# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Prof. Lisa Berreau' _publ_contact_author_email lisa.berreau@usu.edu loop_ _publ_author_name L.Berreau K.Grubel G.Ingle A.Fuller A.Arif data_usu167 #(Compound 3.CH2Cl2) _database_code_depnum_ccdc_archive 'CCDC 821105' #TrackingRef '- Revised_cifs.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H33 N4 Ni O3,Cl O4,C H2 Cl2' _chemical_formula_sum 'C40 H35 Cl3 N4 Ni O7' _chemical_formula_weight 848.78 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' Ni Ni 0.3393 1.1124 '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 23.2096(5) _cell_length_b 15.9822(4) _cell_length_c 11.9687(2) _cell_angle_alpha 90.00 _cell_angle_beta 117.2760(12) _cell_angle_gamma 90.00 _cell_volume 3946.02(15) _cell_formula_units_Z 4 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 1.018 _cell_measurement_theta_min 27.485 _cell_measurement_theta_max 28307 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.429 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1752 _exptl_absorpt_coefficient_mu 0.749 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8348 _exptl_absorpt_correction_T_max 0.8646 _exptl_absorpt_process_details 'DENZO-SMN (Otwinowski & Minor, 1997)' _exptl_special_details ; The program Denzo-SMN (Otwinowski & Minor, 1997) uses a scaling algorithm (Fox & Holmes, 1966) which effectively corrects for absorption effects. High redundancy data were used in the scaling program hence the 'multi-scan' code word was used. No transmission coefficients are available from the program (only scale factors for each frame). The scale factors in the experimental table are calculated from the 'size' command in the SHELXL-97 input file. ; _diffrn_ambient_temperature 150(1) _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 'Nonius KappaCCD Diffractometer' _diffrn_measurement_method 'Phi and Omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8111 _diffrn_reflns_av_R_equivalents 0.0445 _diffrn_reflns_av_sigmaI/netI 0.0459 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.83 _diffrn_reflns_theta_max 27.47 _reflns_number_total 8104 _reflns_number_gt 7110 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'WinGX, Ortep3' _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 Rfactors 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^)+(0.0777P)^2^+7.9130P] 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 constr _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 0.510(15) _refine_ls_number_reflns 8104 _refine_ls_number_parameters 498 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0683 _refine_ls_R_factor_gt 0.0539 _refine_ls_wR_factor_ref 0.1445 _refine_ls_wR_factor_gt 0.1320 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _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 Ni1 Ni 0.23881(2) 0.20936(3) 0.63266(3) 0.02431(13) Uani 1 1 d . . . Cl1 Cl -0.04478(6) 0.25206(7) 0.70212(10) 0.0338(2) Uani 1 1 d . . . Cl2 Cl 0.27362(13) 0.43572(15) 0.3462(2) 0.0959(7) Uani 1 1 d . . . Cl3 Cl 0.31631(10) 0.51997(13) 0.5836(2) 0.0796(5) Uani 1 1 d . . . O1 O 0.15927(13) 0.14793(18) 0.5171(3) 0.0266(6) Uani 1 1 d . . . O2 O 0.19209(14) 0.3185(2) 0.5798(3) 0.0297(6) Uani 1 1 d . . . O3 O 0.02065(14) 0.2799(2) 0.4480(3) 0.0371(7) Uani 1 1 d . . . H3N H 0.0121 0.2834 0.5089 0.045 Uiso 1 1 calc R . . O4 O -0.0083(2) 0.2981(3) 0.6540(4) 0.0680(13) Uani 1 1 d . . . O5 O -0.06591(18) 0.1736(2) 0.6358(4) 0.0480(9) Uani 1 1 d . . . O6 O -0.1020(3) 0.2977(3) 0.6809(6) 0.0719(14) Uani 1 1 d . . . O7 O -0.0066(2) 0.2359(3) 0.8338(3) 0.0547(10) Uani 1 1 d . . . N1 N 0.29369(16) 0.1026(2) 0.6787(3) 0.0305(8) Uani 1 1 d . . . N2 N 0.32138(17) 0.2603(2) 0.7799(3) 0.0298(8) Uani 1 1 d . . . N3 N 0.21450(17) 0.2043(2) 0.7832(3) 0.0267(7) Uani 1 1 d . . . N4 N 0.29309(18) 0.2409(3) 0.5282(4) 0.0320(8) Uani 1 1 d . . . C1 C 0.2810(2) 0.0333(3) 0.6079(5) 0.0364(10) Uani 1 1 d . . . H1 H 0.2393 0.0273 0.5379 0.044 Uiso 1 1 calc R . . C2 C 0.3257(3) -0.0292(4) 0.6324(7) 0.0593(17) Uani 1 1 d . . . H2 H 0.3155 -0.0780 0.5817 0.071 Uiso 1 1 calc R . . C3 C 0.3865(3) -0.0182(4) 0.7345(8) 0.082(3) Uani 1 1 d . . . H3 H 0.4184 -0.0606 0.7547 0.098 Uiso 1 1 calc R . . C4 C 0.4011(3) 0.0525(4) 0.8062(8) 0.071(2) Uani 1 1 d . . . H4 H 0.4430 0.0607 0.8745 0.085 Uiso 1 1 calc R . . C5 C 0.3530(2) 0.1120(3) 0.7765(5) 0.0406(11) Uani 1 1 d . . . C6 C 0.3631(2) 0.1890(3) 0.8530(5) 0.0416(12) Uani 1 1 d . . . H6A H 0.4091 0.2060 0.8882 0.050 Uiso 1 1 calc R . . H6B H 0.3540 0.1763 0.9243 0.050 Uiso 1 1 calc R . . C7 C 0.2991(2) 0.3083(3) 0.8588(4) 0.0336(10) Uani 1 1 d . . . H7A H 0.2803 0.3622 0.8177 0.040 Uiso 1 1 calc R . . H7B H 0.3363 0.3202 0.9415 0.040 Uiso 1 1 calc R . . C8 C 0.2492(2) 0.2585(3) 0.8764(4) 0.0327(9) Uani 1 1 d . . . C9 C 0.2382(3) 0.2686(4) 0.9809(5) 0.0435(12) Uani 1 1 d . . . H9 H 0.2642 0.3060 1.0466 0.052 Uiso 1 1 calc R . . C10 C 0.1888(3) 0.2235(4) 0.9880(5) 0.0501(14) Uani 1 1 d . . . H10 H 0.1797 0.2306 1.0571 0.060 Uiso 1 1 calc R . . C11 C 0.1530(3) 0.1677(4) 0.8918(5) 0.0449(13) Uani 1 1 d . . . H11 H 0.1187 0.1362 0.8937 0.054 Uiso 1 1 calc R . . C12 C 0.1680(2) 0.1593(3) 0.7945(4) 0.0336(10) Uani 1 1 d . . . H12 H 0.1444 0.1194 0.7310 0.040 Uiso 1 1 calc R . . C13 