# Copyright The Royal Society of Chemistry, 1998 # CCDC Number: 182/1072 data_dmt15 _audit_creation_method SHELXL-97 _chemical_name_systematic ; (1-carboxymethyl-4-methylene-1,4,8,11-tetraazacyclotetradecane) -cobalt (III) percholorate ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H59 B Co N4 O2' _chemical_formula_weight 805.74 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 Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.8555(5) _cell_length_b 17.4488(6) _cell_length_c 17.2455(6) _cell_angle_alpha 90.00 _cell_angle_beta 110.2770(10) _cell_angle_gamma 90.00 _cell_volume 4193.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 9620 _cell_measurement_theta_min 1.33 _cell_measurement_theta_max 28.32 _exptl_crystal_description Prism _exptl_crystal_colour Orange _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.276 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1716 _exptl_absorpt_coefficient_mu 0.454 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8048 _exptl_absorpt_correction_T_max 0.8834 _exptl_absorpt_process_details '(Blessing, 1995)' _exptl_special_details ; The hydrogens on carbon atoms C13, C72, and C76 were located in difference maps and allowed to refine with a thermal parameter 20% greater than the carbon atom to which they are attached. The remaining hydrogen atoms were placed in calculated positions and refined with a riding model with U~iso~ constrained to be 1.2 (1.5 for methyl groups) times U~eq~ of the carrier atom. ; _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 'Siemens SMART CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 'none' _diffrn_reflns_number 25441 _diffrn_reflns_av_R_equivalents 0.0285 _diffrn_reflns_av_sigmaI/netI 0.0337 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 26.00 _reflns_number_total 8199 _reflns_number_gt 6384 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART (Siemens, 1994a)' _computing_cell_refinement 'Siemens SMART (Siemens, 1994a)' _computing_data_reduction 'Siemens SHELXTL (Siemens, 1994b)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL (Siemens, 1994b)' _computing_publication_material 'Siemens SHELXTL (Siemens, 1994b)' _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 'w=1/[\s^2^(Fo^2^)+(0.0746P)^2^+2.9123P] 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 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8199 _refine_ls_number_parameters 529 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0680 _refine_ls_R_factor_gt 0.0504 _refine_ls_wR_factor_ref 0.1492 _refine_ls_wR_factor_gt 0.1356 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _refine_ls_shift/su_max 0.021 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co Co 0.04577(2) 0.499572(19) 0.80751(2) 0.03162(12) Uani 1 d . . . O1 O -0.02305(13) 0.54041(10) 0.87949(11) 0.0375(4) Uani 1 d . . . O2 O 0.00352(18) 0.60586(14) 0.99671(13) 0.0572(6) Uani 1 d . . . N1 N 0.05178(18) 0.58993(13) 0.74594(15) 0.0422(5) Uani 1 d . . . N2 N 0.16572(17) 0.53466(15) 0.89526(16) 0.0458(6) Uani 1 d . . . N3 N 0.05479(17) 0.39582(13) 0.85717(14) 0.0391(5) Uani 1 d . . . N4 N -0.07472(16) 0.46238(13) 0.72640(14) 0.0373(5) Uani 1 d . . . C1 C 0.1188(3) 0.64568(18) 0.8023(2) 0.0567(8) Uani 1 d . . . H1A H 0.0854 0.6748 0.8326 0.068 Uiso 1 calc R . . H1B H 0.1423 0.6818 0.7701 0.068 Uiso 1 calc R . . C2 C 0.2010(2) 0.6032(2) 0.8614(2) 0.0607(9) Uani 1 d . . . H2A H 0.2367 0.6372 0.9069 0.073 Uiso 1 calc R . . H2B H 0.2447 0.5865 0.8332 0.073 Uiso 1 calc R . . C3 C 0.2468(2) 0.4783(2) 0.9215(2) 0.0599(9) Uani 1 d . . . H3A H 0.2993 0.5005 0.9676 0.072 Uiso 1 calc R . . H3B H 0.2705 0.4711 0.8756 0.072 Uiso 1 calc R . . C4 C 0.2230(2) 0.4005(2) 0.9479(2) 0.0600(9) Uani 1 d . . . H4A H 0.2004 0.4074 0.9945 0.072 Uiso 1 calc R . . H4B H 0.2818 0.3698 0.9674 0.072 Uiso 1 calc R . . C5 C 0.1477(2) 0.35618(18) 0.8806(2) 0.0516(8) Uani 1 d . . . H5A H 0.1674 0.3513 0.8322 