# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Makoto Tadokoro' _publ_contact_author_address ; Chemistry Tokyo University of Science, Faculty of Science Kagurazaka 1-3 Shinjuku-ku Tokyo 162-8601 JAPAN ; _publ_contact_author_email TADOKORO@RS.KAGU.TUS.AC.JP _publ_section_title ; Structures and Phase Transition of Multi-Layered Water Nanotube Confined to Nanochannels ; loop_ _publ_author_name 'Makoto Tadokoro' 'Syoko Fukui' "Shun'Ichi Ishimaru" 'Kiyoshi Isobe' 'Hiroshi Kitagawa' 'Tadamori Kitajima' ; Y.Nagao ; 'Kazuhiro Nakasuji' # Attachment 'CoTMALT.cif' data_29266 _database_code_depnum_ccdc_archive 'CCDC 220823' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C81 H183 Co3 N36 O78' _chemical_formula_weight 3086.42 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' 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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 16.7257(19) _cell_length_b 29.142(3) _cell_length_c 32.264(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.939(4) _cell_angle_gamma 90.00 _cell_volume 15705(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.305 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6504 _exptl_absorpt_coefficient_mu 0.416 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16262 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0762 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 27.48 _reflns_number_total 16262 _reflns_number_gt 10351 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1097P)^2^+59.6587P] 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 SHELXL _refine_ls_extinction_coef 0.00003(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 16262 _refine_ls_number_parameters 900 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1432 _refine_ls_R_factor_gt 0.0950 _refine_ls_wR_factor_ref 0.2621 _refine_ls_wR_factor_gt 0.2281 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.090 _refine_ls_shift/su_max 0.038 _refine_ls_shift/su_mean 0.004 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co -0.00088(3) 0.16745(2) 0.083057(19) 0.02811(18) Uani 1 1 d . . . Co2 Co 1.0000 0.13234(3) 0.7500 0.0273(2) Uani 1 2 d S . . O1 O 0.0590(2) 0.04497(12) 0.57277(13) 0.0462(9) Uani 1 1 d . . . O2 O -0.0601(2) 0.04568(11) 0.60166(12) 0.0427(9) Uani 1 1 d . . . O3 O -0.2136(2) 0.19501(14) 0.56773(17) 0.0669(14) Uani 1 1 d . . . O4 O -0.1515(2) 0.25517(13) 0.59691(15) 0.0582(12) Uani 1 1 d . . . O5 O 0.1472(2) 0.25236(12) 0.55906(15) 0.0549(11) Uani 1 1 d . . . O6 O 0.2101(2) 0.19636(13) 0.59535(13) 0.0470(9) Uani 1 1 d . . . O7 O 0.55862(19) 0.41899(11) 0.73453(13) 0.0433(9) Uani 1 1 d . . . O8 O 0.7116(2) 0.26940(13) 0.76411(17) 0.0654(14) Uani 1 1 d . . . O9 O 0.6501(2) 0.21143(13) 0.73037(16) 0.0605(12) Uani 1 1 d . . . O10 O 0.3067(10) 0.1101(5) 0.0473(3) 0.350(12) Uani 1 1 d . . . O11 O 0.2290(5) 0.0474(3) 0.0936(3) 0.148(3) Uani 1 1 d . . . O12 O 0.4256(3) 0.1615(2) 0.08437(18) 0.0924(17) Uani 1 1 d . . . O13 O 0.4754(7) 0.0275(4) 0.0685(3) 0.199(4) Uani 1 1 d . . . O14 O 0.5740(3) 0.16548(16) 0.04682(17) 0.0755(14) Uani 1 1 d . . . O15 O 0.7914(4) 0.0478(2) 0.0413(2) 0.120(2) Uani 1 1 d . . . O16 O 0.9202(4) 0.3408(3) 0.0419(2) 0.154(4) Uani 1 1 d . . . O17 O 0.7017(4) 0.1137(2) 0.0869(2) 0.114(2) Uani 1 1 d . . . O18 O 0.6076(4) 0.0483(2) 0.1217(2) 0.1033(19) Uani 1 1 d . . . O19 O 0.6722(4) 0.1396(2) 0.2207(2) 0.1036(19) Uani 1 1 d . . . O20 O 0.5490(3) 0.0825(2) 0.19197(19) 0.0944(18) Uani 1 1 d . . . O21 O 0.4139(3) 0.12928(19) 0.16395(17) 0.0850(16) Uani 1 1 d . . . O22 O 0.2987(3) 0.06014(18) 0.17143(17) 0.0802(15) Uani 1 1 d . . . O23 O 0.5000 0.0226(3) 0.2500 0.083(2) Uani 1 2 d S . . O24 O 0.4207(4) 0.1960(2) 0.2295(2) 0.121(2) Uani 1 1 d . . . O25 O 0.2211(2) 0.07415(16) 0.24339(16) 0.0664(12) Uani 1 1 d . . . O26 O 0.2640(4) 0.1798(2) 0.3468(3) 0.133(3) Uani 1 1 d . . . O27 O 0.2139(3) 0.0432(2) 0.5492(2) 0.104(2) Uani 1 1 d . . . O28 O 0.3329(3) 0.0987(2) 0.5871(2) 0.103(2) Uani 1 1 d . . . O29 O 0.4452(3) 0.0413(2) 0.62434(19) 0.1011(19) Uani 1 1 d . . . O30 O 0.5734(5) 0.1461(4) 0.5801(3) 0.193(5) Uani 1 1 d . . . O31 O 0.7154(3) 0.11624(18) 0.53710(17) 0.0881(16) Uani 1 1 d . . . O32 O 0.7807(2) 0.04036(14) 0.57745(14) 0.0586(11) Uani 1 1 d . . . O33 O 0.6964(3) 0.02667(17) 0.64706(14) 0.0691(12) Uani 1 1 d . . . O34 O 0.5787(3) 0.09241(19) 0.65128(17) 0.0831(15) Uani 1 1 d . . . O35 O 0.3844(3) 0.01590(17) 0.69695(16) 0.0758(14) Uani 1 1 d . . . O36 O 0.2596(3) 0.1331(2) 0.65590(18) 0.0946(19) Uani 1 1 d . . . O37 O 0.2929(3) 0.08497(16) 0.72897(15) 0.0669(12) Uani 1 1 d . . . O38 O 0.5730(3) 0.12949(14) 0.73054(16) 0.0640(12) Uani 1 1 d . . . O39 O 0.7832(3) 0.01606(17) 0.72201(15) 0.0743(14) Uani 1 1 d . . . O40 O 0.009(4) 0.4609(15) 0.0058(12) 0.54(4) Uani 0.50 1 d P . . N1 N -0.0999(2) 0.17058(13) 0.04948(12) 0.0291(8) Uani 1 1 d . . . N2 N -0.2191(2) 0.20248(14) 0.03892(13) 0.0347(9) Uani 1 1 d . . . N3 N -0.0492(2) 0.21613(13) 0.11397(12) 0.0302(8) Uani 1 1 d . . . N4 N -0.1494(2) 0.26532(14) 0.11793(13) 0.0352(9) Uani 1 1 d . . . N5 N 0.0506(2) 0.21295(12) 0.05010(12) 0.0284(8) Uani 1 1 d . . . N6 N 0.1540(2) 0.25839(14) 0.04267(13) 0.0377(9) Uani 1 1 d . . . N7 N 0.0984(2) 0.17033(12) 0.11651(12) 0.0295(8) Uani 1 1 d . . . N8 N 0.2191(2) 0.20042(14) 0.12587(13) 0.0384(10) Uani 1 1 d . . . N9 N 0.0406(2) 0.11696(13) 0.05157(12) 0.0311(8) Uani 1 1 d . . . N10 N 0.0546(2) 0.04186(14) 0.04454(13) 0.0359(9) Uani 1 1 d . . . N11 N -0.0438(2) 0.11844(12) 0.11611(12) 0.0285(8) Uani 1 1 d . . . N12 N -0.0598(2) 0.04381(13) 0.12465(13) 0.0352(9) Uani 1 1 d . . . N13 N 0.9011(2) 0.13578(13) 0.71591(12) 0.0308(8) Uani 1 1 d . . . N14 N 0.7823(2) 0.16749(14) 0.70547(13) 0.0365(9) Uani 1 1 d . . . N15 N 0.9493(2) 0.17953(12) 0.78192(12) 0.0290(8) Uani 1 1 d . . . N16 N 0.8470(2) 0.22647(14) 0.78759(13) 0.0351(9) Uani 1 1 d . . . N17 N 1.0426(2) 0.08226(12) 0.71788(12) 0.0276(8) Uani 1 1 d . . . N18 N 1.0575(2) 0.00787(12) 0.71003(12) 