) 0.5317(6) 0.4713(9) 0.0479(15) 0.58(1) Uiso H4 h 0.653(7) 0.781(3) 0.146(6) 0.0489 1.0000 Uiso H8 h 0.943(7) 0.737(4) 0.505(6) 0.0570 1.0000 Uiso H21 h 0.2733(5) 0.6720(4) 0.2057(5) 0.0559 1.0000 Uiso H22 h 0.2416(5) 0.6274(4) 0.0286(5) 0.0559 1.0000 Uiso H31 h 0.3124(6) 0.7920(3) 0.0556(5) 0.0572 1.0000 Uiso H32 h 0.4210(6) 0.7301(3) -0.0342(5) 0.0572 1.0000 Uiso H51 h 0.5161(6) 0.9062(3) 0.1885(6) 0.0635 1.0000 Uiso H52 h 0.4652(6) 0.8521(3) 0.3296(6) 0.0635 1.0000 Uiso H61 h 0.7180(7) 0.9495(3) 0.4215(6) 0.0744 1.0000 Uiso H62 h 0.8167(7) 0.8779(3) 0.3373(6) 0.0744 1.0000 Uiso H71 h 0.8863(6) 0.8587(3) 0.6175(6) 0.0637 1.0000 Uiso H72 h 0.6846(6) 0.8293(3) 0.5890(6) 0.0637 1.0000 Uiso H91 h 0.8141(8) 0.7172(4) 0.7426(6) 0.0812 1.0000 Uiso H92 h 0.9834(8) 0.6690(4) 0.7140(6) 0.0812 1.0000 Uiso H101 h 0.8338(9) 0.5435(4) 0.7133(6) 0.0842 1.0000 Uiso H102 h 0.6475(9) 0.5967(4) 0.6584(6) 0.0842 1.0000 Uiso H1201 h 0.9434(14) 0.4773(6) 0.5082(13) 0.0575 0.4214 Uiso H1202 h 0.7805(14) 0.4491(6) 0.3513(13) 0.0575 0.4214 Uiso H1211 h 0.9985(9) 0.5670(6) 0.5549(9) 0.0575 0.5786 Uiso H1212 h 0.9254(9) 0.4651(6) 0.4952(9) 0.0575 0.5786 Uiso H1301 h 1.0416(8) 0.5753(5) 0.3798(7) 0.0954 0.4214 Uiso H1302 h 0.9473(8) 0.5067(5) 0.2317(7) 0.0954 0.4214 Uiso H1311 h 1.0523(8) 0.5648(5) 0.3270(7) 0.0954 0.5786 Uiso H1312 h 0.8936(8) 0.4941(5) 0.2447(7) 0.0954 0.5786 Uiso H141 h 0.9010(6) 0.6769(3) 0.2108(5) 0.0566 1.0000 Uiso H151 h 0.6580(7) 0.6598(3) -0.0107(5) 0.0657 1.0000 Uiso H152 h 0.7632(7) 0.5640(3) -0.0008(5) 0.0657 1.0000 Uiso H161 h 0.4469(7) 0.5541(3) -0.0409(6) 0.0664 1.0000 Uiso H162 h 0.5741(7) 0.4865(3) 0.0930(6) 0.0664 1.0000 Uiso H171 h 0.3470(7) 0.5481(3) 0.3477(6) 0.0697 1.0000 Uiso H172 h 0.3766(7) 0.4676(3) 0.2307(6) 0.0697 1.0000 Uiso H181 h 0.5558(11) 0.4766(4) 0.5222(9) 0.1103 1.0000 Uiso H182 h 0.6346(11) 0.4360(4) 0.3866(9) 0.1103 1.0000 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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.02734(18) 0.02425(17) 0.02576(18) -0.0006(2) 0.00935(14) -0.0005(2) Cl1 0.0441(5) 0.0508(6) 0.0406(5) 0.0119(4) 0.0159(4) 0.0054(4) Cl2 0.0415(5) 0.0436(5) 0.0396(5) 0.0054(4) 0.0099(4) 0.0003(4) O1 0.0603(18) 0.0638(19) 0.0444(15) 0.0019(14) 0.0253(14) -0.0049(15) O2 0.081(2) 0.0537(18) 0.075(2) 0.0201(17) 0.039(2) -0.0022(18) O3 0.062(3) 0.131(4) 0.152(5) 0.073(4) 0.045(3) 0.035(3) O4 0.110(4) 0.081(3) 0.066(2) -0.019(2) 