C 0.3541(3) 0.3133(4) 0.7252(5) 0.0429(13) Uani 1 1 d . . . H13A H 0.4000 0.3212 0.7875 0.052 Uiso 1 1 calc R . . H13B H 0.3331 0.3689 0.7043 0.052 Uiso 1 1 calc R . . C14 C 0.3508(2) 0.2739(3) 0.6090(4) 0.0382(11) Uani 1 1 d . . . C15 C 0.4034(3) 0.2760(4) 0.5829(6) 0.0557(16) Uani 1 1 d . . . H15 H 0.4431 0.3008 0.6408 0.067 Uiso 1 1 calc R . . C16 C 0.3972(3) 0.2419(5) 0.4729(7) 0.0662(19) Uani 1 1 d . . . H16 H 0.4329 0.2409 0.4547 0.079 Uiso 1 1 calc R . . C17 C 0.3379(3) 0.2090(4) 0.3891(6) 0.0550(16) Uani 1 1 d . . . H17 H 0.3322 0.1867 0.3111 0.066 Uiso 1 1 calc R . . C18 C 0.2868(3) 0.2086(3) 0.4187(5) 0.0376(11) Uani 1 1 d . . . C19 C 0.2208(2) 0.1791(3) 0.3250(4) 0.0372(10) Uani 1 1 d . . . C20 C 0.2146(3) 0.1020(4) 0.2636(5) 0.0534(15) Uani 1 1 d . . . H20 H 0.2510 0.0663 0.2857 0.064 Uiso 1 1 calc R . . C21 C 0.1534(4) 0.0794(4) 0.1691(5) 0.0623(19) Uani 1 1 d . . . H21 H 0.1484 0.0273 0.1275 0.075 Uiso 1 1 calc R . . C22 C 0.1015(4) 0.1293(5) 0.1356(5) 0.063(2) Uani 1 1 d . . . H22 H 0.0608 0.1121 0.0704 0.076 Uiso 1 1 calc R . . C23 C 0.1068(3) 0.2071(4) 0.1960(5) 0.0527(15) Uani 1 1 d . . . H23 H 0.0703 0.2426 0.1723 0.063 Uiso 1 1 calc R . . C24 C 0.1678(2) 0.2299(4) 0.2918(4) 0.0395(11) Uani 1 1 d . . . H24 H 0.1725 0.2814 0.3347 0.047 Uiso 1 1 calc R . . C25 C 0.10218(19) 0.1751(3) 0.4868(3) 0.0240(8) Uani 1 1 d . . . C26 C 0.05061(19) 0.1082(3) 0.4432(4) 0.0264(8) Uani 1 1 d . . . C27 C 0.0493(2) 0.0500(3) 0.3549(4) 0.0309(9) Uani 1 1 d . . . H27 H 0.0788 0.0549 0.3206 0.037 Uiso 1 1 calc R . . C28 C 0.0043(2) -0.0157(3) 0.3169(4) 0.0411(12) Uani 1 1 d . . . H28 H 0.0031 -0.0551 0.2565 0.049 Uiso 1 1 calc R . . C29 C -0.0386(2) -0.0228(3) 0.3683(5) 0.0398(11) Uani 1 1 d . . . H29 H -0.0698 -0.0665 0.3414 0.048 Uiso 1 1 calc R . . C30 C -0.0357(2) 0.0330(3) 0.4573(5) 0.0358(10) Uani 1 1 d . . . H30 H -0.0641 0.0267 0.4940 0.043 Uiso 1 1 calc R . . C31 C 0.0086(2) 0.0994(3) 0.4949(4) 0.0325(9) Uani 1 1 d . . . H31 H 0.0097 0.1383 0.5558 0.039 Uiso 1 1 calc R . . C32 C 0.08657(19) 0.2585(3) 0.4925(4) 0.0289(9) Uani 1 1 d . . . C33 C 0.1306(2) 0.3258(3) 0.5260(4) 0.0283(9) Uani 1 1 d . . . C34 C 0.1072(2) 0.4140(3) 0.4933(5) 0.0449(13) Uani 1 1 d . . . C35 C 0.0712(3) 0.4374(5) 0.3696(7) 0.0699(19) Uani 1 1 d . . . H35 H 0.0551 0.3955 0.3064 0.084 Uiso 1 1 calc R . . C36 C 0.0579(4) 0.5208(5) 0.3351(10) 0.091(3) Uani 1 1 d . . . H36 H 0.0333 0.5367 0.2496 0.110 Uiso 1 1 calc R . . C37 C 0.0808(4) 0.5777(5) 0.4266(10) 0.096(3) Uani 1 1 d . . . H37 H 0.0707 0.6349 0.4049 0.116 Uiso 1 1 calc R . . C38 C 0.1182(5) 0.5576(5) 0.5501(11) 0.113(4) Uani 1 1 d . . . H38 H 0.1335 0.5991 0.6140 0.136 Uiso 1 1 calc R . . C39 C 0.1325(4) 0.4742(4) 0.5777(8) 0.080(2) Uani 1 1 d . . . H39 H 0.1621 0.4592 0.6614 0.096 Uiso 1 1 calc R . . C40 C 0.2513(3) 0.4699(5) 0.4511(8) 0.078(2) Uani 1 1 d . . . H40A H 0.2351 0.4221 0.4813 0.094 Uiso 1 1 calc R . . H40B H 0.2152 0.5101 0.4100 0.094 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 Ni1 0.0162(2) 0.0314(3) 0.0237(2) -0.0042(2) 0.00768(17) -0.0009(2) Cl1 0.0345(5) 0.0327(6) 0.0351(5) -0.0012(4) 0.0168(4) 0.0038(4) Cl2 0.1089(17) 0.0884(14) 0.0828(14) 0.0027(11) 0.0373(12) -0.0115(13) Cl3 0.0801(12) 0.0654(11) 0.0813(12) 0.0124(9) 0.0267(10) -0.0071(9) O1 0.0191(14) 0.0317(16) 0.0268(14) -0.0056(12) 0.0087(11) 0.0009(12) O2 0.0231(14) 0.0310(15) 0.0305(15) -0.0018(12) 0.0085(12) -0.0023(12) O3 0.0182(15) 0.0387(18) 0.0467(18) 0.0038(15) 0.0082(13) 0.0042(13) O4 0.076(3) 0.087(3) 0.052(2) -0.013(2) 0.038(2) -0.035(3) O5 0.045(2) 0.039(2) 0.049(2) -0.0095(17) 0.0127(17) -0.0036(17) O6 0.068(3) 0.059(3) 0.097(4) 0.004(2) 0.044(3) 0.029(2) O7 0.055(2) 0.071(3) 0.0316(18) -0.0023(17) 0.0134(17) -0.009(2) N1 0.0185(17) 0.035(2) 0.0352(19) -0.0028(16) 0.0100(15) -0.0007(15) N2 0.0183(16) 0.040(2) 0.0274(17) -0.0090(15) 0.0075(14) -0.0050(15) N3 0.0243(17) 0.0312(19) 0.0233(16) -0.0041(14) 0.0099(14) 0.0011(14) N4 0.0254(17) 0.039(2) 0.0339(19) -0.0062(16) 0.0161(15) -0.0069(16) C1 0.026(2) 0.033(2) 0.049(3) -0.002(2) 0.017(2) 0.0001(18) C2 0.044(3) 0.035(3) 0.091(5) -0.016(3) 0.023(3) 0.004(2) C3 0.041(3) 0.046(4) 0.118(6) -0.022(4) 0.001(4) 0.017(3) C4 0.030(3) 0.052(4) 0.102(5) -0.008(3) 0.006(3) 0.014(2) C5 0.023(2) 0.039(3) 0.053(3) 0.003(2) 0.012(2) 0.007(2) C6 0.019(2) 0.055(3) 0.034(2) -0.005(2) -0.0022(18) 0.007(2) C7 0.028(2) 0.042(3) 0.028(2) -0.0123(18) 0.0102(18) -0.0056(18) C8 0.030(2) 0.037(2) 0.028(2) -0.0059(18) 0.0107(18) -0.0009(18) C9 0.049(3) 0.052(3) 0.030(2) -0.010(2) 0.018(2) -0.008(2) C10 0.065(4) 0.059(3) 0.038(3) -0.007(2) 0.034(3) -0.010(3) C11 0.046(3) 0.060(4) 0.032(2) -0.002(2) 0.021(2) -0.008(3) C12 0.030(2) 0.041(3) 0.030(2) -0.0002(19) 0.0141(18) -0.0002(19) C13 0.026(2) 0.063(3) 0.039(3) -0.018(2) 0.014(2) -0.019(2) C14 0.030(2) 0.053(3) 0.034(2) -0.006(2) 0.0169(19) -0.008(2) C15 0.033(3) 0.088(5) 0.053(3) -0.016(3) 0.025(2) -0.018(3) C16 0.048(4) 0.101(6) 0.076(4) -0.014(4) 0.050(3) -0.013(3) C17 0.055(4) 0.073(5) 0.058(4) -0.009(3) 0.044(3) -0.007(3) C18 0.042(3) 0.043(3) 0.036(2) -0.008(2) 0.025(2) -0.004(2) C19 0.043(3) 0.048(3) 0.027(2) -0.004(2) 0.022(2) -0.010(2) C20 0.079(4) 0.055(3) 0.041(3) -0.008(2) 0.040(3) -0.020(3) C21 0.097(5) 0.063(4) 