Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Robert LaDuca' _publ_contact_author_address ; Lyman Briggs School/Chemistry Michigan State University E-30 Holmes Hall East Lansing MI 48825 UNITED STATES OF AMERICA ; _publ_contact_author_email LADUCA@MSU.EDU _publ_section_title ; Oxoanion and Cation Effects on the Structural Morphology of Coordination Polymers Incorporating a Kinked Organodiimine Tethering Ligand ; loop_ _publ_author_name R.LaDuca W.R.Knapp S.M.Krishnan N.Patel R.M.Supkowski # Attachment 'coclo4dpafinal.cif' data_mono _database_code_depnum_ccdc_archive 'CCDC 632670' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C80 H84 Cl4 Co2 N24 O24' _chemical_formula_weight 2025.37 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' 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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.028(4) _cell_length_b 16.175(4) _cell_length_c 33.771(7) _cell_angle_alpha 90.00 _cell_angle_beta 100.799(4) _cell_angle_gamma 90.00 _cell_volume 9137(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description fragment _exptl_crystal_colour pink _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.76 _exptl_crystal_size_min 0.52 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.472 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4184 _exptl_absorpt_coefficient_mu 0.567 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.794 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 ? _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 108061 _diffrn_reflns_av_R_equivalents 0.0398 _diffrn_reflns_av_sigmaI/netI 0.0369 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 28.31 _reflns_number_total 22130 _reflns_number_gt 14592 _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^)+(0.0731P)^2^+20.6825P] 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 22130 _refine_ls_number_parameters 1264 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.1027 _refine_ls_R_factor_gt 0.0617 _refine_ls_wR_factor_ref 0.1828 _refine_ls_wR_factor_gt 0.1545 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.003 _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 0.0000 0.5000 0.5000 0.01377(12) Uani 1 2 d S . . Co2 Co 0.25121(2) 0.49037(2) 0.251029(11) 0.01470(10) Uani 1 1 d . . . Co3 Co 0.5000 0.0000 0.5000 0.01323(12) Uani 1 2 d S . . Cl1 Cl 0.11910(6) 0.33133(8) 0.82199(3) 0.0491(3) Uani 1 1 d . . . Cl2 Cl 0.13775(5) 0.66717(6) 0.92452(2) 0.0340(2) Uani 1 1 d . . . Cl3 Cl 0.38482(6) 0.67318(7) 0.67919(3) 0.0418(2) Uani 1 1 d . . . Cl4 Cl 0.33485(5) 0.34392(6) 0.57824(2) 0.0335(2) Uani 1 1 d . . . O1 O 0.25356(13) 0.44221(15) 0.30892(7) 0.0226(5) Uani 1 1 d D . . H1A H 0.2902(16) 0.423(2) 0.3266(9) 0.027 Uiso 1 1 d D . . H1B H 0.2092(13) 0.425(2) 0.3035(11) 0.027 Uiso 1 1 d D . . O1W O 0.12797(15) 0.47974(17) 0.34644(7) 0.0342(6) Uani 1 1 d D . . H1WA H 0.150(2) 0.503(2) 0.3304(10) 0.041 Uiso 1 1 d D . . H1WB H 0.221(2) 0.464(2) 0.3215(11) 0.041 Uiso 1 1 d D . . O1A O 0.0509(2) 0.2825(3) 0.82691(11) 0.0781(11) Uani 1 1 d . . . O1B O 0.1213(2) 0.3408(3) 0.78169(9) 0.0875(14) Uani 1 1 d . . . O1C O 0.1890(3) 0.2790(3) 0.83885(13) 0.0991(15) Uani 1 1 d . . . O1D O 0.1258(3) 0.4015(3) 0.84550(16) 0.1177(18) Uani 1 1 d . . . O2 O 0.24969(13) 0.54440(15) 0.19454(7) 0.0240(5) Uani 1 1 d D . . H2A H 0.2242(19) 0.579(2) 0.1763(9) 0.029 Uiso 1 1 d D . . H2B H 0.2919(15) 0.535(2) 0.1832(10) 0.029 Uiso 1 1 d D . . O2W O -0.12734(14) 0.39940(16) 0.58923(7) 0.0347(6) Uani 1 1 d . . . H2WA H 0.273(2) 0.579(2) 0.2109(10) 0.042 Uiso 1 1 d D . . H2WB H 0.2016(13) 0.554(3) 0.1832(12) 0.042 Uiso 1 1 d D . . O2A O 0.20890(18) 0.7126(2) 0.92184(9) 0.0559(8) Uani 1 1 d . . . O2B O 0.1428(2) 0.6357(2) 0.96382(8) 0.0576(9) Uani 1 1 d . . . O2C O 0.0709(2) 0.7236(2) 0.91546(12) 0.0708(10) Uani 1 1 d . . . O2D O 0.12551(18) 0.6024(2) 0.89556(9) 0.0615(9) Uani 1 1 d . . . O3 O 0.50880(12) 0.06387(14) 0.55628(6) 0.0209(4) Uani 1 1 d D . . H3A H 0.4648(12) 0.070(2) 0.5632(10) 0.025 Uiso 1 1 d D . . H3B H 0.5461(15) 0.077(2) 0.5743(8) 0.025 Uiso 1 1 d D . . O3WA O 0.3761(2) 0.3979(2) 0.08902(10) 0.0309(7) Uani 0.80 1 d P . . O3A O 0.4375(3) 0.7335(3) 0.66859(15) 0.1122(18) Uani 1 1 d . . . O3C O 0.4268(3) 0.6309(3) 0.71251(11) 0.1046(17) Uani 1 1 d . . . O3D O 0.3630(4) 0.6219(3) 0.64672(13) 0.127(2) Uani 1 1 d . . . O3B O 0.3233(3) 0.7157(3) 0.69265(18) 0.1206(19) Uani 1 1 d . . . O3WB O 0.3789(8) 0.4502(12) 0.0916(4) 0.040(3) Uani 0.20 1 d P . . O4WA O 0.3703(2) 0.5191(3) 0.15313(10) 0.0357(8) Uani 0.80 1 d P . . O4A O 0.33310(19) 0.38275(19) 0.54001(8) 0.0486(7) Uani 1 1 d . . . O4B O 0.3997(2) 0.2860(2) 0.58560(11) 0.0638(9) Uani 1 1 d . . . O4C O 0.3465(2) 0.4027(2) 0.60983(8) 0.0566(8) Uani 1 1 d . . . O4D O 0.26224(19) 0.2998(3) 0.57809(10) 0.0696(11) Uani 1 1 d . . . O4WB O 0.3697(8) 0.5727(11) 0.1559(4) 0.035(3) Uani 0.20 1 d P . . O4 O 0.00853(12) 0.43552(13) 0.55601(6) 0.0204(4) Uani 1 1 d D . . H4A H 0.0434(15) 0.431(2) 0.5763(8) 0.025 Uiso 1 1 d D . . H4B H -0.0367(12) 0.428(2) 0.5606(10) 0.025 Uiso 1 1 d D . . N1 N 0.22264(19) 0.4160(2) 0.04780(11) 0.0443(8) Uani 1 1 d . . . N2 N -0.01382(18) 0.3825(2) -0.01195(9) 0.0370(7) Uani 1 1 d . . . H2N H -0.0453 0.3686 0.0049 0.044 Uiso 1 1 calc R . . N3 N -0.1390(2) 0.3981(2) -0.13124(9) 0.0433(8) Uani 1 1 d . . . N4 N -0.13906(14) 0.92630(15) 0.27178(7) 0.0200(5) Uani 1 1 d . . . N5 N 0.06628(17) 0.78668(18) 0.31657(9) 0.0319(7) Uani 1 1 d . . . H5N H 0.0891 0.8016 0.3411 0.038 Uiso 1 1 calc R . . N6 N 0.18885(15) 0.59427(15) 0.27104(7) 0.0208(5) Uani 1 1 d . . . N7 N 0.36300(14) 0.55346(15) 0.27235(7) 0.0199(5) Uani 1 1 d . . . N8 N 0.57255(19) 0.6871(2) 0.31459(9) 0.0437(9) Uani 1 1 d . . . H8N H 0.5985 0.6696 0.3381 0.052 Uiso 1 1 calc R . . N9 N 0.68858(15) 0.88455(16) 0.26863(8) 0.0237(5) Uani 1 1 d . . . N10 N 0.37486(18) 0.6026(2) 0.87713(9) 0.0361(7) Uani 1 1 d . . . N11 N 0.24890(18) 0.6389(2) 0.75905(9) 0.0345(7) Uani 1 1 d . . . H11N H 0.2758 0.6696 0.7447 0.041 Uiso 1 1 calc R . . N12 N 0.0293(2) 0.5620(3) 0.69064(11) 0.0508(10) Uani 1 1 d . . . N13 N 0.36099(19) 0.3849(2) 0.37386(9) 0.0407(8) Uani 1 1 d . . . N14 N 0.47253(18) 0.3731(2) 0.49578(9) 0.0381(7) Uani 1 1 d . . . H14N H 0.4389 0.3625 0.5120 0.046 Uiso 1 1 calc R . . N15 N 0.7094(2) 0.4001(2) 0.55703(11) 0.0464(9) Uani 1 1 d . . . N16 N 0.40072(15) 0.07950(15) 0.47580(7) 0.0209(5) Uani 1 1 d . . . N17 N 0.20222(17) 0.22649(18) 0.42743(8) 0.0311(7) Uani 1 1 d . . . H17N H 0.1853 0.2186 0.4015 0.037 Uiso 1 1 calc R . . N18 N 0.06633(14) 0.40204(15) 0.47690(7) 0.0192(5) Uani 1 1 d . . . N19 N 0.4714(2) 0.4443(2) 0.81311(11) 0.0512(9) Uani 1 1 d . . . N20 N 0.25406(17) 0.3703(2) 0.74162(9) 0.0379(7) Uani 1 1 d . . . H20N H 0.2306 0.3330 0.7544 0.045 Uiso 1 1 calc R . . N21 N 0.11819(18) 0.4172(2) 0.62644(9) 0.0388(7) Uani 1 1 d . . . N22 N 0.57632(15) 0.09072(16) 0.47880(8) 0.0222(5) Uani 1 1 d . . . N23 N 0.69133(17) 0.28720(18) 0.43131(8) 0.0310(7) Uani 1 1 d . . . H23N H 0.6677 0.3017 0.4069 0.037 Uiso 1 1 calc R . . N24 N 0.89208(14) 0.43134(15) 0.47848(7) 0.0189(5) Uani 1 1 d . . . C1 C 0.1671(2) 0.3789(3) 0.06458(12) 0.0433(10) Uani 1 1 d . . . H1 H 0.1823 0.3593 0.0915 0.052 Uiso 1 1 calc R . . C2 C 0.0894(2) 0.3671(2) 0.04549(11) 0.0387(9) Uani 1 1 d . . . H2 H 0.0526 0.3401 0.0591 0.046 Uiso 1 1 calc R . . C3 C 0.0649(2) 0.3950(2) 0.00594(11) 0.0338(8) Uani 1 1 d . . . C4 C 0.1216(2) 0.4366(2) -0.01170(12) 0.0379(8) Uani 1 1 d . . . H4 H 0.1079 0.4584 -0.0382 0.045 Uiso 1 1 calc R . . C5 C 0.1981(2) 0.4450(3) 0.01050(13) 0.0442(10) Uani 1 1 d . . . H5 H 0.2361 0.4735 -0.0017 0.053 Uiso 1 1 calc R . . C6 C -0.1752(2) 0.3988(2) -0.09956(11) 0.0359(8) Uani 1 1 d . . . H6 H -0.2318 0.4025 -0.1043 0.043 Uiso 1 1 calc R . . C7 C -0.1348(2) 0.3946(2) -0.06001(10) 0.0310(7) Uani 1 1 d . . . H7 H -0.1636 0.3962 -0.0385 0.037 Uiso 1 1 calc R . . C8 C -0.0518(2) 0.3880(2) -0.05193(10) 0.0323(8) Uani 1 1 d . . . C9 C -0.0141(2) 0.3843(3) -0.08512(11) 0.0463(11) Uani 1 1 d . . . H9 H 0.0422 0.3781 -0.0815 0.056 Uiso 1 1 calc R . . C10 C -0.0596(2) 0.3898(3) -0.12325(12) 0.0524(12) Uani 1 1 d . . . H10 H -0.0327 0.3875 -0.1454 0.063 Uiso 1 1 calc R . . C11 C -0.1017(2) 0.9280(2) 0.31029(10) 0.0344(8) Uani 1 1 d . . . H11 H -0.1229 0.9630 0.3283 0.041 Uiso 1 1 calc R . . C12 C -0.0348(2) 0.8828(2) 0.32563(11) 0.0379(9) Uani 1 1 d . . . H12 H -0.0112 0.8869 0.3534 0.046 Uiso 1 1 calc R . . C13 C -0.00150(18) 0.83063(19) 0.30037(10) 0.0235(6) Uani 1 1 d . . . C14 C -0.0384(2) 0.8298(2) 0.26048(10) 0.0318(8) Uani 1 1 d . . . H14 H -0.0173 0.7969 0.2417 0.038 Uiso 1 1 calc R . . C15 C -0.1062(2) 0.8767(2) 0.24784(10) 0.0304(7) Uani 1 1 d . . . H15 H -0.1311 0.8735 0.2202 0.036 Uiso 1 1 calc R . . C16 C 0.1156(2) 0.6160(2) 0.25296(10) 0.0326(8) Uani 1 1 d . . . H16 H 0.0924 0.5873 0.2291 0.039 Uiso 1 1 calc R . . C17 C 0.0710(2) 0.6777(2) 0.26648(11) 0.0378(9) Uani 1 1 d . . . H17 H 0.0182 0.6890 0.2527 0.045 Uiso 1 1 calc R . . C18 C 0.10420(19) 0.72266(19) 0.30035(9) 0.0241(6) Uani 1 1 d . . . C19 C 0.17993(19) 0.69885(19) 0.32032(9) 0.0248(7) Uani 1 1 d . . . H19 H 0.2045 0.7263 0.3443 0.030 Uiso 1 1 calc R . . C20 C 0.21876(19) 0.6353(2) 0.30506(10) 0.0256(7) Uani 1 1 d . . . H20 H 0.2699 0.6195 0.3195 0.031 Uiso 1 1 calc R . . C21 C 0.41858(19) 0.5292(2) 0.30362(10) 0.0295(7) Uani 1 1 d . . . H21 H 0.4097 0.4788 0.3166 0.035 Uiso 1 1 calc R . . C22 C 0.4874(2) 0.5717(2) 0.31823(11) 0.0363(9) Uani 1 1 d . . . H22 H 0.5245 0.5509 0.3405 0.044 Uiso 1 1 calc R . . C23 C 0.5023(2) 0.6462(2) 0.29987(10) 0.0289(7) Uani 1 1 d . . . C24 C 0.44388(19) 0.67392(19) 0.26830(9) 0.0250(7) Uani 1 1 d . . . H24 H 0.4502 0.7252 0.2555 0.030 Uiso 1 1 calc R . . C25 C 0.37696(18) 0.62640(19) 0.25579(9) 0.0227(6) Uani 1 1 d . . . H25 H 0.3380 0.6463 0.2340 0.027 Uiso 1 1 calc R . . C26 C 0.63444(19) 0.8386(2) 0.24469(9) 0.0253(7) Uani 1 1 d . . . H26 H 0.6236 0.8517 0.2168 0.030 Uiso 1 1 calc R . . C27 C 0.59295(19) 0.7735(2) 0.25735(9) 0.0261(7) Uani 1 1 d . . . H27 H 0.5543 0.7440 0.2387 0.031 Uiso 1 1 calc R . . C28 C 0.6085(2) 0.7519(2) 0.29775(10) 0.0302(7) Uani 1 1 d . . . C29 C 0.6687(2) 0.7949(2) 0.32270(11) 0.0401(9) Uani 1 1 d . . . H29 H 0.6844 0.7796 0.3502 0.048 Uiso 1 1 calc R . . C30 C 0.7056(2) 0.8603(2) 0.30719(10) 0.0365(9) Uani 1 1 d . . . H30 H 0.7456 0.8899 0.3250 0.044 Uiso 1 1 calc R . . C31 C 0.4092(2) 0.6299(3) 0.84712(11) 0.0396(9) Uani 1 1 d . . . H31 H 0.4647 0.6424 0.8531 0.048 Uiso 1 1 calc R . . C32 C 0.3694(2) 0.6412(2) 0.80810(11) 0.0378(9) Uani 1 1 d . . . H32 H 0.3973 0.6606 0.7881 0.045 Uiso 1 1 calc R . . C33 C 0.2876(2) 