0.0316(8) Uani 1 1 d . . . C1 C -0.1384(3) 0.14902(16) 0.01592(16) 0.0357(11) Uani 1 1 d . . . C2 C -0.2120(3) 0.16882(18) 0.00942(16) 0.0394(12) Uani 1 1 d . . . C3 C -0.0304(3) 0.24617(18) 0.14519(15) 0.0385(11) Uani 1 1 d . . . C4 C -0.0919(3) 0.27692(19) 0.14828(17) 0.0441(13) Uani 1 1 d . . . C5 C -0.1513(2) 0.20254(15) 0.06256(14) 0.0288(9) Uani 1 1 d . . . C6 C -0.1218(3) 0.22886(15) 0.09765(15) 0.0308(10) Uani 1 1 d . . . C7 C 0.0327(3) 0.24145(16) 0.01706(15) 0.0351(11) Uani 1 1 d . . . C8 C 0.0973(3) 0.26963(19) 0.01234(17) 0.0437(13) Uani 1 1 d . . . C9 C 0.1343(3) 0.15137(17) 0.15173(16) 0.0377(11) Uani 1 1 d . . . C10 C 0.2097(3) 0.16992(19) 0.15749(16) 0.0417(12) Uani 1 1 d . . . C11 C 0.1242(3) 0.22450(15) 0.06489(15) 0.0310(10) Uani 1 1 d . . . C12 C 0.1518(3) 0.19994(16) 0.10192(14) 0.0297(9) Uani 1 1 d . . . C13 C 0.0870(3) 0.10989(17) 0.01852(15) 0.0366(11) Uani 1 1 d . . . C14 C 0.0962(3) 0.06304(19) 0.01403(16) 0.0435(12) Uani 1 1 d . . . C15 C -0.0924(3) 0.11223(16) 0.14894(16) 0.0369(11) Uani 1 1 d . . . C16 C -0.1019(3) 0.06633(17) 0.15417(16) 0.0393(11) Uani 1 1 d . . . C17 C 0.0218(2) 0.07555(15) 0.06641(14) 0.0294(10) Uani 1 1 d . . . C18 C -0.0259(3) 0.07627(15) 0.10242(15) 0.0308(10) Uani 1 1 d . . . C19 C 0.8646(3) 0.11559(16) 0.68197(15) 0.0350(11) Uani 1 1 d . . . C20 C 0.7906(3) 0.13500(18) 0.67497(17) 0.0407(12) Uani 1 1 d . . . C21 C 0.9670(3) 0.20820(17) 0.81462(15) 0.0366(11) Uani 1 1 d . . . C22 C 0.9035(3) 0.23767(17) 0.81842(17) 0.0390(11) Uani 1 1 d . . . C23 C 0.8491(3) 0.16668(15) 0.72992(15) 0.0299(9) Uani 1 1 d . . . C24 C 0.8772(3) 0.19148(15) 0.76619(15) 0.0291(9) Uani 1 1 d . . . C25 C 1.0905(3) 0.07546(17) 0.68499(16) 0.0363(11) Uani 1 1 d . . . C26 C 1.1003(3) 0.02889(16) 0.68019(16) 0.0375(11) Uani 1 1 d . . . C27 C 1.0247(3) 0.04097(15) 0.73218(15) 0.0300(10) Uani 1 1 d . . . C28 C -0.0013(3) 0.11734(15) 0.58564(14) 0.0294(9) Uani 1 1 d . . . C29 C -0.0733(3) 0.14153(16) 0.58533(15) 0.0313(10) Uani 1 1 d . . . C30 C -0.0737(3) 0.18926(16) 0.58306(14) 0.0318(10) Uani 1 1 d . . . C31 C -0.0017(3) 0.21316(14) 0.58130(14) 0.0304(10) Uani 1 1 d . . . C32 C 0.0708(3) 0.18922(15) 0.58126(14) 0.0298(10) Uani 1 1 d . . . C33 C 0.0708(3) 0.14170(15) 0.58393(15) 0.0295(9) Uani 1 1 d . . . C34 C -0.0009(3) 0.06571(16) 0.58693(16) 0.0347(10) Uani 1 1 d . . . C35 C -0.1522(3) 0.21519(18) 0.58244(19) 0.0442(13) Uani 1 1 d . . . C36 C 0.1484(3) 0.21466(16) 0.57887(17) 0.0363(11) Uani 1 1 d . . . C37 C 0.5000 0.3471(2) 0.7500 0.0279(13) Uani 1 2 d S . . C38 C 0.5720(3) 0.32307(16) 0.74955(15) 0.0309(10) Uani 1 1 d . . . C39 C 0.5725(3) 0.27516(15) 0.74928(15) 0.0306(10) Uani 1 1 d . . . C40 C 0.5000 0.2509(2) 0.7500 0.0289(13) Uani 1 2 d S . . C41 C 0.5000 0.3993(2) 0.7500 0.0340(15) Uani 1 2 d S . . C42 C 0.6509(3) 0.25009(17) 0.74813(18) 0.0386(12) Uani 1 1 d . . . H1 H -0.1169 0.1244 0.0002 0.043 Uiso 1 1 d . . . H2 H -0.2513 0.1608 -0.0119 0.048 Uiso 1 1 d . . . H3 H 0.0180 0.2456 0.1624 0.047 Uiso 1 1 d . . . H4 H -0.0940 0.3023 0.1674 0.053 Uiso 1 1 d . . . H5 H -0.2642 0.2220 0.0420 0.043 Uiso 1 1 d . . . H6 H -0.1996 0.2803 0.1125 0.043 Uiso 1 1 d . . . H7 H -0.0162 0.2416 0.0003 0.043 Uiso 1 1 d . . . H8 H 0.1022 0.2930 -0.0083 0.052 Uiso 1 1 d . . . H9 H 0.1106 0.1293 0.1695 0.045 Uiso 1 1 d . . . H10 H 0.2486 0.1625 0.1793 0.051 Uiso 1 1 d . . . H11 H 0.2055 0.2722 0.0471 0.047 Uiso 1 1 d . . . H12 H 0.2650 0.2192 0.1219 0.047 Uiso 1 1 d . . . H13 H 0.1096 0.1332 0.0017 0.045 Uiso 1 1 d . . . H14 H 0.1255 0.0479 -0.0067 0.052 Uiso 1 1 d . . . H15 H -0.1162 0.1361 0.1648 0.045 Uiso 1 1 d . . . H16 H -0.1325 0.0517 0.1748 0.047 Uiso 1 1 d . . . H17 H 0.0500 0.0096 0.0492 0.045 Uiso 1 1 d . . . H18 H -0.0560 0.0117 0.1212 0.044 Uiso 1 1 d . . . H19 H 0.8874 0.0920 0.6654 0.043 Uiso 1 1 d . . . H20 H 0.7517 0.1273 0.6533 0.050 Uiso 1 1 d . . . H21 H 1.0153 0.2078 0.8317 0.046 Uiso 1 1 d . . . H22 H 0.8992 0.2613 0.8389 0.047 Uiso 1 1 d . . . H23 H 0.7371 0.1868 0.7085 0.044 Uiso 1 1 d . . . H24 H 0.7959 0.2406 0.7825 0.043 Uiso 1 1 d . . . H25 H 1.1152 0.1000 0.6702 0.040 Uiso 1 1 d . . . H26 H 1.1311 0.0137 0.6602 0.066 Uiso 1 1 d . . . H27 H 1.0516 -0.0243 0.7141 0.025 Uiso 1 1 d . . . H28 H -0.1230 0.1251 0.5867 0.038 Uiso 1 1 d . . . H29 H -0.0020 0.2460 0.5801 0.036 Uiso 1 1 d . . . H30 H 0.1208 0.1255 0.5847 0.036 Uiso 1 1 d . . . H31 H 0.6214 0.3395 0.7495 0.037 Uiso 1 1 d . . . H32 H 0.5000 0.2100 0.7500 0.040 Uiso 1 2 d S . . 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 0.0273(3) 0.0233(3) 0.0339(3) 0.0016(2) 0.0026(2) 0.0011(2) Co2 0.0266(4) 0.0198(4) 0.0358(5) 0.000 0.0034(3) 0.000 O1 0.0402(19) 0.0266(18) 0.073(3) -0.0110(17) 0.0104(18) 0.0015(15) O2 0.0357(19) 0.0244(17) 0.069(3) 0.0039(16) 0.0070(17) -0.0027(14) O3 0.0283(19) 0.038(2) 0.131(4) -0.005(2) -0.019(2) 0.0078(16) O4 0.037(2) 0.034(2) 0.104(4) -0.018(2) 0.013(2) 0.0066(16) O5 0.039(2) 0.028(2) 0.098(3) 0.019(2) 0.007(2) -0.0033(15) O6 0.0286(18) 0.041(2) 0.071(3) 0.0097(18) -0.0069(17) -0.0057(15) O7 0.0337(18) 0.0215(17) 0.075(3) 0.0059(17) 0.0067(17) -0.0014(13) O8 0.0290(19) 0.029(2) 0.136(4) -0.015(2) -0.018(2) 0.0082(15) O9 0.034(2) 0.033(2) 0.115(4) -0.022(2) 0.009(2) 0.0052(15) O10 0.51(2) 0.43(2) 0.096(7) 0.044(9) -0.074(10) -0.388(19) O11 0.182(7) 0.121(6) 0.132(6) 0.009(5) -0.073(6) -0.040(6) O12 0.079(4) 0.097(4) 0.101(4) 0.021(3) 0.008(3) -0.011(3) O13 0.277(13) 0.176(9) 0.146(8) 0.027(7) 0.024(8) -0.036(9) O14 0.076(3) 0.055(3) 0.096(4) -0.011(3) 0.008(3) -0.008(2) O15 0.161(6) 0.082(4) 0.121(5) 0.032(4) 0.041(5) 0.023(4) O16 0.108(5) 0.219(9) 0.134(6) -0.088(7) 0.004(5) 0.031(6) O17 0.127(5) 0.089(4) 0.129(6) 0.046(4) 0.048(4) 0.029(4) O18 0.118(5) 0.073(4) 0.121(5) 0.014(4) 0.026(4) 0.001(3) O19 0.112(5) 0.096(5) 0.103(5) -0.007(4) 0.015(4) 0.017(4) O20 0.078(4) 0.099(4) 0.106(4) 0.022(4) 0.003(3) 0.010(3) O21 0.083(4) 0.086(4) 0.086(4) 0.014(3) 0.004(3) 0.010(3) O22 0.082(3) 0.077(3) 0.082(4) 