0.032(3) -0.014(3) 0.034(3) -0.037(4) C22 0.064(4) 0.094(5) 0.029(3) -0.015(3) 0.019(3) -0.045(4) C23 0.042(3) 0.085(5) 0.028(2) 0.004(3) 0.014(2) -0.017(3) C24 0.039(3) 0.054(3) 0.027(2) -0.004(2) 0.017(2) -0.014(2) C25 0.0210(19) 0.031(2) 0.0203(18) -0.0018(16) 0.0098(15) -0.0007(16) C26 0.0168(18) 0.031(2) 0.0247(19) 0.0030(16) 0.0033(15) -0.0017(16) C27 0.031(2) 0.035(2) 0.025(2) -0.0028(17) 0.0106(17) -0.0051(18) C28 0.045(3) 0.039(3) 0.029(2) -0.0061(19) 0.008(2) -0.014(2) C29 0.028(2) 0.039(3) 0.040(2) 0.006(2) 0.0043(19) -0.0068(19) C30 0.023(2) 0.039(3) 0.044(3) 0.009(2) 0.0144(19) -0.0018(18) C31 0.021(2) 0.038(2) 0.038(2) 0.0022(19) 0.0132(18) 0.0029(18) C32 0.0163(18) 0.034(2) 0.028(2) 0.0045(17) 0.0035(16) 0.0015(17) C33 0.026(2) 0.030(2) 0.025(2) 0.0016(17) 0.0086(17) 0.0026(18) C34 0.028(2) 0.032(3) 0.056(3) 0.006(2) 0.003(2) 0.0047(19) C35 0.055(4) 0.070(4) 0.074(4) 0.027(4) 0.020(3) 0.017(3) C36 0.057(4) 0.074(5) 0.115(7) 0.048(5) 0.015(4) 0.010(4) C37 0.055(4) 0.057(4) 0.129(7) 0.008(5) 0.000(5) 0.007(4) C38 0.114(7) 0.050(4) 0.135(8) -0.011(5) 0.021(7) 0.027(5) C39 0.090(6) 0.048(4) 0.076(5) -0.002(3) 0.015(4) 0.015(4) C40 0.052(4) 0.058(4) 0.114(6) 0.016(4) 0.029(4) 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 Ni1 O1 1.986(3) . ? Ni1 O2 1.998(3) . ? Ni1 N1 2.048(4) . ? Ni1 N2 2.084(3) . ? Ni1 N3 2.122(4) . ? Ni1 N4 2.202(4) . ? Cl1 O4 1.427(4) . ? Cl1 O6 1.431(4) . ? Cl1 O7 1.434(4) . ? Cl1 O5 1.444(4) . ? Cl2 C40 1.655(9) . ? Cl3 C40 1.799(8) . ? O1 C25 1.279(5) . ? O2 C33 1.274(5) . ? O3 C32 1.412(5) . ? O3 H3N 0.8400 . ? N1 C1 1.342(6) . ? N1 C5 1.346(6) . ? N2 C13 1.476(7) . ? N2 C7 1.481(6) . ? N2 C6 1.490(6) . ? N3 C8 1.349(6) . ? N3 C12 1.356(6) . ? N4 C14 1.348(6) . ? N4 C18 1.353(6) . ? C1 C2 1.371(7) . ? C1 H1 0.9500 . ? C2 C3 1.392(9) . ? C2 H2 0.9500 . ? C3 C4 1.365(10) . ? C3 H3 0.9500 . ? C4 C5 1.382(7) . ? C4 H4 0.9500 . ? C5 C6 1.487(7) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.497(7) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.397(7) . ? C9 C10 1.389(8) . ? C9 H9 0.9500 . ? C10 C11 1.390(8) . ? C10 H10 0.9500 . ? C11 C12 1.366(7) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.496(7) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.392(7) . ? C15 C16 1.370(9) . ? C15 H15 0.9500 . ? C16 C17 1.383(10) . ? C16 H16 0.9500 . ? C17 C18 1.384(7) . ? C17 H17 0.9500 . ? C18 C19 1.502(7) . ? C19 C24 1.372(8) . ? C19 C20 1.408(8) . ? C20 C21 1.397(9) . ? C20 H20 0.9500 . ? C21 C22 1.342(11) . ? C21 H21 0.9500 . ? C22 C23 1.415(10) . ? C22 H22 0.9500 . ? C23 C24 1.401(7) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C32 1.390(6) . ? C25 C26 1.509(6) . ? C26 C31 1.381(6) . ? C26 C27 1.398(6) . ? C27 C28 1.400(6) . ? C27 H27 0.9500 . ? C28 C29 1.394(8) . ? C28 H28 0.9500 . ? C29 C30 1.368(7) . ? C29 H29 0.9500 . ? C30 C31 1.400(7) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 C33 1.409(6) . ? C33 C34 1.496(7) . ? C34 C39 1.322(9) . ? C34 C35 1.377(9) . ? C35 C36 1.388(10) . ? C35 H35 0.9500 . ? C36 C37 1.332(13) . ? C36 H36 0.9500 . ? C37 C38 1.366(14) . ? C37 H37 0.9500 . ? C38 C39 1.376(11) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? 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 Ni1 O2 90.84(12) . . ? O1 Ni1 N1 92.31(13) . . ? O2 Ni1 N1 173.30(14) . . ? O1 Ni1 N2 169.33(14) . . ? O2 Ni1 N2 94.72(14) . . ? N1 Ni1 N2 83.13(15) . . ? O1 Ni1 N3 92.78(13) . . ? O2 Ni1 N3 89.15(13) . . ? N1 Ni1 N3 96.59(15) . . ? N2 Ni1 N3 78.23(14) . . ? O1 Ni1 N4 108.01(13) . . ? O2 Ni1 N4 89.34(14) . . ? N1 Ni1 N4 84.06(15) . . ? N2 Ni1 N4 81.20(15) . . ? N3 Ni1 N4 159.18(14) . . ? O4 Cl1 O6 109.8(3) . . ? O4 Cl1 O7 110.7(3) . . ? O6 Cl1 O7 110.1(3) . . ? O4 Cl1 O5 109.9(3) . . ? O6 Cl1 O5 106.9(3) . . ? O7 Cl1 O5 109.3(2) . . ? C25 O1 Ni1 122.8(3) . . ? C33 O2 Ni1 124.0(3) . . ? C32 O3 H3N 109.5 . . ? C1 N1 C5 118.9(4) . . ? C1 N1 Ni1 126.0(3) . . ? C5 N1 Ni1 113.7(3) . . ? C13 N2 C7 112.7(4) . . ? C13 N2 C6 111.8(4) . . ? C7 N2 C6 110.1(4) . . ? C13 N2 Ni1 108.0(3) . . ? C7 N2 Ni1 106.7(3) . . ? C6 N2 Ni1 107.2(3) . . ? C8 N3 C12 117.4(4) . . ? C8 N3 Ni1 112.8(3) . . ? C12 N3 Ni1 129.7(3) . . ? C14 N4 C18 118.3(4) . . ? C14 N4 Ni1 108.7(3) . . ? C18 N4 Ni1 128.8(3) . . ? N1 C1 C2 122.7(5) . . ? N1 C1 H1 118.7 . . ? C2 C1 H1 118.7 . . ? C1 C2 C3 117.4(5) . . ? C1 C2 H2 121.3 . . ? C3 C2 H2 121.3 . . ? C4 C3 C2 121.1(6) . . ? C4 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? C3 C4 C5 118.0(6) . . ? C3 C4 H4 121.0 . . ? C5 C4 H4 121.0 . . ? N1 C5 C4 122.0(5) . . ? N1 C5 C6 116.0(4) . . ? C4 C5 C6 122.0(5) . . ? C5 C6 N2 113.3(4) . . ? C5 C6 H6A 108.9 . . ? N2 C6 H6A 108.9 . . ? C5 C6 H6B 108.9 . . ? N2 C6 H6B 108.9 . . ? H6A C6 H6B 107.7 . . ? N2 C7 C8 109.5(4) . . ? N2 C7 H7A 109.8 . . ? C8 C7 H7A 109.8 . . ? N2 C7 H7B 109.8 . . ? C8 C7 H7B 109.8 . . ? H7A C7 H7B 108.2 . . ? N3 C8 C9 122.0(4) . . ? N3 C8 C7 115.6(4) . . ? C9 C8 C7 122.4(4) . . ? C10 C9 C8 119.3(5) . . ? C10 C9 H9 120.4 . . ? C8 C9 H9 120.4 . . ? C9 C10 C11 118.7(5) . . ? C9 C10 H10 120.7 . . ? C11 C10 H10 120.7 . . ? C12 C11 C10 118.7(5) . . ? C12 C11 H11 120.7 . . ? C10 C11 H11 120.7 . . ? N3 C12 C11 123.9(5) . . ? N3 C12 H12 118.0 . . ? C11 C12 H12 118.0 . . ? N2 C13 C14 110.7(4) . . ? N2 C13 H13A 109.5 . . ? C14 C13 H13A 109.5 . . ? N2 C13 H13B 109.5 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 108.1 . . ? N4 C14 C15 122.2(5) . . ? N4 C14 C13 116.2(4) . . ? C15 C14 C13 121.4(5) . . ? C16 C15 C14 119.3(5) . . ? C16 C15 H15 120.4 . . ? C14 C15 H15 120.4 . . ? C15 C16 C17 118.6(5) . . ? C15 C16 H16 120.7 . . ? C17 C16 H16 120.7 . . ? C16 C17 C18 120.0(5) . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? N4 C18 C17 121.5(5) . . ? N4 C18 C19 117.6(4) . . ? C17 C18 C19 120.7(5) . . ? C24 C19 C20 120.2(5) . . ? C24 C19 C18 120.2(4) . . ? C20 C19 C18 119.3(5) . . ? C21 C20 C19 118.1(6) . . ? C21 C20 H20 121.0 . . ? C19 C20 H20 121.0 . . ? C22 C21 C20 121.9(6) . . ? C22 C21 H21 119.0 . . ? C20 C21 H21 119.0 . . ? C21 C22 C23 120.8(5) . . ? C21 C22 H22 119.6 . . ? C23 C22 H22 119.6 . . ? C24 C23 C22 117.8(6) . . ? C24 C23 H23 121.1 . . ? C22 C23 H23 121.1 . . ? C19 C24 C23 121.2(5) . . ? C19 C24 H24 119.4 . . ? C23 C24 H24 119.4 . . ? O1 C25 C32 124.8(4) . . ? O1 C25 C26 114.3(4) . . ? C32 C25 C26 120.9(4) . . ? C31 C26 C27 119.7(4) . . ? C31 C26 C25 121.9(4) . . ? C27 C26 C25 118.2(4) . . ? C26 C27 C28 119.9(4) . . ? C26 C27 H27 120.1 . . ? C28 C27 H27 120.1 . . ? C29 C28 C27 119.7(5) . . ? C29 C28 H28 120.1 . . ? C27 C28 H28 120.1 . . ? C30 C29 C28 120.0(4) . . ? C30 C29 H29 120.0 . . ? C28 C29 H29 120.0 . . ? C29 C30 C31 120.8(4) . . ? C29 C30 H30 119.6 . . ? C31 C30 H30 119.6 . . ? C26 C31 C30 119.9(4) . . ? C26 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? C25 C32 C33 125.0(4) . . ? C25 C32 O3 118.4(4) . . ? C33 C32 O3 116.1(4) . . ? O2 C33 C32 124.9(4) . . ? O2 C33 C34 113.9(4) . . ? C32 C33 C34 121.1(4) . . ? C39 C34 C35 117.4(6) . . ? C39 C34 C33 120.4(5) . . ? C35 C34 C33 120.4(6) . . ? C34 C35 C36 121.6(8) . . ? C34 C35 H35 119.2 . . ? C36 C35 H35 119.2 . . ? C37 C36 C35 117.4(8) . . ? C37 C36 H36 121.3 . . ? C35 C36 H36 121.3 . . ? C36 C37 C38 123.1(8) . . ? C36 C37 H37 118.5 . . ? C38 C37 H37 118.5 . . ? C37 C38 C39 116.8(9) . . ? C37 C38 H38 121.6 . . ? C39 C38 H38 121.6 . . ? C34 C39 C38 123.2(8) . . ? C34 C39 H39 118.4 . . ? C38 C39 H39 118.4 . . ? Cl2 C40 Cl3 112.9(4) . . ? Cl2 C40 H40A 109.0 . . ? Cl3 C40 H40A 109.0 . . ? Cl2 C40 H40B 109.0 . . ? Cl3 C40 H40B 109.0 . . ? H40A C40 H40B 107.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Ni1 O1 C25 -28.9(3) . . . . ? N1 Ni1 O1 C25 157.0(3) . . . . ? N2 Ni1 O1 C25 92.6(8) . . . . ? N3 Ni1 O1 C25 60.3(3) . . . . ? N4 Ni1 O1 C25 -118.5(3) . . . . ? O1 Ni1 O2 C33 19.0(3) . . . . ? N1 Ni1 O2 C33 137.1(11) . . . . ? N2 Ni1 O2 C33 -151.9(3) . . . . ? N3 Ni1 O2 C33 -73.7(3) . . . . ? N4 Ni1 O2 C33 127.0(3) . . . . ? O1 Ni1 N1 C1 24.4(4) . . . . ? O2 Ni1 N1 C1 -93.6(12) . . . . ? N2 Ni1 N1 C1 -165.3(4) . . . . ? N3 Ni1 N1 C1 117.4(4) . . . . ? N4 Ni1 N1 C1 -83.5(4) . . . . ? O1 Ni1 N1 C5 -169.2(3) . . . . ? O2 Ni1 N1 C5 72.7(13) . . . . ? N2 Ni1 N1 C5 1.1(3) . . . . ? N3 Ni1 N1 C5 -76.2(4) . . . . ? N4 Ni1 N1 C5 82.9(3) . . . . ? O1 Ni1 N2 C13 170.6(7) . . . . ? O2 Ni1 N2 C13 -68.2(3) . . . . ? N1 Ni1 N2 C13 105.5(3) . . . . ? N3 Ni1 N2 C13 -156.3(3) . . . . ? N4 Ni1 N2 C13 20.4(3) . . . . ? O1 Ni1 N2 C7 -67.9(9) . . . . ? O2 Ni1 N2 C7 53.2(3) . . . . ? N1 Ni1 N2 C7 -133.1(3) . . . . ? N3 Ni1 N2 C7 -34.9(3) . . . . ? N4 Ni1 N2 C7 141.8(3) . . . . ? O1 Ni1 N2 C6 50.0(9) . . . . ? O2 Ni1 N2 C6 171.2(3) . . . . ? N1 Ni1 N2 C6 -15.1(3) . . . . ? N3 Ni1 N2 C6 83.1(3) . . . . ? N4 Ni1 N2 C6 -100.2(3) . . . . ? O1 Ni1 N3 C8 -164.3(3) . . . . ? O2 Ni1 N3 C8 -73.5(3) . . . . ? N1 Ni1 N3 C8 103.0(3) . . . . ? N2 Ni1 N3 C8 21.5(3) . . . . ? N4 Ni1 N3 C8 12.4(6) . . . . ? O1 Ni1 N3 C12 11.5(4) . . . . ? O2 Ni1 N3 C12 102.3(4) . . . . ? N1 Ni1 N3 C12 -81.2(4) . . . . ? N2 Ni1 N3 C12 -162.7(4) . . . . ? N4 Ni1 N3 C12 -171.8(4) . . . . ? O1 Ni1 N4 C14 -172.9(3) . . . . ? O2 Ni1 N4 C14 96.4(3) . . . . ? N1 Ni1 N4 C14 -82.4(3) . . . . ? N2 Ni1 N4 C14 1.5(3) . . . . ? N3 Ni1 N4 C14 10.5(6) . . . . ? O1 Ni1 N4 C18 -16.6(5) . . . . ? O2 Ni1 N4 C18 -107.3(4) . . . . ? N1 Ni1 N4 C18 73.9(4) . . . . ? N2 Ni1 N4 C18 157.8(4) . . . . ? N3 Ni1 N4 C18 166.8(4) . . . . ? C5 N1 C1 C2 1.1(8) . . . . ? Ni1 N1 C1 C2 166.9(5) . . . . ? N1 C1 C2 C3 -0.8(10) . . . . ? C1 C2 C3 C4 -0.7(13) . . . . ? C2 C3 C4 C5 1.8(14) . . . . ? C1 N1 C5 C4 0.0(8) . . . . ? Ni1 N1 C5 C4 -167.4(5) . . . . ? C1 N1 C5 C6 -178.4(5) . . . . ? Ni1 N1 C5 C6 14.2(6) . . . . ? C3 C4 C5 N1 -1.4(11) . . . . ? C3 C4 C5 C6 176.8(7) . . . . ? N1 C5 C6 N2 -28.1(7) . . . . ? C4 C5 C6 N2 153.5(6) . . . . ? C13 N2 C6 C5 -91.6(5) . . . . ? C7 N2 C6 C5 142.3(4) . . . . ? Ni1 N2 C6 C5 26.6(5) . . . . ? C13 N2 C7 C8 161.9(4) . . . . ? C6 N2 C7 C8 -72.5(4) . . . . ? Ni1 N2 C7 C8 43.6(4) . . . . ? C12 N3 C8 C9 0.0(7) . . . . ? Ni1 N3 C8 C9 176.3(4) . . . . ? C12 N3 C8 C7 -178.8(4) . . . . ? Ni1 N3 C8 C7 -2.4(5) . . . . ? N2 C7 C8 N3 -27.7(5) . . . . ? N2 C7 C8 C9 153.6(5) . . . . ? N3 C8 C9 C10 -2.0(8) . . . . ? C7 C8 C9 C10 176.7(5) . . . . ? C8 C9 C10 C11 1.8(9) . . . . ? C9 C10 C11 C12 0.3(9) . . . . ? C8 N3 C12 C11 2.3(7) . . . . ? Ni1 N3 C12 C11 -173.3(4) . . . . ? C10 C11 C12 N3 -2.5(8) . . . . ? C7 N2 C13 C14 -156.2(4) . . . . ? C6 N2 C13 C14 79.1(5) . . . . ? Ni1 N2 C13 C14 -38.6(5) . . . . ? C18 