0.6240(2) 0.79813(10) 0.0292(7) Uani 1 1 d . . . C34 C 0.2510(2) 0.5962(2) 0.82942(11) 0.0342(8) Uani 1 1 d . . . H34 H 0.1955 0.5839 0.8246 0.041 Uiso 1 1 calc R . . C35 C 0.2967(2) 0.5869(2) 0.86731(11) 0.0357(8) Uani 1 1 d . . . H35 H 0.2705 0.5678 0.8881 0.043 Uiso 1 1 calc R . . C36 C 0.0620(2) 0.5228(3) 0.72463(14) 0.0465(10) Uani 1 1 d . . . H36 H 0.0344 0.4761 0.7323 0.056 Uiso 1 1 calc R . . C37 C 0.1328(2) 0.5450(2) 0.74938(12) 0.0372(8) Uani 1 1 d . . . H37 H 0.1528 0.5145 0.7731 0.045 Uiso 1 1 calc R . . C38 C 0.1741(2) 0.6131(2) 0.73879(10) 0.0318(8) Uani 1 1 d . . . C39 C 0.1407(2) 0.6554(3) 0.70341(11) 0.0394(9) Uani 1 1 d . . . H39 H 0.1666 0.7026 0.6951 0.047 Uiso 1 1 calc R . . C40 C 0.0695(2) 0.6277(3) 0.68090(12) 0.0451(10) Uani 1 1 d . . . H40 H 0.0477 0.6571 0.6570 0.054 Uiso 1 1 calc R . . C41 C 0.4396(2) 0.3714(3) 0.38473(12) 0.0480(11) Uani 1 1 d . . . H41 H 0.4693 0.3640 0.3638 0.058 Uiso 1 1 calc R . . C42 C 0.4808(2) 0.3673(3) 0.42391(11) 0.0427(10) Uani 1 1 d . . . H42 H 0.5368 0.3577 0.4295 0.051 Uiso 1 1 calc R . . C43 C 0.4385(2) 0.3775(2) 0.45538(10) 0.0318(8) Uani 1 1 d . . . C44 C 0.3562(2) 0.3897(2) 0.44452(10) 0.0314(7) Uani 1 1 d . . . H44 H 0.3244 0.3956 0.4647 0.038 Uiso 1 1 calc R . . C45 C 0.3214(2) 0.3931(2) 0.40431(11) 0.0352(8) Uani 1 1 d . . . H45 H 0.2653 0.4019 0.3977 0.042 Uiso 1 1 calc R . . C46 C 0.6851(2) 0.4314(3) 0.52051(13) 0.0437(10) Uani 1 1 d . . . H46 H 0.7234 0.4608 0.5088 0.052 Uiso 1 1 calc R . . C47 C 0.6085(2) 0.4247(2) 0.49805(12) 0.0395(9) Uani 1 1 d . . . H47 H 0.5954 0.4484 0.4719 0.047 Uiso 1 1 calc R . . C48 C 0.5516(2) 0.3827(2) 0.51465(11) 0.0339(8) Uani 1 1 d . . . C49 C 0.5755(2) 0.3508(3) 0.55350(12) 0.0446(10) Uani 1 1 d . . . H49 H 0.5384 0.3225 0.5664 0.054 Uiso 1 1 calc R . . C50 C 0.6535(3) 0.3609(3) 0.57277(13) 0.0495(11) Uani 1 1 d . . . H50 H 0.6687 0.3383 0.5991 0.059 Uiso 1 1 calc R . . C51 C 0.38533(18) 0.15038(18) 0.49362(9) 0.0218(6) Uani 1 1 d . . . H51 H 0.4213 0.1666 0.5174 0.026 Uiso 1 1 calc R . . C52 C 0.32104(18) 0.20117(19) 0.47985(9) 0.0234(6) Uani 1 1 d . . . H52 H 0.3129 0.2500 0.4942 0.028 Uiso 1 1 calc R . . C53 C 0.26823(19) 0.1801(2) 0.44476(9) 0.0244(7) Uani 1 1 d . . . C54 C 0.2858(2) 0.1095(2) 0.42454(11) 0.0390(9) Uani 1 1 d . . . H54 H 0.2534 0.0941 0.3996 0.047 Uiso 1 1 calc R . . C55 C 0.3510(2) 0.0621(2) 0.44129(11) 0.0359(9) Uani 1 1 d . . . H55 H 0.3612 0.0136 0.4273 0.043 Uiso 1 1 calc R . . C56 C 0.11453(18) 0.34903(18) 0.50042(9) 0.0209(6) Uani 1 1 d . . . H56 H 0.1167 0.3524 0.5287 0.025 Uiso 1 1 calc R . . C57 C 0.16129(18) 0.28987(19) 0.48658(9) 0.0223(6) Uani 1 1 d . . . H57 H 0.1942 0.2541 0.5049 0.027 Uiso 1 1 calc R . . C58 C 0.15933(18) 0.28344(18) 0.44534(9) 0.0212(6) Uani 1 1 d . . . C59 C 0.1077(2) 0.3363(2) 0.42009(9) 0.0278(7) Uani 1 1 d . . . H59 H 0.1034 0.3331 0.3917 0.033 Uiso 1 1 calc R . . C60 C 0.06302(19) 0.3933(2) 0.43674(9) 0.0258(7) Uani 1 1 d . . . H60 H 0.0279 0.4283 0.4190 0.031 Uiso 1 1 calc R . . C61 C 0.4173(3) 0.3976(3) 0.82659(13) 0.0523(12) Uani 1 1 d . . . H61 H 0.4298 0.3790 0.8537 0.063 Uiso 1 1 calc R . . C62 C 0.3450(2) 0.3744(3) 0.80411(12) 0.0447(10) Uani 1 1 d . . . H62 H 0.3092 0.3411 0.8156 0.054 Uiso 1 1 calc R . . C63 C 0.3248(2) 0.4009(2) 0.76391(11) 0.0343(8) Uani 1 1 d . . . C64 C 0.3789(2) 0.4514(3) 0.74956(13) 0.0410(9) Uani 1 1 d . . . H64 H 0.3675 0.4725 0.7228 0.049 Uiso 1 1 calc R . . C65 C 0.4503(2) 0.4704(3) 0.77521(14) 0.0478(10) Uani 1 1 d . . . H65 H 0.4870 0.5048 0.7649 0.057 Uiso 1 1 calc R . . C66 C 0.1746(2) 0.4696(3) 0.64397(11) 0.0386(9) Uani 1 1 d . . . H66 H 0.1817 0.5188 0.6297 0.046 Uiso 1 1 calc R . . C67 C 0.2238(2) 0.4585(2) 0.68107(11) 0.0353(8) Uani 1 1 d . . . H67 H 0.2636 0.4981 0.6914 0.042 Uiso 1 1 calc R . . C68 C 0.2133(2) 0.3877(2) 0.70289(10) 0.0320(8) Uani 1 1 d . . . C69 C 0.1543(2) 0.3323(3) 0.68533(12) 0.0427(9) Uani 1 1 d . . . H69 H 0.1450 0.2830 0.6991 0.051 Uiso 1 1 calc R . . C70 C 0.1096(2) 0.3493(3) 0.64801(12) 0.0441(10) Uani 1 1 d . . . H70 H 0.0699 0.3104 0.6367 0.053 Uiso 1 1 calc R . . C71 C 0.62938(18) 0.13864(19) 0.50272(9) 0.0229(6) Uani 1 1 d . . . H71 H 0.6395 0.1273 0.5308 0.027 Uiso 1 1 calc R . . C72 C 0.67048(19) 0.2035(2) 0.48927(9) 0.0257(7) Uani 1 1 d . . . H72 H 0.7071 0.2356 0.5078 0.031 Uiso 1 1 calc R . . C73 C 0.65715(18) 0.2210(2) 0.44810(9) 0.0244(7) Uani 1 1 d . . . C74 C 0.6035(2) 0.1708(2) 0.42279(10) 0.0399(9) Uani 1 1 d . . . H74 H 0.5935 0.1796 0.3945 0.048 Uiso 1 1 calc R . . C75 C 0.5648(2) 0.1077(2) 0.43918(10) 0.0368(9) Uani 1 1 d . . . H75 H 0.5280 0.0746 0.4214 0.044 Uiso 1 1 calc R . . C76 C 0.88580(18) 0.35241(18) 0.49028(9) 0.0214(6) Uani 1 1 d . . . H76 H 0.9287 0.3299 0.5093 0.026 Uiso 1 1 calc R . . C77 C 0.82094(18) 0.30229(19) 0.47640(9) 0.0231(6) Uani 1 1 d . . . H77 H 0.8194 0.2472 0.4860 0.028 Uiso 1 1 calc R . . C78 C 0.75808(18) 0.33342(19) 0.44826(9) 0.0227(6) Uani 1 1 d . . . C79 C 0.76337(19) 0.4151(2) 0.43547(10) 0.0278(7) Uani 1 1 d . . . H79 H 0.7218 0.4387 0.4161 0.033 Uiso 1 1 calc R . . C80 C 0.83033(18) 0.46072(19) 0.45163(9) 0.0243(7) Uani 1 1 d . . . H80 H 0.8328 0.5165 0.4432 0.029 Uiso 1 1 calc R . . 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 0.0117(2) 0.0128(3) 0.0165(3) -0.00036(19) 0.0018(2) -0.00025(19) Co2 0.01317(18) 0.01574(18) 0.01462(19) 0.00024(14) 0.00112(14) -0.00002(15) Co3 0.0121(2) 0.0120(2) 0.0149(3) 0.00033(19) 0.0008(2) -0.00011(19) Cl1 0.0351(5) 0.0830(8) 0.0273(5) -0.0038(5) 0.0011(4) -0.0112(5) Cl2 0.0340(4) 0.0461(5) 0.0206(4) -0.0034(3) 0.0021(3) -0.0063(4) Cl3 0.0426(5) 0.0559(6) 0.0255(4) -0.0042(4) 0.0027(4) -0.0021(4) Cl4 0.0336(4) 0.0459(5) 0.0196(4) 0.0013(3) 0.0013(3) -0.0034(4) O1 0.0162(11) 0.0330(12) 0.0180(11) 0.0034(9) 0.0020(9) 0.0019(9) O1W 0.0273(13) 0.0466(15) 0.0307(13) -0.0017(11) 0.0104(10) -0.0028(11) O1A 0.078(3) 0.096(3) 0.069(2) 0.005(2) 0.035(2) -0.024(2) O1B 0.071(2) 0.154(4) 0.0333(17) 0.015(2) 0.0007(16) -0.050(3) O1C 0.076(3) 0.137(4) 0.081(3) 0.022(3) 0.008(2) 0.023(3) O1D 0.127(4) 0.100(4) 0.119(4) -0.044(3) 0.003(3) -0.009(3) O2 0.0184(11) 0.0338(13) 0.0183(11) 0.0062(9) -0.0005(9) -0.0019(10) O2W 0.0269(12) 0.0462(15) 0.0318(13) -0.0050(11) 0.0078(10) -0.0077(11) O2A 0.0516(18) 0.074(2) 0.0427(17) 0.0052(15) 0.0108(14) -0.0250(16) O2B 0.080(2) 0.062(2) 0.0290(15) 0.0073(14) 0.0063(15) -0.0262(17) O2C 0.056(2) 0.057(2) 0.096(3) 0.0060(19) 0.0048(19) 0.0063(17) O2D 0.0445(17) 0.086(2) 0.0506(19) -0.0362(18) 0.0002(14) -0.0045(17) O3 0.0149(10) 0.0282(11) 0.0193(11) -0.0048(9) 0.0024(8) 0.0006(9) O3WA 0.0259(17) 0.0401(19) 0.0272(17) -0.0053(16) 0.0062(13) -0.0054(16) O3A 0.142(4) 0.089(3) 0.133(4) 0.051(3) 0.095(3) 0.013(3) O3C 0.168(5) 0.074(3) 0.052(2) 0.020(2) -0.031(3) -0.026(3) O3D 0.191(5) 0.091(3) 0.067(3) -0.040(2) -0.057(3) 0.018(3) O3B 0.078(3) 0.110(4) 0.190(6) -0.039(4) 0.067(3) -0.006(3) O3WB 0.021(6) 0.073(11) 0.027(7) -0.010(8) 0.007(5) 0.000(8) O4WA 0.0280(17) 0.048(2) 0.0329(18) -0.0036(17) 0.0093(13) -0.0012(18) O4A 0.066(2) 0.0556(18) 0.0251(13) 0.0074(12) 0.0115(13) -0.0093(15) O4B 0.055(2) 0.055(2) 0.082(2) 0.0104(18) 0.0167(18) 0.0147(16) O4C 0.069(2) 0.065(2) 0.0299(15) -0.0166(14) -0.0065(14) 0.0096(17) O4D 0.0494(19) 0.107(3) 0.0479(19) 0.0216(19) -0.0033(15) -0.0360(19) O4WB 0.019(6) 0.060(9) 0.024(7) 0.006(7) -0.002(5) -0.006(7) O4 0.0155(10) 0.0257(11) 0.0198(11) 0.0036(9) 0.0026(8) 0.0003(9) N1 0.0320(17) 0.051(2) 0.047(2) -0.0097(16) 0.0015(15) 0.0085(15) N2 0.0325(16) 0.052(2) 0.0249(15) 0.0054(14) 0.0019(12) 0.0022(14) N3 0.0368(18) 0.065(2) 0.0266(16) 0.0127(15) 0.0019(13) 0.0125(16) N4 0.0171(12) 0.0203(12) 0.0220(13) -0.0006(10) 0.0018(10) 0.0011(10) N5 0.0283(15) 0.0347(16) 0.0285(15) -0.0105(12) -0.0054(12) 0.0170(13) N6 0.0189(12) 0.0221(12) 0.0205(13) 0.0001(10) 0.0009(10) 0.0034(10) N7 0.0167(12) 0.0206(12) 0.0216(13) 0.0012(10) 0.0018(10) -0.0022(10) N8 0.0411(18) 0.055(2) 0.0262(15) 0.0210(14) -0.0171(13) -0.0305(16) N9 0.0218(13) 0.0254(13) 0.0218(13) 0.0033(10) -0.0010(10) -0.0053(11) N10 0.0304(16) 0.0474(19) 0.0281(16) 0.0117(14) -0.0005(12) 0.0061(14) N11 0.0321(16) 0.0434(17) 0.0257(15) 0.0056(13) -0.0006(12) -0.0054(13) N12 0.0271(17) 0.071(3) 0.052(2) -0.0232(19) 0.0014(16) 0.0028(17) N13 0.0310(16) 0.063(2) 0.0265(16) 0.0121(15) 0.0020(13) 0.0107(15) N14 0.0289(15) 0.059(2) 0.0254(15) 0.0087(14) 0.0027(12) 0.0003(15) N15 0.0315(17) 0.059(2) 0.046(2) -0.0128(17) 0.0012(15) 0.0023(16) N16 0.0191(12) 0.0208(12) 0.0211(13) -0.0017(10) -0.0011(10) 0.0054(10) N17 0.0329(15) 0.0367(16) 0.0201(14) -0.0072(12) -0.0045(11) 0.0223(13) N18 0.0167(12) 0.0176(12) 0.0226(13) -0.0023(10) 0.0021(10) 0.0015(9) N19 0.0323(18) 0.065(2) 0.052(2) -0.0177(19) -0.0038(16) 0.0036(17) N20 0.0261(15) 0.054(2) 0.0314(16) 0.0086(14) -0.0012(13) -0.0046(14) N21 0.0319(16) 0.056(2) 0.0266(16) 0.0023(14) 0.0010(13) 0.0046(15) N22 0.0227(13) 0.0226(13) 0.0201(13) 0.0024(10) 0.0011(10) -0.0064(10) N23 0.0301(15) 0.0383(16) 0.0200(13) 0.0092(12) -0.0073(11) -0.0193(13) N24 0.0156(12) 0.0182(12) 0.0222(13) -0.0002(10) 0.0016(10) -0.0029(9) C1 0.040(2) 0.053(2) 0.033(2) -0.0033(18) -0.0038(17) 0.0107(19) C2 0.041(2) 0.042(2) 0.0316(19) -0.0010(16) 0.0044(16) 0.0065(17) C3 0.0319(18) 0.0352(19) 0.0329(19) -0.0009(15) 0.0026(15) 0.0106(15) C4 0.037(2) 0.041(2) 0.036(2) 0.0038(16) 0.0072(16) 0.0093(17) C5 0.038(2) 0.041(2) 0.055(3) -0.0034(19) 0.0105(19) 0.0027(18) C6 0.0318(19) 0.043(2) 0.0323(19) 0.0113(16) 0.0037(15) 0.0010(16) C7 0.0311(18) 0.0323(18) 0.0298(18) 0.0048(14) 0.0064(14) 0.0024(15) C8 0.0360(19) 0.0338(18) 0.0267(17) 0.0059(14) 0.0048(14) 0.0110(15) C9 0.0300(19) 0.078(3) 0.030(2) 0.006(2) 0.0052(16) 0.023(2) C10 0.039(2) 0.089(4) 0.031(2) 0.013(2) 0.0095(17) 0.022(2) C11 0.0325(18) 0.0377(19) 0.0289(18) -0.0115(15) -0.0043(15) 0.0172(16) C12 0.0354(19) 0.043(2) 0.0283(18) -0.0149(16) -0.0118(15) 0.0188(17) C13 0.0194(14) 0.0219(15) 0.0278(16) -0.0017(12) 0.0011(12) 0.0040(12) C14 0.0356(19) 0.0350(18) 0.0250(17) -0.0018(14) 0.0058(14) 0.0166(15) C15 0.0345(18) 0.0343(18) 0.0208(16) -0.0011(13) 0.0013(14) 0.0105(15) C16 0.0295(18) 0.0340(18) 0.0290(18) -0.0087(14) -0.0082(14) 0.0097(15) C17 0.0286(18) 0.038(2) 0.040(2) -0.0105(16) -0.0112(15) 0.0151(15) C18 0.0236(15) 0.0244(15) 0.0236(16) -0.0005(12) 0.0021(12) 0.0081(13) C19 0.0252(16) 0.0248(15) 0.0215(15) -0.0053(12) -0.0034(12) 0.0058(13) C20 0.0205(15) 0.0273(16) 0.0262(16) -0.0034(13) -0.0032(12) 0.0064(13) C21 0.0249(16) 0.0299(17) 0.0308(18) 0.0129(14) -0.0023(14) -0.0114(14) C22 0.0294(18) 0.045(2) 0.0280(18) 0.0187(16) -0.0100(14) -0.0161(16) C23 0.0263(16) 0.0347(18) 0.0232(16) 