Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Barbara Sieklucka' 'Rafal Kania' 'Krzysztof Lewinski' _publ_contact_author_name 'Dr Barbara Sieklucka' _publ_contact_author_address ; Faculty of Chemistry Jagiellonian University Ingardena 3 Krakow 30-060 POLAND ; _publ_contact_author_email SIEKLUCK@CHEMIA.UJ.EDU.PL _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Self-assembly of tetranuclear {[Co(N4)]2[W(CN)8]2}2- square of alternating aliphatic tetramine Co(III) and octacyanotungstate(IV) corners ; data_kco _database_code_CSD 196411 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety '(C6 H18 N4 Co 3+)2, (C8 N8 W 4+)2, (K 1+)2, (H2 O)9' _chemical_formula_sum 'C28 H54 N24 O9 Co2 K2 W2' _chemical_formula_weight 1434.72 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source K K 0.2009 0.2494 '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' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 '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' H H 0.0000 0.0000 '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 11.7830(2) _cell_length_b 13.0640(2) _cell_length_c 16.4650(2) _cell_angle_alpha 84.7700(8) _cell_angle_beta 83.4290(7) _cell_angle_gamma 88.5950(6) _cell_volume 2507.12(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour 'dark violet' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.901 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1404 _exptl_absorpt_coefficient_mu 5.460 _exptl_absorpt_correction_type 'multi-scan (DENZO-SMN; Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.4081 _exptl_absorpt_correction_T_max 0.6113 _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 'Nonius KappaCCD' _diffrn_measurement_method '\f and \w scans with the \k offsets' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21401 _diffrn_reflns_av_R_equivalents 0.0876 _diffrn_reflns_av_sigmaI/netI 0.0974 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.25 _diffrn_reflns_theta_max 29.66 _reflns_number_total 14037 _reflns_number_gt 11087 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius BV, 1997-2000)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.1312P)^2^+50.6314P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0013(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 14037 _refine_ls_number_parameters 605 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1182 _refine_ls_R_factor_gt 0.0978 _refine_ls_wR_factor_ref 0.2745 _refine_ls_wR_factor_gt 0.2612 _refine_ls_goodness_of_fit_ref 1.142 _refine_ls_restrained_S_all 1.142 _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 W1 W 0.23449(4) 0.70579(3) 0.06396(3) 0.02373(16) Uani 1 d . . . W2 W 0.23902(4) 0.29387(3) 0.44774(3) 0.02526(16) Uani 1 d . . . Co1 Co 0.24634(14) 0.31467(13) 0.13045(10) 0.0263(3) Uani 1 d . . . Co2 Co 0.27379(15) 0.68691(13) 0.37510(10) 