N4 C14 C15 0.3(8) . . . . ? Ni1 N4 C14 C15 159.4(5) . . . . ? C18 N4 C14 C13 176.6(5) . . . . ? Ni1 N4 C14 C13 -24.3(6) . . . . ? N2 C13 C14 N4 43.8(7) . . . . ? N2 C13 C14 C15 -139.9(6) . . . . ? N4 C14 C15 C16 -1.4(10) . . . . ? C13 C14 C15 C16 -177.5(6) . . . . ? C14 C15 C16 C17 2.2(12) . . . . ? C15 C16 C17 C18 -2.0(11) . . . . ? C14 N4 C18 C17 0.0(8) . . . . ? Ni1 N4 C18 C17 -154.4(5) . . . . ? C14 N4 C18 C19 -174.7(5) . . . . ? Ni1 N4 C18 C19 31.0(7) . . . . ? C16 C17 C18 N4 0.9(10) . . . . ? C16 C17 C18 C19 175.4(6) . . . . ? N4 C18 C19 C24 49.7(7) . . . . ? C17 C18 C19 C24 -125.0(6) . . . . ? N4 C18 C19 C20 -135.7(5) . . . . ? C17 C18 C19 C20 49.7(7) . . . . ? C24 C19 C20 C21 0.0(7) . . . . ? C18 C19 C20 C21 -174.6(5) . . . . ? C19 C20 C21 C22 0.7(8) . . . . ? C20 C21 C22 C23 -0.5(9) . . . . ? C21 C22 C23 C24 -0.2(8) . . . . ? C20 C19 C24 C23 -0.8(7) . . . . ? C18 C19 C24 C23 173.8(4) . . . . ? C22 C23 C24 C19 0.9(7) . . . . ? Ni1 O1 C25 C32 22.7(5) . . . . ? Ni1 O1 C25 C26 -157.0(3) . . . . ? O1 C25 C26 C31 127.8(4) . . . . ? C32 C25 C26 C31 -51.9(6) . . . . ? O1 C25 C26 C27 -47.3(5) . . . . ? C32 C25 C26 C27 133.1(4) . . . . ? C31 C26 C27 C28 1.6(6) . . . . ? C25 C26 C27 C28 176.7(4) . . . . ? C26 C27 C28 C29 -0.4(7) . . . . ? C27 C28 C29 C30 -1.4(7) . . . . ? C28 C29 C30 C31 2.1(7) . . . . ? C27 C26 C31 C30 -0.9(6) . . . . ? C25 C26 C31 C30 -175.8(4) . . . . ? C29 C30 C31 C26 -1.0(7) . . . . ? O1 C25 C32 C33 3.6(7) . . . . ? C26 C25 C32 C33 -176.7(4) . . . . ? O1 C25 C32 O3 175.8(4) . . . . ? C26 C25 C32 O3 -4.5(6) . . . . ? Ni1 O2 C33 C32 -2.0(6) . . . . ? Ni1 O2 C33 C34 -178.8(3) . . . . ? C25 C32 C33 O2 -15.2(7) . . . . ? O3 C32 C33 O2 172.4(4) . . . . ? C25 C32 C33 C34 161.4(5) . . . . ? O3 C32 C33 C34 -11.0(7) . . . . ? O2 C33 C34 C39 -48.1(8) . . . . ? C32 C33 C34 C39 135.0(7) . . . . ? O2 C33 C34 C35 116.4(6) . . . . ? C32 C33 C34 C35 -60.6(8) . . . . ? C39 C34 C35 C36 -4.5(11) . . . . ? C33 C34 C35 C36 -169.4(7) . . . . ? C34 C35 C36 C37 -0.6(13) . . . . ? C35 C36 C37 C38 2.3(16) . . . . ? C36 C37 C38 C39 0.9(18) . . . . ? C35 C34 C39 C38 8.1(14) . . . . ? C33 C34 C39 C38 173.0(9) . . . . ? C37 C38 C39 C34 -6.5(17) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3N O4 0.84 2.01 2.852(6) 177.1 . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.972 _refine_diff_density_min -0.684 _refine_diff_density_rms 0.082 #===END data_usu163 #(Compound 4.Et2O) _database_code_depnum_ccdc_archive 'CCDC 821106' #TrackingRef '- Revised_cifs.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H33 N4 Ni O2,Cl O4,C4 H10 O' _chemical_formula_sum 'C43 H43 Cl N4 Ni O7' _chemical_formula_weight 821.97 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pcab loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z+1/2' 'x+1/2, -y, -z+1/2' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, y-1/2, -z-1/2' '-x-1/2, y, z-1/2' 'x-1/2, -y-1/2, z' _cell_length_a 16.0204(3) _cell_length_b 19.2924(6) _cell_length_c 25.0918(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7755.2(4) _cell_formula_units_Z 8 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 32251 _cell_measurement_theta_min 1.018 _cell_measurement_theta_max 27.485 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.408 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3440 _exptl_absorpt_coefficient_mu 0.627 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7967 _exptl_absorpt_correction_T_max 0.9400 _exptl_absorpt_process_details 'DENZO-SMN (Otwinowoski & Minor, 1997)' _exptl_special_details ; The program Denzo-SMN (Otwinowski & Minor, 1997) uses a scaling algorithm (Fox & Holmes, 1966) which effectively corrects for absorption effects. High redundancy data were used in the scaling program hence the 'multi-scan' code word was used. No transmission coefficients are available from the program (only scale factors for each frame). The scale factors in the experimental table are calculated from the 'size' command in the SHELXL-97 input file. ; _diffrn_ambient_temperature 150(1) _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 'Nonius KappaCCD Diffractometer' _diffrn_measurement_method 'Phi and Omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16226 _diffrn_reflns_av_R_equivalents 0.0767 _diffrn_reflns_av_sigmaI/netI 0.1004 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 27.49 _reflns_number_total 8868 _reflns_number_gt 5176 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'WinGX, Ortep3' _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 Rfactors 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^)+(0.0422P)^2^+7.1972P] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8868 _refine_ls_number_parameters 677 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1242 _refine_ls_R_factor_gt 0.0552 _refine_ls_wR_factor_ref 0.1275 _refine_ls_wR_factor_gt 0.1015 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _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 C1 C 0.26395(19) 0.19249(17) 0.33867(15) 0.0253(8) Uani 1 1 d . . . C2 C 0.3003(2) 0.23136(18) 0.37833(15) 0.0280(8) Uani 1 1 d . . . C3 C 0.2781(2) 0.21786(19) 0.43044(15) 0.0286(8) Uani 1 1 d . . . C4 C 0.2198(2) 0.16791(18) 0.44101(14) 0.0268(8) Uani 1 1 d . . . C5 C 0.18485(18) 0.13103(16) 0.39944(13) 0.0225(7) Uani 1 1 d . . . C6 C 0.1161(2) 0.07923(19) 0.40842(15) 0.0279(8) Uani 1 1 d . . . C7 C 0.1464(2) -0.03872(18) 0.37645(15) 0.0258(8) Uani 1 1 d . . . C8 C 0.24006(19) -0.03239(17) 0.37048(13) 0.0244(7) Uani 1 1 d . . . C9 C 0.2961(2) -0.06497(19) 0.40355(15) 0.0313(8) Uani 1 1 d . . . C10 C 0.3811(2) -0.0570(2) 0.39446(16) 0.0360(9) Uani 1 1 d . . . C11 C 0.4065(2) -0.0174(2) 0.35142(16) 0.0364(9) Uani 1 1 d . . . C12 C 0.3470(2) 0.01354(19) 0.31994(15) 0.0288(8) Uani 1 1 d . . . C13 C 0.0174(2) 0.02082(19) 0.34979(15) 0.0245(8) Uani 1 1 d . . . C14 C -0.01204(19) 0.07793(17) 0.31371(13) 0.0243(7) Uani 1 1 d . . . C15 C -0.0963(2) 0.0927(2) 0.31040(16) 0.0312(9) Uani 1 1 d . . . C16 C -0.1236(2) 0.1378(2) 0.27199(16) 0.0386(10) Uani 1 1 d . . . C17 C -0.0665(2) 0.1681(2) 0.23830(16) 0.0340(9) Uani 1 1 d . . . C18 C 0.01847(19) 0.15394(17) 0.24443(13) 0.0244(7) Uani 1 1 d . . . C19 C 0.08071(19) 0.18895(17) 0.20933(13) 0.0233(7) Uani 1 1 d . . . C20 C 0.0823(2) 0.1741(2) 0.15558(15) 0.0320(9) Uani 1 1 d . . . C21 C 0.1361(2) 0.2095(2) 0.12193(16) 0.0400(10) Uani 1 1 d . . . C22 C 0.1877(2) 0.2603(2) 0.14163(16) 0.0400(10) Uani 1 1 d . . . C23 C 0.1862(2) 0.2755(2) 0.19518(15) 0.0371(9) Uani 1 1 d . . . C24 C 0.1336(2) 0.23963(19) 0.22936(15) 0.0300(8) Uani 1 1 d . . . C25 C 0.15055(18) -0.03222(16) 0.20786(13) 0.0211(7) Uani 1 1 d . . . C26 C 0.11024(18) -0.09595(17) 0.18549(13) 0.0214(7) Uani 1 1 d . . . C27 C 0.03389(19) -0.11731(19) 0.20728(14) 0.0261(8) Uani 1 1 d . . . C28 C -0.0077(2) -0.17442(19) 0.18769(14) 0.0291(8) Uani 1 1 d . . . C29 C 0.0259(2) -0.21218(19) 0.14630(15) 0.0312(9) Uani 1 1 d . . . C30 C 0.1019(2) -0.19254(19) 0.12507(15) 0.0295(8) Uani 1 1 d . . . C31 C 0.1432(2) -0.13459(18) 0.14397(13) 0.0253(8) Uani 1 1 d . . . C32 C 0.21095(19) 0.00339(18) 0.17789(14) 0.0215(7) Uani 1 1 d . . . C33 C 0.25220(17) 0.06465(17) 0.19308(12) 0.0201(7) Uani 1 1 d . . . C34 C 0.32055(18) 0.09280(16) 0.15780(13) 0.0205(7) Uani 1 1 d . . . C35 C 0.3778(2) 0.13933(17) 0.17994(14) 0.0247(8) Uani 1 1 d . . . C36 C 0.4444(2) 0.16447(19) 0.15050(15) 0.0295(8) Uani 1 1 d . . . C37 C 0.4549(2) 0.14418(18) 0.09828(15) 0.0289(8) Uani 1 1 d . . . C38 C 0.3985(2) 0.09850(19) 0.07557(14) 0.0283(8) Uani 1 1 d . . . C39 C 0.3313(2) 0.07324(18) 0.10470(13) 0.0240(7) Uani 1 1 d . . . C40 C 0.0617(3) 0.2968(3) 0.5139(2) 0.0524(12) Uani 1 1 d . . . C41 C -0.0189(3) 0.3291(2) 0.49713(18) 0.0475(11) Uani 1 1 d . . . C42 C -0.1054(3) 0.4272(2) 0.51140(18) 0.0437(10) Uani 1 1 d . . . C43 C -0.1097(3) 0.4934(3) 0.5416(2) 0.0485(11) Uani 1 1 d . . . N1 N 0.20645(15) 0.14298(14) 0.34838(10) 0.0216(6) Uani 1 1 d . . . N2 N 0.10631(14) 0.02872(13) 0.36428(10) 0.0212(6) Uani 1 1 d . . . N3 N 0.26496(15) 0.00669(13) 0.32871(11) 0.0231(6) Uani 1 1 d . . . N4 N 0.04528(15) 0.10914(13) 0.28210(10) 0.0203(6) Uani 1 1 d . . . O1 O 0.12608(13) -0.01475(11) 0.25402(9) 0.0243(5) Uani 1 1 d . . . O2 O 0.23941(12) 0.09775(11) 0.23587(8) 0.0231(5) Uani 1 1 d . . . O3 O -0.14843(16) 0.15648(14) 0.51664(9) 0.0426(7) Uani 1 1 d . . . O4 O -0.19132(17) 0.09645(16) 0.44057(12) 0.0608(9) Uani 1 1 d . . . O5 O -0.07581(17) 0.05695(13) 0.48926(11) 0.0471(7) Uani 1 1 d . . . O6 O -0.06717(16) 0.15915(15) 0.43915(11) 0.0506(8) Uani 1 1 d . . . O7 O -0.03246(14) 0.39063(13) 0.52720(10) 0.0361(6) Uani 1 1 d . . . Cl1 Cl -0.12103(5) 0.11655(4) 0.47153(3) 0.0278(2) Uani 1 1 d . . . Ni1 Ni 0.16719(2) 0.06631(2) 0.295975(16) 0.01984(12) Uani 1 1 d . . . H1 H 0.2746(16) 0.1974(15) 0.3016(12) 0.010(7) Uiso 1 1 d . . . H2 H 0.3366(19) 0.2657(18) 0.3692(13) 0.028(9) Uiso 1 1 d . . . H3 H 0.300(2) 0.2439(19) 0.4596(14) 0.040(10) Uiso 1 1 d . . . H4 H 0.2049(17) 0.1566(16) 0.4758(13) 0.018(8) Uiso 1 1 d . . . H6A H 0.066(2) 0.1066(17) 0.4131(13) 0.028(9) Uiso 1 1 d . . . H6B H 0.1242(19) 0.0565(17) 0.4407(14) 0.028(10) Uiso 1 1 d . . . H7A H 0.1253(18) -0.0718(17) 0.3488(13) 0.024(9) Uiso 1 1 d . . . H7B H 0.1312(19) -0.0555(17) 0.4125(14) 0.028(9) Uiso 1 1 d . . . H9 H 0.2757(18) -0.0904(17) 0.4343(13) 0.023(9) Uiso 1 1 d . . . H10 H 0.419(2) -0.0767(18) 0.4186(14) 0.034(10) Uiso 1 1 d . . . H11 H 0.463(2) -0.008(2) 0.3429(15) 0.050(12) Uiso 1 1 d . . . H12 H 0.360(2) 0.0380(18) 0.2890(14) 0.032(10) Uiso 1 1 d . . . H13A H 0.0113(18) -0.0241(18) 0.3313(13) 0.026(9) Uiso 1 1 d . . . H13B H -0.016(2) 0.0177(17) 0.3785(13) 0.027(9) Uiso 1 1 d . . . H15 H -0.132(2) 0.0684(19) 0.3334(15) 0.039(10) Uiso 1 1 d . . . H16 H -0.180(2) 0.1459(18) 0.2674(14) 0.038(10) Uiso 1 1 d . . . H17 H -0.0788(19) 0.1978(18) 0.2120(13) 0.026(9) Uiso 1 1 d . . . H20 H 0.047(2) 0.1399(18) 0.1426(13) 0.030(10) Uiso 1 1 d . . . H21 H 0.137(2) 0.1956(18) 0.0866(15) 0.035(10) Uiso 1 1 d . . . H22 H 0.223(2) 0.286(2) 0.1183(14) 0.043(11) Uiso 1 1 d . . . H23 H 0.221(2) 0.316(2) 0.2087(14) 0.050(12) Uiso 1 1 d . . . H24 H 0.1325(17) 0.2512(16) 0.2663(12) 0.017(8) Uiso 1 1 d . . . H27 H 0.0143(18) -0.0912(16) 0.2366(12) 0.020(8) Uiso 1 1 d . . . H28 H -0.060(2) -0.1876(18) 0.2028(13) 0.035(10) Uiso 1 1 d . . . H29 H -0.0021(19) -0.2516(18) 0.1328(12) 0.021(8) Uiso 1 1 d . . . H30 H 0.1231(19) -0.2164(17) 0.0981(13) 0.023(9) Uiso 1 1 d . . . H31 H 