0.0042(13) -0.0020(13) -0.0133(14) C24 0.0273(16) 0.0215(15) 0.0253(16) 0.0049(12) 0.0027(13) -0.0049(13) C25 0.0200(15) 0.0218(15) 0.0252(16) 0.0051(12) 0.0012(12) -0.0007(12) C26 0.0252(16) 0.0297(16) 0.0197(15) 0.0042(12) 0.0014(12) -0.0034(13) C27 0.0250(16) 0.0287(16) 0.0225(16) 0.0005(13) -0.0008(13) -0.0083(13) C28 0.0275(17) 0.0343(18) 0.0262(17) 0.0080(14) -0.0017(13) -0.0149(14) C29 0.042(2) 0.049(2) 0.0239(18) 0.0106(16) -0.0083(15) -0.0243(18) C30 0.037(2) 0.045(2) 0.0224(17) 0.0072(15) -0.0075(14) -0.0222(17) C31 0.0289(18) 0.054(2) 0.034(2) 0.0090(17) -0.0001(15) -0.0079(17) C32 0.0339(19) 0.046(2) 0.0315(19) 0.0088(16) 0.0020(15) -0.0108(17) C33 0.0304(18) 0.0279(17) 0.0276(17) 0.0025(13) 0.0009(14) 0.0019(14) C34 0.0221(16) 0.046(2) 0.0342(19) 0.0068(16) 0.0048(14) 0.0057(15) C35 0.0305(18) 0.045(2) 0.0320(19) 0.0108(16) 0.0070(15) 0.0093(16) C36 0.032(2) 0.052(2) 0.057(3) -0.016(2) 0.0124(19) -0.0035(19) C37 0.0317(19) 0.041(2) 0.039(2) -0.0047(16) 0.0073(16) -0.0001(16) C38 0.0271(17) 0.0373(19) 0.0297(18) -0.0049(15) 0.0017(14) 0.0063(15) C39 0.036(2) 0.046(2) 0.033(2) -0.0030(17) -0.0001(16) 0.0057(17) C40 0.036(2) 0.060(3) 0.036(2) -0.0085(19) -0.0027(17) 0.012(2) C41 0.033(2) 0.079(3) 0.032(2) 0.010(2) 0.0066(16) 0.020(2) C42 0.0291(19) 0.068(3) 0.0306(19) 0.0081(18) 0.0038(15) 0.0155(19) C43 0.0320(18) 0.0369(19) 0.0250(17) 0.0073(14) 0.0016(14) 0.0051(15) C44 0.0294(18) 0.0367(19) 0.0285(18) 0.0084(14) 0.0064(14) 0.0041(15) C45 0.0264(17) 0.049(2) 0.0295(18) 0.0117(16) 0.0042(14) 0.0044(16) C46 0.036(2) 0.048(2) 0.050(2) -0.0119(19) 0.0122(18) -0.0008(18) C47 0.040(2) 0.044(2) 0.034(2) -0.0023(17) 0.0082(17) -0.0001(18) C48 0.0290(18) 0.041(2) 0.0295(18) -0.0035(15) 0.0003(14) 0.0045(15) C49 0.037(2) 0.062(3) 0.032(2) 0.0099(19) 0.0016(16) -0.0006(19) C50 0.039(2) 0.069(3) 0.036(2) 0.003(2) -0.0062(18) 0.004(2) C51 0.0198(14) 0.0213(14) 0.0222(15) -0.0030(12) -0.0013(12) 0.0020(12) C52 0.0252(16) 0.0190(14) 0.0249(16) -0.0046(12) 0.0019(13) 0.0050(12) C53 0.0236(15) 0.0276(16) 0.0196(15) -0.0018(12) -0.0016(12) 0.0113(13) C54 0.039(2) 0.043(2) 0.0275(18) -0.0169(16) -0.0139(15) 0.0224(17) C55 0.0359(19) 0.0341(19) 0.0312(19) -0.0140(15) -0.0103(15) 0.0207(16) C56 0.0213(14) 0.0213(14) 0.0202(15) 0.0014(11) 0.0039(12) 0.0022(12) C57 0.0219(15) 0.0228(15) 0.0213(15) 0.0026(12) 0.0014(12) 0.0075(12) C58 0.0195(14) 0.0209(14) 0.0213(15) -0.0039(12) -0.0014(12) 0.0054(12) C59 0.0308(17) 0.0329(17) 0.0172(15) -0.0023(13) -0.0019(13) 0.0141(14) C60 0.0265(16) 0.0279(16) 0.0205(15) -0.0008(12) -0.0020(12) 0.0126(13) C61 0.037(2) 0.079(3) 0.037(2) -0.012(2) -0.0029(18) 0.007(2) C62 0.033(2) 0.067(3) 0.033(2) -0.0038(19) 0.0046(16) 0.0004(19) C63 0.0245(17) 0.043(2) 0.0337(19) -0.0069(16) 0.0018(14) 0.0046(15) C64 0.0284(19) 0.047(2) 0.046(2) -0.0022(18) 0.0037(17) 0.0030(17) C65 0.028(2) 0.051(3) 0.063(3) -0.010(2) 0.0057(19) 0.0002(18) C66 0.039(2) 0.051(2) 0.0267(18) 0.0027(16) 0.0064(16) 0.0022(18) C67 0.0305(18) 0.046(2) 0.0293(18) -0.0006(16) 0.0062(15) -0.0008(16) C68 0.0236(16) 0.047(2) 0.0250(17) 0.0024(15) 0.0040(13) 0.0054(15) C69 0.035(2) 0.050(2) 0.039(2) 0.0101(18) -0.0036(17) -0.0061(18) C70 0.034(2) 0.054(3) 0.041(2) 0.0032(19) -0.0007(17) -0.0057(18) C71 0.0218(15) 0.0289(16) 0.0163(14) 0.0022(12) -0.0009(12) -0.0085(13) C72 0.0244(16) 0.0309(17) 0.0194(15) 0.0013(12) -0.0019(12) -0.0114(13) C73 0.0221(15) 0.0254(15) 0.0244(16) 0.0049(12) 0.0010(12) -0.0102(13) C74 0.046(2) 0.049(2) 0.0206(17) 0.0081(15) -0.0047(15) -0.0291(19) C75 0.045(2) 0.041(2) 0.0197(16) 0.0047(14) -0.0062(15) -0.0274(17) C76 0.0199(14) 0.0183(14) 0.0252(15) 0.0016(12) 0.0021(12) -0.0014(11) C77 0.0232(15) 0.0195(14) 0.0266(16) 0.0014(12) 0.0047(13) -0.0044(12) C78 0.0220(15) 0.0253(15) 0.0206(15) 0.0018(12) 0.0037(12) -0.0111(12) C79 0.0244(16) 0.0313(17) 0.0237(16) 0.0095(13) -0.0055(13) -0.0082(13) C80 0.0240(16) 0.0219(15) 0.0258(16) 0.0058(12) 0.0016(13) -0.0070(12) _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 O4 2.141(2) . ? Co1 O4 2.141(2) 3_566 ? Co1 N24 2.154(2) 1_455 ? Co1 N24 2.154(2) 3_666 ? Co1 N18 2.174(2) 3_566 ? Co1 N18 2.174(2) . ? Co2 O2 2.094(2) . ? Co2 O1 2.098(2) . ? Co2 N7 2.161(2) . ? Co2 N9 2.163(3) 2_645 ? Co2 N6 2.163(3) . ? Co2 N4 2.183(2) 2_545 ? Co3 O3 2.144(2) . ? Co3 O3 2.144(2) 3_656 ? Co3 N16 2.159(2) . ? Co3 N16 2.159(2) 3_656 ? Co3 N22 2.169(2) 3_656 ? Co3 N22 2.169(2) . ? Cl1 O1B 1.377(3) . ? Cl1 O1D 1.378(5) . ? Cl1 O1A 1.440(4) . ? Cl1 O1C 1.484(4) . ? Cl2 O2B 1.409(3) . ? Cl2 O2D 1.422(3) . ? Cl2 O2A 1.434(3) . ? Cl2 O2C 1.447(3) . ? Cl3 O3D 1.370(4) . ? Cl3 O3C 1.393(4) . ? Cl3 O3B 1.399(4) . ? Cl3 O3A 1.416(4) . ? Cl4 O4C 1.415(3) . ? Cl4 O4D 1.427(3) . ? Cl4 O4A 1.431(3) . ? Cl4 O4B 1.434(3) . ? O3WA O3WB 0.852(17) . ? O4WA O4WB 0.871(16) . ? N1 C1 1.333(5) . ? N1 C5 1.336(5) . ? N2 C3 1.379(5) . ? N2 C8 1.386(4) . ? N3 C6 1.330(5) . ? N3 C10 1.335(5) . ? N4 C15 1.334(4) . ? N4 C11 1.337(4) . ? N4 Co2 2.183(2) 2 ? N5 C13 1.379(4) . ? N5 C18 1.386(4) . ? N6 C16 1.329(4) . ? N6 C20 1.342(4) . ? N7 C21 1.338(4) . ? N7 C25 1.346(4) . ? N8 C23 1.377(4) . ? N8 C28 1.388(4) . ? N9 C26 1.333(4) . ? N9 C30 1.338(4) . ? N9 Co2 2.163(3) 2_655 ? N10 C35 1.335(5) . ? N10 C31 1.336(5) . ? N11 C33 1.382(4) . ? N11 C38 1.392(4) . ? N12 C40 1.338(6) . ? N12 C36 1.338(6) . ? N13 C41 1.338(5) . ? N13 C45 1.338(5) . ? N14 C43 1.381(4) . ? N14 C48 1.386(4) . ? N15 C46 1.326(5) . ? N15 C50 1.334(6) . ? N16 C55 1.336(4) . ? N16 C51 1.343(4) . ? N17 C58 1.383(4) . ? N17 C53 1.386(4) . ? N18 C56 1.340(4) . ? N18 C60 1.354(4) . ? N19 C65 1.331(6) . ? N19 C61 1.336(6) . ? N20 C63 1.386(4) . ? N20 C68 1.390(4) . ? N21 C66 1.334(5) . ? N21 C70 1.341(5) . ? N22 C71 1.340(4) . ? N22 C75 1.344(4) . ? N23 C73 1.390(4) . ? N23 C78 1.391(4) . ? N24 C80 1.340(4) . ? N24 C76 1.348(4) . ? N24 Co1 2.154(2) 1_655 ? C1 C2 1.371(5) . ? C2 C3 1.398(5) . ? C3 C4 1.397(5) . ? C4 C5 1.383(5) . ? C6 C7 1.385(5) . ? C7 C8 1.393(5) . ? C8 C9 1.393(5) . ? C9 C10 1.376(5) . ? C11 C12 1.372(5) . ? C12 C13 1.393(4) . ? C13 C14 1.376(4) . ? C14 C15 1.381(5) . ? C16 C17 1.382(5) . ? C17 C18 1.384(5) . ? C18 C19 1.393(4) . ? C19 C20 1.373(4) . ? C21 C22 1.368(4) . ? C22 C23 1.400(5) . ? C23 C24 1.389(4) . ? C24 C25 1.374(4) . ? C26 C27 1.380(4) . ? C27 C28 1.385(4) . ? C28 C29 1.386(5) . ? C29 C30 1.383(5) . ? C31 C32 1.376(5) . ? C32 C33 1.399(5) . ? C33 C34 1.398(5) . ? C34 C35 1.375(5) . ? C36 C37 1.380(5) . ? C37 C38 1.389(5) . ? C38 C39 1.402(5) . ? C39 C40 1.379(5) . ? C41 C42 1.378(5) . ? C42 C43 1.401(5) . ? C43 C44 1.395(5) . ? C44 C45 1.377(5) . ? C46 C47 1.385(5) . ? C47 C48 1.386(5) . ? C48 C49 1.398(5) . ? C49 C50 1.375(5) . ? C51 C52 1.378(4) . ? C52 C53 1.389(4) . ? C53 C54 1.393(4) . ? C54 C55 1.379(4) . ? C56 C57 1.381(4) . ? C57 C58 1.391(4) . ? C58 C59 1.396(4) . ? C59 C60 1.381(4) . ? C61 C62 1.372(6) . ? C62 C63 1.403(5) . ? C63 C64 1.386(6) . ? C64 C65 1.388(5) . ? C66 C67 1.381(5) . ? C67 C68 1.391(5) . ? C68 C69 1.393(5) . ? C69 C70 1.373(5) . ? C71 C72 1.384(4) . ? C72 C73 1.395(4) . ? C73 C74 1.390(4) . ? C74 C75 1.384(5) . ? C76 C77 1.380(4) . ? C77 C78 1.386(4) . ? C78 C79 1.398(4) . ? C79 C80 1.382(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 O4 Co1 O4 180.00(6) . 3_566 ? O4 Co1 N24 87.67(9) . 1_455 ? O4 Co1 N24 92.33(9) 3_566 1_455 ? O4 Co1 N24 92.33(9) . 3_666 ? O4 Co1 N24 87.67(9) 3_566 3_666 ? N24 Co1 N24 180.000(1) 1_455 3_666 ? O4 Co1 N18 89.53(9) . 3_566 ? O4 Co1 N18 90.47(9) 3_566 3_566 ? N24 Co1 N18 91.67(9) 1_455 3_566 ? N24 Co1 N18 88.33(9) 3_666 3_566 ? O4 Co1 N18 90.47(9) . . ? O4 Co1 N18 89.53(9) 3_566 . ? N24 Co1 N18 88.33(9) 1_455 . ? N24 Co1 N18 91.67(9) 3_666 . ? N18 Co1 N18 180.00(12) 3_566 . ? O2 Co2 O1 177.11(9) . . ? O2 Co2 N7 88.06(9) . . ? O1 Co2 N7 90.18(9) . . ? O2 Co2 N9 88.64(10) . 2_645 ? O1 Co2 N9 93.72(10) . 2_645 ? N7 Co2 N9 92.14(10) . 2_645 ? O2 Co2 N6 92.14(10) . . ? O1 Co2 N6 85.53(9) . . ? N7 Co2 N6 88.99(10) . . ? N9 Co2 N6 178.65(10) 2_645 . ? O2 Co2 N4 90.92(9) . 2_545 ? O1 Co2 N4 90.87(9) . 2_545 ? N7 Co2 N4 178.75(9) . 2_545 ? N9 Co2 N4 87.11(10) 2_645 2_545 ? N6 Co2 N4 91.77(10) . 2_545 ? O3 Co3 O3 180.0 . 3_656 ? O3 Co3 N16 88.18(9) . . ? O3 Co3 N16 91.82(9) 3_656 . ? O3 Co3 N16 91.82(9) . 3_656 ? O3 Co3 N16 88.18(9) 3_656 3_656 ? N16 Co3 N16 180.00(13) . 3_656 ? O3 Co3 N22 88.86(9) . 3_656 ? O3 Co3 N22 91.14(9) 3_656 3_656 ? N16 Co3 N22 93.03(10) . 3_656 ? N16 Co3 N22 86.97(10) 3_656 3_656 ? O3 Co3 N22 91.14(9) . . ? O3 Co3 N22 88.86(9) 3_656 . ? N16 Co3 N22 86.97(10) . . ? N16 Co3 N22 93.03(10) 3_656 . ? N22 Co3 N22 180.00(12) 3_656 . ? O1B Cl1 O1D 117.6(3) . . ? O1B Cl1 O1A 110.3(2) . . ? O1D Cl1 O1A 111.6(3) . . ? O1B Cl1 O1C 105.9(3) . . ? O1D Cl1 O1C 105.9(3) . . ? O1A Cl1 O1C 104.4(3) . . ? O2B Cl2 O2D 110.9(2) . . ? O2B Cl2 O2A 109.97(18) . . ? O2D Cl2 O2A 110.5(2) . . ? O2B Cl2 O2C 109.5(2) . . ? O2D Cl2 O2C 108.2(2) . . ? O2A Cl2 O2C 107.7(2) . . ? O3D Cl3 O3C 111.8(3) . . ? O3D Cl3 O3B 116.8(4) . . ? O3C Cl3 O3B 106.3(4) . . ? O3D Cl3 O3A 107.7(4) . . ? O3C Cl3 O3A 106.8(3) . . ? O3B Cl3 O3A 107.0(3) . . ? O4C Cl4 O4D 109.7(2) . . ? O4C Cl4 O4A 111.20(19) . . ? O4D Cl4 O4A 110.17(18) . . ? O4C Cl4 O4B 108.3(2) . . ? O4D Cl4 O4B 108.2(2) . . ? O4A Cl4 O4B 109.2(2) . . ? C1 N1 C5 115.9(3) . . ? C3 N2 C8 130.9(3) . . ? C6 N3 C10 116.2(3) . . ? C15 N4 C11 115.1(3) . . ? C15 N4 Co2 120.7(2) . 2 ? C11 N4 Co2 124.0(2) . 2 ? C13 N5 C18 130.2(3) . . ? C16 N6 C20 115.8(3) . . ? C16 N6 Co2 122.4(2) . . ? C20 N6 Co2 121.5(2) . . ? C21 N7 C25 115.6(3) . . ? C21 N7 Co2 124.9(2) . . ? C25 N7 Co2 119.3(2) . . ? C23 N8 C28 129.5(3) . . ? C26 N9 C30 115.2(3) . . ? C26 N9 Co2 124.7(2) . 2_655 ? C30 N9 Co2 120.1(2) . 2_655 ? C35 N10 C31 115.6(3) . . ? C33 N11 C38 130.2(3) . . ? C40 N12 C36 116.0(4) . . ? C41 N13 C45 115.3(3) . . ? C43 N14 C48 129.8(3) . . ? C46 N15 C50 115.5(3) . . ? C55 N16 C51 115.2(3) . . ? C55 N16 Co3 121.9(2) . . ? C51 N16 Co3 122.9(2) . . ? C58 N17 C53 128.9(3) . . ? C56 N18 C60 115.6(3) . . ? C56 N18 Co1 123.7(2) . . ? C60 N18 Co1 120.58(19) . . ? C65 N19 C61 115.4(4) . . ? C63 N20 C68 132.0(3) . . ? C66 N21 C70 115.0(3) . . ? C71 N22 C75 115.9(3) . . ? C71 N22 Co3 124.8(2) . . ? C75 N22 Co3 118.9(2) . . ? C73 N23 C78 128.2(3) . . ? C80 N24 C76 116.1(3) . . ? C80 N24 Co1 123.9(2) . 1_655 ? C76 N24 Co1 119.9(2) . 