0.0274(3) Uani 1 d . . . K1 K 0.1772(5) 0.0520(4) 0.7989(4) 0.0749(13) Uani 1 d . . . K2 K 0.1743(9) 0.4669(6) 0.7875(5) 0.129(3) Uani 1 d . . . O1 O 0.3836(15) 0.0424(17) 0.8641(16) 0.113(8) Uani 1 d . . . O2 O 0.0977(16) -0.0427(16) 0.6735(12) 0.092(5) Uani 1 d . . . O3 O 0.185(3) 0.2570(18) 0.7730(14) 0.156(12) Uani 1 d . . . O4 O 0.3643(17) -0.0504(17) 0.6766(16) 0.122(8) Uani 1 d . . . O5 O 0.0835(16) 0.6562(16) 0.7249(10) 0.088(5) Uani 1 d . . . O6 O 0.4327(17) 0.4188(17) 0.7809(11) 0.098(6) Uani 1 d . . . O7 O -0.0284(17) 0.4437(16) 0.7169(14) 0.107(7) Uani 1 d . . . C11 C 0.2577(11) 0.6919(9) 0.1908(7) 0.028(2) Uani 1 d . . . N11 N 0.2745(10) 0.6887(9) 0.2592(6) 0.032(2) Uani 1 d . . . C12 C 0.0622(13) 0.6667(15) 0.0512(9) 0.049(4) Uani 1 d . . . N12 N -0.0276(13) 0.6405(13) 0.0416(13) 0.067(5) Uani 1 d . . . C13 C 0.3431(13) 0.8331(11) 0.0762(9) 0.039(3) Uani 1 d . . . N13 N 0.4039(15) 0.8985(13) 0.0831(13) 0.066(5) Uani 1 d . . . C14 C 0.4091(13) 0.6564(16) 0.0548(8) 0.052(5) Uani 1 d . . . N14 N 0.5006(11) 0.6206(13) 0.0510(10) 0.052(3) Uani 1 d . . . C15 C 0.1157(13) 0.8152(13) 0.1202(11) 0.046(4) Uani 1 d . . . N15 N 0.0543(17) 0.8710(16) 0.1513(15) 0.088(7) Uani 1 d . . . C16 C 0.2110(17) 0.8143(15) -0.0384(10) 0.055(4) Uani 1 d . . . N16 N 0.199(2) 0.8722(17) -0.0956(14) 0.101(8) Uani 1 d . . . C17 C 0.2585(15) 0.6226(14) -0.0460(9) 0.047(4) Uani 1 d . . . N17 N 0.2710(19) 0.5806(17) -0.1030(10) 0.077(6) Uani 1 d . . . C18 C 0.2216(11) 0.5454(11) 0.1061(8) 0.032(3) Uani 1 d . . . N18 N 0.2220(10) 0.4590(9) 0.1240(7) 0.034(2) Uani 1 d . . . C21 C 0.2536(11) 0.4556(11) 0.4068(7) 0.031(2) Uani 1 d . . . N21 N 0.2605(10) 0.5412(9) 0.3881(6) 0.031(2) Uani 1 d . . . C22 C 0.2382(10) 0.3065(10) 0.3179(8) 0.030(2) Uani 1 d . . . N22 N 0.2341(10) 0.3091(9) 0.2480(7) 0.035(2) Uani 1 d . . . C23 C 0.0656(12) 0.3444(16) 0.4484(9) 0.048(4) Uani 1 d . . . N23 N -0.0272(11) 0.3761(12) 0.4452(11) 0.054(4) Uani 1 d . . . C24 C 0.4097(14) 0.3284(16) 0.4585(8) 0.051(4) Uani 1 d . . . N24 N 0.5025(12) 0.3600(14) 0.4650(12) 0.063(4) Uani 1 d . . . C25 C 0.3560(14) 0.1747(12) 0.4032(10) 0.045(3) Uani 1 d . . . N25 N 0.4146(17) 0.1115(14) 0.3809(14) 0.079(6) Uani 1 d . . . C26 C 0.2456(17) 0.1877(15) 0.5540(10) 0.056(5) Uani 1 d . . . N26 N 0.249(2) 0.1292(17) 0.6115(13) 0.097(8) Uani 1 d . . . C27 C 0.1322(15) 0.1675(11) 0.4271(9) 0.042(3) Uani 1 d . . . N27 N 0.0751(15) 0.1047(13) 0.4141(12) 0.067(5) Uani 1 d . . . C28 C 0.2141(17) 0.3768(15) 0.5571(10) 0.053(4) Uani 1 d . . . N28 N 0.205(2) 0.4183(17) 0.6161(11) 0.088(7) Uani 1 d . . . N30 N 0.2757(14) 0.1686(10) 0.1281(8) 0.047(3) Uani 1 d . . . N31 N 0.2596(10) 0.3239(9) 0.0119(6) 0.032(2) Uani 1 d . . . H311 H 0.2019 0.3630 -0.0059 0.070 Uiso 1 calc R . . H312 H 0.3257 0.3544 -0.0087 0.070 Uiso 1 calc R . . C32 C 0.256(3) 0.2214(16) -0.0181(12) 