0.041(3) -0.032(3) O5 0.082(3) 0.133(4) 0.087(3) 0.019(3) 0.018(2) -0.056(3) O6 0.090(3) 0.188(7) 0.065(3) 0.004(4) 0.036(2) 0.004(4) O7 0.119(4) 0.059(3) 0.145(5) -0.021(3) -0.034(4) 0.025(3) O8 0.089(3) 0.117(4) 0.050(2) 0.028(2) 0.011(2) 0.036(3) N1 0.0418(18) 0.0397(17) 0.0347(16) -0.0053(13) 0.0068(14) -0.0033(14) N4 0.049(2) 0.0283(15) 0.0444(18) 0.0076(13) 0.0229(16) 0.0082(14) N8 0.0365(17) 0.054(2) 0.052(2) -0.0161(17) 0.0085(16) -0.0113(16) N11 0.0420(18) 0.0469(19) 0.0401(18) 0.0090(15) 0.0149(15) 0.0058(16) C2 0.0360(16) 0.063(3) 0.0407(18) -0.008(2) 0.0038(15) 0.003(2) C3 0.047(2) 0.057(3) 0.039(2) 0.0040(18) -0.0015(18) 0.015(2) C5 0.068(3) 0.0299(18) 0.061(3) 0.0046(17) 0.033(2) 0.0103(18) C6 0.078(3) 0.041(2) 0.067(3) -0.016(2) 0.041(3) -0.020(2) C7 0.052(2) 0.053(2) 0.054(2) -0.029(2) 0.022(2) -0.018(2) C9 0.079(3) 0.072(4) 0.052(2) -0.001(3) -0.016(2) 0.002(3) C10 0.094(4) 0.074(4) 0.043(3) 0.014(2) 0.015(3) 0.020(3) C13 0.064(3) 0.107(4) 0.068(3) 0.022(3) 0.036(3) 0.048(3) C14 0.047(2) 0.050(2) 0.045(2) 0.0013(18) 0.0282(18) 0.0083(18) C15 0.067(3) 0.055(2) 0.042(2) -0.0049(18) 0.030(2) 0.010(2) C16 0.075(3) 0.049(2) 0.041(2) -0.0187(19) 0.015(2) 0.000(2) C17 0.067(3) 0.047(2) 0.060(3) -0.008(2) 0.027(2) -0.028(2) C18 0.118(6) 0.066(4) 0.091(5) 0.044(3) 0.001(4) -0.037(4) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Co1 . O1 . 2.452(4) yes Co1 . N1 . 1.943(3) yes Co1 . N4 . 1.964(3) yes Co1 . N8 . 1.968(3) yes Co1 . N11 . 1.926(3) yes Co1 . C14 . 1.984(4) yes Cl1 . O1 . 1.445(3) yes Cl1 . O2 . 1.409(3) yes Cl1 . O3 . 1.401(4) yes Cl1 . O4 . 1.463(4) yes Cl2 . O5 . 1.422(4) yes Cl2 . O6 . 1.420(5) yes Cl2 . O7 . 1.402(5) yes Cl2 . O8 . 1.407(4) yes N1 . C2 . 1.484(6) yes N1 . C16 . 1.503(6) yes N1 . C17 . 1.524(6) yes N4 . C3 . 1.518(6) yes N4 . C5 . 1.486(5) yes N4 . H4 . 0.93(5) no N8 . C7 . 1.494(6) yes N8 . C9 . 1.499(7) yes N8 . H8 . 0.99(6) no N11 . C10 . 1.474(6) yes N11 . C18 . 1.476(7) yes N11 . C120 . 1.494(7) yes N11 . C121 . 1.503(6) yes C2 . C3 . 1.509(7) yes C2 . H21 . 1.000 no C2 . H22 . 1.000 no C3 . H31 . 1.000 no C3 . H32 . 1.000 no C5 . C6 . 1.505(7) yes C5 . H51 . 1.000 no C5 . H52 . 1.000 no C6 . C7 . 1.486(7) yes C6 . H61 . 1.000 no C6 . H62 . 1.000 no C7 . H71 . 1.000 no C7 . H72 . 1.000 no C9 . C10 . 1.514(9) yes C9 . H91 . 1.000 no C9 . H92 . 1.000 no C10 . H101 . 1.000 no C10 . H102 . 1.000 no C13 . C14 . 1.521(7) yes C13 . C120 . 