0.021(3) 0.006(3) 0.012(3) O23 0.074(5) 0.088(5) 0.085(5) 0.000 -0.013(4) 0.000 O24 0.150(6) 0.095(5) 0.124(6) -0.015(4) 0.053(5) -0.004(4) O25 0.048(2) 0.060(3) 0.091(3) 0.005(2) 0.002(2) 0.010(2) O26 0.124(5) 0.072(4) 0.209(8) 0.008(5) 0.062(5) -0.001(4) O27 0.078(4) 0.092(4) 0.144(6) -0.028(4) 0.027(4) -0.006(3) O28 0.072(4) 0.116(5) 0.120(5) 0.020(4) 0.001(3) -0.014(3) O29 0.083(4) 0.121(5) 0.098(4) 0.009(4) -0.001(3) -0.006(4) O30 0.103(6) 0.299(13) 0.179(9) 0.146(9) 0.016(5) 0.020(7) O31 0.108(4) 0.071(3) 0.083(4) 0.003(3) -0.019(3) 0.003(3) O32 0.052(2) 0.048(2) 0.076(3) 0.004(2) 0.004(2) -0.0057(19) O33 0.077(3) 0.068(3) 0.062(3) 0.001(2) 0.004(2) 0.001(2) O34 0.086(4) 0.083(4) 0.081(4) 0.003(3) 0.006(3) 0.012(3) O35 0.088(3) 0.059(3) 0.079(3) -0.003(3) -0.005(3) 0.002(3) O36 0.086(4) 0.106(4) 0.092(4) 0.055(3) 0.005(3) 0.003(3) O37 0.073(3) 0.056(3) 0.071(3) 0.004(2) -0.003(2) -0.006(2) O38 0.057(3) 0.045(2) 0.091(3) -0.003(2) 0.011(2) -0.0021(19) O39 0.083(3) 0.073(3) 0.067(3) 0.011(3) 0.004(2) 0.018(3) O40 1.00(11) 0.41(6) 0.24(4) -0.18(5) 0.23(5) -0.26(8) N1 0.0278(19) 0.027(2) 0.033(2) -0.0017(16) 0.0045(15) -0.0013(15) N2 0.030(2) 0.032(2) 0.041(2) -0.0049(17) -0.0023(17) 0.0036(16) N3 0.0298(19) 0.025(2) 0.036(2) 0.0015(16) 0.0011(16) 0.0034(15) N4 0.033(2) 0.033(2) 0.039(2) -0.0072(17) -0.0016(17) 0.0061(16) N5 0.0325(19) 0.0191(18) 0.034(2) 0.0035(15) 0.0006(16) 0.0004(14) N6 0.037(2) 0.032(2) 0.043(2) 0.0098(18) -0.0037(18) -0.0076(17) N7 0.0268(18) 0.025(2) 0.036(2) 0.0079(16) 0.0029(15) -0.0012(15) N8 0.028(2) 0.040(2) 0.047(3) 0.0098(19) -0.0001(17) -0.0013(17) N9 0.031(2) 0.027(2) 0.036(2) 0.0013(16) 0.0043(16) 0.0012(15) N10 0.040(2) 0.029(2) 0.040(2) 0.0019(17) 0.0135(18) 0.0044(17) N11 0.0274(18) 0.0225(19) 0.036(2) 0.0005(15) 0.0041(16) 0.0006(14) N12 0.038(2) 0.024(2) 0.045(2) 0.0038(17) 0.0084(18) -0.0001(16) N13 0.032(2) 0.0224(19) 0.038(2) -0.0038(16) 0.0040(16) -0.0014(15) N14 0.030(2) 0.034(2) 0.046(2) -0.0074(18) -0.0015(17) 0.0031(16) N15 0.0281(19) 0.0238(19) 0.035(2) -0.0006(15) -0.0021(16) 0.0007(14) N16 0.033(2) 0.028(2) 0.044(2) -0.0068(17) -0.0007(17) 0.0073(16) N17 0.0283(18) 0.0189(18) 0.036(2) 0.0031(15) 0.0029(15) -0.0010(14) N18 0.032(2) 0.0217(19) 0.042(2) -0.0027(16) 0.0069(17) 0.0014(15) C1 0.037(3) 0.030(3) 0.040(3) -0.006(2) 0.001(2) -0.0037(19) C2 0.031(2) 0.045(3) 0.041(3) -0.012(2) -0.003(2) -0.003(2) C3 0.034(3) 0.046(3) 0.035(3) -0.006(2) -0.004(2) 0.004(2) C4 0.046(3) 0.039(3) 0.046(3) -0.013(2) -0.005(2) 0.011(2) C5 0.025(2) 0.024(2) 0.037(2) 0.0020(18) 0.0048(18) 0.0016(17) C6 0.032(2) 0.025(2) 0.036(3) -0.0001(19) 0.0039(19) 0.0027(18) C7 0.045(3) 0.028(2) 0.031(2) 0.0072(19) -0.003(2) 0.000(2) C8 0.048(3) 0.040(3) 0.042(3) 0.014(2) -0.008(2) -0.005(2) C9 0.039(3) 0.035(3) 0.040(3) 0.011(2) 0.003(2) 0.004(2) C10 0.033(3) 0.052(3) 0.039(3) 0.014(2) -0.007(2) 0.002(2) C11 0.032(2) 0.025(2) 0.035(2) 0.0015(18) -0.0011(19) 0.0035(18) C12 0.027(2) 0.030(2) 0.032(2) 0.0042(19) 0.0023(18) 0.0048(18) C13 0.038(3) 0.036(3) 0.036(3) 0.003(2) 0.007(2) 0.000(2) C14 0.048(3) 0.044(3) 0.040(3) 0.000(2) 0.017(2) 0.008(2) C15 0.039(3) 0.029(3) 0.044(3) -0.004(2) 0.012(2) 0.002(2) C16 0.042(3) 0.035(3) 0.042(3) 0.002(2) 0.013(2) -0.005(2) C17 0.023(2) 0.028(2) 0.038(3) 0.0013(19) 0.0059(18) 0.0011(17) C18 0.027(2) 0.024(2) 0.042(3) 0.0008(19) 0.0033(19) 0.0015(17) C19 0.033(2) 0.032(3) 0.040(3) -0.009(2) 0.006(2) -0.0017(19) C20 0.033(3) 0.036(3) 0.052(3) -0.009(2) -0.004(2) -0.001(2) C21 0.036(3) 0.038(3) 0.036(3) -0.007(2) -0.004(2) 0.005(2) C22 0.040(3) 0.029(3) 0.048(3) -0.011(2) 0.002(2) 0.007(2) C23 0.027(2) 0.021(2) 0.041(3) -0.0035(19) 0.0036(19) -0.0010(17) C24 0.029(2) 0.020(2) 0.039(3) -0.0032(18) 0.0041(19) 0.0001(16) C25 0.035(2) 0.034(3) 0.040(3) -0.002(2) 0.011(2) -0.003(2) C26 0.038(3) 0.025(2) 0.050(3) -0.002(2) 0.012(2) 0.0081(19) C27 0.028(2) 0.024(2) 0.038(3) -0.0030(18) 0.0075(18) 0.0021(17) C28 0.029(2) 0.027(2) 0.032(2) -0.0023(18) 0.0019(18) 0.0005(18) C29 0.033(2) 0.025(2) 0.036(3) -0.0032(19) 0.0005(19) 0.0002(18) C30 0.028(2) 0.034(3) 0.033(2) -0.0031(19) -0.0001(19) 0.0005(18) C31 0.035(2) 0.021(2) 0.035(2) 0.0013(18) 0.0040(19) -0.0001(18) C32 0.029(2) 0.028(2) 0.033(2) -0.0006(18) 0.0009(18) -0.0031(17) C33 0.026(2) 0.026(2) 0.036(3) 0.0002(18) 0.0000(18) 0.0013(17) C34 0.029(2) 0.028(2) 0.047(3) -0.001(2) 0.001(2) 0.0006(19) C35 0.036(3) 0.032(3) 0.065(4) 0.004(2) 0.004(2) 0.007(2) C36 0.032(2) 0.025(2) 0.053(3) -0.003(2) 0.005(2) -0.0040(18) C37 0.028(3) 0.020(3) 0.037(4) 0.000 0.003(3) 0.000 C38 0.025(2) 0.028(2) 0.039(3) 0.0010(19) 0.0009(18) -0.0001(17) C39 0.029(2) 0.021(2) 0.042(3) -0.0016(19) 0.0003(19) 0.0038(17) C40 0.025(3) 0.032(3) 0.030(3) 0.000 0.002(2) 0.000 C41 0.027(3) 0.017(3) 0.058(4) 0.000 0.000(3) 0.000 C42 0.023(2) 0.027(3) 0.066(4) -0.002(2) 0.002(2) 0.0049(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N5 1.930(4) . ? Co1 N1 1.934(4) . ? Co1 N3 1.935(4) . ? Co1 N7 1.936(4) . ? Co1 N9 1.937(4) . ? Co1 N11 1.942(4) . ? Co2 N15 1.939(4) 2_756 ? Co2 N15 1.939(4) . ? Co2 N13 1.942(4) 2_756 ? Co2 N13 1.942(4) . ? Co2 N17 1.946(4) 2_756 ? Co2 N17 1.946(4) . ? O1 C34 1.276(5) . ? O2 C34 1.263(6) . ? O3 C35 1.255(6) . ? O4 C35 1.255(6) . ? O5 C36 1.271(6) . ? O6 C36 1.256(6) . ? O7 C41 1.261(4) . ? O8 C42 1.249(6) . ? O9 C42 1.264(6) . ? N1 C5 1.349(5) . ? N1 C1 1.382(6) . ? N2 C5 1.334(6) . ? N2 C2 1.376(6) . ? N3 C6 1.350(6) . ? N3 C3 1.359(6) . ? N4 C6 1.342(6) . ? N4 C4 1.379(6) . ? N5 C11 1.340(6) . ? N5 C7 1.372(6) . ? N6 C11 1.332(6) . ? N6 C8 1.368(6) . ? N7 C12 1.344(6) . ? N7 C9 1.373(6) . ? N8 C12 1.333(6) . ? N8 C10 1.368(6) . ? N9 C17 1.342(6) . ? N9 C13 1.366(6) . ? N10 C17 1.343(6) . ? N10 C14 1.380(6) . ? N11 C18 1.345(6) . ? N11 C15 1.380(6) . ? N12 C18 1.331(6) . ? N12 C16 1.379(6) . ? N13 C23 1.345(5) . ? N13 C19 1.360(6) . ? N14 C23 1.335(6) . ? N14 C20 1.378(6) . ? N15 C24 1.330(5) . ? N15 C21 1.366(6) . ? N16 C24 1.345(6) . ? N16 C22 1.375(6) . ? N17 C27 1.328(6) . ? N17 C25 1.377(6) . ? N18 C27 1.335(6) . ? N18 C26 1.373(6) . ? C1 C2 1.365(7) . ? C3 C4 1.372(7) . ? C5 C6 1.434(6) . ? C7 C8 1.371(7) . ? C9 C10 1.376(7) . ? C11 C12 1.448(6) . ? C13 C14 1.383(7) . ? C15 C16 1.358(7) . ? C17 C18 1.443(6) . ? C19 C20 1.370(7) . ? C21 C22 1.377(6) . ? C23 C24 1.434(6) . ? C25 C26 1.377(7) . ? C27 C27 1.449(9) 2_756 ? C28 C29 1.395(6) . ? C28 C33 1.403(6) . ? C28 C34 1.505(6) . ? C29 C30 1.393(7) . ? C30 C31 1.395(6) . ? C30 C35 1.514(7) . ? C31 C32 1.399(6) . ? C32 C33 1.388(6) . ? C32 C36 1.501(6) . ? C37 C38 1.393(5) 2_656 ? C37 C38 1.393(5) . ? C37 C41 1.521(9) . ? C38 C39 1.396(6) . ? C39 C40 1.406(5) . ? C39 C42 1.503(6) . ? C40 C39 1.406(5) 2_656 ? C41 O7 1.261(4) 2_656 ? 