0.1965(19) -0.1227(16) 0.1289(11) 0.020(8) Uiso 1 1 d . . . H32 H 0.2251(16) -0.0156(15) 0.1482(12) 0.008(8) Uiso 1 1 d . . . H35 H 0.3664(16) 0.1522(15) 0.2162(12) 0.011(7) Uiso 1 1 d . . . H36 H 0.484(2) 0.193(2) 0.1668(14) 0.044(11) Uiso 1 1 d . . . H37 H 0.502(2) 0.1610(18) 0.0779(13) 0.034(10) Uiso 1 1 d . . . H38 H 0.406(2) 0.0831(18) 0.0389(15) 0.036(10) Uiso 1 1 d . . . H39 H 0.296(2) 0.0418(19) 0.0888(14) 0.036(10) Uiso 1 1 d . . . H40A H 0.064(2) 0.289(2) 0.5513(16) 0.044(12) Uiso 1 1 d . . . H40B H 0.071(2) 0.250(2) 0.4940(15) 0.054(12) Uiso 1 1 d . . . H40C H 0.114(2) 0.329(2) 0.5067(15) 0.048(12) Uiso 1 1 d . . . H41A H -0.066(2) 0.299(2) 0.5038(16) 0.056(13) Uiso 1 1 d . . . H41B H -0.018(2) 0.3412(19) 0.4574(16) 0.041(11) Uiso 1 1 d . . . H42A H -0.159(3) 0.397(2) 0.5202(16) 0.066(13) Uiso 1 1 d . . . H42B H -0.104(2) 0.4366(18) 0.4741(15) 0.034(10) Uiso 1 1 d . . . H43A H -0.110(2) 0.485(2) 0.5808(19) 0.066(14) Uiso 1 1 d . . . H43B H -0.158(2) 0.5204(19) 0.5336(14) 0.034(10) Uiso 1 1 d . . . H43C H -0.060(3) 0.525(2) 0.5325(17) 0.065(13) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0243(17) 0.0236(19) 0.028(2) -0.0017(17) 0.0025(15) -0.0023(14) C2 0.0237(17) 0.0206(19) 0.040(2) -0.0040(18) -0.0013(16) -0.0024(15) C3 0.0318(19) 0.0251(19) 0.029(2) -0.0071(17) -0.0085(16) 0.0011(15) C4 0.0311(18) 0.027(2) 0.0224(19) -0.0006(17) -0.0028(15) 0.0012(15) C5 0.0241(16) 0.0205(17) 0.0229(18) -0.0016(15) -0.0012(14) 0.0044(13) C6 0.034(2) 0.029(2) 0.021(2) -0.0045(17) 0.0035(16) -0.0008(16) C7 0.0305(18) 0.0212(18) 0.026(2) 0.0033(17) 0.0010(16) -0.0019(14) C8 0.0276(17) 0.0191(17) 0.0263(19) -0.0011(16) -0.0010(15) 0.0001(14) C9 0.0320(19) 0.028(2) 0.034(2) 0.0058(19) -0.0006(17) -0.0023(16) C10 0.033(2) 0.033(2) 0.042(2) 0.007(2) -0.0066(18) 0.0072(17) C11 0.0261(19) 0.036(2) 0.048(3) 0.005(2) -0.0015(18) 0.0030(17) C12 0.0247(18) 0.028(2) 0.034(2) 0.0037(18) 0.0030(16) 0.0031(15) C13 0.0221(17) 0.023(2) 0.028(2) 0.0021(18) 0.0028(15) -0.0060(14) C14 0.0247(17) 0.0230(19) 0.0251(18) -0.0032(15) -0.0003(14) -0.0018(14) C15 0.0242(18) 0.034(2) 0.036(2) 0.0048(19) 0.0012(16) -0.0039(16) C16 0.0209(19) 0.045(3) 0.050(3) 0.008(2) -0.0025(17) 0.0013(17) C17 0.031(2) 0.033(2) 0.038(2) 0.012(2) -0.0067(17) 0.0035(16) C18 0.0265(17) 0.0204(18) 0.0262(18) -0.0012(16) -0.0022(15) 0.0008(14) C19 0.0253(16) 0.0227(18) 0.0218(18) 0.0031(16) -0.0014(14) 0.0054(14) C20 0.037(2) 0.027(2) 0.032(2) -0.0035(18) -0.0019(17) -0.0066(17) C21 0.052(2) 0.043(2) 0.025(2) -0.003(2) 0.0026(19) -0.005(2) C22 0.039(2) 0.043(3) 0.038(2) 0.014(2) 0.0057(18) -0.0065(18) C23 0.037(2) 0.041(2) 0.034(2) 0.0088(19) -0.0041(17) -0.0141(18) C24 0.0344(19) 0.032(2) 0.0231(19) -0.0025(18) -0.0015(16) -0.0042(16) C25 0.0224(16) 0.0185(16) 0.0222(17) 0.0028(15) -0.0065(14) 0.0027(13) C26 0.0223(16) 0.0202(17) 0.0217(17) 0.0018(15) -0.0033(14) 0.0011(13) C27 0.0268(17) 0.0267(19) 0.0247(19) -0.0045(17) 0.0026(15) 0.0020(14) C28 0.0226(17) 0.031(2) 0.034(2) -0.0061(17) 0.0027(15) -0.0062(15) C29 0.0321(19) 0.025(2) 0.037(2) -0.0046(18) -0.0063(17) -0.0074(16) C30 0.0326(19) 0.027(2) 0.029(2) -0.0087(18) 0.0006(16) 0.0019(16) C31 0.0233(17) 0.027(2) 0.0260(19) -0.0016(16) 0.0009(15) 0.0009(14) C32 0.0241(17) 0.0230(19) 0.0173(18) -0.0009(16) 0.0017(14) -0.0011(14) C33 0.0162(14) 0.0198(16) 0.0244(18) 0.0006(16) -0.0030(13) 0.0043(13) C34 0.0202(16) 0.0189(16) 0.0224(17) 0.0032(15) -0.0010(13) 0.0008(13) C35 0.0301(18) 0.0214(18) 0.0226(19) -0.0041(16) 0.0047(15) -0.0018(14) C36 0.0276(18) 0.028(2) 0.033(2) -0.0036(18) 0.0050(16) -0.0053(16) C37 0.0279(18) 0.026(2) 0.033(2) 0.0067(17) 0.0067(16) 0.0026(15) C38 0.0328(19) 0.032(2) 0.0196(19) 0.0009(17) 0.0026(15) 0.0040(16) C39 0.0264(17) 0.0246(18) 0.0210(17) 0.0002(16) 0.0004(15) -0.0008(15) C40 0.077(3) 0.038(3) 0.042(3) -0.002(2) 0.004(3) 0.010(3) C41 0.057(3) 0.050(3) 0.036(3) -0.009(2) 0.009(2) -0.015(2) C42 0.044(2) 0.055(3) 0.032(2) 0.006(2) -0.0052(19) -0.005(2) C43 0.041(3) 0.051(3) 0.053(3) 0.003(3) 0.010(2) 0.007(2) N1 0.0220(13) 0.0202(15) 0.0226(15) 0.0000(13) -0.0005(12) 0.0009(11) N2 0.0210(13) 0.0207(15) 0.0221(15) 0.0007(12) 0.0019(11) -0.0029(11) N3 0.0245(14) 0.0196(15) 0.0251(15) -0.0001(13) 0.0006(12) 0.0032(11) N4 0.0207(13) 0.0157(14) 0.0245(15) -0.0026(12) -0.0006(11) 0.0003(11) O1 0.0285(12) 0.0221(12) 0.0221(12) -0.0032(11) 0.0036(10) -0.0037(10) O2 0.0237(11) 0.0235(13) 0.0223(13) -0.0024(11) 0.0034(9) -0.0026(10) O3 0.0614(17) 0.0394(16) 0.0270(14) -0.0029(13) 0.0072(12) 0.0137(13) O4 0.0490(17) 0.063(2) 0.070(2) -0.0126(18) -0.0282(15) -0.0068(15) O5 0.0670(18) 0.0308(15) 0.0433(17) 0.0075(13) -0.0029(14) 0.0209(13) O6 0.0466(16) 0.0472(18) 0.0581(19) 0.0157(15) 0.0237(14) 0.0055(13) O7 0.0384(14) 0.0357(16) 0.0343(15) -0.0073(13) -0.0010(12) -0.0039(12) Cl1 0.0320(4) 0.0266(4) 0.0250(4) 0.0014(4) -0.0023(4) 0.0035(4) Ni1 0.0212(2) 0.0185(2) 0.0198(2) -0.00057(19) 0.00182(17) -0.00185(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.349(4) . ? C1 C2 1.375(5) . ? C1 H1 0.95(3) . ? C2 C3 1.380(5) . ? C2 H2 0.91(3) . ? C3 C4 1.368(5) . ? C3 H3 0.96(4) . ? C4 C5 1.381(4) . ? C4 H4 0.93(3) . ? C5 N1 1.347(4) . ? C5 C6 1.504(5) . ? C6 N2 1.484(4) . ? C6 H6A 0.97(3) . ? C6 H6B 0.93(3) . ? C7 