1_655 ? N1 C1 C2 124.1(4) . . ? C1 C2 C3 119.6(4) . . ? N2 C3 C4 125.2(3) . . ? N2 C3 C2 117.6(3) . . ? C4 C3 C2 117.2(3) . . ? C5 C4 C3 118.2(4) . . ? N1 C5 C4 125.0(4) . . ? N3 C6 C7 123.7(3) . . ? C6 C7 C8 119.7(3) . . ? N2 C8 C9 125.5(3) . . ? N2 C8 C7 117.8(3) . . ? C9 C8 C7 116.7(3) . . ? C10 C9 C8 119.2(4) . . ? N3 C10 C9 124.5(4) . . ? N4 C11 C12 124.5(3) . . ? C11 C12 C13 119.8(3) . . ? C14 C13 N5 125.3(3) . . ? C14 C13 C12 116.3(3) . . ? N5 C13 C12 118.4(3) . . ? C13 C14 C15 119.9(3) . . ? N4 C15 C14 124.4(3) . . ? N6 C16 C17 124.5(3) . . ? C16 C17 C18 119.2(3) . . ? C17 C18 N5 124.8(3) . . ? C17 C18 C19 116.9(3) . . ? N5 C18 C19 118.2(3) . . ? C20 C19 C18 119.5(3) . . ? N6 C20 C19 124.0(3) . . ? N7 C21 C22 124.6(3) . . ? C21 C22 C23 119.1(3) . . ? N8 C23 C24 124.8(3) . . ? N8 C23 C22 118.1(3) . . ? C24 C23 C22 117.1(3) . . ? C25 C24 C23 119.2(3) . . ? N7 C25 C24 124.3(3) . . ? N9 C26 C27 125.0(3) . . ? C26 C27 C28 118.9(3) . . ? C27 C28 C29 117.1(3) . . ? C27 C28 N8 125.2(3) . . ? C29 C28 N8 117.6(3) . . ? C30 C29 C28 119.4(3) . . ? N9 C30 C29 124.2(3) . . ? N10 C31 C32 124.3(3) . . ? C31 C32 C33 119.5(3) . . ? N11 C33 C34 125.3(3) . . ? N11 C33 C32 118.0(3) . . ? C34 C33 C32 116.6(3) . . ? C35 C34 C33 119.0(3) . . ? N10 C35 C34 125.0(3) . . ? N12 C36 C37 124.8(4) . . ? C36 C37 C38 118.6(4) . . ? C37 C38 N11 124.9(3) . . ? C37 C38 C39 117.5(3) . . ? N11 C38 C39 117.4(3) . . ? C40 C39 C38 119.0(4) . . ? N12 C40 C39 124.0(4) . . ? N13 C41 C42 125.1(4) . . ? C41 C42 C43 118.8(3) . . ? N14 C43 C44 118.8(3) . . ? N14 C43 C42 124.3(3) . . ? C44 C43 C42 116.8(3) . . ? C45 C44 C43 119.4(3) . . ? N13 C45 C44 124.6(3) . . ? N15 C46 C47 125.3(4) . . ? C46 C47 C48 118.4(4) . . ? C47 C48 N14 124.2(3) . . ? C47 C48 C49 117.2(3) . . ? N14 C48 C49 118.5(3) . . ? C50 C49 C48 119.1(4) . . ? N15 C50 C49 124.4(4) . . ? N16 C51 C52 124.5(3) . . ? C51 C52 C53 119.2(3) . . ? N17 C53 C52 124.9(3) . . ? N17 C53 C54 118.0(3) . . ? C52 C53 C54 117.1(3) . . ? C55 C54 C53 119.0(3) . . ? N16 C55 C54 124.8(3) . . ? N18 C56 C57 124.8(3) . . ? C56 C57 C58 118.9(3) . . ? N17 C58 C57 124.9(3) . . ? N17 C58 C59 117.7(3) . . ? C57 C58 C59 117.4(3) . . ? C60 C59 C58 119.5(3) . . ? N18 C60 C59 123.7(3) . . ? N19 C61 C62 124.8(4) . . ? C61 C62 C63 119.0(4) . . ? C64 C63 N20 126.0(4) . . ? C64 C63 C62 117.3(4) . . ? N20 C63 C62 116.6(4) . . ? C63 C64 C65 118.3(4) . . ? N19 C65 C64 125.2(4) . . ? N21 C66 C67 125.7(4) . . ? C66 C67 C68 118.1(4) . . ? N20 C68 C67 125.0(3) . . ? N20 C68 C69 117.6(3) . . ? C67 C68 C69 117.2(3) . . ? C70 C69 C68 119.6(4) . . ? N21 C70 C69 124.4(4) . . ? N22 C71 C72 124.5(3) . . ? C71 C72 C73 118.9(3) . . ? C74 C73 N23 118.5(3) . . ? C74 C73 C72 117.4(3) . . ? N23 C73 C72 124.1(3) . . ? C75 C74 C73 119.4(3) . . ? N22 C75 C74 123.9(3) . . ? N24 C76 C77 124.0(3) . . ? C76 C77 C78 119.1(3) . . ? C77 C78 N23 123.6(3) . . ? C77 C78 C79 118.0(3) . . ? N23 C78 C79 118.4(3) . . ? C80 C79 C78 118.6(3) . . ? N24 C80 C79 124.2(3) . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 1.558 _refine_diff_density_min -0.969 _refine_diff_density_rms 0.090 # Attachment 'coso4dpafinal.cif' data_ortho _database_code_depnum_ccdc_archive 'CCDC 632671' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H20 Co N6 O7 S' _chemical_formula_weight 2189.64 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' 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' S S 0.1246 0.1234 '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 orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 16.992(3) _cell_length_b 15.164(3) _cell_length_c 17.489(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4506.5(14) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.614 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2248 _exptl_absorpt_coefficient_mu 0.911 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.665 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 ? _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 51997 _diffrn_reflns_av_R_equivalents 0.1125 _diffrn_reflns_av_sigmaI/netI 0.0646 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 28.29 _reflns_number_total 5562 _reflns_number_gt 3874 _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^)+(0.0564P)^2^+20.5481P] 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 5562 _refine_ls_number_parameters 355 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.1085 _refine_ls_R_factor_gt 0.0692 _refine_ls_wR_factor_ref 0.1715 _refine_ls_wR_factor_gt 0.1518 _refine_ls_goodness_of_fit_ref 1.113 _refine_ls_restrained_S_all 1.113 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.18284(3) 0.01304(4) 0.45184(3) 0.01370(16) Uani 1 1 d . . . S1 S 0.04097(10) 0.07633(15) 0.32781(10) 0.0235(4) Uani 0.85 1 d P . . O1 O 0.07686(18) -0.0617(2) 0.46820(19) 0.0241(7) Uani 1 1 d D . . H1A H 0.044(2) -0.035(3) 0.439(2) 0.029 Uiso 1 1 d D . . H1B H 0.058(3) -0.070(4) 0.5128(15) 0.029 Uiso 1 1 d D . . O2 O 0.12289(18) 0.0709(3) 0.3564(2) 0.0354(9) Uani 1 1 d . . . O3 O -0.0139(2) 0.0569(3) 0.3904(2) 0.0378(9) Uani 1 1 d . . . O4 O 0.0301(2) 0.1719(3) 0.3035(2) 0.0465(12) Uani 1 1 d . . . O5 O 0.0269(2) 0.0185(3) 0.2638(2) 0.0502(12) Uani 1 1 d . . . N1 N 0.28253(19) 0.0904(2) 0.4190(2) 0.0136(7) Uani 1 1 d . . . N2 N 0.6399(2) 0.3852(2) 0.4703(2) 0.0174(7) Uani 1 1 d . . . N3 N 0.4924(2) 0.2121(3) 0.3484(2) 0.0237(9) Uani 1 1 d D . . H3N H 0.503(3) 0.202(3) 0.2986(14) 0.028 Uiso 1 1 d D . . N4 N 0.2346(2) -0.4404(2) 0.0465(2) 0.0171(7) Uani 1 1 d . . . N5 N 0.3066(2) -0.2954(2) 0.2396(2) 0.0222(8) Uani 1 1 d D . . H5N H 0.347(2) -0.323(3) 0.261(3) 0.027 Uiso 1 1 d D . . N6 N 0.2214(2) -0.0897(2) 0.3763(2) 0.0173(7) Uani 1 1 d . . . C1 C 0.6198(2) 0.3992(3) 0.3972(3) 0.0173(9) Uani 1 1 d . . . H1 H 0.6386 0.4499 0.3734 0.021 Uiso 1 1 calc R . . C2 C 0.5730(2) 0.3430(3) 0.3551(3) 0.0193(9) Uani 1 1 d . . . H2 H 0.5614 0.3552 0.3042 0.023 Uiso 1 1 calc R . . C3 C 0.5434(2) 0.2680(3) 0.3901(3) 0.0189(9) Uani 1 1 d . . . C4 C 0.5667(3) 0.2499(3) 0.4648(3) 0.0275(11) Uani 1 1 d . . . H4 H 0.5511 0.1981 0.4890 0.033 Uiso 1 1 calc R . . C5 C 0.6134(3) 0.3105(3) 0.5022(3) 0.0262(11) Uani 1 1 d . . . H5 H 0.6274 0.2989 0.5526 0.031 Uiso 1 1 calc R . . C6 C 0.3118(2) 0.0822(3) 0.3478(2) 0.0167(8) Uani 1 1 d . . . H6 H 0.2838 0.0484 0.3127 0.020 Uiso 1 1 calc R . . C7 C 0.3808(2) 0.1209(3) 0.3238(3) 0.0185(9) Uani 1 1 d . . . H7 H 0.3984 0.1127 0.2739 0.022 Uiso 1 1 calc R . . C8 C 0.4246(2) 0.1729(3) 0.3746(3) 0.0150(8) Uani 1 1 d . . . C9 C 0.3935(2) 0.1850(3) 0.4478(3) 0.0175(8) Uani 1 1 d . . . H9 H 0.4192 0.2205 0.4833 0.021 Uiso 1 1 calc R . . C10 C 0.3234(2) 0.1430(3) 0.4665(2) 0.0176(9) Uani 1 1 d . . . H10 H 0.3033 0.1518 0.5154 0.021 Uiso 1 1 calc R . . C11 C 0.2948(3) -0.1220(3) 0.3816(3) 0.0198(9) Uani 1 1 d . . . H11 H 0.3276 -0.0991 0.4193 0.024 Uiso 1 1 calc R . . C12 C 0.3243(3) -0.1866(3) 0.3350(3) 0.0212(9) Uani 1 1 d . . . H12 H 0.3762 -0.2052 0.3404 0.025 Uiso 1 1 calc R . . C13 C 0.2757(3) -0.2247(3) 0.2788(3) 0.0186(9) Uani 1 1 d . . . C14 C 0.2000(2) -0.1905(3) 0.2717(3) 0.0204(9) Uani 1 1 d . . . H14 H 0.1659 -0.2119 0.2345 0.024 Uiso 1 1 calc R . . C15 C 0.1764(3) -0.1243(3) 0.3206(3) 0.0211(9) Uani 1 1 d . . . H15 H 0.1258 -0.1021 0.3147 0.025 Uiso 1 1 calc R . . C16 C 0.2067(3) -0.3591(3) 0.0605(3) 0.0207(9) Uani 1 1 d . . . H16 H 0.1711 -0.3355 0.0257 0.025 Uiso 1 1 calc R . . C17 C 0.2268(3) -0.3083(3) 0.1225(3) 0.0203(9) Uani 1 1 d . . . H17 H 0.2047 -0.2526 0.1288 0.024 Uiso 1 1 calc R . . C18 C 0.2804(3) -0.3405(3) 0.1758(3) 0.0182(9) Uani 1 1 d . . . C19 C 0.3129(3) -0.4240(3) 0.1607(3) 0.0243(10) Uani 1 1 d . . . H19 H 0.3506 -0.4480 0.1931 0.029 Uiso 1 1 calc R . . C20 C 0.2881(3) -0.4695(3) 0.0971(3) 0.0202(9) Uani 1 1 d . . . H20 H 0.3101 -0.5248 0.0884 0.024 Uiso 1 1 calc R . . O2WA O 0.0061(5) 0.4537(5) 0.3769(6) 0.050(2) Uani 0.50 1 d P . . O2WB O 0.5248(6) 0.0300(6) 0.5304(6) 0.060(3) Uani 0.50 1 d P . . O1WA O 0.0635(3) -0.2078(5) 0.1290(4) 0.0424(15) Uani 0.67 1 d P . . O1WB O -0.0466(6) 0.3638(7) 0.3524(6) 0.029(2) Uani 0.33 1 d P . . S1A S 0.0314(6) 0.1138(7) 0.3483(9) 0.033(3) Uani 0.15 1 d P . . 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 0.0089(2) 0.0176(3) 0.0146(3) 0.0014(2) -0.0005(2) -0.0017(2) S1 0.0106(7) 0.0397(12) 0.0203(8) 0.0161(8) -0.0036(6) -0.0058(8) O1 0.0139(15) 0.035(2) 0.0234(18) 0.0055(15) -0.0010(13) -0.0050(13) O2 0.0115(15) 0.068(3) 0.0263(18) 0.0200(18) -0.0045(13) -0.0110(16) O3 0.0173(16) 0.055(3) 0.041(2) 0.0188(19) 0.0017(15) -0.0009(16) O4 0.0279(19) 0.065(3) 0.047(2) 0.037(2) -0.0190(18) -0.0204(19) O5 0.031(2) 0.086(3) 0.033(2) 0.013(2) -0.0113(17) -0.012(2) N1 0.0087(15) 0.0161(17) 0.0160(17) -0.0001(14) 0.0023(13) 0.0018(13) N2 0.0113(16) 0.0180(18) 0.0228(19) 0.0033(14) -0.0030(14) -0.0015(14) N3 0.0152(17) 0.028(2) 0.028(2) -0.0078(18) 0.0059(16) -0.0106(16) N4 0.0140(16) 0.0200(19) 0.0173(18) -0.0002(15) 0.0004(14) 0.0013(14) N5 0.025(2) 0.0178(18) 0.023(2) -0.0058(15) -0.0123(16) 0.0087(15) N6 0.0160(17) 0.0172(18) 0.0188(18) -0.0021(14) -0.0030(14) -0.0038(14) C1 0.0146(19) 0.016(2) 0.022(2) 0.0036(17) -0.0013(16) -0.0014(16) C2 0.018(2) 0.025(2) 0.015(2) -0.0013(17) 0.0022(17) -0.0026(17) C3 0.0096(18) 0.013(2) 0.034(3) -0.0025(18) 0.0007(17) -0.0005(15) C4 0.025(2) 0.021(2) 0.036(3) 0.009(2) -0.007(2) -0.0051(19) C5 0.023(2) 0.025(2) 0.030(3) 0.014(2) -0.010(2) -0.0075(19) C6 0.0129(18) 0.019(2) 0.018(2) -0.0011(17) -0.0024(16) -0.0010(16) C7 0.018(2) 0.020(2) 0.018(2) -0.0035(17) 0.0050(17) -0.0008(17) C8 0.0096(17) 0.0105(19) 0.025(2) -0.0006(16) 0.0023(16) -0.0013(15) C9 0.0142(19) 0.016(2) 0.022(2) -0.0018(18) -0.0036(17) -0.0016(15) C10 0.018(2) 0.016(2) 0.019(2) -0.0002(16) 0.0003(17) 0.0002(16) C11 0.017(2) 0.023(2) 0.019(2) -0.0024(18) -0.0055(17) -0.0028(17) C12 0.020(2) 0.019(2) 0.024(2) -0.0007(18) -0.0077(18) 0.0040(18) C13 0.022(2) 0.016(2) 0.018(2) 0.0014(17) -0.0023(17) -0.0015(17) C14 0.016(2) 0.025(2) 0.021(2) -0.0014(18) -0.0049(17) -0.0048(17) C15 0.0138(19) 0.027(2) 0.022(2) -0.0018(18) -0.0008(17) -0.0018(18) C16 0.021(2) 0.019(2) 0.022(2) 0.0042(18) -0.0055(18) 0.0060(17) C17 0.020(2) 0.019(2) 0.021(2) -0.0017(18) -0.0060(17) 0.0049(17) C18 0.020(2) 0.014(2) 0.020(2) -0.0034(17) -0.0028(17) -0.0002(16) C19 0.021(2) 0.024(2) 0.028(2) -0.0057(19) -0.0114(19) 0.0074(19) C20 0.020(2) 0.014(2) 0.026(2) -0.0063(18) -0.0044(18) 0.0046(16) O2WA 0.049(5) 0.029(4) 0.072(6) 0.010(4) 0.001(5) -0.003(4) O2WB 0.080(7) 0.039(5) 0.062(6) 0.011(4) -0.011(5) 0.012(5) O1WA 0.029(3) 0.058(4) 0.040(4) -0.001(3) 0.001(3) -0.006(3) O1WB 0.032(6) 0.031(6) 0.024(5) -0.001(5) 0.001(4) 0.005(5) S1A 0.009(4) 0.021(5) 0.069(9) 0.019(5) -0.007(5) 0.000(4) _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 N1 2.139(3) . ? Co1 O2 2.143(3) . ? Co1 N6 2.145(4) . ? Co1 O1 2.147(3) . ? Co1 N4 2.174(4) 7_556 ? Co1 N2 2.184(4) 4_456 ? S1 O5 1.442(5) . ? S1 O3 1.468(4) . ? S1 O2 1.481(4) . ? S1 O4 1.522(5) . ? O1 H1A 0.853(19) . ? O1 H1B 0.852(19) . ? O2 S1A 1.691(11) . ? O3 S1A 1.372(12) . ? O4 S1A 1.180(12) . ? N1 C10 1.345(5) . ? N1 C6 1.348(5) . ? N2 C5 1.340(6) . ? N2 C1 1.341(6) . ? N3 C8 1.374(5) . ? N3 C3 1.415(6) . ? N3 H3N 0.903(19) . ? N4 C20 1.344(6) . ? N4 C16 1.344(6) . ? N5 C13 1.376(6) . ? N5 C18 1.383(6) . ? N5 H5N 0.882(19) . ? N6 C11 1.344(5) . ? N6 C15 1.345(6) . ? C1 C2 1.379(6) . ? C1 H1 0.9300 . ? C2 C3 1.387(6) . ? C2 H2 0.9300 . ? C3 C4 1.393(7) . ? C4 C5 1.380(7) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.377(6) . ? C6 H6 0.9300 . ? C7 C8 1.402(6) . ? C7 H7 0.9300 . ? C8 C9 1.397(6) . ? C9 C10 1.390(6) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.369(6) . ? C11 H11 0.9300 . ? C12 C13 1.407(6) . ? C12 H12 0.9300 . ? C13 C14 1.394(6) . ? C14 C15 1.378(6) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.372(6) . ? C16 H16 0.9300 . ? C17 C18 1.393(6) . ? C17 H17 0.9300 . ? C18 C19 1.406(6) . ? C19 C20 1.375(6) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? 