0.062 Uiso 1 calc R . . H5B H 0.1414 0.3045 0.9005 0.062 Uiso 1 calc R . . C6 C -0.0241(2) 0.34772(16) 0.80246(19) 0.0464(7) Uani 1 d . . . H6A H -0.0396 0.3063 0.8341 0.056 Uiso 1 calc R . . H6B H -0.0055 0.3251 0.7582 0.056 Uiso 1 calc R . . C7 C -0.1083(2) 0.39954(17) 0.76720(18) 0.0439(7) Uani 1 d . . . H7A H -0.1618 0.3720 0.7271 0.053 Uiso 1 calc R . . H7B H -0.1295 0.4197 0.8110 0.053 Uiso 1 calc R . . C8 C -0.1486(2) 0.52214(18) 0.69134(19) 0.0450(7) Uani 1 d . . . H8A H -0.1616 0.5490 0.7363 0.054 Uiso 1 calc R . . H8B H -0.2084 0.4980 0.6562 0.054 Uiso 1 calc R . . C9 C -0.1150(2) 0.57871(18) 0.64114(19) 0.0521(8) Uani 1 d . . . H9A H -0.0939 0.5503 0.6015 0.062 Uiso 1 calc R . . H9B H -0.1696 0.6107 0.6095 0.062 Uiso 1 calc R . . C10 C -0.0351(2) 0.62979(17) 0.6909(2) 0.0509(8) Uani 1 d . . . H10A H -0.0163 0.6625 0.6528 0.061 Uiso 1 calc R . . H10B H -0.0593 0.6634 0.7248 0.061 Uiso 1 calc R . . C13 C 0.0915(3) 0.5256(2) 0.7157(2) 0.0538(8) Uani 1 d . . . H13A H 0.057(3) 0.507(2) 0.661(3) 0.065 Uiso 1 d . . . H13B H 0.158(3) 0.524(2) 0.723(2) 0.065 Uiso 1 d . . . C11 C 0.1375(2) 0.5571(2) 0.96801(19) 0.0555(8) Uani 1 d . . . H11A H 0.1718 0.6041 0.9924 0.067 Uiso 1 calc R . . H11B H 0.1582 0.5167 1.0099 0.067 Uiso 1 calc R . . C12 C 0.0311(2) 0.57030(15) 0.94686(17) 0.0414(6) Uani 1 d . . . B B 0.0402(2) 0.25097(16) 0.56325(17) 0.0297(6) Uani 1 d . . . C21 C 0.06598(18) 0.20045(14) 0.64945(15) 0.0308(5) Uani 1 d . . . C22 C 0.19403(19) 0.26955(16) 0.51719(17) 0.0398(6) Uani 1 d . . . H22A H 0.1721 0.2280 0.4809 0.048 Uiso 1 calc R . . C23 C 0.2807(2) 0.3039(2) 0.5231(2) 0.0540(8) Uani 1 d . . . H23A H 0.3168 0.2843 0.4923 0.065 Uiso 1 calc R . . C24 C 0.3141(2) 0.3661(2) 0.5735(2) 0.0557(9) Uani 1 d . . . H24A H 0.3727 0.3893 0.5775 0.067 Uiso 1 calc R . . C25 C 0.2599(2) 0.39426(17) 0.6187(2) 0.0494(8) Uani 1 d . . . H25A H 0.2811 0.4374 0.6529 0.059 Uiso 1 calc R . . C26 C 0.1744(2) 0.35856(15) 0.61319(18) 0.0399(6) Uani 1 d . . . H26A H 0.1391 0.3783 0.6445 0.048 Uiso 1 calc R . . C31 C 0.13832(18) 0.29428(14) 0.56287(16) 0.0331(5) Uani 1 d . . . C32 C 0.14815(19) 0.21099(15) 0.71895(15) 0.0351(6) Uani 1 d . . . H32A H 0.1910 0.2503 0.7179 0.042 Uiso 1 calc R . . C33 C 0.1699(2) 0.16600(17) 0.79004(17) 0.0450(7) Uani 1 d . . . H33A H 0.2265 0.1751 0.8350 0.054 Uiso 1 calc R . . C34 C 0.1088(2) 0.10845(17) 0.79454(18) 0.0462(7) Uani 1 d . . . H34A H 0.1231 0.0780 0.8422 0.055 Uiso 1 calc R . . C35 C 0.0262(2) 0.09629(16) 0.72767(18) 0.0453(7) Uani 1 d . . . H35A H -0.0166 0.0574 0.7300 0.054 Uiso 1 calc R . . C36 C 0.0054(2) 0.14073(15) 0.65704(17) 0.0379(6) Uani 1 d . . . H36A H -0.0512 0.1307 0.6124 0.045 Uiso 1 calc R . . C41 C -0.04491(18) 0.31406(13) 0.55466(15) 0.0296(5) Uani 1 d . . . C42 C -0.12401(19) 0.29852(15) 0.57870(17) 0.0373(6) Uani 1 d . . . H42A H -0.1227 0.2542 0.6100 0.045 Uiso 1 calc R . . C43 C -0.2038(2) 0.34538(17) 0.55850(18) 0.0433(7) Uani 1 d . . . H43A H -0.2555 0.3321 0.5755 0.052 Uiso 1 calc R . . C44 C -0.2083(2) 0.41199(17) 0.51333(17) 0.0420(6) Uani 1 d . . . H44A H -0.2628 0.4436 0.4988 0.050 Uiso 1 calc R . . C45 C -0.1311(2) 0.43073(15) 0.49033(16) 0.0393(6) Uani 1 d . . . H45A H -0.1322 0.4762 0.4607 0.047 Uiso 1 calc R . . C46 C -0.05166(19) 0.38295(14) 0.51062(16) 0.0349(6) Uani 1 d . . . H46A H 0.0000 0.3973 0.4942 0.042 Uiso 1 calc R . . C51 C -0.00209(17) 0.19293(14) 0.48293(15) 0.0289(5) Uani 1 d . . . C52 C -0.07226(19) 0.21466(15) 0.40862(16) 0.0350(6) Uani 1 d . . . H52A H -0.0971 0.2647 0.4040 0.042 Uiso 1 calc R . . C53 C -0.1072(2) 0.16550(16) 0.34085(17) 0.0421(6) Uani 1 d . . . H53A H -0.1539 0.1829 0.2917 0.051 Uiso 1 calc R . . C54 C -0.0733(2) 0.09139(16) 0.34593(17) 0.0421(6) Uani 1 d . . . H54A H -0.0968 0.0578 0.3008 0.051 Uiso 1 calc R . . C55 C -0.0041(2) 0.06758(15) 0.41843(17) 0.0398(6) Uani 1 d . . . H55A H 0.0196 0.0172 0.4230 0.048 Uiso 1 calc R . . C56 