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 N5 Co1 N1 93.03(15) . . ? N5 Co1 N3 89.46(16) . . ? N1 Co1 N3 83.43(16) . . ? N5 Co1 N7 83.27(15) . . ? N1 Co1 N7 174.81(15) . . ? N3 Co1 N7 92.87(16) . . ? N5 Co1 N9 92.92(16) . . ? N1 Co1 N9 93.53(16) . . ? N3 Co1 N9 176.24(16) . . ? N7 Co1 N9 90.30(16) . . ? N5 Co1 N11 174.79(15) . . ? N1 Co1 N11 90.69(15) . . ? N3 Co1 N11 94.59(16) . . ? N7 Co1 N11 93.25(15) . . ? N9 Co1 N11 83.21(16) . . ? N15 Co2 N15 89.6(2) 2_756 . ? N15 Co2 N13 83.18(15) 2_756 2_756 ? N15 Co2 N13 92.61(15) . 2_756 ? N15 Co2 N13 92.61(15) 2_756 . ? N15 Co2 N13 83.18(15) . . ? N13 Co2 N13 174.1(2) 2_756 . ? N15 Co2 N17 175.31(15) 2_756 2_756 ? N15 Co2 N17 93.86(15) . 2_756 ? N13 Co2 N17 93.53(15) 2_756 2_756 ? N13 Co2 N17 90.92(16) . 2_756 ? N15 Co2 N17 93.86(15) 2_756 . ? N15 Co2 N17 175.30(15) . . ? N13 Co2 N17 90.92(15) 2_756 . ? N13 Co2 N17 93.53(15) . . ? N17 Co2 N17 82.8(2) 2_756 . ? C5 N1 C1 106.3(4) . . ? C5 N1 Co1 113.5(3) . . ? C1 N1 Co1 140.2(3) . . ? C5 N2 C2 107.1(4) . . ? C6 N3 C3 106.4(4) . . ? C6 N3 Co1 113.1(3) . . ? C3 N3 Co1 140.1(3) . . ? C6 N4 C4 107.2(4) . . ? C11 N5 C7 106.5(4) . . ? C11 N5 Co1 113.8(3) . . ? C7 N5 Co1 139.3(3) . . ? C11 N6 C8 107.3(4) . . ? C12 N7 C9 106.2(4) . . ? C12 N7 Co1 113.5(3) . . ? C9 N7 Co1 140.3(3) . . ? C12 N8 C10 107.4(4) . . ? C17 N9 C13 107.2(4) . . ? C17 N9 Co1 113.5(3) . . ? C13 N9 Co1 139.2(3) . . ? C17 N10 C14 106.4(4) . . ? C18 N11 C15 106.4(4) . . ? C18 N11 Co1 113.4(3) . . ? C15 N11 Co1 140.1(3) . . ? C18 N12 C16 106.3(4) . . ? C23 N13 C19 106.9(4) . . ? C23 N13 Co2 113.0(3) . . ? C19 N13 Co2 140.1(3) . . ? C23 N14 C20 107.3(4) . . ? C24 N15 C21 106.9(4) . . ? C24 N15 Co2 113.3(3) . . ? C21 N15 Co2 139.5(3) . . ? C24 N16 C22 106.8(4) . . ? C27 N17 C25 106.7(4) . . ? C27 N17 Co2 113.5(3) . . ? C25 N17 Co2 139.6(3) . . ? C27 N18 C26 107.3(4) . . ? C2 C1 N1 108.0(4) . . ? C1 C2 N2 107.7(4) . . ? N3 C3 C4 109.2(4) . . ? C3 C4 N4 106.6(4) . . ? N2 C5 N1 110.9(4) . . ? N2 C5 C6 134.4(4) . . ? N1 C5 C6 114.7(4) . . ? N4 C6 N3 110.6(4) . . ? N4 C6 C5 134.1(4) . . ? N3 C6 C5 115.3(4) . . ? C8 C7 N5 107.9(4) . . ? N6 C8 C7 107.4(4) . . ? N7 C9 C10 108.2(4) . . ? N8 C10 C9 107.1(4) . . ? N6 C11 N5 110.9(4) . . ? N6 C11 C12 134.3(4) . . ? N5 C11 C12 114.7(4) . . ? N8 C12 N7 111.1(4) . . ? N8 C12 C11 134.2(4) . . ? N7 C12 C11 114.7(4) . . ? N9 C13 C14 107.5(4) . . ? N10 C14 C13 107.7(4) . . ? C16 C15 N11 107.5(4) . . ? C15 C16 N12 108.4(4) . . ? N9 C17 N10 111.1(4) . . ? N9 C17 C18 115.1(4) . . ? N10 C17 C18 133.8(4) . . ? N12 C18 N11 111.4(4) . . ? N12 C18 C17 133.8(4) . . ? N11 C18 C17 114.8(4) . . ? N13 C19 C20 108.6(4) . . ? C19 C20 N14 106.8(4) . . ? N15 C21 C22 108.2(4) . . ? N16 C22 C21 107.0(4) . . ? N14 C23 N13 110.4(4) . . ? N14 C23 C24 134.7(4) . . ? N13 C23 C24 114.9(4) . . ? N15 C24 N16 111.1(4) . . ? N15 C24 C23 115.6(4) . . ? N16 C24 C23 133.2(4) . . ? N17 C25 C26 107.8(4) . . ? N18 C26 C25 106.9(4) . . ? N17 C27 N18 111.2(4) . . ? N17 C27 C27 115.0(2) . 2_756 ? N18 C27 C27 133.7(3) . 2_756 ? C29 C28 C33 119.2(4) . . ? C29 C28 C34 120.5(4) . . ? C33 C28 C34 120.3(4) . . ? C30 C29 C28 120.5(4) . . ? C29 C30 C31 119.9(4) . . ? C29 C30 C35 120.1(4) . . ? C31 C30 C35 120.0(4) . . ? C30 C31 C32 120.1(4) . . ? C33 C32 C31 119.7(4) . . ? C33 C32 C36 119.9(4) . . ? C31 C32 C36 120.4(4) . . ? C32 C33 C28 120.7(4) . . ? O2 C34 O1 124.2(4) . . ? O2 C34 C28 118.1(4) . . ? O1 C34 C28 117.8(4) . . ? O3 C35 O4 124.6(5) . . ? O3 C35 C30 117.6(5) . . ? O4 C35 C30 117.8(5) . . ? O6 C36 O5 124.9(4) . . ? O6 C36 C32 117.6(4) . . ? O5 C36 C32 117.5(4) . . ? C38 C37 C38 119.7(6) 2_656 . ? C38 C37 C41 120.1(3) 2_656 . ? C38 C37 C41 120.1(3) . . ? C37 C38 C39 120.5(4) . . ? C38 C39 C40 119.8(4) . . ? C38 C39 C42 119.5(4) . . ? C40 C39 C42 120.7(4) . . ? C39 C40 C39 119.5(6) . 2_656 ? O7 C41 O7 125.8(6) 2_656 . ? O7 C41 C37 117.1(3) 2_656 . ? O7 C41 C37 117.1(3) . . ? O8 C42 O9 125.4(4) . . ? O8 C42 C39 117.5(4) . . ? O9 C42 C39 117.1(4) . . ? _diffrn_measured_fraction_theta_max 0.902 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.902 _refine_diff_density_max 1.022 _refine_diff_density_min -0.570 _refine_diff_density_rms 0.084 # Attachment 'CoTMART.cif' data_master_file_afc7*.xtl _database_code_depnum_ccdc_archive 'CCDC 286770' _audit_creation_date 'Fri Oct 14 15:42:20 2005' _audit_creation_method 'by teXsan' _audit_update_record ? _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (2000). teXsan. Single Crystal Structure Analysis Software. Version 1.11. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. ; #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C27 H67 Co N12 O29 ' _chemical_formula_moiety ? _chemical_formula_weight 1082.82 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,y,1/2-z -x,-y,-z x,-y,1/2+z 1/2+x,1/2+y,z 1/2-x,1/2+y,1/2-z 1/2-x,1/2-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 16.403(5) _cell_length_b 29.471(7) _cell_length_c 10.954(6) _cell_angle_alpha 90 _cell_angle_beta 90.24(3) _cell_angle_gamma 90 _cell_volume 5295(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 11.8 _cell_measurement_theta_max 14.7 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description prismatic _exptl_crystal_colour orange _exptl_crystal_size_max 0.490 _exptl_crystal_size_mid 0.280 _exptl_crystal_size_min 0.250 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.358 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.418 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.964 _exptl_absorpt_correction_T_max 0.999 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 5016 _diffrn_reflns_av_R_equivalents 0.044 _diffrn_reflns_theta_max 24.99 _diffrn_measured_fraction_theta_max 0.9991 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.9991 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 0 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 2.38 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 3.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 3.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 4648 _reflns_number_gt 2157 _reflns_threshold_expression F^2^>3.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0880 _refine_ls_wR_factor_ref 0.1304 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 2157 _refine_ls_number_parameters 257 _refine_ls_goodness_of_fit_ref 1.228 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.01000|Fo|^2^]' _refine_ls_shift/su_max 0.9941 _refine_diff_density_max 0.56 _refine_diff_density_min -0.41 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Co Co 0.349 0.972 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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(1) Co 0.5000 0.14414(5) 0.7500 0.0558(5) Uani 1.00 d S . . O(1) O 0.2845(4) -0.2144(2) 0.7308(8) 0.100(3) Uani 1.00 d . . . O(2) O 0.3491(4) -0.2710(3) 0.818(1) 0.130(4) Uani 1.00 d . . . O(3) O 0.5593(4) -0.0657(2) 0.7028(7) 0.084(2) Uani 1.00 d . . . O(4) O 0.724(1) -0.0578(6) 0.738(2) 0.248(7) Uiso 1.00 d . . . O(5) O 0.716(1) 0.0286(7) 0.844(2) 0.288(9) Uiso 1.00 d . . . O(6) O 0.812(3) -0.033(2) 0.540(5) 0.526(9) Uiso 1.00 d . . . O(7) O 0.828(6) -0.129(2) 0.796(8) 0.795(5) Uiso 1.00 d . . . O(8) O 0.868(4) -0.196(2) 0.603(6) 0.597(8) Uiso 1.00 d . . . O(9) O 0.751(2) 0.1426(8) 0.417(2) 0.305(9) Uiso 1.00 d . . . O(10) O 0.855(3) 0.154(2) 0.631(4) 0.546(8) Uiso 1.00 d . . . O(11) O 0.150(3) 0.044(2) -0.005(6) 0.623(6) Uiso 1.00 d . . . O(12) O 0.005(6) 0.067(4) 0.07(1) 0.957(3) Uiso 1.00 d . . . O(13) O 0.789(2) 0.082(1) 0.699(4) 0.46(1) Uiso 1.00 d . . . O(14) O 0.948(2) 0.158(1) 0.923(3) 0.43(1) Uiso 1.00 d . . . O(15) O 1.0000 -0.004(9) 0.7500 1.244(2) Uiso 1.00 d S . . N(1) N 0.5983(4) 0.1474(2) 0.8473(6) 0.061(2) Uani 1.00 d . . . N(2) N 0.7166(4) 0.1800(3) 0.8817(7) 0.074(2) Uani 1.00 d . . . N(3) N 0.5540(4) 0.1900(2) 0.6571(6) 0.060(2) Uani 1.00 d . . . N(4) N 0.6569(4) 0.2384(2) 0.6424(7) 0.072(2) Uani 1.00 d . . . N(5) N 0.5432(4) 0.0946(2) 0.6542(6) 0.061(2) Uani 1.00 d . . . N(6) N 0.5583(5) 0.0214(2) 0.6284(7) 0.071(2) Uani 1.00 d . . . C(1) C 0.6334(5) 0.1278(3) 0.9482(8) 0.069(3) Uani 1.00 d . . . C(2) C 0.7062(6) 0.1470(4) 0.9701(9) 0.083(3) Uani 1.00 d . . . C(3) C 0.5378(6) 0.2194(3) 0.5599(8) 0.072(3) Uani 1.00 d . . . C(4) C 0.6036(7) 0.2479(4) 0.5500(10) 0.089(4) Uani 1.00 d . . . C(5) C 0.6517(5) 0.1782(3) 0.8112(8) 0.062(3) Uani 1.00 d . . . C(6) C 0.6245(5) 0.2043(3) 0.7036(7) 0.059(2) Uani 1.00 d . . . C(7) C 0.5920(6) 0.0883(3) 0.5531(8) 0.076(3) Uani 1.00 d . . . C(8) C 0.6001(6) 0.0417(4) 0.5368(9) 0.083(3) Uani 1.00 d . . . C(9) C 0.5243(4) 0.0542(2) 0.6984(7) 0.054(2) Uani 1.00 d . . . C(10) C 0.5000 -0.1364(3) 0.7500 0.054(3) Uani 1.00 d S . . C(11) C 0.4275(5) -0.1601(3) 0.7570(8) 0.063(3) Uani 1.00 d . . . C(12) C 0.4266(5) -0.2072(3) 0.7587(8) 0.067(3) Uani 1.00 d . . . C(13) C 0.5000 -0.2320(4) 0.7500 0.065(4) Uani 1.00 d S . . C(14) C 0.3468(5) -0.2327(4) 0.769(1) 0.079(3) Uani 1.00 d . . . C(15) C 0.5000 -0.0858(5) 0.7500 0.068(4) Uani 1.00 d S . . H(1) H 0.6099 0.1040 0.9959 0.0852 Uiso 1.00 calc . . . H(2) H 0.7431 0.1394 1.0332 0.0992 Uiso 1.00 calc . . . H(3) H 0.4903 0.2190 0.5093 0.0867 Uiso 1.00 calc . . . H(4) H 0.6107 0.2701 0.4887 0.1085 Uiso 1.00 calc . . . H(5) H 0.7619 0.1997 0.8742 0.0907 Uiso 1.00 calc . . . H(6) H 0.7064 0.2522 0.6582 0.0909 Uiso 1.00 calc . . . H(7) H 0.6154 0.1114 0.5041 0.0931 Uiso 1.00 calc . . . H(8) H 0.6310 0.0267 0.4762 0.1007 Uiso 1.00 calc . . . H(9) H 0.5529 -0.0104 0.6418 0.0839 Uiso 1.00 calc . . . H(10) H 0.3788 -0.1436 0.7621 0.0732 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Co(1) 0.0546(9) 0.0519(10) 0.061(1) 0.0000 0.0017(7) 0.0000 O(1) 0.067(4) 0.079(5) 0.154(7) -0.015(4) -0.016(4) 0.012(5) O(2) 0.070(5) 0.094(6) 0.23(1) -0.018(4) -0.014(5) 0.043(6) O(3) 0.083(4) 0.056(4) 0.112(5) -0.010(3) 0.021(4) 0.002(4) N(1) 0.059(4) 0.062(4) 0.063(4) -0.001(3) 0.007(3) 0.013(3) N(2) 0.059(4) 0.083(5) 0.081(5) -0.011(4) -0.007(4) 0.020(4) N(3) 0.064(4) 0.057(4) 0.060(4) -0.004(3) -0.002(3) 0.004(3) N(4) 0.072(5) 0.063(4) 0.082(5) -0.013(4) -0.018(4) 0.020(4) N(5) 0.061(4) 0.061(4) 0.061(4) 0.003(3) 0.012(3) -0.001(3) N(6) 0.081(5) 0.056(4) 0.076(5) 0.003(4) 0.011(4) -0.003(4) C(1) 0.063(5) 0.078(6) 0.067(6) 0.002(5) 0.003(4) 0.014(5) C(2) 0.071(6) 0.103(8) 0.076(6) 0.008(6) -0.009(5) 0.026(6) C(3) 0.079(6) 0.071(6) 0.065(6) -0.005(5) -0.009(4) 0.008(5) C(4) 0.098(8) 0.085(7) 0.084(7) -0.023(6) -0.017(6) 0.027(6) C(5) 0.052(5) 0.070(5) 0.064(5) -0.001(4) 0.004(4) 0.000(4) C(6) 0.062(5) 0.054(5) 0.060(5) -0.008(4) -0.004(4) 0.008(4) C(7) 0.087(6) 0.072(6) 0.070(6) -0.009(5) 0.023(5) -0.001(5) C(8) 0.086(6) 0.084(7) 0.079(7) 0.009(5) 0.031(5) -0.003(5) C(9) 0.052(4) 0.049(5) 0.062(5) 0.001(3) 0.003(3) 0.002(4) C(10) 0.052(6) 0.041(6) 0.068(7) 0.0000 0.002(5) 0.0000 C(11) 0.064(5) 0.059(5) 0.066(5) 0.003(4) 0.004(4) -0.002(4) C(12) 0.070(5) 0.067(6) 0.064(5) -0.007(4) 0.002(4) 0.002(4) C(13) 0.064(7) 0.067(8) 0.065(8) 0.0000 0.012(6) 0.0000 C(14) 0.051(5) 0.066(6) 0.121(8) -0.009(5) -0.007(5) 0.004(6) C(15) 0.057(7) 0.070(8) 0.076(9) 0.0000 0.005(6) 0.0000 #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SHELXS97 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; 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(1) N(1) 1.931(7) . . yes Co(1) N(1) 1.931(7) . 