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 Co1 O2 86.73(13) . . ? N1 Co1 N6 89.49(13) . . ? O2 Co1 N6 87.84(15) . . ? N1 Co1 O1 171.71(13) . . ? O2 Co1 O1 85.48(13) . . ? N6 Co1 O1 87.40(13) . . ? N1 Co1 N4 99.30(13) . 7_556 ? O2 Co1 N4 173.02(14) . 7_556 ? N6 Co1 N4 88.70(14) . 7_556 ? O1 Co1 N4 88.31(13) . 7_556 ? N1 Co1 N2 92.57(13) . 4_456 ? O2 Co1 N2 92.16(15) . 4_456 ? N6 Co1 N2 177.94(13) . 4_456 ? O1 Co1 N2 90.54(13) . 4_456 ? N4 Co1 N2 91.08(14) 7_556 4_456 ? O5 S1 O3 110.6(3) . . ? O5 S1 O2 112.6(3) . . ? O3 S1 O2 109.5(2) . . ? O5 S1 O4 110.0(3) . . ? O3 S1 O4 108.8(3) . . ? O2 S1 O4 105.1(2) . . ? Co1 O1 H1A 103(4) . . ? Co1 O1 H1B 121(4) . . ? H1A O1 H1B 112(4) . . ? S1 O2 S1A 24.1(4) . . ? S1 O2 Co1 137.1(2) . . ? S1A O2 Co1 131.2(5) . . ? S1A O3 S1 27.9(5) . . ? S1A O4 S1 25.9(7) . . ? S1 O5 S1A 9.7(3) . . ? C10 N1 C6 115.8(4) . . ? C10 N1 Co1 124.6(3) . . ? C6 N1 Co1 119.4(3) . . ? C5 N2 C1 116.5(4) . . ? C5 N2 Co1 116.7(3) . 4_556 ? C1 N2 Co1 124.6(3) . 4_556 ? C8 N3 C3 126.9(4) . . ? C8 N3 H3N 115(3) . . ? C3 N3 H3N 119(3) . . ? C20 N4 C16 114.8(4) . . ? C20 N4 Co1 127.5(3) . 7 ? C16 N4 Co1 117.5(3) . 7 ? C13 N5 C18 131.7(4) . . ? C13 N5 H5N 118(3) . . ? C18 N5 H5N 110(3) . . ? C11 N6 C15 115.8(4) . . ? C11 N6 Co1 120.4(3) . . ? C15 N6 Co1 123.8(3) . . ? N2 C1 C2 123.9(4) . . ? N2 C1 H1 118.0 . . ? C2 C1 H1 118.0 . . ? C1 C2 C3 118.7(4) . . ? C1 C2 H2 120.6 . . ? C3 C2 H2 120.6 . . ? C2 C3 C4 118.3(4) . . ? C2 C3 N3 119.0(4) . . ? C4 C3 N3 122.7(4) . . ? C5 C4 C3 118.5(4) . . ? C5 C4 H4 120.8 . . ? C3 C4 H4 120.8 . . ? N2 C5 C4 124.0(4) . . ? N2 C5 H5 118.0 . . ? C4 C5 H5 118.0 . . ? N1 C6 C7 123.9(4) . . ? N1 C6 H6 118.1 . . ? C7 C6 H6 118.1 . . ? C6 C7 C8 119.9(4) . . ? C6 C7 H7 120.0 . . ? C8 C7 H7 120.0 . . ? N3 C8 C9 124.5(4) . . ? N3 C8 C7 118.4(4) . . ? C9 C8 C7 117.0(4) . . ? C10 C9 C8 118.7(4) . . ? C10 C9 H9 120.7 . . ? C8 C9 H9 120.7 . . ? N1 C10 C9 124.7(4) . . ? N1 C10 H10 117.7 . . ? C9 C10 H10 117.7 . . ? N6 C11 C12 124.0(4) . . ? N6 C11 H11 118.0 . . ? C12 C11 H11 118.0 . . ? C11 C12 C13 119.6(4) . . ? C11 C12 H12 120.2 . . ? C13 C12 H12 120.2 . . ? N5 C13 C14 126.7(4) . . ? N5 C13 C12 116.4(4) . . ? C14 C13 C12 116.8(4) . . ? C15 C14 C13 119.0(4) . . ? C15 C14 H14 120.5 . . ? C13 C14 H14 120.5 . . ? N6 C15 C14 124.7(4) . . ? N6 C15 H15 117.7 . . ? C14 C15 H15 117.7 . . ? N4 C16 C17 124.9(4) . . ? N4 C16 H16 117.5 . . ? C17 C16 H16 117.5 . . ? C16 C17 C18 119.6(4) . . ? C16 C17 H17 120.2 . . ? C18 C17 H17 120.2 . . ? N5 C18 C17 125.2(4) . . ? N5 C18 C19 118.1(4) . . ? C17 C18 C19 116.6(4) . . ? C20 C19 C18 118.9(4) . . ? C20 C19 H19 120.5 . . ? C18 C19 H19 120.5 . . ? N4 C20 C19 125.1(4) . . ? N4 C20 H20 117.4 . . ? C19 C20 H20 117.4 . . ? O2WB O2WA O1WB 117.9(7) 4_456 . ? O2WB O2WB O2WA 128.1(11) 5_656 4_556 ? O1WA O1WB O2WA 144.1(9) 3 . ? O4 S1A O3 144.7(9) . . ? O4 S1A O2 111.1(8) . . ? O3 S1A O2 103.2(7) . . ? O4 S1A O5 92.6(9) . . ? O3 S1A O5 85.5(6) . . ? O2 S1A O5 79.9(6) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.125 _refine_diff_density_min -0.768 _refine_diff_density_rms 0.132 # Attachment 'cono3dpafinal.cif' data_mono2 _database_code_depnum_ccdc_archive 'CCDC 632672' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H40 Co2 N16 O14' _chemical_formula_weight 1086.74 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' 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 Cc 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' _cell_length_a 24.00(2) _cell_length_b 15.522(16) _cell_length_c 16.523(17) _cell_angle_alpha 90.00 _cell_angle_beta 133.517(3) _cell_angle_gamma 90.00 _cell_volume 4463(8) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.617 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2232 _exptl_absorpt_coefficient_mu 0.831 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.751 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 ? _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 26859 _diffrn_reflns_av_R_equivalents 0.0427 _diffrn_reflns_av_sigmaI/netI 0.0636 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 28.56 _reflns_number_total 10675 _reflns_number_gt 9318 _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^)+(0.0316P)^2^+19.2133P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.063(16) _refine_ls_number_reflns 10675 _refine_ls_number_parameters 673 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0659 _refine_ls_R_factor_gt 0.0545 _refine_ls_wR_factor_ref 0.1229 _refine_ls_wR_factor_gt 0.1183 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.093 _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 0.74090(3) 0.99134(4) 1.00112(4) 0.01345(13) Uani 1 1 d . . . Co2 Co 0.82874(3) 0.49898(4) 1.58671(4) 0.01463(13) Uani 1 1 d . . . N1 N 0.7129(2) 0.9200(2) 1.8676(3) 0.0158(7) Uani 1 1 d . . . N2 N 0.7556(2) 0.5992(2) 1.5658(3) 0.0185(8) Uani 1 1 d . . . N3 N 0.6348(2) 0.7696(3) 1.5974(3) 0.0230(9) Uani 1 1 d D . . H3N H 0.5842(12) 0.773(4) 1.546(3) 0.028 Uiso 1 1 d D . . N4 N 0.6703(2) 1.0969(2) 0.8935(3) 0.0175(8) Uani 1 1 d . . . N5 N 0.3401(2) 1.4407(2) 0.5562(3) 0.0164(7) Uani 1 1 d . . . N6 N 0.5425(2) 1.3095(3) 0.6901(3) 0.0206(8) Uani 1 1 d D . . H6N H 0.556(3) 1.335(3) 0.657(4) 0.025 Uiso 1 1 d D . . N7 N 0.8137(2) 0.8925(2) 1.1231(3) 0.0169(8) Uani 1 1 d . . . N8 N 0.8658(2) 0.5818(2) 1.5276(3) 0.0179(8) Uani 1 1 d . . . N9 N 0.9402(2) 0.7360(3) 1.4078(3) 0.0205(8) Uani 1 1 d D . . H9N H 0.9903(12) 0.737(3) 1.450(4) 0.025 Uiso 1 1 d D . . N10 N 0.9004(2) 0.3964(2) 1.6153(3) 0.0174(8) Uani 1 1 d . . . N11 N 1.2324(2) 0.0640(2) 1.9361(3) 0.0201(8) Uani 1 1 d . . . N12 N 1.0312(2) 0.1866(3) 1.6591(3) 0.0222(8) Uani 1 1 d D . . H12N H 1.004(3) 0.161(3) 1.593(3) 0.027 Uiso 1 1 d D . . N13 N 0.6124(2) 0.9085(3) 0.9936(3) 0.0257(9) Uani 1 1 d . . . N14 N 0.9369(2) 0.5769(3) 1.8332(3) 0.0248(9) Uani 1 1 d . . . N15 N 0.9178(2) 0.9072(3) 0.8892(3) 0.0278(9) Uani 1 1 d . . . N16 N 1.1410(2) 0.8753(3) 1.6005(4) 0.0261(9) Uani 1 1 d . . . O1 O 0.74299(19) 1.0491(2) 1.1192(3) 0.0212(7) Uani 1 1 d D . . H1A H 0.7835(17) 1.042(4) 1.186(2) 0.025 Uiso 1 1 d D . . H1B H 0.7004(16) 1.029(3) 1.093(4) 0.025 Uiso 1 1 d D . . O2 O 0.8109(2) 0.4311(2) 1.6773(3) 0.0236(7) Uani 1 1 d D . . H2A H 0.7649(15) 0.417(3) 1.643(4) 0.028 Uiso 1 1 d D . . H2B H 0.833(3) 0.456(3) 1.739(3) 0.028 Uiso 1 1 d D . . O3 O 0.63527(19) 0.9237(2) 0.9441(3) 0.0222(7) Uani 1 1 d . . . O4 O 0.6139(3) 0.9675(3) 1.0453(4) 0.0504(12) Uani 1 1 d . . . O5 O 0.5879(2) 0.8366(2) 0.9870(3) 0.0322(8) Uani 1 1 d . . . O6 O 0.9788(2) 0.6388(3) 1.8913(3) 0.0366(9) Uani 1 1 d . . . O7 O 0.93037(19) 0.5539(2) 1.7530(3) 0.0249(7) Uani 1 1 d . . . O8 O 0.8992(3) 0.5403(3) 1.8499(4) 0.0524(13) Uani 1 1 d . . . O9 O 0.8698(2) 0.9674(3) 0.8348(3) 0.0394(10) Uani 1 1 d . . . O10 O 0.9817(2) 0.9233(3) 0.9836(3) 0.0443(11) Uani 1 1 d . . . O11 O 0.9022(3) 0.8345(3) 0.8509(3) 0.0415(10) Uani 1 1 d . . . O12 O 1.0765(2) 0.8565(3) 1.5637(3) 0.0424(10) Uani 1 1 d . . . O13 O 1.1964(2) 0.8790(3) 1.7017(3) 0.0479(11) Uani 1 1 d . . . O14 O 1.1509(3) 0.8883(4) 1.5374(4) 0.0566(13) Uani 1 1 d . . . C1 C 0.7583(2) 0.8609(3) 1.8790(4) 0.0180(9) Uani 1 1 d . . . H1 H 0.8076 0.8541 1.9491 0.022 Uiso 1 1 calc R . . C2 C 0.7366(3) 0.8089(3) 1.7926(4) 0.0199(9) Uani 1 1 d . . . H2 H 0.7702 0.7680 1.8051 0.024 Uiso 1 1 calc R . . C3 C 0.6635(3) 0.8194(3) 1.6871(4) 0.0175(9) Uani 1 1 d . . . C4 C 0.6163(3) 0.8831(3) 1.6740(4) 0.0195(9) Uani 1 1 d . . . H4 H 0.5676 0.8935 1.6043 0.023 Uiso 1 1 calc R . . C5 C 0.6426(3) 0.9296(3) 1.7651(4) 0.0230(10) Uani 1 1 d . . . H5 H 0.6099 0.9702 1.7553 0.028 Uiso 1 1 calc R . . C6 C 0.7871(3) 0.6732(3) 1.6231(4) 0.0220(10) Uani 1 1 d . . . H6 H 0.8367 0.6860 1.6558 0.026 Uiso 1 1 calc R . . C7 C 0.7507(3) 0.7313(3) 1.6365(4) 0.0201(9) Uani 1 1 d . . . H7 H 0.7755 0.7813 1.6779 0.024 Uiso 1 1 calc R . . C8 C 0.6753(3) 0.7134(3) 1.5862(4) 0.0201(9) Uani 1 1 d . . . C9 C 0.6397(3) 0.6398(3) 1.5216(4) 0.0241(10) Uani 1 1 d . . . H9 H 0.5891 0.6271 1.4843 0.029 Uiso 1 1 calc R . . C10 C 0.6818(3) 0.5863(3) 1.5146(4) 0.0248(10) Uani 1 1 d . . . H10 H 0.6575 0.5371 1.4709 0.030 Uiso 1 1 calc R . . C11 C 0.6880(3) 1.1436(3) 0.8455(4) 0.0287(11) Uani 1 1 d . . . H11 H 0.7306 1.1273 0.8578 0.034 Uiso 1 1 calc R . . C12 C 0.6467(3) 1.2139(3) 0.7793(5) 0.0278(11) Uani 1 1 d . . . H12 H 0.6615 1.2446 0.7483 0.033 Uiso 1 1 calc R . . C13 C 0.5819(2) 1.2389(3) 0.7589(4) 0.0197(9) Uani 1 1 d . . . C14 C 0.5625(3) 1.1911(3) 0.8072(4) 0.0229(10) Uani 1 1 d . . . H14 H 0.5199 1.2055 0.7958 0.028 Uiso 1 1 calc R . . C15 C 0.6080(3) 1.1213(3) 0.8726(4) 0.0199(10) Uani 1 1 d . . . H15 H 0.5944 1.0892 0.9043 0.024 Uiso 1 1 calc R . . C16 C 0.3738(3) 1.3848(3) 0.6405(4) 0.0267(11) Uani 1 1 d . . . H16 H 0.3503 1.3754 0.6668 0.032 Uiso 1 1 calc R . . C17 C 0.4414(3) 1.3396(3) 0.6920(4) 0.0260(10) Uani 1 1 d . . . H17 H 0.4633 1.3038 0.7527 0.031 Uiso 1 1 calc R . . C18 C 0.4756(3) 1.3496(3) 0.6492(4) 0.0173(9) Uani 1 1 d . . . C19 C 0.4417(3) 1.4085(3) 0.5627(4) 0.0214(10) Uani 1 1 d . . . H19 H 0.4634 1.4193 0.5339 0.026 Uiso 1 1 calc R . . C20 C 0.3755(3) 1.4506(3) 0.5199(4) 0.0228(10) Uani 1 1 d . . . H20 H 0.3537 1.4888 0.4614 0.027 Uiso 1 1 calc R . . C21 C 0.8893(3) 0.9018(3) 1.2092(4) 0.0204(9) Uani 1 1 d . . . H21 H 0.9144 0.9444 1.2048 0.024 Uiso 1 1 calc R . . C22 C 0.9327(3) 0.8515(3) 1.3047(4) 0.0215(10) Uani 1 1 d . . . H22 H 0.9853 0.8606 1.3625 0.026 Uiso 1 1 calc R . . C23 C 0.8962(3) 0.7868(3) 1.3129(4) 0.0168(9) Uani 1 1 d . . . C24 C 0.8181(3) 0.7741(3) 1.2219(4) 0.0179(9) Uani 1 1 