0.074(7) Uani 1 d . . . H321 H 0.1789 0.2070 -0.0275 0.070 Uiso 1 calc R . . H322 H 0.3043 0.2207 -0.0701 0.070 Uiso 1 calc R . . C33 C 0.296(2) 0.1416(16) 0.0400(13) 0.072(6) Uani 1 d . . . H331 H 0.3771 0.1296 0.0257 0.070 Uiso 1 calc R . . H332 H 0.2570 0.0782 0.0353 0.070 Uiso 1 calc R . . N34 N 0.0840(11) 0.2835(12) 0.1381(8) 0.047(3) Uani 1 d . . . H341 H 0.0461 0.3110 0.1817 0.070 Uiso 1 calc R . . H342 H 0.0547 0.3106 0.0926 0.070 Uiso 1 calc R . . C35 C 0.071(2) 0.1668(15) 0.1472(13) 0.066(6) Uani 1 d . . . H351 H 0.0051 0.1483 0.1866 0.070 Uiso 1 calc R . . H352 H 0.0578 0.1432 0.0949 0.070 Uiso 1 calc R . . C36 C 0.176(2) 0.1165(15) 0.1758(13) 0.071(6) Uani 1 d . . . H361 H 0.1772 0.1227 0.2339 0.070 Uiso 1 calc R . . H362 H 0.1777 0.0440 0.1669 0.070 Uiso 1 calc R . . N37 N 0.4122(10) 0.3258(12) 0.1308(7) 0.043(3) Uani 1 d . . . H371 H 0.4414 0.3631 0.0848 0.070 Uiso 1 calc R . . H372 H 0.4263 0.3591 0.1740 0.070 Uiso 1 calc R . . C38 C 0.4686(19) 0.225(2) 0.1355(13) 0.078(7) Uani 1 d . . . H381 H 0.5274 0.2246 0.1722 0.070 Uiso 1 calc R . . H382 H 0.5046 0.2115 0.0815 0.070 Uiso 1 calc R . . C39 C 0.385(2) 0.1466(16) 0.1656(13) 0.070(6) Uani 1 d . . . H391 H 0.3696 0.1448 0.2248 0.070 Uiso 1 calc R . . H392 H 0.4148 0.0798 0.1518 0.070 Uiso 1 calc R . . N40 N 0.2910(19) 0.8358(10) 0.3709(8) 0.066(5) Uani 1 d . . . N41 N 0.2674(10) 0.6843(9) 0.4935(6) 0.032(2) Uani 1 d . . . H411 H 0.2114 0.6422 0.5173 0.070 Uiso 1 calc R . . H412 H 0.3340 0.6597 0.5096 0.070 Uiso 1 calc R . . C42 C 0.246(2) 0.7881(17) 0.5198(10) 0.064(5) Uani 1 d . . . H421 H 0.1639 0.8017 0.5277 0.070 Uiso 1 calc R . . H422 H 0.2759 0.7933 0.5716 0.070 Uiso 1 calc R . . C43 C 0.300(3) 0.8634(15) 0.4575(13) 0.085(8) Uani 1 d . . . H431 H 0.3800 0.8683 0.4653 0.070 Uiso 1 calc R . . H432 H 0.2644 0.9303 0.4644 0.070 Uiso 1 calc R . . N44 N 0.1090(12) 0.7117(13) 0.3788(8) 0.053(4) Uani 1 d . . . H441 H 0.0821 0.6832 0.3372 0.070 Uiso 1 calc R . . H442 H 0.0735 0.6827 0.4263 0.070 Uiso 1 calc R . . C45 C 0.085(2) 0.827(2) 0.3718(15) 0.086(9) Uani 1 d . . . H451 H 0.0259 0.8432 0.3362 0.070 Uiso 1 calc R . . H452 H 0.0589 0.8490 0.4255 0.070 Uiso 1 calc R . . C46 C 0.191(3) 0.8818(16) 0.3376(11) 0.097(11) Uani 1 d . . . H461 H 0.2011 0.8806 0.2784 0.070 Uiso 1 calc R . . H462 H 0.1841 0.9530 0.3499 0.070 Uiso 1 calc R . . N47 N 0.4404(11) 0.6787(13) 0.3591(8) 0.050(3) Uani 1 d . . . H471 H 0.4662 0.6443 0.4034 0.070 Uiso 1 calc R . . H472 H 0.4631 0.6439 0.3152 0.070 Uiso 1 calc R . . C48 C 0.490(3) 0.784(3) 0.3463(17) 0.111(13) Uani 1 d . . . H481 H 0.5134 0.8039 0.3972 0.070 Uiso 1 calc R . . H482 H 0.5561 0.7857 0.3054 0.070 Uiso 1 calc R . . C49 C 0.400(3) 0.8566(19) 0.3181(15) 0.104(12) Uani 1 d . . . H491 H 0.3907 0.8478 0.2614 0.070 Uiso 1 calc R . . H492 H 0.4230 0.9269 0.3212 0.070 Uiso 1 calc