2_656 yes Co(1) N(3) 1.912(7) . . yes Co(1) N(3) 1.912(7) . 2_656 yes Co(1) N(5) 1.935(7) . . yes Co(1) N(5) 1.935(7) . 2_656 yes O(1) C(14) 1.23(1) . . yes O(2) C(14) 1.25(1) . . yes O(3) C(15) 1.252(8) . . yes N(1) C(1) 1.37(1) . . yes N(1) C(5) 1.33(1) . . yes N(2) C(2) 1.38(1) . . yes N(2) C(5) 1.31(1) . . yes N(2) H(5) 0.948 . . no N(3) C(3) 1.40(1) . . yes N(3) C(6) 1.33(1) . . yes N(4) C(4) 1.36(1) . . yes N(4) C(6) 1.32(1) . . yes N(4) H(6) 0.924 . . no N(5) C(7) 1.38(1) . . yes N(5) C(9) 1.321(9) . . yes N(6) C(8) 1.36(1) . . yes N(6) C(9) 1.355(10) . . yes N(6) H(9) 0.954 . . no C(1) C(2) 1.34(1) . . yes C(1) H(1) 0.957 . . no C(2) H(2) 0.944 . . no C(3) C(4) 1.37(1) . . yes C(3) H(3) 0.955 . . no C(4) H(4) 0.944 . . no C(5) C(6) 1.47(1) . . yes C(7) C(8) 1.39(1) . . yes C(7) H(7) 0.950 . . no C(8) H(8) 0.946 . . no C(9) C(9) 1.39(1) . 2_656 yes C(10) C(11) 1.381(10) . . yes C(10) C(11) 1.381(10) . 2_656 yes C(10) C(15) 1.49(2) . . yes C(11) C(12) 1.39(1) . . yes C(11) H(10) 0.938 . . no C(12) C(13) 1.41(1) . . yes C(12) C(14) 1.51(1) . . 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 N(1) Co(1) N(1) 174.3(4) . . 2_656 yes N(1) Co(1) N(3) 82.6(3) . . . yes N(1) Co(1) N(3) 93.3(3) . . 2_656 yes N(1) Co(1) N(5) 91.7(3) . . . yes N(1) Co(1) N(5) 92.6(3) . . 2_656 yes N(1) Co(1) N(3) 93.3(3) 2_656 . . yes N(1) Co(1) N(3) 82.6(3) 2_656 . 2_656 yes N(1) Co(1) N(5) 92.6(3) 2_656 . . yes N(1) Co(1) N(5) 91.7(3) 2_656 . 2_656 yes N(3) Co(1) N(3) 89.9(4) . . 2_656 yes N(3) Co(1) N(5) 94.2(3) . . . yes N(3) Co(1) N(5) 173.8(3) . . 2_656 yes N(3) Co(1) N(5) 173.8(3) 2_656 . . yes N(3) Co(1) N(5) 94.2(3) 2_656 . 2_656 yes N(5) Co(1) N(5) 81.9(4) . . 2_656 yes Co(1) N(1) C(1) 140.4(6) . . . yes Co(1) N(1) C(5) 114.9(5) . . . yes C(1) N(1) C(5) 104.7(7) . . . yes C(2) N(2) C(5) 106.4(7) . . . yes C(2) N(2) H(5) 126.2 . . . no C(5) N(2) H(5) 127.4 . . . no Co(1) N(3) C(3) 139.3(6) . . . yes Co(1) N(3) C(6) 115.1(5) . . . yes C(3) N(3) C(6) 104.9(7) . . . yes C(4) N(4) C(6) 106.0(7) . . . yes C(4) N(4) H(6) 127.4 . . . no C(6) N(4) H(6) 126.6 . . . no Co(1) N(5) C(7) 138.6(6) . . . yes Co(1) N(5) C(9) 113.2(5) . . . yes C(7) N(5) C(9) 108.1(7) . . . yes C(8) N(6) C(9) 108.3(7) . . . yes C(8) N(6) H(9) 126.5 . . . no C(9) N(6) H(9) 125.2 . . . no N(1) C(1) C(2) 109.7(8) . . . yes N(1) C(1) H(1) 125.5 . . . no C(2) C(1) H(1) 124.8 . . . no N(2) C(2) C(1) 106.4(8) . . . yes N(2) C(2) H(2) 126.7 . . . no C(1) C(2) H(2) 126.8 . . . no N(3) C(3) C(4) 107.1(8) . . . yes N(3) C(3) H(3) 125.8 . . . no C(4) C(3) H(3) 127.1 . . . no N(4) C(4) C(3) 108.5(8) . . . yes N(4) C(4) H(4) 126.1 . . . no C(3) C(4) H(4) 125.4 . . . no N(1) C(5) N(2) 112.7(7) . . . yes N(1) C(5) C(6) 113.5(7) . . . yes N(2) C(5) C(6) 133.7(8) . . . yes N(3) C(6) N(4) 113.4(7) . . . yes N(3) C(6) C(5) 113.6(7) . . . yes N(4) C(6) C(5) 133.0(8) . . . yes N(5) C(7) C(8) 106.9(8) . . . yes N(5) C(7) H(7) 126.4 . . . no C(8) C(7) H(7) 126.7 . . . no N(6) C(8) C(7) 106.9(8) . . . yes N(6) C(8) H(8) 126.0 . . . no C(7) C(8) H(8) 127.0 . . . no N(5) C(9) N(6) 109.7(7) . . . yes N(5) C(9) C(9) 115.8(4) . . 2_656 yes N(6) C(9) C(9) 134.5(4) . . 2_656 yes C(11) C(10) C(11) 119(1) . . 2_656 yes C(11) C(10) C(15) 120.4(5) . . . yes C(11) C(10) C(15) 120.4(5) 2_656 . . yes C(10) C(11) C(12) 121.1(8) . . . yes C(10) C(11) H(10) 118.4 . . . no C(12) C(11) H(10) 120.5 . . . no C(11) C(12) C(13) 120.4(8) . . . yes C(11) C(12) C(14) 120.4(8) . . . yes C(13) C(12) C(14) 119.1(9) . . . yes C(12) C(13) C(12) 117(1) . . 2_656 yes O(1) C(14) O(2) 124.6(9) . . . yes O(1) C(14) C(12) 118.2(9) . . . yes O(2) C(14) C(12) 117.1(8) . . . yes O(3) C(15) O(3) 123(1) . . 2_656 yes O(3) C(15) C(10) 118.2(6) . . . yes O(3) C(15) C(10) 118.2(6) 2_656 . . yes #------------------------------------------------------------------------------ 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Co(1) N(1) C(1) C(2) -179.1(7) . . . . yes Co(1) N(1) C(5) N(2) 178.4(6) . . . . yes Co(1) N(1) C(5) C(6) 0.6(9) . . . . yes Co(1) N(1) C(1) C(2) -179.1(7) . 2_656 2_656 2_656 yes Co(1) N(1) C(5) N(2) 178.4(6) . 2_656 2_656 2_656 yes Co(1) N(1) C(5) C(6) 0.6(9) . 2_656 2_656 2_656 yes Co(1) N(3) C(3) C(4) 172.6(8) . . . . yes Co(1) N(3) C(6) N(4) -175.0(6) . . . . yes Co(1) N(3) C(6) C(5) 6.3(9) . . . . yes Co(1) N(3) C(3) C(4) 172.6(8) . 2_656 2_656 2_656 yes Co(1) N(3) C(6) N(4) -175.0(6) . 2_656 2_656 2_656 yes Co(1) N(3) C(6) C(5) 6.3(9) . 2_656 2_656 2_656 yes Co(1) N(5) C(7) C(8) 178.1(7) . . . . yes Co(1) N(5) C(9) N(6) -178.5(5) . . . . yes Co(1) N(5) C(9) C(9) 1(1) . . . 2_656 yes Co(1) N(5) C(7) C(8) 178.1(7) . 2_656 2_656 2_656 yes Co(1) N(5) C(9) N(6) -178.5(5) . 2_656 2_656 2_656 yes Co(1) N(5) C(9) C(9) 1(1) . 2_656 2_656 . yes O(1) C(14) C(12) C(11) 27(1) . . . . yes O(1) C(14) C(12) C(13) -152.4(9) . . . . yes O(2) C(14) C(12) C(11) -151(1) . . . . yes O(2) C(14) C(12) C(13) 28(1) . . . . yes O(3) C(15) C(10) C(11) -155.8(6) . . . . yes O(3) C(15) C(10) C(11) 24.2(6) . . . 2_656 yes N(1) Co(1) N(1) C(1) 136.2(9) . . 2_656 2_656 yes N(1) Co(1) N(1) C(5) -42.8(6) . . 2_656 2_656 yes N(1) Co(1) N(3) C(3) -172.9(9) . . . . yes N(1) Co(1) N(3) C(6) -4.8(6) . . . . yes N(1) Co(1) N(3) C(3) 3.1(9) . . 2_656 2_656 yes N(1) Co(1) N(3) C(6) 171.1(6) . . 2_656 2_656 yes N(1) Co(1) N(5) C(7) -85.0(9) . . . . yes N(1) Co(1) N(5) C(9) 91.7(6) . . . . yes N(1) Co(1) N(5) C(7) 91.2(9) . . 2_656 2_656 yes N(1) Co(1) N(5) C(9) -92.0(6) . . 2_656 2_656 yes N(1) C(1) C(2) N(2) 0(1) . . . . yes N(1) C(5) N(2) C(2) 1(1) . . . . yes N(1) C(5) C(6) N(3) -4(1) . . . . yes N(1) C(5) C(6) N(4) 177.2(9) . . . . yes N(2) C(5) N(1) C(1) -0.9(10) . . . . yes N(2) C(5) C(6) N(3) 178.3(9) . . . . yes N(2) C(5) C(6) N(4) 0(1) . . . . yes N(3) Co(1) N(1) C(1) -178.9(10) . . . . yes N(3) Co(1) N(1) C(5) 2.2(6) . . . . yes N(3) Co(1) N(1) C(1) 91.6(9) . . 