d . . . H24 H 0.7920 0.7306 1.2230 0.022 Uiso 1 1 calc R . . C25 C 0.7802(3) 0.8264(3) 1.1306(4) 0.0200(9) Uani 1 1 d . . . H25 H 0.7282 0.8161 1.0697 0.024 Uiso 1 1 calc R . . C26 C 0.8228(3) 0.6479(3) 1.4580(4) 0.0200(9) Uani 1 1 d . . . H26 H 0.7757 0.6579 1.4358 0.024 Uiso 1 1 calc R . . C27 C 0.8448(3) 0.7012(3) 1.4182(4) 0.0218(9) Uani 1 1 d . . . H27 H 0.8139 0.7476 1.3730 0.026 Uiso 1 1 calc R . . C28 C 0.9137(3) 0.6861(3) 1.4453(4) 0.0173(9) Uani 1 1 d . . . C29 C 0.9611(3) 0.6206(3) 1.5229(4) 0.0204(9) Uani 1 1 d . . . H29 H 1.0092 0.6102 1.5486 0.024 Uiso 1 1 calc R . . C30 C 0.9347(3) 0.5720(3) 1.5600(4) 0.0180(9) Uani 1 1 d . . . H30 H 0.9668 0.5289 1.6117 0.022 Uiso 1 1 calc R . . C31 C 0.9538(3) 0.3590(3) 1.7142(4) 0.0211(10) Uani 1 1 d . . . H31 H 0.9614 0.3807 1.7737 0.025 Uiso 1 1 calc R . . C32 C 0.9985(3) 0.2905(3) 1.7350(4) 0.0208(10) Uani 1 1 d . . . H32 H 1.0339 0.2665 1.8061 0.025 Uiso 1 1 calc R . . C33 C 0.9908(2) 0.2575(3) 1.6505(4) 0.0181(9) Uani 1 1 d . . . C34 C 0.9345(3) 0.2952(3) 1.5450(4) 0.0191(9) Uani 1 1 d . . . H34 H 0.9257 0.2743 1.4843 0.023 Uiso 1 1 calc R . . C35 C 0.8927(2) 0.3627(3) 1.5321(4) 0.0173(9) Uani 1 1 d . . . H35 H 0.8565 0.3874 1.4616 0.021 Uiso 1 1 calc R . . C36 C 1.2165(3) 0.1456(3) 1.9429(4) 0.0195(9) Uani 1 1 d . . . H36 H 1.2521 0.1736 2.0113 0.023 Uiso 1 1 calc R . . C37 C 1.1516(3) 0.1903(3) 1.8564(4) 0.0200(9) Uani 1 1 d . . . H37 H 1.1436 0.2464 1.8662 0.024 Uiso 1 1 calc R . . C38 C 1.0989(3) 0.1499(3) 1.7545(4) 0.0200(9) Uani 1 1 d . . . C39 C 1.1167(3) 0.0668(3) 1.7446(4) 0.0242(10) Uani 1 1 d . . . H39 H 1.0836 0.0383 1.6764 0.029 Uiso 1 1 calc R . . C40 C 1.1826(3) 0.0284(3) 1.8353(4) 0.0244(10) Uani 1 1 d . . . H40 H 1.1936 -0.0263 1.8264 0.029 Uiso 1 1 calc R . . 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 0.0142(3) 0.0103(3) 0.0146(3) -0.0005(2) 0.0095(2) 0.0000(2) Co2 0.0163(3) 0.0111(3) 0.0164(3) -0.0003(2) 0.0112(3) -0.0009(2) N1 0.0127(17) 0.0167(18) 0.0170(18) -0.0002(14) 0.0099(16) 0.0000(14) N2 0.022(2) 0.0120(17) 0.024(2) 0.0000(15) 0.0170(18) -0.0001(15) N3 0.018(2) 0.028(2) 0.020(2) -0.0026(16) 0.0120(17) 0.0050(17) N4 0.0184(19) 0.0124(17) 0.0216(19) -0.0014(14) 0.0137(17) -0.0023(14) N5 0.0191(19) 0.0113(18) 0.0181(18) 0.0005(14) 0.0125(16) 0.0003(14) N6 0.022(2) 0.0201(19) 0.027(2) 0.0107(16) 0.0196(18) 0.0103(16) N7 0.022(2) 0.0102(17) 0.0174(18) -0.0005(14) 0.0129(17) 0.0010(15) N8 0.0199(19) 0.0128(17) 0.0196(19) 0.0008(14) 0.0130(17) -0.0018(15) N9 0.0130(18) 0.025(2) 0.0195(19) 0.0079(16) 0.0095(16) 0.0017(16) N10 0.0157(18) 0.0181(19) 0.0165(18) -0.0014(15) 0.0103(16) -0.0020(15) N11 0.0180(19) 0.019(2) 0.0205(19) 0.0001(16) 0.0122(17) 0.0015(16) N12 0.022(2) 0.021(2) 0.0137(18) -0.0005(15) 0.0083(17) 0.0051(16) N13 0.014(2) 0.038(3) 0.023(2) -0.0058(18) 0.0122(18) -0.0035(18) N14 0.023(2) 0.027(2) 0.018(2) 0.0000(17) 0.0113(18) 0.0026(18) N15 0.028(2) 0.032(2) 0.019(2) 0.0036(18) 0.0144(19) 0.0000(19) N16 0.023(2) 0.028(2) 0.031(2) 0.0037(18) 0.020(2) 0.0026(17) O1 0.0200(17) 0.0255(18) 0.0161(16) 0.0022(13) 0.0117(15) 0.0009(14) O2 0.0264(19) 0.0226(18) 0.0270(18) -0.0008(14) 0.0204(17) -0.0041(14) O3 0.0199(17) 0.0296(18) 0.0195(16) 0.0019(14) 0.0145(15) -0.0041(14) O4 0.067(3) 0.041(2) 0.078(3) -0.028(2) 0.064(3) -0.022(2) O5 0.033(2) 0.034(2) 0.034(2) -0.0048(17) 0.0250(18) -0.0140(17) O6 0.037(2) 0.042(2) 0.030(2) -0.0184(17) 0.0233(18) -0.0152(18) O7 0.0213(17) 0.036(2) 0.0204(16) -0.0054(15) 0.0155(15) 0.0000(15) O8 0.077(3) 0.061(3) 0.043(2) -0.019(2) 0.051(3) -0.036(3) O9 0.039(2) 0.041(2) 0.0260(19) 0.0049(17) 0.0176(18) 0.0109(18) O10 0.037(2) 0.040(2) 0.0229(19) 0.0048(17) 0.0077(18) -0.0020(18) O11 0.058(3) 0.034(2) 0.029(2) -0.0014(17) 0.028(2) -0.0062(19) O12 0.0210(19) 0.074(3) 0.031(2) 0.010(2) 0.0175(18) -0.0044(19) O13 0.029(2) 0.055(3) 0.036(2) -0.015(2) 0.013(2) -0.007(2) O14 0.068(3) 0.075(4) 0.062(3) -0.003(3) 0.058(3) -0.012(3) C1 0.013(2) 0.024(2) 0.014(2) 0.0007(17) 0.0082(18) -0.0006(17) C2 0.021(2) 0.017(2) 0.023(2) 0.0022(18) 0.016(2) 0.0056(18) C3 0.021(2) 0.017(2) 0.017(2) -0.0042(17) 0.014(2) 0.0010(17) C4 0.020(2) 0.019(2) 0.020(2) -0.0017(17) 0.014(2) -0.0002(18) C5 0.022(2) 0.025(3) 0.027(3) -0.002(2) 0.019(2) 0.0040(19) C6 0.019(2) 0.021(2) 0.028(2) 0.0001(19) 0.018(2) 0.0001(18) C7 0.022(2) 0.017(2) 0.023(2) -0.0032(18) 0.016(2) -0.0015(18) C8 0.024(2) 0.019(2) 0.018(2) 0.0001(17) 0.015(2) 0.0053(18) C9 0.014(2) 0.026(3) 0.025(2) -0.007(2) 0.011(2) -0.0035(19) C10 0.026(3) 0.024(2) 0.028(2) -0.010(2) 0.020(2) -0.005(2) C11 0.020(2) 0.035(3) 0.034(3) 0.013(2) 0.020(2) 0.014(2) C12 0.028(3) 0.029(3) 0.041(3) 0.014(2) 0.029(3) 0.006(2) C13 0.014(2) 0.013(2) 0.020(2) 0.0037(17) 0.0068(19) 0.0067(17) C14 0.026(2) 0.023(2) 0.029(3) 0.008(2) 0.023(2) 0.0104(19) C15 0.024(2) 0.018(2) 0.026(2) 0.0086(19) 0.020(2) 0.0070(19) C16 0.029(3) 0.028(3) 0.036(3) 0.007(2) 0.028(3) 0.009(2) C17 0.029(3) 0.018(2) 0.032(3) 0.012(2) 0.021(2) 0.0086(19) C18 0.018(2) 0.0111(19) 0.022(2) 0.0004(16) 0.0133(19) 0.0005(16) C19 0.024(2) 0.017(2) 0.032(3) 0.0041(19) 0.023(2) 0.0044(19) C20 0.023(2) 0.021(2) 0.024(2) 0.0045(19) 0.016(2) 0.0047(19) C21 0.021(2) 0.021(2) 0.023(2) 0.0029(18) 0.017(2) 0.0001(18) C22 0.014(2) 0.026(2) 0.020(2) 0.0058(19) 0.010(2) 0.0032(19) C23 0.023(2) 0.016(2) 0.017(2) 0.0010(17) 0.0152(19) 0.0025(17) C24 0.020(2) 0.013(2) 0.022(2) 0.0019(17) 0.015(2) -0.0003(17) C25 0.021(2) 0.016(2) 0.019(2) -0.0004(17) 0.012(2) -0.0008(18) C26 0.015(2) 0.020(2) 0.023(2) 0.0004(18) 0.012(2) 0.0031(17) C27 0.021(2) 0.017(2) 0.022(2) 0.0036(18) 0.013(2) 0.0036(18) C28 0.018(2) 0.017(2) 0.014(2) -0.0018(17) 0.0095(19) -0.0023(17) C29 0.020(2) 0.017(2) 0.023(2) 0.0031(18) 0.015(2) 0.0032(17) C30 0.018(2) 0.011(2) 0.017(2) 0.0038(17) 0.0097(19) 0.0030(17) C31 0.017(2) 0.026(2) 0.018(2) 0.0012(19) 0.010(2) 0.0014(18) C32 0.023(2) 0.025(2) 0.015(2) 0.0037(18) 0.014(2) 0.0011(19) C33 0.013(2) 0.019(2) 0.020(2) 0.0034(17) 0.0103(19) 0.0012(17) C34 0.018(2) 0.018(2) 0.015(2) -0.0051(17) 0.0092(19) -0.0008(17) C35 0.017(2) 0.017(2) 0.012(2) 0.0007(16) 0.0075(18) 0.0008(17) C36 0.020(2) 0.024(2) 0.016(2) -0.0047(18) 0.013(2) -0.0045(19) C37 0.019(2) 0.017(2) 0.023(2) -0.0018(17) 0.014(2) -0.0005(17) C38 0.017(2) 0.017(2) 0.025(2) 0.0025(18) 0.014(2) 0.0038(17) C39 0.019(2) 0.027(3) 0.018(2) -0.0090(19) 0.009(2) -0.0018(19) C40 0.023(2) 0.017(2) 0.023(2) -0.0021(18) 0.012(2) 0.0057(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 O1 2.116(4) . ? Co1 N1 2.122(4) 1_554 ? Co1 N4 2.137(4) . ? Co1 N7 2.149(4) . ? Co1 N5 2.151(4) 4_575 ? Co1 O3 2.265(4) . ? Co2 O2 2.102(4) . ? Co2 N11 2.137(4) 4_454 ? Co2 N8 2.144(4) . ? Co2 N10 2.144(4) . ? Co2 N2 2.188(4) . ? Co2 O7 2.235(4) . ? N1 C1 1.335(6) . ? N1 C5 1.342(6) . ? N2 C6 1.342(6) . ? N2 C10 1.351(6) . ? N3 C3 1.365(6) . ? N3 C8 1.409(6) . ? N3 H3N 0.88(2) . ? N4 C15 1.337(6) . ? N4 C11 1.341(6) . ? N5 C16 1.340(6) . ? N5 C20 1.344(6) . ? N6 C13 1.380(6) . ? N6 C18 1.388(6) . ? N6 H6N 0.89(2) . ? N7 C21 1.335(6) . ? N7 C25 1.361(6) . ? N8 C26 1.344(6) . ? N8 C30 1.350(6) . ? N9 C23 1.384(6) . ? N9 C28 1.389(6) . ? N9 H9N 0.882(19) . ? N10 C31 1.329(6) . ? N10 C35 1.360(6) . ? N11 C40 1.330(6) . ? N11 C36 1.351(6) . ? N12 C38 1.386(6) . ? N12 C33 1.408(6) . ? N12 H12N 0.89(2) . ? N13 O5 1.230(6) . ? N13 O4 1.237(6) . ? N13 O3 1.281(5) . ? N14 O6 1.236(6) . ? N14 O8 1.249(6) . ? N14 O7 1.274(5) . ? N15 O11 1.219(6) . ? N15 O10 1.247(6) . ? N15 O9 1.258(6) . ? N16 O13 1.227(6) . ? N16 O14 1.234(6) . ? N16 O12 1.248(6) . ? O1 H1A 0.831(19) . ? O1 H1B 0.848(19) . ? O2 H2A 0.850(19) . ? O2 H2B 0.849(19) . ? C1 C2 1.392(6) . ? C1 H1 0.9300 . ? C2 C3 1.389(6) . ? C2 H2 0.9300 . ? C3 C4 1.404(6) . ? C4 C5 1.370(7) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.375(6) . ? C6 H6 0.9300 . ? C7 C8 1.405(7) . ? C7 H7 0.9300 . ? C8 C9 1.384(7) . ? C9 C10 1.374(7) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.370(7) . ? C11 H11 0.9300 . ? C12 C13 1.402(7) . ? C12 H12 0.9300 . ? C13 C14 1.384(7) . ? C14 C15 1.381(6) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.394(7) . ? C16 H16 0.9300 . ? C17 C18 1.414(7) . ? C17 H17 0.9300 . ? C18 C19 1.392(6) . ? C19 C20 1.379(7) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 C22 1.387(6) . ? C21 H21 0.9300 . ? C22 C23 1.398(6) . ? C22 H22 0.9300 . ? C23 C24 1.390(6) . ? C24 C25 1.369(6) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 C27 1.369(7) . ? C26 H26 0.9300 . ? C27 C28 1.405(7) . ? C27 H27 0.9300 . ? C28 C29 1.401(6) . ? C29 C30 1.371(7) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C32 1.377(7) . ? C31 H31 0.9300 . ? C32 C33 1.374(7) . ? C32 H32 0.9300 . ? C33 C34 1.401(6) . ? C34 C35 1.361(6) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C36 C37 1.373(6) . ? C36 H36 0.9300 . ? C37 C38 1.376(7) . ? C37 H37 0.9300 . ? C38 C39 1.404(7) . ? C39 C40 1.355(7) . ? C39 H39 0.9300 . ? C40 H40 0.9300 . ? 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 Co1 N1 165.71(14) . 1_554 ? O1 Co1 N4 86.82(16) . . ? N1 Co1 N4 91.88(16) 1_554 . ? O1 Co1 N7 87.13(15) . . ? N1 Co1 N7 94.22(16) 1_554 . ? N4 Co1 N7 173.88(14) . . ? O1 Co1 N5 94.88(14) . 4_575 ? N1 Co1 N5 99.33(14) 1_554 4_575 ? N4 Co1 N5 89.31(16) . 4_575 ? N7 Co1 N5 90.29(16) . 4_575 ? O1 Co1 O3 83.64(13) . . ? N1 Co1 O3 82.12(13) 1_554 . ? N4 Co1 O3 89.48(15) . . ? N7 Co1 O3 90.77(15) . . ? N5 Co1 O3 178.14(14) 4_575 . ? O2 Co2 N11 90.72(17) . 4_454 ? O2 Co2 N8 167.77(15) . . ? N11 Co2 N8 101.47(17) 4_454 . ? O2 Co2 N10 89.81(15) . . ? N11 Co2 N10 88.69(16) 4_454 . ? N8 Co2 N10 91.37(16) . . ? O2 Co2 N2 86.20(15) . . ? N11 Co2 N2 91.98(17) 4_454 . ? N8 Co2 N2 92.40(16) . . ? N10 Co2 N2 175.97(15) . . ? O2 Co2 O7 84.31(16) . . ? N11 Co2 O7 174.51(15) 4_454 . ? N8 Co2 O7 83.54(17) . . ? N10 Co2 O7 88.96(15) . . ? N2 Co2 O7 90.03(15) . . ? C1 N1 C5 116.6(4) . . ? C1 N1 Co1 124.7(3) . 1_556 ? C5 N1 Co1 118.5(3) . 1_556 ? C6 N2 C10 115.3(4) . . ? C6 N2 Co2 119.7(3) . . ? C10 N2 Co2 123.8(3) . . ? C3 N3 C8 127.9(4) . . ? C3 N3 H3N 110(4) . . ? C8 N3 H3N 122(4) . . ? C15 N4 C11 116.5(4) . . ? C15 N4 Co1 122.4(3) . . ? C11 N4 Co1 121.0(3) . . ? C16 N5 C20 115.1(4) . . ? C16 N5 Co1 117.2(3) . 4_474 ? C20 N5 Co1 127.6(3) . 4_474 ? C13 N6 C18 131.5(4) . . ? C13 N6 H6N 122(3) . . ? C18 N6 H6N 106(3) . . ? C21 N7 C25 116.0(4) . . ? C21 N7 Co1 123.6(3) . . ? C25 N7 Co1 118.3(3) . . ? C26 N8 C30 115.8(4) . . ? C26 N8 Co2 122.1(3) . . ? C30 N8 Co2 122.1(3) . . ? C23 N9 C28 126.6(4) . . ? C23 N9 H9N 116(4) . . ? C28 N9 H9N 117(3) . . ? C31 N10 C35 114.8(4) . . ? C31 N10 Co2 122.9(3) . . ? C35 N10 Co2 122.3(3) . . ? C40 N11 C36 115.6(4) . . ? C40 N11 Co2 126.0(3) . 