1.447(8) yes C13 . C121 . 1.487(7) yes C13 . H1301 . 1.000 no C13 . H1302 . 1.000 no C13 . H1311 . 1.000 no C13 . H1312 . 1.000 no C14 . C15 . 1.532(6) yes C14 . H141 . 1.000 no C15 . C16 . 1.509(7) yes C15 . H151 . 1.000 no C15 . H152 . 1.000 no C16 . H161 . 1.000 no C16 . H162 . 1.000 no C17 . C18 . 1.477(9) yes C17 . H171 . 1.000 no C17 . H172 . 1.000 no C18 . H181 . 1.000 no C18 . H182 . 1.000 no C120 . H1201 . 1.000 no C120 . H1202 . 1.000 no C121 . H1211 . 1.000 no C121 . H1212 . 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 . Co1 . N1 . 88.5(1) yes O1 . Co1 . N4 . 86.7(1) yes O1 . Co1 . N8 . 84.6(1) yes O1 . Co1 . N11 . 92.7(1) yes O1 . Co1 . C14 . 177.3(1) yes N1 . Co1 . N4 . 87.32(16) yes N1 . Co1 . N8 . 171.19(17) yes N4 . Co1 . N8 . 97.72(16) yes N1 . Co1 . N11 . 89.01(15) yes N4 . Co1 . N11 . 176.29(17) yes N8 . Co1 . N11 . 85.86(18) yes N1 . Co1 . C14 . 88.87(18) yes N4 . Co1 . C14 . 92.34(16) yes N8 . Co1 . C14 . 98.11(18) yes N11 . Co1 . C14 . 88.10(16) yes O1 . Cl1 . O2 . 110.9(2) yes O1 . Cl1 . O3 . 109.9(3) yes O2 . Cl1 . O3 . 114.4(3) yes O1 . Cl1 . O4 . 104.9(2) yes O2 . Cl1 . O4 . 107.5(3) yes O3 . Cl1 . O4 . 108.8(4) yes O5 . Cl2 . O6 . 109.4(3) yes O5 . Cl2 . O7 . 107.0(4) yes O6 . Cl2 . O7 . 108.1(5) yes O5 . Cl2 . O8 . 111.9(3) yes O6 . Cl2 . O8 . 110.9(3) yes O7 . Cl2 . O8 . 109.4(3) yes Co1 . O1 . Cl1 . 163.6(2) yes Co1 . N1 . C2 . 105.3(3) yes Co1 . N1 . C16 . 110.6(3) yes C2 . N1 . C16 . 112.1(3) yes Co1 . N1 . C17 . 104.3(3) yes C2 . N1 . C17 . 111.4(4) yes C16 . N1 . C17 . 112.6(4) yes Co1 . N4 . C3 . 108.8(3) yes Co1 . N4 . C5 . 116.6(3) yes C3 . N4 . C5 . 112.5(3) yes Co1 . N4 . H4 . 105.3(31) no C3 . N4 . H4 . 109.6(30) no C5 . N4 . H4 . 103.6(31) no Co1 . N8 . C7 . 117.5(3) yes Co1 . N8 . C9 . 108.5(3) yes C7 . N8 . C9 . 109.2(4) yes Co1 . N8 . H8 . 114.5(29) no C7 . N8 . H8 . 103.8(31) no C9 . N8 . H8 . 102.1(30) no Co1 . N11 . C10 . 106.3(3) yes Co1 . N11 . C18 . 108.2(3) yes C10 . N11 . C18 . 110.7(5) yes Co1 . N11 . C120 . 111.6(4) yes C10 . N11 . C120 . 126.0(6) yes C18 . N11 . C120 . 92.5(6) yes Co1 . N11 . C121 . 109.6(3) yes C10 . N11 . C121 . 102.9(5) yes C18 . N11 . C121 . 118.6(6) yes N1 . C2 . C3 . 108.5(3) yes N1 . C2 . H21 . 109.7 no C3 . C2 . H21 . 109.7 no N1 . C2 . H22 . 109.7 no C3 . C2 . H22 . 109.7 no H21 . C2 . H22 . 109.467 no N4 . C3 . C2 . 109.9(3) yes N4 . C3 . H31 . 109.4 no C2 . C3 . H31 . 