C 0.03058(19) 0.11743(15) 0.48452(16) 0.0353(6) Uani 1 d . . . H56A H 0.0784 0.0998 0.5328 0.042 Uiso 1 calc R . . C60 C -0.2618(3) 0.6092(3) 0.8258(3) 0.0755(11) Uani 1 d . . . H60A H -0.3033 0.5799 0.7793 0.113 Uiso 1 calc R . . H60B H -0.2971 0.6240 0.8613 0.113 Uiso 1 calc R . . H60C H -0.2071 0.5780 0.8569 0.113 Uiso 1 calc R . . C61 C -0.2270(2) 0.6805(2) 0.7943(2) 0.0560(8) Uani 1 d . . . C62 C -0.1442(3) 0.7165(2) 0.8429(2) 0.0630(9) Uani 1 d . . . H62A H -0.1096 0.6965 0.8954 0.076 Uiso 1 calc R . . C63 C -0.1112(3) 0.7816(2) 0.8158(3) 0.0709(11) Uani 1 d . . . H63A H -0.0543 0.8051 0.8500 0.085 Uiso 1 calc R . . C64 C -0.1616(3) 0.8129(2) 0.7378(3) 0.0717(11) Uani 1 d . . . C65 C -0.2427(3) 0.7756(2) 0.6903(2) 0.0691(10) Uani 1 d . . . H65A H -0.2777 0.7946 0.6374 0.083 Uiso 1 calc R . . C66 C -0.2744(3) 0.7105(2) 0.7183(2) 0.0655(10) Uani 1 d . . . H66A H -0.3304 0.6862 0.6837 0.079 Uiso 1 calc R . . C67 C -0.1307(5) 0.8858(3) 0.7083(4) 0.117(2) Uani 1 d . . . H67A H -0.1867 0.9165 0.6794 0.176 Uiso 1 calc R . . H67B H -0.0964 0.8738 0.6711 0.176 Uiso 1 calc R . . H67C H -0.0889 0.9143 0.7553 0.176 Uiso 1 calc R . . C70 C -0.0201(3) 0.8404(2) 1.0416(2) 0.0637(9) Uani 1 d . . . H70A H -0.0174 0.8370 1.0985 0.096 Uiso 1 calc R . . H70B H 0.0317 0.8104 1.0348 0.096 Uiso 1 calc R . . H70C H -0.0811 0.8206 1.0052 0.096 Uiso 1 calc R . . C71 C -0.0099(2) 0.9229(2) 1.0203(2) 0.0505(7) Uani 1 d . . . C72 C -0.0657(3) 0.9536(2) 0.9449(2) 0.0571(8) Uani 1 d . . . H72 H -0.102(3) 0.924(2) 0.896(2) 0.069 Uiso 1 d . . . C76 C 0.0556(3) 0.9706(2) 1.0748(2) 0.0589(9) Uani 1 d . . . H76 H 0.099(3) 0.949(2) 1.129(2) 0.071 Uiso 1 d . . . 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 Co 0.0365(2) 0.02894(19) 0.0343(2) -0.00670(14) 0.01846(15) -0.00423(14) O1 0.0441(11) 0.0365(10) 0.0369(10) -0.0030(8) 0.0203(9) 0.0024(8) O2 0.0873(17) 0.0526(13) 0.0407(11) -0.0022(10) 0.0335(12) 0.0195(12) N1 0.0527(14) 0.0341(12) 0.0482(14) -0.0055(10) 0.0282(12) -0.0063(10) N2 0.0391(13) 0.0450(14) 0.0527(15) -0.0126(12) 0.0153(11) -0.0040(11) N3 0.0467(13) 0.0310(11) 0.0401(12) -0.0024(10) 0.0158(11) 0.0015(10) N4 0.0401(12) 0.0347(12) 0.0385(12) -0.0029(10) 0.0152(10) -0.0042(10) C1 0.063(2) 0.0397(17) 0.073(2) -0.0108(16) 0.0311(18) -0.0156(15) C2 0.0499(19) 0.0538(19) 0.078(2) -0.0181(18) 0.0213(18) -0.0223(16) C3 0.0378(17) 0.065(2) 0.072(2) -0.0120(18) 0.0118(16) 0.0012(15) C4 0.0526(19) 0.060(2) 0.059(2) -0.0028(17) 0.0092(16) 0.0177(16) C5 0.0573(19) 0.0423(16) 0.0570(19) -0.0018(14) 0.0220(16) 0.0122(14) C6 0.0596(19) 0.0329(15) 0.0488(17) -0.0012(12) 0.0212(15) -0.0081(13) C7 0.0449(16) 0.0431(16) 0.0436(16) -0.0031(13) 0.0152(13) -0.0121(13) C8 0.0443(16) 0.0441(16) 0.0423(16) -0.0032(13) 0.0095(13) 0.0028(13) C9 0.064(2) 0.0459(17) 0.0439(17) 0.0030(14) 0.0160(15) 0.0109(15) C10 0.073(2) 0.0339(15) 0.0515(18) 0.0064(13) 0.0285(17) 0.0063(14) C13 0.059(2) 0.0534(19) 0.058(2) -0.0110(16) 0.0325(18) -0.0033(16) C11 0.061(2) 0.0556(19) 0.0434(17) -0.0181(15) 0.0093(15) 0.0033(15) C12 0.0618(18) 0.0316(14) 0.0351(14) 0.0020(11) 0.0223(13) 0.0065(13) B 0.0313(14) 0.0252(13) 0.0312(14) 0.0014(11) 0.0089(11) -0.0002(11) C21 0.0354(13) 0.0248(12) 0.0326(13) -0.0003(10) 0.0124(11) 0.0039(10) C22 0.0370(14) 0.0412(15) 0.0402(15) 0.0060(12) 0.0118(12) 0.0010(12) C23 0.0393(16) 0.068(2) 0.0571(19) 0.0116(17) 0.0199(15) 0.0012(15) C24 0.0329(15) 0.063(2) 0.063(2) 0.0207(17) 0.0061(15) -0.0113(14) C25 0.0425(16) 0.0372(15) 0.0525(18) 0.0103(13) -0.0037(14) -0.0096(13) C26 0.0384(15) 0.0318(14) 0.0437(15) 0.0029(12) 0.0070(12) 0.0006(11) C31 0.0314(13) 0.0288(13) 0.0347(13) 0.0082(10) 0.0058(10) 0.0027(10) C32 0.0394(14) 0.0325(13) 0.0325(13) -0.0012(11) 0.0114(11) 0.0047(11) C33 0.0500(17) 0.0471(17) 0.0334(14) 0.0010(12) 0.0088(13) 0.0120(14) C34 0.0630(19) 0.0428(16) 0.0341(14) 0.0082(12) 0.0184(14) 0.0124(14) C35 0.0625(19) 0.0326(14) 0.0459(16) 