4 ? C36 N11 Co2 118.2(3) . 4 ? C38 N12 C33 128.5(4) . . ? C38 N12 H12N 121(4) . . ? C33 N12 H12N 110(4) . . ? O5 N13 O4 121.1(4) . . ? O5 N13 O3 119.9(4) . . ? O4 N13 O3 118.9(4) . . ? O6 N14 O8 120.5(4) . . ? O6 N14 O7 118.5(4) . . ? O8 N14 O7 120.9(4) . . ? O11 N15 O10 120.6(5) . . ? O11 N15 O9 121.0(4) . . ? O10 N15 O9 118.5(4) . . ? O13 N16 O14 119.1(5) . . ? O13 N16 O12 119.4(4) . . ? O14 N16 O12 121.5(5) . . ? Co1 O1 H1A 115(4) . . ? Co1 O1 H1B 97(4) . . ? H1A O1 H1B 122(4) . . ? Co2 O2 H2A 117(4) . . ? Co2 O2 H2B 110(4) . . ? H2A O2 H2B 112(4) . . ? N13 O3 Co1 131.9(3) . . ? N14 O7 Co2 129.3(3) . . ? N1 C1 C2 124.1(4) . . ? N1 C1 H1 117.9 . . ? C2 C1 H1 117.9 . . ? C3 C2 C1 118.4(4) . . ? C3 C2 H2 120.8 . . ? C1 C2 H2 120.8 . . ? N3 C3 C2 123.6(4) . . ? N3 C3 C4 118.8(4) . . ? C2 C3 C4 117.6(4) . . ? C5 C4 C3 119.3(4) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? N1 C5 C4 123.8(4) . . ? N1 C5 H5 118.1 . . ? C4 C5 H5 118.1 . . ? N2 C6 C7 124.3(4) . . ? N2 C6 H6 117.8 . . ? C7 C6 H6 117.8 . . ? C6 C7 C8 118.5(4) . . ? C6 C7 H7 120.8 . . ? C8 C7 H7 120.8 . . ? C9 C8 C7 118.6(4) . . ? C9 C8 N3 119.8(4) . . ? C7 C8 N3 121.6(4) . . ? C10 C9 C8 117.8(4) . . ? C10 C9 H9 121.1 . . ? C8 C9 H9 121.1 . . ? N2 C10 C9 125.4(4) . . ? N2 C10 H10 117.3 . . ? C9 C10 H10 117.3 . . ? N4 C11 C12 123.7(4) . . ? N4 C11 H11 118.2 . . ? C12 C11 H11 118.2 . . ? C11 C12 C13 119.0(4) . . ? C11 C12 H12 120.5 . . ? C13 C12 H12 120.5 . . ? N6 C13 C14 126.2(4) . . ? N6 C13 C12 115.8(4) . . ? C14 C13 C12 118.1(4) . . ? C15 C14 C13 118.3(4) . . ? C15 C14 H14 120.9 . . ? C13 C14 H14 120.9 . . ? N4 C15 C14 124.4(4) . . ? N4 C15 H15 117.8 . . ? C14 C15 H15 117.8 . . ? N5 C16 C17 125.1(5) . . ? N5 C16 H16 117.4 . . ? C17 C16 H16 117.4 . . ? C16 C17 C18 118.1(4) . . ? C16 C17 H17 120.9 . . ? C18 C17 H17 120.9 . . ? N6 C18 C19 117.2(4) . . ? N6 C18 C17 125.6(4) . . ? C19 C18 C17 117.0(4) . . ? C20 C19 C18 119.4(4) . . ? C20 C19 H19 120.3 . . ? C18 C19 H19 120.3 . . ? N5 C20 C19 125.1(5) . . ? N5 C20 H20 117.4 . . ? C19 C20 H20 117.4 . . ? N7 C21 C22 123.9(4) . . ? N7 C21 H21 118.1 . . ? C22 C21 H21 118.1 . . ? C21 C22 C23 119.0(4) . . ? C21 C22 H22 120.5 . . ? C23 C22 H22 120.5 . . ? N9 C23 C24 123.6(4) . . ? N9 C23 C22 118.6(4) . . ? C24 C23 C22 117.7(4) . . ? C25 C24 C23 119.1(4) . . ? C25 C24 H24 120.5 . . ? C23 C24 H24 120.5 . . ? N7 C25 C24 124.2(4) . . ? N7 C25 H25 117.9 . . ? C24 C25 H25 117.9 . . ? N8 C26 C27 123.3(4) . . ? N8 C26 H26 118.4 . . ? C27 C26 H26 118.4 . . ? C26 C27 C28 120.4(4) . . ? C26 C27 H27 119.8 . . ? C28 C27 H27 119.8 . . ? N9 C28 C29 118.8(4) . . ? N9 C28 C27 124.5(4) . . ? C29 C28 C27 116.5(4) . . ? C30 C29 C28 118.4(4) . . ? C30 C29 H29 120.8 . . ? C28 C29 H29 120.8 . . ? N8 C30 C29 125.3(4) . . ? N8 C30 H30 117.4 . . ? C29 C30 H30 117.4 . . ? N10 C31 C32 124.8(5) . . ? N10 C31 H31 117.6 . . ? C32 C31 H31 117.6 . . ? C33 C32 C31 119.8(4) . . ? C33 C32 H32 120.1 . . ? C31 C32 H32 120.1 . . ? C32 C33 C34 116.7(4) . . ? C32 C33 N12 125.9(4) . . ? C34 C33 N12 117.3(4) . . ? C35 C34 C33 119.4(4) . . ? C35 C34 H34 120.3 . . ? C33 C34 H34 120.3 . . ? N10 C35 C34 124.5(4) . . ? N10 C35 H35 117.8 . . ? C34 C35 H35 117.8 . . ? N11 C36 C37 124.8(4) . . ? N11 C36 H36 117.6 . . ? C37 C36 H36 117.6 . . ? C36 C37 C38 118.2(4) . . ? C36 C37 H37 120.9 . . ? C38 C37 H37 120.9 . . ? C37 C38 N12 125.0(4) . . ? C37 C38 C39 117.6(4) . . ? N12 C38 C39 117.2(4) . . ? C40 C39 C38 119.5(4) . . ? C40 C39 H39 120.2 . . ? C38 C39 H39 120.2 . . ? N11 C40 C39 124.1(4) . . ? N11 C40 H40 118.0 . . ? C39 C40 H40 118.0 . . ? _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.033 _refine_diff_density_min -0.700 _refine_diff_density_rms 0.095 data_tri _database_code_depnum_ccdc_archive 'CCDC 632673' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H42 Cd Cl2 N12 O12' _chemical_formula_weight 1066.16 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' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 '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 10.5491(16) _cell_length_b 14.136(2) _cell_length_c 16.082(3) _cell_angle_alpha 87.483(3) _cell_angle_beta 86.253(3) _cell_angle_gamma 89.096(3) _cell_volume 2390.6(6) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rhomb _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.481 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1088 _exptl_absorpt_coefficient_mu 0.640 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.882 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 ? _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 29848 _diffrn_reflns_av_R_equivalents 0.0975 _diffrn_reflns_av_sigmaI/netI 0.1648 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.27 _diffrn_reflns_theta_max 28.39 _reflns_number_total 11452 _reflns_number_gt 5721 _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^)+(0.0405P)^2^+2.2915P] 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 11452 _refine_ls_number_parameters 635 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.1581 _refine_ls_R_factor_gt 0.0543 _refine_ls_wR_factor_ref 0.1366 _refine_ls_wR_factor_gt 0.0996 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.0000 0.0000 0.5000 0.01861(15) Uani 1 2 d S . . Cd2 Cd -0.5000 0.5000 0.0000 0.01825(15) Uani 1 2 d S . . Cl3 Cl 0.34697(13) 0.93697(9) 0.11848(9) 0.0304(3) Uani 1 1 d . . . Cl4 Cl 0.87469(14) 0.40968(10) 0.34294(10) 0.0361(4) Uani 1 1 d . . . O1 O 0.4507(4) 0.9596(3) 0.1673(3) 0.0454(11) Uani 1 1 d . . . O1W O 0.3493(4) -0.0524(3) 0.3499(3) 0.0404(11) Uani 1 1 d D . . H1WA H 0.381(5) -0.107(2) 0.361(3) 0.048 Uiso 1 1 d D . . H1WB H 0.340(6) -0.046(4) 0.2980(14) 0.048 Uiso 1 1 d D . . O2 O 0.3250(4) 1.0115(3) 0.0586(3) 0.0530(13) Uani 1 1 d . . . O2WA O -0.1107(9) 0.4685(7) 0.0946(6) 0.036(2) Uani 0.50 1 d P . . O2WB O -0.0983(10) 0.4711(7) 0.0388(7) 0.044(3) Uani 0.50 1 d P . . O3 O 0.3730(5) 0.8503(3) 0.0785(3) 0.0669(15) Uani 1 1 d . . . O4 O 0.2359(4) 0.9267(3) 0.1742(3) 0.0615(14) Uani 1 1 d . . . O5 O 0.9626(4) 0.4536(3) 0.3922(3) 0.0527(12) Uani 1 1 d . . . O6 O 0.9408(4) 0.3433(3) 0.2918(3) 0.0548(13) Uani 1 1 d . . . O7 O 0.7789(5) 0.3629(4) 0.3933(3) 0.0849(19) Uani 1 1 d . . . O8 O 0.8207(5) 0.4801(4) 0.2887(4) 0.0914(19) Uani 1 1 d . . . O9 O -0.3330(3) 0.5670(3) 0.0664(3) 0.0317(10) Uani 1 1 d D . . H9A H -0.264(3) 0.536(3) 0.062(3) 0.038 Uiso 1 1 d D . . H9B H -0.319(6) 0.622(3) 0.084(5) 0.11(3) Uiso 1 1 d D . . O10 O 0.1593(3) 0.0623(2) 0.4074(2) 0.0292(9) Uani 1 1 d D . . H10A H 0.219(4) 0.022(2) 0.396(3) 0.035 Uiso 1 1 d D . . H10B H 0.193(4) 0.1160(18) 0.395(3) 0.035 Uiso 1 1 d D . . N1 N 0.3469(4) -0.4495(3) 0.0995(3) 0.0274(11) Uani 1 1 d . . . N2 N 0.0801(5) -0.3845(3) 0.2946(3) 0.0468(15) Uani 1 1 d . . . H2A H 0.0335 -0.4318 0.3116 0.056 Uiso 1 1 calc R . . N3 N 0.0139(4) -0.1402(3) 0.4287(3) 0.0230(10) Uani 1 1 d . . . N4 N -0.1497(4) 0.0492(3) 0.4071(3) 0.0245(10) Uani 1 1 d . . . N5 N -0.4229(4) 0.1210(3) 0.2364(3) 0.0288(11) Uani 1 1 d . . . H5A H -0.4759 0.0767 0.2300 0.035 Uiso 1 1 calc R . . N6 N -0.4789(4) 0.3655(3) 0.0851(3) 0.0241(10) Uani 1 1 d . . . N7 N -0.7201(5) 0.2319(3) 0.3945(3) 0.0459(14) Uani 1 1 d . . . N8 N -0.4878(5) 0.4713(3) 0.3795(3) 0.0445(14) Uani 1 1 d . . . H8A H -0.4079 0.4579 0.3750 0.053 Uiso 1 1 calc R . . N9 N -0.5677(6) 0.7620(4) 0.3790(3) 0.0491(15) Uani 1 1 d . . . N10 N -0.2447(4) 0.7404(3) 0.1061(3) 0.0336(12) Uani 1 1 d . . . N11 N -0.0232(4) 0.9816(3) 0.1202(3) 0.0328(12) Uani 1 1 d . . . H11A H 0.0533 0.9676 0.1322 0.039 Uiso 1 1 calc R . . N12 N -0.0798(5) 1.2760(3) 0.0850(3) 0.0376(13) Uani 1 1 d . . . C1 C 0.2485(6) -0.5044(4) 0.1243(4) 0.052(2) Uani 1 1 d . . . H1 H 0.2403 -0.5604 0.0970 0.063 Uiso 1 1 calc R . . C2 C 0.1587(6) -0.4847(4) 0.1869(4) 0.055(2) Uani 1 1 d . . . H2 H 0.0931 -0.5267 0.2013 0.066 Uiso 1 1 calc R . . C3 C 0.1673(5) -0.4010(4) 0.2286(3) 0.0318(14) Uani 1 1 d . . . C4 C 0.2684(5) -0.3425(4) 0.2039(3) 0.0311(14) Uani 1 1 d . . . H4 H 0.2786 -0.2858 0.2296 0.037 Uiso 1 1 calc R . . C5 C 0.3532(5) -0.3698(4) 0.1406(3) 0.0302(14) Uani 1 1 d . . . H5 H 0.4203 -0.3296 0.1251 0.036 Uiso 1 1 calc R . . C6 C 0.0532(5) -0.1354(4) 0.3484(3) 0.0261(13) Uani 1 1 d . . . H6 H 0.0653 -0.0756 0.3230 0.031 Uiso 1 1 calc R . . C7 C 0.0772(5) -0.2120(4) 0.3003(3) 0.0267(13) Uani 1 1 d . . . H7 H 0.1060 -0.2042 0.2446 0.032 Uiso 1 1 calc R . . C8 C 0.0574(5) -0.3019(4) 0.3372(4) 0.0315(14) Uani 1 1 d . . . C9 C 0.0114(6) -0.3092(4) 0.4201(4) 0.0396(16) Uani 1 1 d . . . H9 H -0.0065 -0.3679 0.4463 0.047 Uiso 1 1 calc R . . C10 C -0.0071(5) -0.2271(4) 0.4625(3) 0.0336(14) Uani 1 1 d . . . C11 C -0.1310(5) 0.1194(4) 0.3497(3) 0.0246(13) Uani 1 1 d . . . H11 H -0.0546 0.1515 0.3483 0.029 Uiso 1 1 calc R . . C12 C -0.2165(5) 0.1478(4) 0.2923(3) 0.0260(13) Uani 1 1 d . . . H12 H -0.1979 0.1973 0.2537 0.031 Uiso 1 1 calc R . . C13 C -0.3315(5) 0.1006(3) 0.2934(3) 0.0236(12) Uani 1 1 d . . . C14 C -0.3509(5) 0.0252(4) 0.3509(4) 0.0312(14) Uani 1 1 d . . . C15 C -0.2607(5) 0.0026(4) 0.4058(3) 0.0324(14) Uani 1 1 d . . . H15 H -0.2763 -0.0475 0.4444 0.039 Uiso 1 1 calc R . . C16 C -0.5241(5) 0.2802(4) 0.0687(3) 0.0288(13) Uani 1 1 d . . . H16 H -0.5691 0.2758 0.0212 0.035 Uiso 1 1 calc R . . C17 C -0.5084(5) 0.1996(4) 0.1172(3) 0.0299(14) Uani 1 1 d . . . H17 H -0.5428 0.1428 0.1031 0.036 Uiso 1 1 calc R . . C18 C -0.4393(5) 0.2042(4) 0.1885(3) 0.0234(12) Uani 1 1 d . . . C19 C -0.3967(5) 0.2917(3) 0.2074(3) 0.0242(12) Uani 1 1 d . . . H19 H -0.3540 0.2986 0.2555 0.029 Uiso 1 1 calc R . . C20 C -0.4174(5) 0.3683(4) 0.1554(3) 0.0271(13) Uani 1 1 d . . . H20 H -0.3869 0.4264 0.1695 0.033 Uiso 1 1 calc R . . C21 C -0.7637(6) 0.3183(5) 0.3719(5) 0.060(2) Uani 1 1 d . . . H21 H -0.8478 0.3237 0.3580 0.072 Uiso 1 1 calc R . . C22 C -0.6933(6) 0.3990(4) 0.3680(4) 0.0465(17) Uani 1 1 d . . . H22 H -0.7303 0.4569 0.3531 0.056 Uiso 1 1 calc R . . C23 C -0.5670(5) 0.3943(4) 0.3862(4) 0.0320(14) Uani 1 1 d . . . C24 C -0.5185(6) 0.3048(4) 0.4089(4) 0.0380(15) Uani 1 1 d . . . H24 H -0.4340 0.2972 0.4214 0.046 Uiso 1 1 calc R . . C25 C -0.5978(6) 0.2283(4) 0.4124(4) 0.0406(16) Uani 1 1 d . . . H25 H -0.5639 0.1697 0.4284 0.049 Uiso 1 1 calc R . . C26 C -0.6471(6) 0.6996(5) 0.4149(4) 0.0462(17) Uani 1 1 d . . . H26 H -0.7223 0.7226 0.4406 0.055 Uiso 1 1 calc R . . C27 C -0.6277(6) 0.6029(4) 0.4176(4) 0.0391(15) Uani 1 1 d . . . H27 H -0.6874 0.5627 0.4448 0.047 Uiso 1 1 calc R . . C28 C -0.5179(6) 0.5672(4) 0.3789(4) 0.0397(16) Uani 1 1 d . . . C29 C -0.4323(6) 0.6309(4) 0.3422(4) 0.0479(18) Uani 1 1 d . . . H29 H -0.3560 0.6096 0.3169 0.057 Uiso 1 1 calc R . . C30 C -0.4592(7) 0.7258(5) 0.3431(4) 0.0536(19) Uani 1 1 d . . . H30 H -0.3998 0.7675 0.3178 0.064 Uiso 1 1 calc R . . C31 C -0.1193(6) 0.7384(4) 0.1002(4) 0.0358(15) Uani 1 1 d . . . H31 H -0.0788 0.6802 0.0926 0.043 Uiso 1 1 calc R . . C32 C -0.0444(5) 0.8166(4) 0.1045(3) 0.0294(13) Uani 1 1 d . . . H32 H 0.0437 0.8106 0.0998 0.035 Uiso 1 1 calc R . . C33 C -0.1019(5) 0.9046(4) 0.1159(3) 0.0248(12) Uani 1 1 d . . . C34 C -0.2347(5) 0.9076(4) 0.1249(4) 0.0314(14) Uani 1 1 d . . . C35 C -0.2986(5) 0.8244(4) 0.1188(4) 0.0348(15) Uani 1 1 d . . . H35 H -0.3869 0.8272 0.1242 0.042 Uiso 1 1 calc R . . C36 C 0.0211(6) 1.2371(4) 0.1202(4) 0.0363(15) Uani 1 1 d . . . H36 H 0.0816 1.2777 0.1376 0.044 Uiso 1 1 calc R . . C37 C 0.0418(6) 1.1416(4) 0.1327(4) 0.0367(15) Uani 1 1 d . . . H37 H 0.1147 1.1192 0.1570 0.044 Uiso 1 1 calc R . . C38 C -0.0486(5) 1.0779(4) 0.1083(3) 0.0290(13) Uani 1 1 d . . . C39 C -0.1538(5) 1.1175(4) 0.0715(3) 0.0277(13) Uani 1 1 d . . . H39 H -0.2159 1.0789 0.0531 0.033 Uiso 1 1 calc R . . C40 C -0.1647(5) 1.2148(4) 0.0625(4) 0.0339(14) Uani 1 1 d . . . H40 H -0.2370 1.2396 0.0390 0.041 Uiso 1 1 calc R . . H10 H -0.0357 -0.2324 0.5188 0.041 Uiso 1 1 d R . . H14 H -0.4258 -0.0097 0.3523 0.041 Uiso 1 1 d R . . H34 H -0.2789 0.9639 0.1345 0.041 Uiso 1 1 d R . . 