109.4 no N4 . C3 . H32 . 109.4 no C2 . C3 . H32 . 109.4 no H31 . C3 . H32 . 109.467 no N4 . C5 . C6 . 110.6(4) yes N4 . C5 . H51 . 109.2 no C6 . C5 . H51 . 109.2 no N4 . C5 . H52 . 109.2 no C6 . C5 . H52 . 109.2 no H51 . C5 . H52 . 109.467 no C5 . C6 . C7 . 115.4(4) yes C5 . C6 . H61 . 108.0 no C7 . C6 . H61 . 108.0 no C5 . C6 . H62 . 108.0 no C7 . C6 . H62 . 108.0 no H61 . C6 . H62 . 109.467 no N8 . C7 . C6 . 113.0(4) yes N8 . C7 . H71 . 108.6 no C6 . C7 . H71 . 108.6 no N8 . C7 . H72 . 108.6 no C6 . C7 . H72 . 108.6 no H71 . C7 . H72 . 109.467 no N8 . C9 . C10 . 112.0(4) yes N8 . C9 . H91 . 108.8 no C10 . C9 . H91 . 108.8 no N8 . C9 . H92 . 108.8 no C10 . C9 . H92 . 108.8 no H91 . C9 . H92 . 109.467 no N11 . C10 . C9 . 110.2(5) yes N11 . C10 . H101 . 109.3 no C9 . C10 . H101 . 109.3 no N11 . C10 . H102 . 109.3 no C9 . C10 . H102 . 109.3 no H101 . C10 . H102 . 109.467 no C14 . C13 . C120 . 113.8(5) yes C14 . C13 . C121 . 114.7(4) yes C14 . C13 . H1301 . 108.4 no C120 . C13 . H1301 . 108.4 no C14 . C13 . H1302 . 108.4 no C120 . C13 . H1302 . 108.4 no H1301 . C13 . H1302 . 109.467 no C14 . C13 . H1311 . 108.1 no C121 . C13 . H1311 . 108.1 no C14 . C13 . H1312 . 108.1 no C121 . C13 . H1312 . 108.1 no H1311 . C13 . H1312 . 109.467 no Co1 . C14 . C13 . 107.8(3) yes Co1 . C14 . C15 . 104.4(3) yes C13 . C14 . C15 . 113.9(4) yes Co1 . C14 . H141 . 115.38 no C13 . C14 . H141 . 106.2 no C15 . C14 . H141 . 109.4 no C14 . C15 . C16 . 110.6(4) yes C14 . C15 . H151 . 109.2 no C16 . C15 . H151 . 109.2 no C14 . C15 . H152 . 109.2 no C16 . C15 . H152 . 109.2 no H151 . C15 . H152 . 109.466 no N1 . C16 . C15 . 110.2(3) yes N1 . C16 . H161 . 109.3 no C15 . C16 . H161 . 109.3 no N1 . C16 . H162 . 109.3 no C15 . C16 . H162 . 109.3 no H161 . C16 . H162 . 109.467 no N1 . C17 . C18 . 110.4(4) yes N1 . C17 . H171 . 109.3 no C18 . C17 . H171 . 109.3 no N1 . C17 . H172 . 109.3 no C18 . C17 . H172 . 109.3 no H171 . C17 . H172 . 109.466 no N11 . C18 . C17 . 115.1(4) yes N11 . C18 . H181 . 108.0 no C17 . C18 . H181 . 108.0 no N11 . C18 . H182 . 108.0 no C17 . C18 . H182 . 108.0 no H181 . C18 . H182 . 109.467 no N11 . C120 . C13 . 112.5(6) yes N11 . C120 . H1201 . 108.7 no C13 . C120 . H1201 . 108.7 no N11 . C120 . H1202 . 108.7 no C13 . C120 . H1202 . 108.7 no H1201 . C120 . H1202 . 109.467 no N11 . C121 . C13 . 109.7(5) yes N11 . C121 . H1211 . 109.4 no C13 . C121 . H1211 . 109.4 no N11 . C121 . H1212 . 