0.0053(12) 0.0253(15) -0.0001(13) C36 0.0444(15) 0.0313(13) 0.0360(14) 0.0022(11) 0.0114(12) -0.0010(11) C41 0.0325(12) 0.0247(12) 0.0300(12) -0.0036(10) 0.0088(10) 0.0000(10) C42 0.0386(14) 0.0329(13) 0.0410(14) -0.0017(11) 0.0145(12) -0.0023(11) C43 0.0348(14) 0.0471(16) 0.0487(16) -0.0056(13) 0.0155(13) -0.0004(12) C44 0.0375(14) 0.0459(16) 0.0367(14) -0.0064(12) 0.0055(12) 0.0122(12) C45 0.0503(16) 0.0300(13) 0.0347(14) 0.0010(11) 0.0110(12) 0.0084(12) C46 0.0389(14) 0.0298(13) 0.0365(13) 0.0016(11) 0.0137(11) 0.0031(11) C51 0.0282(12) 0.0277(12) 0.0315(13) 0.0031(10) 0.0112(10) -0.0006(9) C52 0.0383(14) 0.0284(13) 0.0365(14) 0.0031(11) 0.0108(11) 0.0043(11) C53 0.0427(15) 0.0411(15) 0.0334(14) -0.0009(12) 0.0017(12) 0.0030(12) C54 0.0456(16) 0.0378(15) 0.0388(15) -0.0096(12) 0.0094(12) -0.0023(12) C55 0.0482(16) 0.0280(13) 0.0408(15) -0.0031(11) 0.0124(12) 0.0047(11) C56 0.0376(14) 0.0308(13) 0.0326(13) 0.0011(11) 0.0062(11) 0.0047(11) C60 0.071(3) 0.083(3) 0.085(3) 0.005(2) 0.043(2) 0.005(2) C61 0.0546(19) 0.061(2) 0.058(2) -0.0086(17) 0.0265(16) 0.0098(16) C62 0.064(2) 0.064(2) 0.060(2) -0.0088(18) 0.0202(18) 0.0096(18) C63 0.062(2) 0.066(2) 0.091(3) -0.019(2) 0.035(2) -0.0029(19) C64 0.088(3) 0.052(2) 0.097(3) 0.002(2) 0.059(3) 0.011(2) C65 0.090(3) 0.060(2) 0.060(2) -0.0007(18) 0.029(2) 0.018(2) C66 0.062(2) 0.061(2) 0.068(2) -0.0065(19) 0.0152(18) 0.0168(18) C67 0.140(5) 0.097(4) 0.156(5) 0.014(4) 0.104(5) -0.006(3) C70 0.059(2) 0.060(2) 0.072(2) 0.0062(18) 0.0230(18) 0.0015(17) C71 0.0418(16) 0.0544(19) 0.0605(19) 0.0025(16) 0.0242(15) 0.0022(14) C72 0.0500(19) 0.060(2) 0.058(2) -0.0021(17) 0.0148(16) -0.0053(16) C76 0.052(2) 0.067(2) 0.055(2) 0.0089(18) 0.0150(16) 0.0013(17) _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 Co N1 1.920(2) . ? Co N4 1.961(2) . ? Co C13 1.980(3) . ? Co N3 1.987(2) . ? Co N2 1.993(2) . ? Co O1 1.9933(17) . ? O1 C12 1.273(3) . ? O2 C12 1.239(3) . ? N1 C13 1.446(4) . ? N1 C10 1.484(4) . ? N1 C1 1.487(4) . ? N2 C3 1.499(4) . ? N2 C2 1.503(4) . ? N2 C11 1.506(4) . ? N3 C5 1.469(4) . ? N3 C6 1.484(4) . ? N4 C7 1.480(3) . ? N4 C8 1.483(4) . ? C1 C2 1.489(5) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C3 C4 1.512(5) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C4 C5 1.515(5) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 C7 1.491(4) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C8 C9 1.507(4) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C9 C10 1.495(5) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C13 H13A 0.96(4) . ? C13 H13B 0.95(4) . ? C11 C12 1.513(5) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? B C31 1.644(4) . ? B C41 1.644(4) . ? B C51 1.654(4) . ? B C21 1.655(4) . ? C21 C32 1.395(4) . ? C21 C36 1.412(4) . ? C22 C23 1.392(4) . ? C22 C31 1.394(4) . ? C22 H22A 0.9400 . ? C23 C24 1.371(5) . ? C23 H23A 0.9400 . ? C24 C25 1.390(5) . ? C24 H24A 0.9400 . ? C25 C26 1.387(4) . ? C25 H25A 0.9400 . ? C26 C31 1.406(4) . ? C26 H26A 0.9400 . ? C32 C33 1.396(4) . ? C32 H32A 0.9400 . ? C33 C34 1.373(4) . ? C33 H33A 0.9400 . ? C34 C35 1.379(4) . ? C34 H34A 0.9400 . ? C35 C36 1.386(4) . ? C35 H35A 0.9400 . ? C36 H36A 0.9400 . ? C41 C42 1.401(4) . ? C41 C46 1.407(3) . ? C42 C43 1.382(4) . ? C42 H42A 0.9400 . ? C43 C44 1.388(4) . ? C43 H43A 0.9400 . ? C44 C45 1.376(4) . ? C44 H44A 0.9400 . ? C45 C46 1.387(4) . ? C45 H45A 0.9400 . ? C46 H46A 0.9400 . ? C51 C52 1.395(3) . ? C51 C56 1.401(4) . ? C52 C53 1.397(4) . ? C52 H52A 0.9400 . ? C53 C54 1.380(4) . ? C53 H53A 0.9400 . ? C54 C55 1.379(4) . ? C54 H54A 0.9400 . ? C55 C56 1.383(4) . ? C55 H55A 0.9400 . ? C56 H56A 0.9400 . ? C60 C61 1.519(5) . ? C60 H60A 0.9700 . ? C60 H60B 0.9700 . ? C60 H60C 0.9700 . ? C61 C66 1.360(5) . ? C61 C62 1.376(5) . ? C62 C63 1.381(5) . ? C62 H62A 0.9400 . ? C63 C64 1.404(6) . ? C63 H63A 0.9400 . ? C64 C65 1.366(6) . ? C64 C67 1.500(6) . ? C65 C66 1.378(6) . ? C65 H65A 0.9400 . ? C66 H66A 0.9400 . ? C67 H67A 0.9700 . ? C67 H67B 0.9700 . ? C67 H67C 0.9700 . ? C70 C71 1.507(5) . ? C70 H70A 0.9700 . ? C70 H70B 0.9700 . ? C70 H70C 0.9700 . ? C71 C76 1.375(5) . ? C71 C72 1.384(5) . ? C72 C76 1.387(5) 3_577 ? C72 H72 0.98(4) . ? C76 C72 1.387(5) 3_577 ? C76 H76 1.00(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Co N4 94.77(10) . . ? N1 Co C13 43.51(12) . . ? N4 Co C13 89.24(14) . . ? N1 Co N3 167.75(9) . . ? N4 Co N3 85.09(10) . . ? C13 Co N3 124.28(12) . . ? N1 Co N2 88.11(11) . . ? N4 Co N2 176.55(10) . . ? C13 Co N2 94.16(14) . . ? N3 Co N2 92.50(10) . . ? N1 Co O1 100.54(9) . . ? N4 Co O1 91.38(9) . . ? C13 Co O1 143.90(12) . . ? N3 Co O1 91.70(8) . . ? N2 Co O1 86.21(9) . . ? C12 O1 Co 114.64(18) . . ? C13 N1 C10 120.4(3) . . ? C13 N1 C1 118.6(3) . . ? C10 N1 C1 110.4(2) . . ? C13 N1 Co 70.44(17) . . ? C10 N1 Co 122.84(19) . . ? C1 N1 Co 109.0(2) . . ? C3 N2 C2 106.7(3) . . ? C3 N2 C11 110.2(3) . . ? C2 N2 C11 110.6(3) . . ? C3 N2 Co 116.2(2) . . ? C2 N2 Co 106.9(2) . . ? C11 N2 Co 106.20(18) . . ? C5 N3 C6 111.6(2) . . ? C5 N3 Co 117.66(19) . . ? C6 N3 Co 108.71(17) . . ? C7 N4 C8 113.0(2) . . ? C7 N4 Co 106.30(17) . . ? C8 N4 Co 114.95(18) . . ? N1 C1 C2 109.1(3) . . ? N1 C1 H1A 109.9 . . ? C2 C1 H1A 109.9 . . ? N1 C1 H1B 109.9 . . ? C2 C1 H1B 109.9 . . ? H1A C1 H1B 108.3 . . ? C1 C2 N2 110.4(3) . . ? C1 C2 H2A 109.6 . . ? N2 C2 H2A 109.6 . . ? C1 C2 H2B 109.6 . . ? N2 C2 H2B 109.6 . . ? H2A C2 H2B 108.1 . . ? N2 C3 C4 115.6(3) . . ? N2 C3 H3A 108.4 . . ? C4 C3 H3A 108.4 . . ? N2 C3 H3B 108.4 . . ? C4 C3 H3B 108.4 . . ? H3A C3 H3B 107.4 . . ? C3 C4 C5 114.6(3) . . ? C3 C4 H4A 108.6 . . ? C5 C4 H4A 108.6 . . ? C3 C4 H4B 108.6 . . ? C5 C4 H4B 108.6 . . ? H4A C4 H4B 107.6 . . ? N3 C5 C4 110.2(2) . . ? N3 C5 H5A 109.6 . . ? C4 C5 H5A 109.6 . . ? N3 C5 H5B 109.6 . . ? C4 C5 H5B 109.6 . . ? H5A C5 H5B 108.1 . . ? N3 C6 C7 106.4(2) . . ? N3 C6 H6A 110.4 . . ? C7 C6 H6A 110.4 . . ? N3 C6 H6B 110.4 . . ? C7 C6 H6B 110.4 . . ? H6A C6 H6B 108.6 . . ? N4 C7 C6 105.7(2) . . ? N4 C7 H7A 110.6 . . ? C6 C7 H7A 110.6 . . ? N4 C7 H7B 110.6 . . ? C6 C7 H7B 110.6 . . ? H7A C7 H7B 108.7 . . ? N4 C8 C9 110.4(3) . . ? N4 C8 H8A 109.6 . . ? C9 C8 H8A 109.6 . . ? N4 C8 H8B 109.6 . . ? C9 C8 H8B 109.6 . . ? H8A C8 H8B 108.1 . . ? C10 C9 C8 114.6(3) . . ? C10 C9 H9A 108.6 . . ? C8 C9 H9A 108.6 . . ? C10 C9 H9B 108.6 . . ? C8 C9 H9B 108.6 . . ? H9A C9 H9B 107.6 . . ? N1 C10 C9 115.4(2) . . ? N1 C10 H10A 108.4 . . ? C9 C10 H10A 108.4 . . ? N1 C10 H10B 108.4 . . ? C9 C10 H10B 108.4 . . ? H10A C10 H10B 107.5 . . ? N1 C13 Co 66.06(15) . . ? N1 C13 H13A 118(2) . . ? Co C13 H13A 119(2) . . ? N1 C13 H13B 120(2) . . ? Co C13 H13B 121(2) . . ? H13A C13 H13B 108(3) . . ? N2 C11 C12 114.1(2) . . ? N2 C11 H11A 108.7 . . ? C12 C11 H11A 108.7 . . ? N2 C11 H11B 108.7 . . ? C12 C11 H11B 108.7 . . ? H11A C11 H11B 107.6 . . ? O2 C12 O1 125.6(3) . . ? O2 C12 C11 118.5(3) . . ? O1 C12 C11 115.8(2) . . ? C31 B C41 110.3(2) . . ? C31 B C51 111.0(2) . . ? C41 B C51 106.1(2) . . ? C31 B C21 108.6(2) . . ? C41 B C21 111.7(2) . . ? C51 B C21 109.18(19) . . ? C32 C21 C36 114.4(2) . . ? C32 C21 B 124.2(2) . . ? C36 C21 B 121.3(2) . . ? C23 C22 C31 122.7(3) . . ? C23 C22 H22A 118.7 . . ? C31 C22 H22A 118.7 . . ? C24 C23 C22 120.7(3) . . ? C24 C23 H23A 119.7 . . ? C22 C23 H23A 119.7 . . ? C23 C24 C25 118.8(3) . . ? C23 C24 H24A 120.6 . . ? C25 C24 H24A 120.6 . . ? C26 C25 C24 119.8(3) . . ? C26 C25 H25A 120.1 . . ? C24 C25 H25A 120.1 . . ? C25 C26 C31 123.0(3) . . ? C25 C26 H26A 118.5 . . ? C31 C26 H26A 118.5 . . ? C22 C31 C26 114.9(2) . . ? C22 C31 B 124.1(2) . . ? C26 C31 B 120.9(2) . . ? C21 C32 C33 123.2(3) . . ? C21 C32 H32A 118.4 . . ? C33 C32 H32A 118.4 . . ? C34 C33 C32 120.3(3) . . ? C34 C33 H33A 119.8 . . ? C32 C33 H33A 119.8 . . ? C33 C34 C35 118.6(3) . . ? C33 C34 H34A 120.7 . . ? C35 C34 H34A 120.7 . . ? C34 C35 C36 120.7(3) . . ? C34 C35 