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 Cd1 0.0202(3) 0.0175(3) 0.0185(3) -0.0031(2) -0.0029(2) 0.0023(2) Cd2 0.0208(3) 0.0164(3) 0.0174(3) -0.0012(2) -0.0008(2) 0.0021(2) Cl3 0.0269(8) 0.0231(7) 0.0421(9) -0.0023(6) -0.0076(7) -0.0043(6) Cl4 0.0268(8) 0.0325(8) 0.0491(10) -0.0050(7) 0.0003(7) -0.0052(7) O1 0.036(3) 0.035(2) 0.068(3) -0.011(2) -0.024(2) -0.004(2) O1W 0.036(3) 0.035(2) 0.050(3) -0.007(2) 0.002(2) 0.009(2) O2 0.080(4) 0.034(2) 0.046(3) 0.013(2) -0.019(2) -0.013(2) O2WA 0.024(5) 0.033(5) 0.052(6) -0.003(6) -0.012(5) -0.002(4) O2WB 0.034(6) 0.028(5) 0.069(7) 0.002(6) -0.007(6) 0.003(4) O3 0.080(4) 0.037(3) 0.091(4) -0.029(3) -0.038(3) 0.016(3) O4 0.028(3) 0.088(4) 0.066(3) 0.015(3) 0.010(2) -0.007(2) O5 0.060(3) 0.048(3) 0.053(3) -0.013(2) -0.014(2) -0.024(2) O6 0.048(3) 0.051(3) 0.065(3) -0.024(3) 0.011(2) 0.001(2) O7 0.065(4) 0.101(4) 0.086(4) -0.023(3) 0.040(3) -0.056(3) O8 0.102(5) 0.076(4) 0.101(5) -0.007(3) -0.049(4) 0.043(3) O9 0.026(2) 0.023(2) 0.048(3) -0.006(2) -0.016(2) 0.0023(18) O10 0.025(2) 0.022(2) 0.039(2) 0.0000(19) 0.0092(19) 0.0005(17) N1 0.029(3) 0.021(2) 0.031(3) -0.005(2) 0.013(2) 0.000(2) N2 0.056(4) 0.022(3) 0.059(4) -0.023(2) 0.038(3) -0.022(2) N3 0.027(3) 0.019(2) 0.023(3) -0.0048(19) 0.001(2) -0.002(2) N4 0.023(3) 0.026(2) 0.025(3) 0.003(2) -0.009(2) 0.004(2) N5 0.035(3) 0.018(2) 0.035(3) 0.008(2) -0.020(2) -0.010(2) N6 0.029(3) 0.016(2) 0.027(3) 0.0031(19) -0.004(2) -0.001(2) N7 0.029(3) 0.033(3) 0.074(4) 0.003(3) 0.009(3) -0.004(2) N8 0.029(3) 0.036(3) 0.067(4) 0.000(3) 0.003(3) -0.002(3) N9 0.061(4) 0.032(3) 0.056(4) -0.010(3) -0.009(3) 0.006(3) N10 0.031(3) 0.024(3) 0.047(3) -0.006(2) -0.008(2) 0.000(2) N11 0.021(3) 0.023(3) 0.055(3) -0.002(2) -0.009(2) 0.004(2) N12 0.045(3) 0.026(3) 0.042(3) -0.009(2) 0.004(3) -0.003(2) C1 0.054(4) 0.033(4) 0.067(5) -0.032(3) 0.038(4) -0.023(3) C2 0.061(5) 0.034(4) 0.066(5) -0.025(3) 0.045(4) -0.027(3) C3 0.039(4) 0.022(3) 0.032(3) -0.009(3) 0.022(3) -0.005(3) C4 0.035(4) 0.020(3) 0.038(4) -0.013(3) 0.009(3) -0.003(3) C5 0.028(3) 0.026(3) 0.036(3) -0.005(3) 0.012(3) -0.005(3) C6 0.032(3) 0.023(3) 0.024(3) -0.005(2) -0.002(3) -0.001(2) C7 0.032(3) 0.029(3) 0.019(3) -0.009(2) 0.003(2) -0.002(3) C8 0.033(3) 0.019(3) 0.041(4) -0.014(3) 0.014(3) -0.006(3) C9 0.053(4) 0.021(3) 0.041(4) -0.004(3) 0.026(3) -0.005(3) C10 0.040(4) 0.027(3) 0.032(3) -0.007(3) 0.015(3) -0.004(3) C11 0.024(3) 0.019(3) 0.032(3) 0.000(2) -0.008(3) -0.006(2) C12 0.033(3) 0.020(3) 0.025(3) 0.006(2) -0.009(3) -0.006(2) C13 0.027(3) 0.020(3) 0.025(3) 0.002(2) -0.012(2) -0.001(2) C14 0.027(3) 0.027(3) 0.041(4) 0.011(3) -0.014(3) -0.010(3) C15 0.033(4) 0.033(3) 0.031(3) 0.012(3) -0.011(3) -0.009(3) C16 0.030(3) 0.030(3) 0.028(3) 0.004(3) -0.012(3) -0.002(3) C17 0.037(4) 0.019(3) 0.036(3) 0.001(3) -0.020(3) -0.003(3) C18 0.023(3) 0.021(3) 0.026(3) 0.005(2) -0.008(2) -0.001(2) C19 0.034(3) 0.019(3) 0.021(3) -0.004(2) -0.011(2) -0.003(2) C20 0.035(4) 0.022(3) 0.025(3) 0.000(2) -0.010(3) -0.002(3) C21 0.029(4) 0.040(4) 0.110(7) 0.015(4) -0.005(4) 0.003(3) C22 0.034(4) 0.033(4) 0.071(5) 0.014(3) -0.005(3) -0.001(3) C23 0.024(3) 0.034(3) 0.037(4) 0.006(3) 0.000(3) 0.000(3) C24 0.035(4) 0.038(4) 0.040(4) 0.001(3) -0.001(3) 0.007(3) C25 0.043(4) 0.033(4) 0.044(4) 0.008(3) 0.008(3) 0.001(3) C26 0.046(4) 0.047(4) 0.046(4) -0.003(3) -0.006(3) 0.004(4) C27 0.041(4) 0.038(4) 0.037(4) 0.005(3) 0.000(3) -0.001(3) C28 0.033(4) 0.034(4) 0.052(4) -0.002(3) -0.003(3) 0.004(3) C29 0.039(4) 0.036(4) 0.067(5) -0.006(3) 0.010(4) -0.004(3) C30 0.056(5) 0.041(4) 0.062(5) 0.004(4) 0.006(4) -0.007(4) C31 0.036(4) 0.030(3) 0.042(4) -0.007(3) -0.010(3) 0.007(3) C32 0.029(3) 0.027(3) 0.032(3) -0.004(3) -0.004(3) 0.000(3) C33 0.025(3) 0.025(3) 0.026(3) -0.001(2) -0.009(2) -0.001(2) C34 0.026(3) 0.020(3) 0.048(4) -0.007(3) -0.002(3) 0.004(2) C35 0.027(3) 0.031(3) 0.047(4) -0.002(3) -0.009(3) 0.001(3) C36 0.033(4) 0.034(4) 0.042(4) -0.003(3) -0.001(3) -0.012(3) C37 0.029(4) 0.033(4) 0.048(4) -0.004(3) -0.001(3) 0.003(3) C38 0.028(3) 0.024(3) 0.036(3) -0.003(3) 0.002(3) -0.002(3) C39 0.025(3) 0.028(3) 0.031(3) -0.006(3) 0.001(3) -0.002(3) C40 0.027(3) 0.031(3) 0.044(4) -0.004(3) 0.001(3) 0.005(3) _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 Cd1 N4 2.322(4) . ? Cd1 N4 2.322(4) 2_556 ? Cd1 O10 2.328(3) 2_556 ? Cd1 O10 2.328(3) . ? Cd1 N3 2.330(4) 2_556 ? Cd1 N3 2.330(4) . ? Cd2 N6 2.310(4) . ? Cd2 N6 2.310(4) 2_465 ? Cd2 N1 2.325(4) 2 ? Cd2 N1 2.325(4) 1_465 ? Cd2 O9 2.351(4) 2_465 ? Cd2 O9 2.351(4) . ? Cl3 O2 1.423(4) . ? Cl3 O3 1.423(4) . ? Cl3 O4 1.433(4) . ? Cl3 O1 1.437(4) . ? Cl4 O7 1.408(4) . ? Cl4 O6 1.420(4) . ? Cl4 O5 1.426(4) . ? Cl4 O8 1.431(5) . ? O2WA O2WB 0.896(10) . ? N1 C5 1.335(6) . ? N1 C1 1.335(7) . ? N1 Cd2 2.325(4) 1_645 ? N2 C3 1.383(6) . ? N2 C8 1.389(6) . ? N3 C6 1.328(6) . ? N3 C10 1.338(6) . ? N4 C11 1.334(6) . ? N4 C15 1.354(6) . ? N5 C13 1.392(6) . ? N5 C18 1.392(6) . ? N6 C20 1.342(6) . ? N6 C16 1.347(6) . ? N7 C25 1.340(7) . ? N7 C21 1.342(7) . ? N8 C23 1.378(7) . ? N8 C28 1.388(7) . ? N9 C26 1.314(8) . ? N9 C30 1.352(8) . ? N10 C31 1.320(7) . ? N10 C35 1.327(6) . ? N11 C33 1.386(6) . ? N11 C38 1.391(6) . ? N12 C40 1.333(7) . ? N12 C36 1.337(7) . ? C1 C2 1.371(7) . ? C2 C3 1.393(7) . ? C3 C4 1.386(7) . ? C4 C5 1.375(7) . ? C6 C7 1.369(7) . ? C7 C8 1.391(7) . ? C8 C9 1.390(7) . ? C9 C10 1.376(7) . ? C11 C12 1.375(7) . ? C12 C13 1.392(7) . ? C13 C14 1.388(7) . ? C14 C15 1.365(7) . ? C16 C17 1.365(7) . ? C17 C18 1.402(7) . ? C18 C19 1.377(7) . ? C19 C20 1.362(7) . ? C21 C22 1.369(8) . ? C22 C23 1.383(8) . ? C23 C24 1.400(7) . ? C24 C25 1.374(8) . ? C26 C27 1.379(8) . ? C27 C28 1.378(8) . ? C28 C29 1.372(8) . ? C29 C30 1.366(8) . ? C31 C32 1.376(7) . ? C32 C33 1.390(7) . ? C33 C34 1.398(7) . ? C34 C35 1.376(7) . ? C36 C37 1.372(8) . ? C37 C38 1.407(7) . ? C38 C39 1.390(7) . ? C39 C40 1.381(7) . ? 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 N4 Cd1 N4 180.00(15) . 2_556 ? N4 Cd1 O10 90.68(15) . 2_556 ? N4 Cd1 O10 89.32(15) 2_556 2_556 ? N4 Cd1 O10 89.32(15) . . ? N4 Cd1 O10 90.68(15) 2_556 . ? O10 Cd1 O10 180.00(16) 2_556 . ? N4 Cd1 N3 93.77(15) . 2_556 ? N4 Cd1 N3 86.23(15) 2_556 2_556 ? O10 Cd1 N3 88.91(14) 2_556 2_556 ? O10 Cd1 N3 91.09(14) . 2_556 ? N4 Cd1 N3 86.23(15) . . ? N4 Cd1 N3 93.77(15) 2_556 . ? O10 Cd1 N3 91.09(14) 2_556 . ? O10 Cd1 N3 88.91(14) . . ? N3 Cd1 N3 180.0 2_556 . ? N6 Cd2 N6 180.0(2) . 2_465 ? N6 Cd2 N1 93.35(15) . 2 ? N6 Cd2 N1 86.65(15) 2_465 2 ? N6 Cd2 N1 86.65(15) . 1_465 ? N6 Cd2 N1 93.35(15) 2_465 1_465 ? N1 Cd2 N1 180.00(19) 2 1_465 ? N6 Cd2 O9 91.53(14) . 2_465 ? N6 Cd2 O9 88.47(14) 2_465 2_465 ? N1 Cd2 O9 93.06(15) 2 2_465 ? N1 Cd2 O9 86.94(15) 1_465 2_465 ? N6 Cd2 O9 88.47(14) . . ? N6 Cd2 O9 91.53(14) 2_465 . ? N1 Cd2 O9 86.94(15) 2 . ? N1 Cd2 O9 93.06(15) 1_465 . ? O9 Cd2 O9 180.00(18) 2_465 . ? O2 Cl3 O3 110.6(3) . . ? O2 Cl3 O4 108.8(3) . . ? O3 Cl3 O4 109.4(3) . . ? O2 Cl3 O1 110.4(3) . . ? O3 Cl3 O1 110.0(3) . . ? O4 Cl3 O1 107.6(3) . . ? O7 Cl4 O6 109.3(3) . . ? O7 Cl4 O5 111.3(3) . . ? O6 Cl4 O5 109.1(3) . . ? O7 Cl4 O8 110.7(4) . . ? O6 Cl4 O8 107.3(3) . . ? O5 Cl4 O8 109.0(3) . . ? C5 N1 C1 114.7(4) . . ? C5 N1 Cd2 124.6(4) . 1_645 ? C1 N1 Cd2 120.5(3) . 1_645 ? C3 N2 C8 128.8(5) . . ? C6 N3 C10 116.0(4) . . ? C6 N3 Cd1 118.2(3) . . ? C10 N3 Cd1 125.7(3) . . ? C11 N4 C15 116.0(4) . . ? C11 N4 Cd1 123.7(3) . . ? C15 N4 Cd1 120.3(3) . . ? C13 N5 C18 128.1(4) . . ? C20 N6 C16 115.3(4) . . ? C20 N6 Cd2 120.7(3) . . ? C16 N6 Cd2 124.0(3) . . ? C25 N7 C21 114.9(5) . . ? C23 N8 C28 129.6(5) . . ? C26 N9 C30 115.5(5) . . ? C31 N10 C35 115.9(5) . . ? C33 N11 C38 130.1(5) . . ? C40 N12 C36 115.2(5) . . ? N1 C1 C2 125.2(5) . . ? C1 C2 C3 119.0(5) . . ? N2 C3 C4 124.5(5) . . ? N2 C3 C2 118.4(5) . . ? C4 C3 C2 117.0(5) . . ? C5 C4 C3 118.9(5) . . ? N1 C5 C4 125.2(5) . . ? N3 C6 C7 124.9(5) . . ? C6 C7 C8 118.1(5) . . ? N2 C8 C9 118.6(5) . . ? N2 C8 C7 123.1(5) . . ? C9 C8 C7 118.3(5) . . ? C10 C9 C8 118.2(5) . . ? N3 C10 C9 124.3(5) . . ? N4 C11 C12 124.7(5) . . ? C11 C12 C13 118.4(5) . . ? C14 C13 N5 118.9(5) . . ? C14 C13 C12 117.7(5) . . ? N5 C13 C12 123.3(5) . . ? C15 C14 C13 119.7(5) . . ? N4 C15 C14 123.5(5) . . ? N6 C16 C17 124.4(5) . . ? C16 C17 C18 118.8(5) . . ? C19 C18 N5 124.8(5) . . ? C19 C18 C17 117.2(5) . . ? N5 C18 C17 118.0(5) . . ? C20 C19 C18 119.8(5) . . ? N6 C20 C19 124.4(5) . . ? N7 C21 C22 124.6(6) . . ? C21 C22 C23 119.9(6) . . ? N8 C23 C22 123.5(5) . . ? N8 C23 C24 119.8(5) . . ? C22 C23 C24 116.6(6) . . ? C25 C24 C23 118.9(6) . . ? N7 C25 C24 125.0(6) . . ? N9 C26 C27 125.2(6) . . ? C28 C27 C26 118.4(6) . . ? C29 C28 C27 117.6(6) . . ? C29 C28 N8 119.3(6) . . ? C27 C28 N8 123.1(6) . . ? C30 C29 C28 119.9(6) . . ? N9 C30 C29 123.4(6) . . ? N10 C31 C32 124.4(5) . . ? C31 C32 C33 119.2(5) . . ? N11 C33 C32 117.5(5) . . ? N11 C33 C34 125.4(5) . . ? C32 C33 C34 117.1(5) . . ? C35 C34 C33 117.9(5) . . ? N10 C35 C34 125.4(5) . . ? N12 C36 C37 124.8(6) . . ? C36 C37 C38 119.2(6) . . ? C39 C38 N11 125.8(5) . . ? C39 C38 C37 116.6(5) . . ? N11 C38 C37 117.6(5) . . ? C40 C39 C38 119.1(5) . . ? N12 C40 C39 125.1(5) . . ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 28.39 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 0.795 _refine_diff_density_min -1.584 _refine_diff_density_rms 0.132