2_656 2_656 yes N(3) Co(1) N(1) C(5) -87.3(6) . . 2_656 2_656 yes N(3) Co(1) N(3) C(3) -79.5(9) . . 2_656 2_656 yes N(3) Co(1) N(3) C(6) 88.5(6) . . 2_656 2_656 yes N(3) Co(1) N(5) C(7) -2.3(10) . . . . yes N(3) Co(1) N(5) C(9) 174.5(6) . . . . yes N(3) Co(1) N(5) C(7) 130(2) . . 2_656 2_656 yes N(3) Co(1) N(5) C(9) -52(2) . . 2_656 2_656 yes N(3) C(3) C(4) N(4) -3(1) . . . . yes N(3) C(6) N(4) C(4) 1(1) . . . . yes N(4) C(6) N(3) C(3) -3(1) . . . . yes N(5) Co(1) N(1) C(1) -84.8(9) . . . . yes N(5) Co(1) N(1) C(5) 96.3(6) . . . . yes N(5) Co(1) N(1) C(1) -2.8(9) . . 2_656 2_656 yes N(5) Co(1) N(1) C(5) 178.3(6) . . 2_656 2_656 yes N(5) Co(1) N(3) C(3) 96.0(9) . . . . yes N(5) Co(1) N(3) C(6) -96.0(6) . . . . yes N(5) Co(1) N(3) C(3) 147(2) . . 2_656 2_656 yes N(5) Co(1) N(3) C(6) -44(2) . . 2_656 2_656 yes N(5) Co(1) N(5) C(7) -177(1) . . 2_656 2_656 yes N(5) Co(1) N(5) C(9) -0.6(4) . . 2_656 2_656 yes N(5) C(7) C(8) N(6) -1(1) . . . . yes N(5) C(9) N(6) C(8) 0.0(10) . . . . yes N(5) C(9) C(9) N(5) -2(1) . . 2_656 2_656 yes N(5) C(9) C(9) N(6) 178.0(7) . . 2_656 2_656 yes N(6) C(9) N(5) C(7) -0.8(9) . . . . yes N(6) C(9) C(9) N(6) -1(2) . . 2_656 2_656 yes C(1) N(1) C(5) C(6) -178.7(7) . . . . yes C(1) C(2) N(2) C(5) -1(1) . . . . yes C(2) N(2) C(5) C(6) 178.7(9) . . . . yes C(2) C(1) N(1) C(5) 0(1) . . . . yes C(3) N(3) C(6) C(5) 178.3(7) . . . . yes C(3) C(4) N(4) C(6) 1(1) . . . . yes C(4) N(4) C(6) C(5) 179.3(10) . . . . yes C(4) C(3) N(3) C(6) 3(1) . . . . yes C(7) N(5) C(9) C(9) 179.5(9) . . . 2_656 yes C(7) C(8) N(6) C(9) 0(1) . . . . yes C(8) N(6) C(9) C(9) 179(1) . . . 2_656 yes C(8) C(7) N(5) C(9) 1(1) . . . . yes C(10) C(11) C(12) C(13) -1(1) . . . . yes C(10) C(11) C(12) C(14) 178.6(8) . . . . yes C(10) C(11) C(12) C(13) -1(1) . 2_656 2_656 . yes C(10) C(11) C(12) C(14) 178.6(8) . 2_656 2_656 2_656 yes C(11) C(10) C(11) C(12) 0.8(6) . . 2_656 2_656 yes C(11) C(12) C(13) C(12) 0.8(6) . . . 2_656 yes C(12) C(11) C(10) C(15) -179.2(6) . . . . yes C(12) C(13) C(12) C(14) -179.4(9) . . 2_656 2_656 yes C(12) C(13) C(12) C(14) -179.4(9) . . 2_656 2_656 yes #------------------------------------------------------------------------------ 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 O(1) N(4) 2.690(10) . 5_445 ? O(1) O(9) 2.73(3) . 3_656 ? O(1) O(7) 3.15(8) . 2_656 ? O(1) O(8) 3.15(6) . 2_656 ? O(1) C(6) 3.564(10) . 5_445 ? O(2) N(2) 2.703(10) . 5_445 ? O(2) O(14) 2.89(4) . 5_445 ? O(2) O(10) 3.03(5) . 5_445 ? O(2) O(8) 3.28(6) . 8_445 ? O(2) C(5) 3.57(1) . 5_445 ? O(3) N(6) 2.693(9) . . ? O(3) O(4) 2.74(2) . . ? O(3) C(1) 3.55(1) . 4_554 ? O(3) C(9) 3.581(9) . . ? O(4) O(6) 2.71(5) . . ? O(4) O(7) 2.77(8) . . ? O(4) O(5) 2.80(3) . . ? O(4) O(9) 3.21(3) . 4_555 ? O(4) O(11) 3.59(7) . 3_656 ? O(5) O(13) 2.55(4) . . ? O(5) O(6) 2.66(6) . 4_555 ? O(5) C(1) 3.42(2) . . ? O(5) N(6) 3.50(2) . . ? O(5) C(8) 3.52(2) . 4_555 ? O(5) O(11) 3.54(7) . 3_656 ? O(5) C(9) 3.59(2) . . ? O(6) O(12) 3.3(1) . 4_655 ? O(7) O(8) 2.97(9) . . ? O(7) O(11) 3.4(1) . 3_656 ? O(7) O(12) 3.6(1) . 3_656 ? O(8) O(14) 2.62(6) . 4_554 ? O(8) C(2) 3.35(6) . 4_554 ? O(8) N(4) 3.42(6) . 6_646 ? O(8) N(2) 3.50(6) . 4_554 ? O(9) O(10) 2.91(5) . . ? O(9) C(7) 3.41(3) . . ? O(9) O(11) 3.45(7) . 2_655 ? O(9) C(11) 3.53(3) . 3_656 ? O(10) O(14) 3.28(7) . 2_756 ? O(10) O(11) 3.51(8) . 2_655 ? O(10) O(14) 3.54(6) . . ? O(10) C(4) 3.57(5) . 7_656 ? O(11) O(13) 2.60(6) . 2_655 ? O(11) O(12) 2.63(9) . . ? O(12) O(15) 2.7(2) . 3_656 ? O(12) O(14) 3.3(1) . 1_454 ? N(2) C(14) 3.57(1) . 5_555 ? N(4) C(14) 3.51(1) . 5_555 ? N(6) C(15) 3.56(1) . . ? C(1) C(11) 3.52(1) . 3_657 ? C(3) C(13) 3.468(9) . 3_656 ? C(3) C(12) 3.56(1) . 3_656 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ # Attachment 'CoTMART(SOUEEZE).cif' data_shelxl _database_code_depnum_ccdc_archive 'CCDC 292075' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H67 Co N12 O29' _chemical_formula_weight 1082.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co .3494 .9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 16.403(5) _cell_length_b 29.471(7) _cell_length_c 10.954(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.24(3) _cell_angle_gamma 90.00 _cell_volume 5295(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 11.8 _cell_measurement_theta_max 14.7 _exptl_crystal_description prismatic _exptl_crystal_colour orange _exptl_crystal_size_max 0.490 _exptl_crystal_size_mid 0.280 _exptl_crystal_size_min 0.250 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.358 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2288 _exptl_absorpt_coefficient_mu 0.418 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.964 _exptl_absorpt_correction_T_max 0.999 _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4917 _diffrn_reflns_av_R_equivalents 0.0447 _diffrn_reflns_av_sigmaI/netI 0.0850 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 24.99 _reflns_number_total 4648 _reflns_number_gt 2251 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'teXsan Ver. 1.11' _computing_publication_material 'teXsan Ver. 1.11' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0919P)^2^+0.0000P] 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 4648 _refine_ls_number_parameters 210 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1126 _refine_ls_R_factor_gt 0.0543 _refine_ls_wR_factor_ref 0.1571 _refine_ls_wR_factor_gt 0.1455 _refine_ls_goodness_of_fit_ref 0.859 _refine_ls_restrained_S_all 0.859 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.5000 0.14403(2) 0.7500 0.0604(2) Uani 1 2 d S . . O1 O 0.28466(17) -0.21465(10) 0.7294(3) 0.1042(10) Uani 1 1 d . . . O2 O 0.34900(17) -0.27136(11) 0.8177(4) 0.1322(14) Uani 1 1 d . . . O3 O 0.55982(16) -0.06547(8) 0.7030(2) 0.0844(8) Uani 1 1 d . . . N1 N 0.59755(16) 0.14746(9) 0.8485(2) 0.0625(7) Uani 1 1 d . . . N2 N 0.71669(18) 0.17993(10) 0.8814(3) 0.0760(8) Uani 