R . . O11 O 0.2710(15) -0.2301(12) 0.7468(9) 0.072(4) Uani 1 d . . . O12 O 0.452(2) 0.621(2) 0.7259(12) 0.128(9) Uani 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 W1 0.0275(3) 0.0232(3) 0.0200(2) 0.00075(16) -0.00260(16) 0.00004(16) W2 0.0294(3) 0.0235(3) 0.0221(2) 0.00234(16) -0.00298(16) -0.00092(16) Co1 0.0337(8) 0.0227(8) 0.0218(7) -0.0015(6) -0.0002(6) -0.0003(6) Co2 0.0390(9) 0.0230(8) 0.0201(7) -0.0022(6) -0.0027(6) -0.0013(6) K1 0.083(3) 0.063(3) 0.082(3) 0.001(2) -0.032(3) -0.001(2) K2 0.215(9) 0.091(5) 0.103(5) -0.034(4) -0.091(6) 0.034(5) O1 0.058(10) 0.119(17) 0.18(2) -0.084(16) -0.026(11) 0.004(10) O2 0.080(11) 0.104(14) 0.091(13) 0.000(11) -0.005(9) -0.022(10) O3 0.31(4) 0.082(15) 0.076(14) 0.020(11) -0.026(19) 0.00(2) O4 0.076(12) 0.104(16) 0.17(2) 0.034(15) 0.015(13) 0.007(11) O5 0.094(12) 0.119(15) 0.051(8) -0.019(9) 0.002(8) -0.004(11) O6 0.099(13) 0.128(17) 0.067(10) -0.016(11) -0.003(9) 0.032(12) O7 0.080(12) 0.104(15) 0.141(19) -0.007(13) -0.020(12) -0.034(11) C11 0.039(6) 0.020(5) 0.025(5) -0.004(4) -0.004(4) 0.001(4) N11 0.049(6) 0.031(5) 0.016(4) 0.001(4) 0.000(4) -0.001(4) C12 0.035(7) 0.074(12) 0.033(7) 0.019(7) -0.003(5) 0.006(7) N12 0.037(7) 0.054(9) 0.113(15) 0.006(9) -0.031(8) -0.004(6) C13 0.043(7) 0.032(7) 0.041(7) 0.002(6) -0.005(6) -0.010(5) N13 0.058(9) 0.045(9) 0.097(14) -0.008(9) -0.010(9) -0.010(7) C14 0.039(8) 0.093(14) 0.016(5) 0.014(7) 0.008(5) 0.004(8) N14 0.033(6) 0.065(9) 0.056(8) -0.004(7) 0.002(6) 0.008(6) C15 0.036(7) 0.041(8) 0.062(10) -0.015(7) -0.001(7) 0.005(6) N15 0.063(11) 0.077(13) 0.126(19) -0.043(13) 0.005(11) 0.024(10) C16 0.066(11) 0.062(11) 0.036(8) 0.016(7) -0.019(7) -0.009(8) N16 0.14(2) 0.073(14) 0.084(14) 0.046(12) -0.046(14) -0.006(13) C17 0.062(10) 0.050(9) 0.031(7) -0.009(6) -0.008(6) 0.001(7) N17 0.107(15) 0.089(14) 0.042(8) -0.032(9) -0.014(9) 0.008(11) C18 0.029(6) 0.041(7) 0.028(6) -0.006(5) -0.008(4) -0.001(5) N18 0.044(6) 0.032(6) 0.027(5) -0.009(4) -0.006(4) -0.002(4) C21 0.035(6) 0.036(7) 0.023(5) -0.002(5) -0.005(4) 0.004(5) N21 0.041(6) 0.029(5) 0.023(5) 0.000(4) -0.006(4) -0.002(4) C22 0.028(6) 0.029(6) 0.029(6) 0.002(5) 0.001(4) 0.003(4) N22 0.043(6) 0.029(6) 0.032(5) -0.002(4) 0.004(4) 0.000(4) C23 0.031(7) 0.088(13) 0.024(6) -0.005(7) -0.004(5) -0.005(7) N23 0.033(7) 0.054(9) 0.075(10) -0.005(7) -0.004(6) -0.001(6) C24 0.046(8) 0.087(13) 0.019(6) 0.015(7) -0.011(5) -0.007(8) N24 0.033(7) 0.075(11) 0.086(12) -0.008(9) -0.021(7) -0.010(7) C25 0.047(8) 0.038(8) 0.050(9) -0.006(6) -0.008(7) 0.011(6) N25 0.078(12) 0.050(10) 0.106(16) -0.006(10) -0.010(11) 0.023(9) C26 0.074(12) 0.056(10) 0.037(8) 0.020(7) -0.018(8) -0.024(9) N26 0.16(2) 0.072(13) 0.062(12) 0.030(10) -0.032(13) -0.026(14) C27 0.060(9) 0.025(6) 0.040(7) -0.002(5) -0.004(6) -0.008(6) N27 0.067(10) 0.049(9) 0.087(13) -0.022(9) -0.004(9) -0.019(8) C28 