H35A 119.6 . . ? C36 C35 H35A 119.6 . . ? C35 C36 C21 122.7(3) . . ? C35 C36 H36A 118.7 . . ? C21 C36 H36A 118.7 . . ? C42 C41 C46 114.5(2) . . ? C42 C41 B 122.8(2) . . ? C46 C41 B 122.0(2) . . ? C43 C42 C41 123.0(3) . . ? C43 C42 H42A 118.5 . . ? C41 C42 H42A 118.5 . . ? C42 C43 C44 120.4(3) . . ? C42 C43 H43A 119.8 . . ? C44 C43 H43A 119.8 . . ? C45 C44 C43 118.6(3) . . ? C45 C44 H44A 120.7 . . ? C43 C44 H44A 120.7 . . ? C44 C45 C46 120.4(3) . . ? C44 C45 H45A 119.8 . . ? C46 C45 H45A 119.8 . . ? C45 C46 C41 123.0(3) . . ? C45 C46 H46A 118.5 . . ? C41 C46 H46A 118.5 . . ? C52 C51 C56 114.6(2) . . ? C52 C51 B 123.3(2) . . ? C56 C51 B 122.1(2) . . ? C51 C52 C53 123.0(2) . . ? C51 C52 H52A 118.5 . . ? C53 C52 H52A 118.5 . . ? C54 C53 C52 120.0(3) . . ? C54 C53 H53A 120.0 . . ? C52 C53 H53A 120.0 . . ? C53 C54 C55 118.8(3) . . ? C53 C54 H54A 120.6 . . ? C55 C54 H54A 120.6 . . ? C54 C55 C56 120.4(2) . . ? C54 C55 H55A 119.8 . . ? C56 C55 H55A 119.8 . . ? C55 C56 C51 123.2(2) . . ? C55 C56 H56A 118.4 . . ? C51 C56 H56A 118.4 . . ? C61 C60 H60A 109.5 . . ? C61 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C61 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C66 C61 C62 117.8(4) . . ? C66 C61 C60 122.3(4) . . ? C62 C61 C60 120.0(4) . . ? C61 C62 C63 121.1(4) . . ? C61 C62 H62A 119.4 . . ? C63 C62 H62A 119.4 . . ? C62 C63 C64 120.6(4) . . ? C62 C63 H63A 119.7 . . ? C64 C63 H63A 119.7 . . ? C65 C64 C63 117.1(4) . . ? C65 C64 C67 120.8(5) . . ? C63 C64 C67 122.1(5) . . ? C64 C65 C66 121.4(4) . . ? C64 C65 H65A 119.3 . . ? C66 C65 H65A 119.3 . . ? C61 C66 C65 122.0(4) . . ? C61 C66 H66A 119.0 . . ? C65 C66 H66A 119.0 . . ? C64 C67 H67A 109.5 . . ? C64 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C64 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C71 C70 H70A 109.5 . . ? C71 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C71 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? C76 C71 C72 117.4(3) . . ? C76 C71 C70 121.3(3) . . ? C72 C71 C70 121.4(3) . . ? C71 C72 C76 121.3(3) . 3_577 ? C71 C72 H72 125(2) . . ? C76 C72 H72 111(2) 3_577 . ? C71 C76 C72 121.4(3) . 3_577 ? C71 C76 H76 119(2) . . ? C72 C76 H76 119(2) 3_577 . ? _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 1.132 _refine_diff_density_min -0.388 _refine_diff_density_rms 0.058 #=END data_dmt7 _chemical_name_systematic ; chloro(1-carboxymethyl-4-methyl-1,4,8,11-tetraazacyclotetradecane)- cobalt (III) perchlorate ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H25 Cl2 Co N4 O6' _chemical_formula_weight 463.20 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' 'Cl' 'Cl' 0.1484 0.1585 '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' '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' _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 8.456(2) _cell_length_b 9.689(3) _cell_length_c 12.161(6) _cell_angle_alpha 90.95(3) _cell_angle_beta 109.51(3) _cell_angle_gamma 96.09(2) _cell_volume 932.4(6) _cell_formula_units_Z 2 _cell_measurement_temperature 292(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 11.45 _cell_measurement_theta_max 14.22 _exptl_crystal_description Prism _exptl_crystal_colour Red _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.650 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 480 _exptl_absorpt_coefficient_mu 1.245 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North et al, 1968)' _exptl_absorpt_correction_T_min 0.6491 _exptl_absorpt_correction_T_max 0.7460 _exptl_special_details ; ? ; _diffrn_ambient_temperature 292(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAD-4' _diffrn_measurement_method '\w/2\q' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 _diffrn_reflns_number 3323 _diffrn_reflns_av_R_equivalents 0.0206 _diffrn_reflns_av_sigmaI/netI 0.0361 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 24.98 _reflns_number_total 3188 _reflns_number_gt 2561 