109.4 no C13 . C121 . H1212 . 109.4 no H1211 . C121 . H1212 . 109.467 no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O3 O8 3.001(7) . 1_455 no O3 N8 3.023(7) . 1_455 no O3 C7 3.561(7) . 1_455 no O3 C120 3.59(1) . 2_656 no O4 O5 3.134(6) . 1_556 no O4 C3 3.345(7) . 1_556 no O4 C18 3.392(7) . 2_656 no O5 N4 3.066(7) . . no O5 C5 3.539(8) . . no O6 C3 3.412(7) . 1_655 no O6 C13 3.41(1) . 2_755 no O6 C7 3.461(6) . 1_554 no O7 C2 3.361(7) . 2_655 no O7 C10 3.468(8) . 2_756 no O7 C17 3.554(7) . 2_655 no C6 C121 3.559(9) . 2_756 no #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Co1 O1 Cl1 O2 . . . . -41.7(8) no Co1 O1 Cl1 O3 . . . . -169.2(7) no Co1 O1 Cl1 O4 . . . . 74.0(7) no Co1 N1 C2 C3 . . . . 47.9(4) no Co1 N1 C16 C15 . . . . -19.8(4) no Co1 N1 C17 C18 . . . . -37.5(5) no Co1 N4 C3 C2 . . . . 16.2(5) no Co1 N4 C5 C6 . . . . 55.5(5) no Co1 N8 C7 C6 . . . . -48.5(5) no Co1 N8 C9 C10 . . . . 4.1(6) no Co1 N11 C10 C9 . . . . -42.5(5) no Co1 N11 C18 C17 . . . . -1.7(8) no Co1 N11 C120 C13 . . . . 20.1(7) no Co1 N11 C120 C121 . . . . 91(1) no Co1 N11 C121 C13 . . . . -34.6(7) no Co1 N11 C121 C120 . . . . -99(1) no Co1 C14 C13 C120 . . . . 22.8(6) no Co1 C14 C13 C121 . . . . -9.0(6) no Co1 C14 C15 C16 . . . . -40.3(4) no Cl1 O1 Co1 N1 . . . . 108.0(7) no Cl1 O1 Co1 N4 . . . . -164.6(7) no Cl1 O1 Co1 N8 . . . . -66.5(7) no Cl1 O1 Co1 N11 . . . . 19.1(7) no Cl1 O1 Co1 C14 . . . . 127(3) no O1 Co1 N1 C2 . . . . 55.2(3) no O1 Co1 N1 C16 . . . . 176.4(3) no O1 Co1 N1 C17 . . . . -62.3(3) no O1 Co1 N4 C3 . . . . -79.9(3) no O1 Co1 N4 C5 . . . . 48.5(3) no O1 Co1 N8 C7 . . . . -54.3(4) no O1 Co1 N8 C9 . . . . 70.1(4) no O1 Co1 N11 C10 . . . . -47.5(3) no O1 Co1 N11 C18 . . . . 71.4(4) no O1 Co1 N11 C120 . . . . 171.7(4) no O1 Co1 N11 C121 . . . . -158.0(4) no O1 Co1 C14 C13 . . . . -116(3) no O1 Co1 C14 C15 . . . . 5(3) no N1 Co1 N4 C3 . . . . 8.7(3) no N1 Co1 N4 C5 . . . . 137.2(4) no N1 Co1 N8 C7 . . . . -93(1) no N1 Co1 N8 C9 . . . . 31(1) no N1 Co1 N11 C10 . . . . -136.0(4) no N1 Co1 N11 C18 . . . . -17.1(4) no N1 Co1 N11 C120 . . . . 83.2(4) no N1 Co1 N11 C121 . . . . 113.5(4) no N1 Co1 C14 C13 . . . . -98.0(3) no N1 Co1 C14 C15 . . . . 23.5(3) no N1 C2 C3 N4 . . . . -42.4(5) no N1 C16 C15 C14 . . . . 40.4(5) no N1 C17 C18 N11 . . . . 26.8(8) no N4 Co1 N1 C2 . . . . -31.5(3) no N4 Co1 N1 C16 . . . . 89.7(3) no N4 Co1 N1 C17 . . . . -149.0(3) no N4 Co1 N8 C7 . . . . 