0.072(11) 0.056(10) 0.030(7) -0.006(7) -0.002(7) 0.014(8) N28 0.135(19) 0.094(15) 0.039(8) -0.024(9) -0.018(10) 0.042(14) N30 0.080(10) 0.024(6) 0.037(6) -0.001(5) -0.001(6) 0.002(6) N31 0.036(6) 0.039(6) 0.021(5) -0.004(4) 0.001(4) -0.001(4) C32 0.14(2) 0.051(11) 0.039(9) -0.022(8) -0.019(11) 0.021(12) C33 0.119(19) 0.047(11) 0.053(11) -0.021(9) -0.011(11) 0.013(11) N34 0.041(7) 0.068(9) 0.034(6) -0.011(6) 0.003(5) -0.026(6) C35 0.088(15) 0.051(11) 0.057(11) 0.001(9) 0.010(10) -0.041(10) C36 0.121(19) 0.036(9) 0.059(11) 0.004(8) -0.028(12) -0.025(10) N37 0.038(6) 0.067(9) 0.025(5) -0.006(5) -0.004(4) 0.007(6) C38 0.061(12) 0.11(2) 0.057(12) 0.005(12) -0.011(9) 0.047(13) C39 0.101(17) 0.049(11) 0.060(11) -0.010(9) -0.011(11) 0.043(11) N40 0.155(17) 0.017(6) 0.027(6) -0.005(5) -0.002(8) -0.017(8) N41 0.040(6) 0.037(6) 0.019(4) 0.000(4) -0.003(4) 0.000(4) C42 0.099(15) 0.070(13) 0.024(7) -0.020(8) 0.001(8) -0.014(11) C43 0.16(3) 0.031(9) 0.061(13) -0.017(9) -0.002(14) -0.018(12) N44 0.051(8) 0.076(11) 0.030(6) 0.001(6) -0.007(5) 0.024(7) C45 0.094(17) 0.096(19) 0.060(13) 0.000(12) 0.002(12) 0.058(15) C46 0.22(3) 0.041(10) 0.030(8) -0.009(7) -0.037(14) 0.053(16) N47 0.042(7) 0.074(10) 0.034(6) -0.004(6) -0.002(5) -0.007(6) C48 0.11(2) 0.15(3) 0.069(16) -0.010(18) 0.015(15) -0.10(2) C49 0.19(3) 0.067(15) 0.061(13) -0.007(11) 0.001(17) -0.09(2) O11 0.104(12) 0.059(9) 0.051(8) 0.008(6) -0.012(7) 0.002(8) O12 0.17(2) 0.14(2) 0.064(11) -0.015(12) 0.026(13) 0.018(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 W1 C11 2.128(12) . ? W1 C14 2.134(16) . ? W1 C16 2.140(15) . ? W1 C12 2.144(16) . ? W1 C18 2.150(14) . ? W1 C13 2.161(14) . ? W1 C15 2.170(15) . ? W1 C17 2.184(15) . ? W2 C24 2.102(16) . ? W2 C22 2.130(13) . ? W2 C23 2.132(15) . ? W2 C26 2.139(15) . ? W2 C21 2.163(14) . ? W2 C28 2.174(16) . ? W2 C27 2.175(15) . ? W2 C25 2.176(15) . ? Co1 N18 1.896(12) . ? Co1 N22 1.919(12) . ? Co1 N31 1.934(10) . ? Co1 N30 1.934(13) . ? Co1 N34 1.953(12) . ? Co1 N37 1.965(13) . ? Co2 N21 1.904(11) . ? Co2 N11 1.905(10) . ? Co2 N41 1.939(10) . ? Co2 N47 1.953(14) . ? Co2 N40 1.955(12) . ? Co2 N44 1.955(14) . ? K1 O3 2.68(2) . ? K1 O2 2.76(2) . ? K1 O1 2.764(18) . ? K1 N16 2.817(18) 1_546 ? K1 N15 2.937(18) 2_566 ? K1 O4 3.17(2) . ? K1 N26 3.18(2) . ? K2 O3 2.77(2) . ? K2 N17 2.792(19) 1_556 ? K2 O7 2.81(2) . ? K2 O5 2.83(2) . ? K2 N28 2.929(18) . ? K2 O6 3.09(2) . ? K2 N12 3.34(2) 2_566 ? C11 N11 1.163(16) . ? C12 N12 1.15(2) . ? N12 K2 3.34(2) 2_566 ? C13 N13 1.15(2) . ? C14 N14 1.16(2) . ? C15 N15 1.13(2) . ? N15 K1 2.937(18) 2_566 ? C16 N16 1.17(2) . ? N16 K1 2.817(18) 1_564 ? C17 N17 1.12(2) . ? N17 K2 2.792(19) 1_554 ? C18 N18 1.139(18) . ? C21 N21 1.135(18) . ? C22 N22 1.155(17) . ? C23 N23 1.16(2) . ? C24 N24 1.20(2) . ? C25 N25 1.12(2) . ? C26 N26 1.17(2) . ? C27 N27 