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD-4 Software (Enraf, 1989)' _computing_cell_refinement 'CAD-4 Software (Enraf, 1989)' _computing_data_reduction 'Local Program' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL (Siemens,1994b)' _computing_publication_material 'Siemens SHELXTL (Siemens,1994b)' _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 'w=1/[\s^2^(Fo^2^)+(0.0970P)^2^+1.9598P] 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 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3188 _refine_ls_number_parameters 228 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0769 _refine_ls_R_factor_gt 0.0571 _refine_ls_wR_factor_ref 0.1694 _refine_ls_wR_factor_gt 0.1546 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co Co 0.22393(8) 0.27736(6) 0.26119(5) 0.0297(2) Uani 1 d . . . Cl1 Cl -0.00250(17) 0.25070(15) 0.09814(12) 0.0485(4) Uani 1 d . . . O1 O 0.4050(4) 0.3017(4) 0.4052(3) 0.0385(8) Uani 1 d . . . O2 O 0.6708(5) 0.3921(5) 0.4900(4) 0.0583(12) Uani 1 d . . . N1 N 0.3290(5) 0.1144(4) 0.2139(4) 0.0347(9) Uani 1 d . . . N2 N 0.3691(6) 0.4038(5) 0.1984(4) 0.0412(10) Uani 1 d . . . N3 N 0.1284(5) 0.4340(5) 0.3119(4) 0.0424(11) Uani 1 d . . . N4 N 0.0984(6) 0.1555(5) 0.3414(4) 0.0446(11) Uani 1 d . . . C1 C 0.4742(8) 0.1835(6) 0.1839(5) 0.0503(14) Uani 1 d . . . H1A H 0.5064 0.1209 0.1341 0.060 Uiso 1 calc R . . H1B H 0.5706 0.2076 0.2544 0.060 Uiso 1 calc R . . C2 C 0.4215(8) 0.3137(6) 0.1209(5) 0.0523(15) Uani 1 d . . . H2A H 0.5153 0.3621 0.1025 0.063 Uiso 1 calc R . . H2B H 0.3285 0.2894 0.0484 0.063 Uiso 1 calc R . . C3 C 0.2888(9) 0.5222(6) 0.1300(5) 0.0583(17) Uani 1 d . . . H3A H 0.3731 0.5775 0.1062 0.070 Uiso 1 calc R . . H3B H 0.1993 0.4838 0.0597 0.070 Uiso 1 calc R . . C4 C 0.2171(9) 0.6155(6) 0.1953(6) 0.0636(19) Uani 1 d . . . H4A H 0.1763 0.6912 0.1465 0.076 Uiso 1 calc R . . H4B H 0.3080 0.6556 0.2643 0.076 Uiso 1 calc R . . C5 C 0.0768(8) 0.5502(6) 0.2331(6) 0.0616(18) Uani 1 d . . . H5A H -0.0180 0.5149 0.1646 0.074 Uiso 1 calc R . . H5B H 0.0397 0.6206 0.2735 0.074 Uiso 1 calc R . . C6 C -0.0184(8) 0.3730(7) 0.3452(6) 0.0604(18) Uani 1 d . . . H6A H -0.0467 0.4397 0.3940 0.072 Uiso 1 calc R . . H6B H -0.1165 0.3479 0.2759 0.072 Uiso 1 calc R . . C7 C 0.0331(8) 0.2473(7) 0.4105(6) 0.0587(16) Uani 1 d . . . H7A H 0.1199 0.2747 0.4852 0.070 Uiso 1 calc R . . H7B H -0.0632 0.1977 0.4250 0.070 Uiso 1 calc R . . C8 C 0.1907(9) 0.0514(7) 0.4178(6) 0.0561(16) Uani 1 d . . . H8A H 0.1146 -0.0014 0.4505 0.067 Uiso 1 calc R . . H8B H 0.2828 0.0996 0.4821 0.067 Uiso 1 calc R . . C9 C 0.2607(9) -0.0476(6) 0.3547(6) 0.0581(16) Uani 1 d . . . H9A H 0.3080 -0.1186 0.4070 0.070 Uiso 1 calc R . . H9B H 0.1690 -0.0932 0.2887 0.070 Uiso 1 calc R . . C10 C 0.3939(8) 0.0210(6) 0.3117(5) 0.0475(14) Uani 1 d . . . H10A H 0.4476 -0.0503 0.2855 0.057 Uiso 1 calc R . . H10B H 0.4796 0.0750 0.3763 0.057 Uiso 1 calc R . . C11 C 0.5193(7) 0.4609(6) 0.3012(5) 0.0480(14) Uani 1 d . . . H11A H 0.6207 0.4607 0.2807 0.058 Uiso 1 calc R . . H11B H 0.5084 0.5565 0.3194 0.058 Uiso 1 calc R . . C12 C 0.5373(7) 0.3804(5) 0.4056(5) 0.0409(12) Uani 1 d . . . C13 C 0.2188(8) 0.0246(6) 0.1094(5) 0.0496(14) Uani 1 d . . . H13A H 0.2755 -0.0531 0.0996 0.074 Uiso 1 calc R . . H13B H 0.1960 0.0778 0.0411 0.074 Uiso 1 calc R . . H13C H 0.1144 -0.0085 0.1205 0.074 Uiso 1 calc R . . Cl2 Cl 0.2620(2) 0.16630(17) 0.78583(14) 0.0565(4) Uani 1 d . . . O3 O 0.320(3) 0.227(2) 0.7053(18) 0.149(6) Uiso 0.50 d P A 1 O4 O 0.4218(15) 0.1471(13) 0.8865(11) 0.073(3) Uiso 0.50 d P A 1 O5 O 0.2200(14) 0.0369(12) 0.7065(11) 0.068(3) Uiso 0.50 d P A 1 O3' O 0.2281(18) 0.2733(14) 0.7026(12) 0.096(4) Uiso 0.50 d P A 2 O4' O 0.4292(16) 0.1966(14) 0.8568(11) 0.079(3) Uiso 0.50 d P A 2 O5' O 0.222(2) 0.0193(17) 0.7597(14) 0.107(5) Uiso 0.50 d P A 2 O6 O 0.1400(9) 0.1797(8) 0.8369(6) 0.111(2) Uiso 1 d . . . 