31.5(4) no N4 Co1 N8 C9 . . . . 156.0(4) no N4 Co1 N11 C10 . . . . -128(3) no N4 Co1 N11 C18 . . . . -9(3) no N4 Co1 N11 C120 . . . . 91(3) no N4 Co1 N11 C121 . . . . 122(3) no N4 Co1 C14 C13 . . . . 174.8(3) no N4 Co1 C14 C15 . . . . -63.7(3) no N4 C5 C6 C7 . . . . -71.9(6) no N8 Co1 N1 C2 . . . . 94(1) no N8 Co1 N1 C16 . . . . -145(1) no N8 Co1 N1 C17 . . . . -24(1) no N8 Co1 N4 C3 . . . . -164.0(3) no N8 Co1 N4 C5 . . . . -35.5(4) no N8 Co1 N11 C10 . . . . 36.9(4) no N8 Co1 N11 C18 . . . . 155.7(4) no N8 Co1 N11 C120 . . . . -103.9(4) no N8 Co1 N11 C121 . . . . -73.7(4) no N8 Co1 C14 C13 . . . . 76.6(3) no N8 Co1 C14 C15 . . . . -161.9(3) no N8 C7 C6 C5 . . . . 68.2(6) no N8 C9 C10 N11 . . . . 25.0(7) no N11 Co1 N1 C2 . . . . 147.9(3) no N11 Co1 N1 C16 . . . . -90.9(3) no N11 Co1 N1 C17 . . . . 30.5(3) no N11 Co1 N4 C3 . . . . 1(3) no N11 Co1 N4 C5 . . . . 129(3) no N11 Co1 N8 C7 . . . . -147.5(4) no N11 Co1 N8 C9 . . . . -23.0(4) no N11 Co1 C14 C13 . . . . -8.9(3) no N11 Co1 C14 C15 . . . . 112.6(3) no N11 C120 C13 C14 . . . . -28.4(8) no N11 C121 C13 C14 . . . . 28.4(8) no N11 C121 C13 C120 . . . . -67(1) no C2 N1 Co1 C14 . . . . -124.0(3) no C2 N1 C16 C15 . . . . 97.2(4) no C2 N1 C17 C18 . . . . -150.6(5) no C2 C3 N4 C5 . . . . -114.6(4) no C3 N4 Co1 C14 . . . . 97.5(3) no C3 N4 C5 C6 . . . . -177.9(4) no C3 C2 N1 C16 . . . . -72.3(4) no C3 C2 N1 C17 . . . . 160.4(3) no C5 N4 Co1 C14 . . . . -134.0(3) no C6 C7 N8 C9 . . . . -172.6(4) no C7 N8 Co1 C14 . . . . 125.1(4) no C7 N8 C9 C10 . . . . 133.3(5) no C9 N8 Co1 C14 . . . . -110.5(4) no C9 C10 N11 C18 . . . . -159.8(5) no C9 C10 N11 C120 . . . . 90.9(7) no C9 C10 N11 C121 . . . . 72.7(6) no C10 N11 Co1 C14 . . . . 135.1(4) no C10 N11 C18 C17 . . . . 114.4(6) no C10 N11 C120 C13 . . . . -111.3(7) no C10 N11 C121 C13 . . . . -147.4(6) no C13 C14 C15 C16 . . . . 77.1(6) no C13 C120 N11 C18 . . . . 130.8(7) no C13 C121 N11 C18 . . . . 90.2(7) no C14 Co1 N1 C16 . . . . -2.7(3) no C14 Co1 N1 C17 . . . . 118.6(3) no C14 Co1 N11 C18 . . . . -106.0(4) no C14 Co1 N11 C120 . . . . -5.6(4) no C14 Co1 N11 C121 . . . . 24.6(4) no C15 C14 C13 C120 . . . . -92.6(7) no C15 C14 C13 C121 . . . . -124.4(6) no C15 C16 N1 C17 . . . . -136.1(4) no C16 N1 C17 C18 . . . . 82.4(5) no C17 C18 N11 C120 . . . . -115.4(7) no C17 C18 N11 C121 . . . . -127.2(6) no #------------------------------------------------------------------------------ #===END