1.12(2) . ? C28 N28 1.15(2) . ? N30 C36 1.48(3) . ? N30 C39 1.50(3) . ? N30 C33 1.52(2) . ? N31 C32 1.47(2) . ? N31 H311 0.9000 . ? N31 H312 0.9000 . ? C32 C33 1.45(3) . ? C32 H321 0.9700 . ? C32 H322 0.9700 . ? C33 H331 0.9700 . ? C33 H332 0.9700 . ? N34 C35 1.53(2) . ? N34 H341 0.9000 . ? N34 H342 0.9000 . ? C35 C36 1.49(3) . ? C35 H351 0.9700 . ? C35 H352 0.9700 . ? C36 H361 0.9700 . ? C36 H362 0.9700 . ? N37 C38 1.45(2) . ? N37 H371 0.9000 . ? N37 H372 0.9000 . ? C38 C39 1.46(3) . ? C38 H381 0.9700 . ? C38 H382 0.9700 . ? C39 H391 0.9700 . ? C39 H392 0.9700 . ? N40 C46 1.45(3) . ? N40 C49 1.49(3) . ? N40 C43 1.52(2) . ? N41 C42 1.47(2) . ? N41 H411 0.9000 . ? N41 H412 0.9000 . ? C42 C43 1.46(3) . ? C42 H421 0.9700 . ? C42 H422 0.9700 . ? C43 H431 0.9700 . ? C43 H432 0.9700 . ? N44 C45 1.52(3) . ? N44 H441 0.9000 . ? N44 H442 0.9000 . ? C45 C46 1.48(4) . ? C45 H451 0.9700 . ? C45 H452 0.9700 . ? C46 H461 0.9700 . ? C46 H462 0.9700 . ? N47 C48 1.50(3) . ? N47 H471 0.9000 . ? N47 H472 0.9000 . ? C48 C49 1.48(4) . ? C48 H481 0.9700 . ? C48 H482 0.9700 . ? C49 H491 0.9700 . ? C49 H492 0.9700 . ? 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 C11 W1 C14 80.9(5) . . ? C11 W1 C16 143.6(6) . . ? C14 W1 C16 108.7(7) . . ? C11 W1 C12 109.0(5) . . ? C14 W1 C12 146.3(8) . . ? C16 W1 C12 82.8(6) . . ? C11 W1 C18 72.9(5) . . ? C14 W1 C18 77.6(6) . . ? C16 W1 C18 142.9(6) . . ? C12 W1 C18 75.0(6) . . ? C11 W1 C13 76.2(5) . . ? C14 W1 C13 69.9(7) . . ? C16 W1 C13 74.8(6) . . ? C12 W1 C13 143.2(7) . . ? C18 W1 C13 137.9(5) . . ? C11 W1 C15 74.2(6) . . ? C14 W1 C15 142.6(7) . . ? C16 W1 C15 78.4(8) . . ? C12 W1 C15 69.7(7) . . ? C18 W1 C15 119.4(6) . . ? C13 W1 C15 77.3(6) . . ? C11 W1 C17 142.4(6) . . ? C14 W1 C17 75.2(7) . . ? C16 W1 C17 72.7(7) . . ? C12 W1 C17 78.5(7) . . ? C18 W1 C17 73.9(6) . . ? C13 W1 C17 120.4(6) . . ? C15 W1 C17 139.2(7) . . ? C24 W2 C22 101.5(5) . . ? C24 W2 C23 148.7(8) . . ? C22 W2 C23 84.1(5) . . ? C24 W2 C26 87.1(6) . . ? C22 W2 C26 144.1(7) . . ? C23 W2 C26 106.4(7) . . ? C24 W2 C21 75.5(6) . . ? C22 W2 C21 73.3(5) . . ? C23 W2 C21 76.8(6) . . ? C26 W2 C21 142.0(6) . . ? C24 W2 C28 80.3(7) . . ? C22 W2 C28 144.8(6) . . ? C23 W2 C28 78.0(7) . . ? C26 W2 C28 70.7(7) . . ? C21 W2 C28 73.3(6) . . ? C24 W2 C27 141.5(7) . . ? C22 W2 C27 76.5(5) . . ? C23 W2 C27 69.9(7) . . ? C26 W2 C27 75.5(6) . . ? C21 W2 C27 136.7(5) . . ? C28 W2 C27 123.5(7) . . ? C24 W2 C25 68.4(7) . . ? C22 W2 C25 74.2(5) . . ? C23 W2 C25 141.4(7) . . ? C26 W2 C25 77.0(8) . . ? C21 W2 C25 124.4(6) . . ? C28 W2 C25 135.7(6) . . ? C27 W2 C25 74.2(6) . . ? N18 Co1 N22 90.6(5) . . ? N18 Co1 N31 88.1(5) . . ? N22 Co1 N31 178.6(5) . . ? N18 Co1 N30 175.5(5) . . ? N22 Co1 N30 93.7(5) . . ? N31 Co1 N30 87.7(5) . . ? N18 Co1 N34 94.2(6) . . ? N22 Co1 N34 89.1(5) . . ? N31 Co1 N34 91.5(5) . . ? N30 Co1 N34 