1 1 d . . . H2 H 0.7581 0.1976 0.8735 0.091 Uiso 0.50 1 calc PR . . N3 N 0.55373(17) 0.19014(9) 0.6564(2) 0.0609(7) Uani 1 1 d . . . N4 N 0.65680(19) 0.23882(10) 0.6432(3) 0.0750(8) Uani 1 1 d . . . H4 H 0.7019 0.2526 0.6584 0.090 Uiso 0.50 1 calc PR . . N5 N 0.54348(17) 0.09542(9) 0.6539(3) 0.0621(7) Uani 1 1 d . . . N6 N 0.55789(18) 0.02120(10) 0.6290(3) 0.0735(8) Uani 1 1 d . . . H6 H 0.5529 -0.0075 0.6401 0.088 Uiso 0.50 1 calc PR . . C1 C 0.6321(2) 0.12812(13) 0.9490(3) 0.0717(10) Uani 1 1 d . . . H1 H 0.6090 0.1052 0.9957 0.086 Uiso 1 1 calc R . . C2 C 0.7055(2) 0.14767(14) 0.9701(4) 0.0866(12) Uani 1 1 d . . . H2A H 0.7416 0.1406 1.0329 0.104 Uiso 1 1 calc R . . C3 C 0.5381(3) 0.21840(13) 0.5606(3) 0.0773(10) Uani 1 1 d . . . H3 H 0.4923 0.2178 0.5103 0.093 Uiso 1 1 calc R . . C4 C 0.6026(3) 0.24797(15) 0.5521(4) 0.0957(14) Uani 1 1 d . . . H4A H 0.6083 0.2706 0.4935 0.115 Uiso 1 1 calc R . . C5 C 0.6512(2) 0.17861(12) 0.8103(3) 0.0636(9) Uani 1 1 d . . . C6 C 0.6250(2) 0.20383(11) 0.7038(3) 0.0623(8) Uani 1 1 d . . . C7 C 0.5924(2) 0.08846(13) 0.5544(3) 0.0764(10) Uani 1 1 d . . . H7 H 0.6156 0.1110 0.5064 0.092 Uiso 1 1 calc R . . C8 C 0.6013(2) 0.04221(14) 0.5374(3) 0.0819(11) Uani 1 1 d . . . H8 H 0.6309 0.0280 0.4761 0.098 Uiso 1 1 calc R . . C9 C 0.52513(19) 0.05404(11) 0.6970(3) 0.0610(8) Uani 1 1 d . . . C10 C 0.5000 -0.13628(15) 0.7500 0.0602(12) Uani 1 2 d S . . C11 C 0.4280(2) -0.16028(12) 0.7585(3) 0.0654(9) Uani 1 1 d . . . H11 H 0.3789 -0.1446 0.7635 0.079 Uiso 1 1 calc R . . C12 C 0.4274(2) -0.20742(12) 0.7596(3) 0.0653(9) Uani 1 1 d . . . C13 C 0.5000 -0.23073(17) 0.7500 0.0672(13) Uani 1 2 d S . . H13 H 0.5000 -0.2623 0.7500 0.081 Uiso 1 2 calc SR . . C14 C 0.3479(2) -0.23290(15) 0.7699(4) 0.0826(11) Uani 1 1 d . . . C15 C 0.5000 -0.08597(18) 0.7500 0.0681(13) Uani 1 2 d S . . 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 0.0580(4) 0.0564(4) 0.0669(4) 0.000 0.0016(3) 0.000 O1 0.0640(17) 0.089(2) 0.159(3) 0.0080(19) -0.0092(18) -0.0142(15) O2 0.076(2) 0.092(2) 0.229(4) 0.049(3) -0.001(2) -0.0170(17) O3 0.0830(18) 0.0602(15) 0.110(2) 0.0014(14) 0.0211(15) -0.0039(13) N1 0.0646(16) 0.0598(16) 0.0632(17) 0.0043(15) 0.0028(14) -0.0018(15) N2 0.0650(19) 0.080(2) 0.082(2) 0.0188(18) -0.0116(16) -0.0069(16) N3 0.0669(18) 0.0559(17) 0.0599(17) 0.0067(14) -0.0052(14) -0.0068(14) N4 0.079(2) 0.0701(19) 0.076(2) 0.0197(16) -0.0150(17) -0.0099(16) N5 0.0654(18) 0.0592(17) 0.0618(18) 0.0019(13) 0.0119(14) -0.0032(13) N6 0.077(2) 0.0654(19) 0.078(2) -0.0077(16) 0.0199(16) 0.0024(15) C1 0.070(2) 0.076(2) 0.069(2) 0.0151(19) -0.0026(19) 0.0030(19) C2 0.080(3) 0.100(3) 0.079(3) 0.022(2) -0.017(2) 0.002(2) C3 0.086(3) 0.076(3) 0.070(2) 0.005(2) -0.013(2) -0.007(2) C4 0.108(3) 0.095(3) 0.084(3) 0.033(2) -0.016(3) -0.026(3) C5 0.055(2) 0.065(2) 0.071(2) 0.0096(18) -0.0035(17) -0.0037(17) C6 0.061(2) 0.060(2) 0.065(2) 0.0085(17) -0.0006(17) -0.0082(17) C7 0.082(3) 0.074(3) 0.073(2) 0.000(2) 0.020(2) -0.006(2) C8 0.090(3) 0.082(3) 0.074(3) -0.006(2) 0.026(2) 0.002(2) C9 0.056(2) 0.064(2) 0.063(2) 0.0029(17) 0.0072(15) 0.0036(16) C10 0.065(3) 0.048(3) 0.068(3) 0.000 0.005(2) 0.000 C11 0.060(2) 0.065(2) 0.071(2) 0.0002(18) 0.0058(17) -0.0015(17) C12 0.069(2) 0.062(2) 0.065(2) 0.0014(17) 0.0023(17) -0.0042(18) C13 0.065(3) 0.058(3) 0.079(3) 0.000 -0.002(3) 0.000 C14 0.057(2) 0.075(3) 0.116(3) 0.002(2) -0.005(2) -0.012(2) C15 0.063(3) 0.068(3) 0.073(3) 0.000 0.001(3) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N5 1.917(3) 2_656 ? Co1 N5 1.917(3) . ? Co1 N3 1.919(3) . ? Co1 N3 1.919(3) 2_656 ? Co1 N1 1.929(3) 2_656 ? Co1 N1 1.929(3) . ? O1 C14 1.249(4) . ? O2 C14 1.248(5) . ? O3 C15 1.264(3) . ? N1 C5 1.340(4) . ? N1 C1 1.361(4) . ? N2 C5 1.325(4) . ? N2 C2 1.372(5) . ? N3 C6 1.339(4) . ? N3 C3 1.364(4) . ? N4 C6 1.334(4) . ? N4 C4 1.361(5) . ? N5 C9 1.342(4) . ? N5 C7 1.371(4) . ? N6 C9 1.336(4) . ? N6 C8 1.379(4) . ? C1 C2 1.354(5) . ? C3 C4 1.374(5) . ? C5 C6 1.447(5) . ? C7 C8 1.384(5) . ? C9 C9 1.427(6) 2_656 ? C10 C11 1.381(4) . ? C10 C11 1.381(4) 2_656 ? C10 C15 1.483(7) . ? C11 C12 1.389(5) . ? C12 C13 1.379(4) . ? C12 C14 1.509(5) . ? C13 C12 1.379(4) 2_656 ? C15 O3 1.264(3) 2_656 ? 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 N5 Co1 N5 83.29(16) 2_656 . ? N5 Co1 N3 174.45(12) 2_656 . ? N5 Co1 N3 93.61(12) . . ? N5 Co1 N3 93.62(12) 2_656 2_656 ? N5 Co1 N3 174.45(12) . 2_656 ? N3 Co1 N3 89.83(16) . 2_656 ? N5 Co1 N1 92.10(12) 2_656 2_656 ? N5 Co1 N1 92.38(12) . 2_656 ? N3 Co1 N1 92.62(12) . 2_656 ? N3 Co1 N1 83.11(12) 2_656 2_656 ? N5 Co1 N1 92.38(12) 2_656 . ? N5 Co1 N1 92.11(12) . . ? N3 Co1 N1 83.11(12) . . ? N3 Co1 N1 92.62(12) 2_656 . ? N1 Co1 N1 173.99(17) 2_656 . ? C5 N1 C1 105.5(3) . . ? C5 N1 Co1 113.9(2) . . ? C1 N1 Co1 140.5(3) . . ? C5 N2 C2 106.6(3) . . ? C6 N3 C3 106.0(3) . . ? C6 N3 Co1 114.1(2) . . ? C3 N3 Co1 139.3(3) . . ? C6 N4 C4 105.2(3) . . ? C9 N5 C7 106.1(3) . . ? C9 N5 Co1 113.7(2) . . ? C7 N5 Co1 140.2(3) . . ? C9 N6 C8 106.9(3) . . ? C2 C1 N1 109.1(3) . . ? C1 C2 N2 107.2(3) . . ? N3 C3 C4 107.3(3) . . ? N4 C4 C3 109.0(4) . . ? N2 C5 N1 111.6(3) . . ? N2 C5 C6 134.1(3) . . ? N1 C5 C6 114.3(3) . . ? N4 C6 N3 112.5(3) . . ? N4 C6 C5 133.1(3) . . ? N3 C6 C5 114.4(3) . . ? N5 C7 C8 108.5(3) . . ? N6 C8 C7 106.8(3) . . ? N6 C9 N5 111.8(3) . . ? N6 C9 C9 133.56(19) . 2_656 ? N5 C9 C9 114.67(18) . 2_656 ? C11 C10 C11 118.4(4) . 2_656 ? C11 C10 C15 120.8(2) . . ? C11 C10 C15 120.8(2) 2_656 . ? C10 C11 C12 121.2(4) . . ? C13 C12 C11 119.5(3) . . ? C13 C12 C14 120.3(3) . . ? C11 C12 C14 120.3(3) . . ? C12 C13 C12 120.2(5) . 2_656 ? O2 C14 O1 123.4(4) . . ? O2 C14 C12 118.2(4) . . ? O1 C14 C12 118.4(4) . . ? O3 C15 O3 122.9(5) 2_656 . ? O3 C15 C10 118.6(2) 2_656 . ? O3 C15 C10 118.6(2) . . ? _diffrn_measured_fraction_theta_max .999 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full .999 _refine_diff_density_max .188 _refine_diff_density_min -.273 _refine_diff_density_rms .051