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 Co 0.0272(4) 0.0265(4) 0.0295(4) -0.0012(2) 0.0024(3) 0.0017(2) Cl1 0.0422(8) 0.0465(8) 0.0405(8) -0.0052(6) -0.0061(6) 0.0021(6) O1 0.0356(19) 0.0384(19) 0.0360(19) 0.0004(15) 0.0048(15) 0.0043(16) O2 0.036(2) 0.058(3) 0.060(3) -0.014(2) -0.0102(19) 0.0028(19) N1 0.037(2) 0.031(2) 0.032(2) -0.0035(17) 0.0060(18) 0.0050(17) N2 0.042(2) 0.037(2) 0.040(2) 0.0041(19) 0.011(2) -0.0045(19) N3 0.036(2) 0.038(2) 0.046(3) -0.005(2) 0.003(2) 0.0088(19) N4 0.043(3) 0.047(3) 0.046(3) 0.007(2) 0.019(2) 0.003(2) C1 0.050(3) 0.053(3) 0.052(3) -0.009(3) 0.025(3) 0.002(3) C2 0.064(4) 0.051(3) 0.047(3) 0.001(3) 0.028(3) -0.005(3) C3 0.075(4) 0.037(3) 0.048(4) 0.012(3) 0.006(3) -0.007(3) C4 0.081(5) 0.033(3) 0.061(4) 0.013(3) 0.002(4) 0.011(3) C5 0.056(4) 0.044(3) 0.066(4) -0.006(3) -0.008(3) 0.022(3) C6 0.038(3) 0.073(4) 0.072(4) -0.016(4) 0.019(3) 0.014(3) C7 0.050(4) 0.075(4) 0.060(4) 0.001(3) 0.032(3) 0.003(3) C8 0.068(4) 0.051(4) 0.054(4) 0.020(3) 0.028(3) 0.000(3) C9 0.073(4) 0.037(3) 0.060(4) 0.017(3) 0.015(3) 0.007(3) C10 0.053(3) 0.036(3) 0.049(3) 0.006(2) 0.009(3) 0.012(3) C11 0.038(3) 0.042(3) 0.053(3) 0.000(3) 0.007(3) -0.009(2) C12 0.033(3) 0.032(3) 0.051(3) -0.009(2) 0.008(2) 0.001(2) C13 0.056(4) 0.038(3) 0.045(3) -0.011(2) 0.005(3) 0.000(3) Cl2 0.0513(9) 0.0637(10) 0.0592(9) 0.0020(7) 0.0272(7) -0.0001(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co O1 1.894(3) . ? Co N3 1.975(4) . ? Co N2 1.982(4) . ? Co N4 1.984(5) . ? Co N1 2.054(4) . ? Co Cl1 2.2376(17) . ? O1 C12 1.284(6) . ? O2 C12 1.239(6) . ? N1 C1 1.491(7) . ? N1 C10 1.497(7) . ? N1 C13 1.497(6) . ? N2 C2 1.476(7) . ? N2 C11 1.501(7) . ? N2 C3 1.513(7) . ? N3 C5 1.496(8) . ? N3 C6 1.497(8) . ? N4 C7 1.480(8) . ? N4 C8 1.484(8) . ? C1 C2 1.517(9) . ? C3 C4 1.493(10) . ? C4 C5 1.494(10) . ? C6 C7 1.489(10) . ? C8 C9 1.502(9) . ? C9 C10 1.494(9) . ? C11 C12 1.474(8) . ? Cl2 O3 1.35(2) . ? Cl2 O4' 1.385(13) . ? Cl2 O6 1.386(7) . ? Cl2 O5' 1.433(16) . ? Cl2 O3' 1.445(14) . ? Cl2 O5 1.506(11) . ? Cl2 O4 1.522(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co N3 88.67(17) . . ? O1 Co N2 86.34(17) . . ? N3 Co N2 92.2(2) . . ? O1 Co N4 87.31(18) . . ? N3 Co N4 87.0(2) . . ? N2 Co N4 173.61(18) . . ? O1 Co N1 89.46(16) . . ? N3 Co N1 178.10(17) . . ? N2 Co N1 88.03(18) . . ? N4 Co N1 92.60(19) . . ? O1 Co Cl1 175.89(12) . . ? N3 Co Cl1 88.32(13) . . ? N2 Co Cl1 96.57(14) . . ? N4 Co Cl1 89.74(15) . . ? N1 Co Cl1 93.53(12) . . ? C12 O1 Co 116.1(4) . . ? C1 N1 C10 109.0(4) . . ? C1 N1 C13 107.3(4) . . ? C10 N1 C13 107.5(4) . . ? C1 N1 Co 103.8(3) . . ? C10 N1 Co 112.7(3) . . ? C13 N1 Co 116.3(3) . . ? C2 N2 C11 110.2(5) . . ? C2 N2 C3 108.8(5) . . ? C11 N2 C3 109.6(4) . . ? C2 N2 Co 105.0(3) . . ? C11 N2 Co 106.4(3) . . ? C3 N2 Co 116.7(4) . . ? C5 N3 C6 109.5(5) . . ? C5 N3 Co 120.1(4) . . ? C6 N3 Co 107.0(4) . . ? C7 N4 C8 109.3(5) . . ? C7 N4 Co 107.2(4) . . ? C8 N4 Co 117.6(4) . . ? N1 C1 C2 108.6(5) . . ? N2 C2 C1 108.1(5) . . ? C4 C3 N2 114.5(5) . . ? C3 C4 C5 116.5(5) . . ? C4 C5 N3 112.5(5) . . ? C7 C6 N3 107.1(5) . . ? N4 C7 C6 109.6(5) . . ? N4 C8 C9 113.2(5) . . ? C10 C9 C8 113.5(5) . . ? C9 C10 N1 114.0(5) . . ? C12 C11 N2 112.5(4) . . ? O2 C12 O1 122.3(6) . . ? O2 C12 C11 121.6(5) . . ? O1 C12 C11 116.0(5) . . ? O3 Cl2 O4' 82.9(10) . . ? O3 Cl2 O6 139.4(10) . . ? O4' Cl2 O6 117.0(6) . . ? O3 Cl2 O5' 110.4(11) . . ? O4' Cl2 O5' 109.8(9) . . ? O6 Cl2 O5' 96.2(7) . . ? O3 Cl2 O3' 38.6(9) . . ? O4' Cl2 O3' 106.6(8) . . ? O6 Cl2 O3' 100.9(7) . . ? O5' Cl2 O3' 126.4(9) . . ? O3 Cl2 O5 85.7(10) . . ? O4' Cl2 O5 116.3(7) . . ? O6 Cl2 O5 111.7(5) . . ? O5' Cl2 O5 26.1(7) . . ? O3' Cl2 O5 101.6(7) . . ? O3 Cl2 O4 104.0(10) . . ? O4' Cl2 O4 23.9(6) . . ? O6 Cl2 O4 105.3(6) . . ? O5' Cl2 O4 91.8(8) . . ? O3' Cl2 O4 130.4(8) . . ? O5 Cl2 O4 106.5(6) . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 1.154 _refine_diff_density_min -0.798 _refine_diff_density_rms 0.106