87.1(7) . . ? N18 Co1 N37 93.4(6) . . ? N22 Co1 N37 87.4(5) . . ? N31 Co1 N37 92.2(5) . . ? N30 Co1 N37 85.5(7) . . ? N34 Co1 N37 171.6(6) . . ? N21 Co2 N11 91.4(5) . . ? N21 Co2 N41 88.1(5) . . ? N11 Co2 N41 178.0(5) . . ? N21 Co2 N47 92.4(6) . . ? N11 Co2 N47 88.4(5) . . ? N41 Co2 N47 93.6(5) . . ? N21 Co2 N40 175.3(5) . . ? N11 Co2 N40 93.1(5) . . ? N41 Co2 N40 87.4(5) . . ? N47 Co2 N40 86.5(8) . . ? N21 Co2 N44 94.0(6) . . ? N11 Co2 N44 86.3(5) . . ? N41 Co2 N44 91.8(5) . . ? N47 Co2 N44 171.8(6) . . ? N40 Co2 N44 87.5(8) . . ? O3 K1 O2 114.1(7) . . ? O3 K1 O1 91.9(9) . . ? O2 K1 O1 132.9(6) . . ? O3 K1 N16 149.2(8) . 1_546 ? O2 K1 N16 96.5(7) . 1_546 ? O1 K1 N16 68.0(8) . 1_546 ? O3 K1 N15 73.6(9) . 2_566 ? O2 K1 N15 90.3(6) . 2_566 ? O1 K1 N15 135.9(7) . 2_566 ? N16 K1 N15 104.2(8) 1_546 2_566 ? O3 K1 O4 110.3(8) . . ? O2 K1 O4 63.7(6) . . ? O1 K1 O4 70.8(7) . . ? N16 K1 O4 85.6(7) 1_546 . ? N15 K1 O4 153.3(7) 2_566 . ? O3 K1 N26 67.3(7) . . ? O2 K1 N26 58.7(6) . . ? O1 K1 N26 102.7(8) . . ? N16 K1 N26 137.9(7) 1_546 . ? N15 K1 N26 108.9(7) 2_566 . ? O4 K1 N26 53.7(7) . . ? O3 K2 N17 129.4(8) . 1_556 ? O3 K2 O7 80.3(9) . . ? N17 K2 O7 142.4(7) 1_556 . ? O3 K2 O5 144.5(7) . . ? N17 K2 O5 86.1(6) 1_556 . ? O7 K2 O5 67.3(6) . . ? O3 K2 N28 67.5(7) . . ? N17 K2 N28 141.5(8) 1_556 . ? O7 K2 N28 64.7(7) . . ? O5 K2 N28 85.0(6) . . ? O3 K2 O6 77.2(9) . . ? N17 K2 O6 70.1(6) 1_556 . ? O7 K2 O6 146.8(7) . . ? O5 K2 O6 123.5(7) . . ? N28 K2 O6 84.1(6) . . ? O3 K2 N12 74.5(7) . 2_566 ? N17 K2 N12 83.4(6) 1_556 2_566 ? O7 K2 N12 84.5(6) . 2_566 ? O5 K2 N12 114.8(5) . 2_566 ? N28 K2 N12 133.9(7) . 2_566 ? O6 K2 N12 112.3(5) . 2_566 ? K1 O3 K2 165.7(10) . . ? N11 C11 W1 176.3(11) . . ? C11 N11 Co2 169.9(12) . . ? N12 C12 W1 175.7(18) . . ? C12 N12 K2 113.6(14) . 2_566 ? N13 C13 W1 177.6(15) . . ? N14 C14 W1 173.9(18) . . ? N15 C15 W1 178(2) . . ? C15 N15 K1 152.2(18) . 2_566 ? N16 C16 W1 178(2) . . ? C16 N16 K1 164(2) . 1_564 ? N17 C17 W1 179.4(18) . . ? C17 N17 K2 147.9(18) . 1_554 ? N18 C18 W1 174.6(12) . . ? C18 N18 Co1 166.4(11) . . ? N21 C21 W2 177.6(11) . . ? C21 N21 Co2 170.7(10) . . ? N22 C22 W2 176.5(12) . . ? C22 N22 Co1 173.3(12) . . ? N23 C23 W2 176.2(15) . . ? N24 C24 W2 172.2(18) . . ? N25 C25 W2 178.4(18) . . ? N26 C26 W2 179(2) . . ? C26 N26 K1 153(2) . . ? N27 C27 W2 177.2(16) . . ? N28 C28 W2 177.0(17) . . ? C28 N28 K2 164.3(19) . . ? C36 N30 C39 113.1(16) . . ? C36 N30 C33 113.4(16) . . ? C39 N30 C33 107.4(16) . . ? C36 N30 Co1 106.5(12) . . ? C39 N30 Co1 106.4(11) . . ? C33 N30 Co1 109.8(11) . . ? C32 N31 Co1 111.1(10) . . ? C32 N31 H311 109.4 . . ? Co1 N31 H311 109.4 . . ? C32 N31 H312 109.4 . . ? Co1 N31 H312 109.4 . . ? H311 N31 H312 108.0 . . ? C33 C32 N31 111.7(15) . . ? C33 C32 H321 109.3 . . ? N31 C32 H321 109.3 . . ? C33 C32 H322 109.3 . . ? N31 C32 H322 109.3 . . ? H321 C32 H322 107.9 . . ? C32 C33 N30 113.1(15) . . ? C32 C33 H331 109.0 . . ? N30 C33 H331 109.0 . . ? C32 C33 H332 109.0 . . ? N30 C33 H332 109.0 . . ? H331 C33 H332 107.8 . . ? C35 N34 Co1 108.6(13) . . ? C35 N34 H341 110.0 . . ? Co1 N34 H341 110.0 . . ? C35 N34 H342 110.0 . . ? Co1 N34 H342 110.0 . . ? H341 N34 H342 108.3 . . ? C36 C35 N34 109.8(15) . . ? C36 C35 H351 109.7 . . ? N34 C35 H351 109.7 . . ? C36 C35 H352 109.7 . . ? N34 C35 H352 109.7 . . ? H351 C35 H352 108.2 . . ? N30 C36 C35 107.7(15) . . ? N30 C36 H361 110.2 . . ? C35 C36 H361 110.2 . . ? N30 C36 H362 110.2 . . ? C35 C36 H362 110.2 . . ? H361 C36 H362 108.5 . . ? C38 N37 Co1 111.9(14) . . ? C38 N37 H371 109.2 . . ? Co1 N37 H371 109.2 . . ? C38 N37 H372 109.2 . . ? Co1 N37 H372 109.2 . . ? H371 N37 H372 107.9 . . ? N37 C38 C39 109.5(16) . . ? N37 C38 H381 109.8 . . ? C39 C38 H381 109.8 . . ? N37 C38 H382 109.8 . . ? C39 C38 H382 109.8 . . ? H381 C38 H382 108.2 . . ? C38 C39 N30 110.4(15) . . ? C38 C39 H391 109.6 . . ? N30 C39 H391 109.6 . . ? C38 C39 H392 109.6 . . ? N30 C39 H392 109.6 . . ? H391 C39 H392 108.1 . . ? C46 N40 C49 114(2) . . ? C46 N40 C43 112.3(18) . . ? C49 N40 C43 110(2) . . ? C46 N40 Co2 106.6(14) . . ? C49 N40 Co2 104.5(14) . . ? C43 N40 Co2 108.0(10) . . ? C42 N41 Co2 110.4(9) . . ? C42 N41 H411 109.6 . . ? Co2 N41 H411 109.6 . . ? C42 N41 H412 109.6 . . ? Co2 N41 H412 109.6 . . ? H411 N41 H412 108.1 . . ? C43 C42 N41 109.5(14) . . ? C43 C42 H421 109.8 . . ? N41 C42 H421 109.8 . . ? C43 C42 H422 109.8 . . ? N41 C42 H422 109.8 . . ? H421 C42 H422 108.2 . . ? C42 C43 N40 112.4(16) . . ? C42 C43 H431 109.1 . . ? N40 C43 H431 109.1 . . ? C42 C43 H432 109.1 . . ? N40 C43 H432 109.1 . . ? H431 C43 H432 107.9 . . ? C45 N44 Co2 109.2(14) . . ? C45 N44 H441 109.8 . . ? Co2 N44 H441 109.8 . . ? C45 N44 H442 109.8 . . ? Co2 N44 H442 109.8 . . ? H441 N44 H442 108.3 . . ? C46 C45 N44 109.5(16) . . ? C46 C45 H451 109.8 . . ? N44 C45 H451 109.8 . . ? C46 C45 H452 109.8 . . ? N44 C45 H452 109.8 . . ? H451 C45 H452 108.2 . . ? N40 C46 C45 111.9(17) . . ? N40 C46 H461 109.2 . . ? C45 C46 H461 109.2 . . ? N40 C46 H462 109.2 . . ? C45 C46 H462 109.2 . . ? H461 C46 H462 107.9 . . ? C48 N47 Co2 110.4(17) . . ? C48 N47 H471 109.6 . . ? Co2 N47 H471 109.6 . . ? C48 N47 H472 109.6 . . ? Co2 N47 H472 109.6 . . ? H471 N47 H472 108.1 . . ? C49 C48 N47 107.9(19) . . ? C49 C48 H481 110.1 . . ? N47 C48 H481 110.1 . . ? C49 C48 H482 110.1 . . ? N47 C48 H482 110.1 . . ? H481 C48 H482 108.4 . . ? C48 C49 N40 109.2(19) . . ? C48 C49 H491 109.8 . . ? N40 C49 H491 109.8 . . ? C48 C49 H492 109.8 . . ? N40 C49 H492 109.8 . . ? H491 C49 H492 108.3 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 29.66 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 8.082 _refine_diff_density_min -3.497 _refine_diff_density_rms 0.430