N2 1.482(4) . ? C7 C8 1.513(4) . ? C7 H7A 1.00(3) . ? C7 H7B 0.99(3) . ? C8 N3 1.351(4) . ? C8 C9 1.375(5) . ? C9 C10 1.389(5) . ? C9 H9 0.97(3) . ? C10 C11 1.384(5) . ? C10 H10 0.94(3) . ? C11 C12 1.375(5) . ? C11 H11 0.94(4) . ? C12 N3 1.339(4) . ? C12 H12 0.93(3) . ? C13 N2 1.478(4) . ? C13 C14 1.502(5) . ? C13 H13A 0.99(3) . ? C13 H13B 0.90(3) . ? C14 N4 1.355(4) . ? C14 C15 1.383(4) . ? C15 C16 1.370(5) . ? C15 H15 0.94(4) . ? C16 C17 1.375(5) . ? C16 H16 0.93(3) . ? C17 C18 1.396(4) . ? C17 H17 0.90(3) . ? C18 N4 1.351(4) . ? C18 C19 1.492(4) . ? C19 C20 1.379(5) . ? C19 C24 1.388(5) . ? C20 C21 1.386(5) . ? C20 H20 0.93(3) . ? C21 C22 1.374(5) . ? C21 H21 0.93(4) . ? C22 C23 1.376(5) . ? C22 H22 0.96(4) . ? C23 C24 1.387(5) . ? C23 H23 1.01(4) . ? C24 H24 0.95(3) . ? C25 O1 1.268(4) . ? C25 C32 1.405(4) . ? C25 C26 1.498(4) . ? C26 C31 1.386(5) . ? C26 C27 1.402(4) . ? C27 C28 1.378(5) . ? C27 H27 0.94(3) . ? C28 C29 1.378(5) . ? C28 H28 0.95(3) . ? C29 C30 1.382(5) . ? C29 H29 0.95(3) . ? C30 C31 1.383(5) . ? C30 H30 0.89(3) . ? C31 H31 0.96(3) . ? C32 C33 1.407(4) . ? C32 H32 0.86(3) . ? C33 O2 1.266(4) . ? C33 C34 1.509(4) . ? C34 C39 1.396(4) . ? C34 C35 1.399(4) . ? C35 C36 1.386(5) . ? C35 H35 0.96(3) . ? C36 C37 1.378(5) . ? C36 H36 0.94(4) . ? C37 C38 1.386(5) . ? C37 H37 0.97(3) . ? C38 C39 1.389(5) . ? C38 H38 0.97(4) . ? C39 H39 0.92(4) . ? C40 C41 1.494(6) . ? C40 H40A 0.95(4) . ? C40 H40B 1.04(4) . ? C40 H40C 1.05(4) . ? C41 O7 1.423(5) . ? C41 H41A 0.97(4) . ? C41 H41B 1.02(4) . ? C42 O7 1.422(5) . ? C42 C43 1.487(6) . ? C42 H42A 1.06(4) . ? C42 H42B 0.95(4) . ? C43 H43A 1.00(5) . ? C43 H43B 0.96(4) . ? C43 H43C 1.02(4) . ? N1 Ni1 2.077(3) . ? N2 Ni1 2.101(3) . ? N3 Ni1 2.110(3) . ? N4 Ni1 2.149(2) . ? O1 Ni1 1.997(2) . ? O2 Ni1 1.995(2) . ? O3 Cl1 1.438(2) . ? O4 Cl1 1.422(3) . ? O5 Cl1 1.430(2) . ? O6 Cl1 1.442(3) . ? 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 C1 C2 123.0(3) . . ? N1 C1 H1 111.7(17) . . ? C2 C1 H1 125.3(18) . . ? C1 C2 C3 118.3(3) . . ? C1 C2 H2 119(2) . . ? C3 C2 H2 123(2) . . ? C4 C3 C2 119.5(3) . . ? C4 C3 H3 118(2) . . ? C2 C3 H3 122(2) . . ? C3 C4 C5 119.5(3) . . ? C3 C4 H4 121.5(19) . . ? C5 C4 H4 118.9(19) . . ? N1 C5 C4 121.7(3) . . ? N1 C5 C6 116.4(3) . . ? C4 C5 C6 121.7(3) . . ? N2 C6 C5 113.7(3) . . ? N2 C6 H6A 111.0(19) . . ? C5 C6 H6A 105.5(19) . . ? N2 C6 H6B 111(2) . . ? C5 C6 H6B 110(2) . . ? H6A C6 H6B 105(3) . . ? N2 C7 C8 109.8(3) . . ? N2 C7 H7A 105.7(18) . . ? C8 C7 H7A 108.5(17) . . ? N2 C7 H7B 111.6(19) . . ? C8 C7 H7B 111.1(18) . . ? H7A C7 H7B 110(3) . . ? N3 C8 C9 122.0(3) . . ? N3 C8 C7 114.5(3) . . ? C9 C8 C7 123.4(3) . . ? C8 C9 C10 119.4(4) . . ? C8 C9 H9 119.3(18) . . ? C10 C9 H9 121.1(18) . . ? C11 C10 C9 118.5(4) . . ? C11 C10 H10 122(2) . . ? C9 C10 H10 119(2) . . ? C12 C11 C10 119.0(3) . . ? C12 C11 H11 117(2) . . ? C10 C11 H11 124(2) . . ? N3 C12 C11 122.9(4) . . ? N3 C12 H12 114(2) . . ? C11 C12 H12 122(2) . . ? N2 C13 C14 112.0(3) . . ? N2 C13 H13A 107.5(18) . . ? C14 C13 H13A 109.2(19) . . ? N2 C13 H13B 113(2) . . ? C14 C13 H13B 110(2) . . ? H13A C13 H13B 105(3) . . ? N4 C14 C15 122.4(3) . . ? N4 C14 C13 117.8(3) . . ? C15 C14 C13 119.6(3) . . ? C16 C15 C14 119.0(3) . . ? C16 C15 H15 124(2) . . ? C14 C15 H15 117(2) . . ? C15 C16 C17 119.4(3) . . ? C15 C16 H16 120(2) . . ? C17 C16 H16 120(2) . . ? C16 C17 C18 119.8(4) . . ? C16 C17 H17 125(2) . . ? C18 C17 H17 115(2) . . ? N4 C18 C17 120.8(3) . . ? N4 C18 C19 119.4(3) . . ? C17 C18 C19 119.9(3) . . ? C20 C19 C24 119.3(3) . . ? C20 C19 C18 119.7(3) . . ? C24 C19 C18 120.9(3) . . ? C19 C20 C21 120.3(4) . . ? C19 C20 H20 119(2) . . ? C21 C20 H20 121(2) . . ? C22 C21 C20 120.4(4) . . ? C22 C21 H21 123(2) . . ? C20 C21 H21 117(2) . . ? C21 C22 C23 119.5(4) . . ? C21 C22 H22 121(2) . . ? C23 C22 H22 120(2) . . ? C22 C23 C24 120.5(4) . . ? C22 C23 H23 119(2) . . ? C24 C23 H23 121(2) . . ? C23 C24 C19 119.9(3) . . ? C23 C24 H24 119.7(18) . . ? C19 C24 H24 120.3(18) . . ? O1 C25 C32 124.9(3) . . ? O1 C25 C26 115.3(3) . . ? C32 C25 C26 119.9(3) . . ? C31 C26 C27 117.9(3) . . ? C31 C26 C25 124.0(3) . . ? C27 C26 C25 118.1(3) . . ? C28 C27 C26 121.2(3) . . ? C28 C27 H27 122.9(18) . . ? C26 C27 H27 115.9(18) . . ? C29 C28 C27 120.2(3) . . ? C29 C28 H28 120(2) . . ? C27 C28 H28 120(2) . . ? C28 C29 C30 119.3(3) . . ? C28 C29 H29 120.7(18) . . ? C30 C29 H29 120.0(18) . . ? C29 C30 C31 120.7(3) . . ? C29 C30 H30 119(2) . . ? C31 C30 H30 120(2) . . ? C30 C31 C26 120.7(3) . . ? C30 C31 H31 118.9(18) . . ? C26 C31 H31 120.4(18) . . ? C25 C32 C33 126.1(3) . . ? C25 C32 H32 115.9(19) . . ? C33 C32 H32 117.9(19) . . ? O2 C33 C32 125.3(3) . . ? O2 C33 C34 115.7(3) . . ? C32 C33 C34 119.0(3) . . ? C39 C34 C35 118.1(3) . . ? C39 C34 C33 123.5(3) . . ? C35 C34 C33 118.3(3) . . ? C36 C35 C34 121.2(3) . . ? C36 C35 H35 124.2(17) . . ? C34 C35 H35 114.6(17) . . ? C37 C36 C35 120.1(3) . . ? C37 C36 H36 120(2) . . ? C35 C36 H36 120(2) . . ? C36 C37 C38 119.5(3) . . ? C36 C37 H37 120(2) . . ? C38 C37 H37 120(2) . . ? C37 C38 C39 120.8(3) . . ? C37 C38 H38 120(2) . . ? C39 C38 H38 119(2) . . ? C38 C39 C34 120.2(3) . . ? C38 C39 H39 119(2) . . ? C34 C39 H39 121(2) . . ? C41 C40 H40A 113(2) . . ? C41 C40 H40B 111(2) . . ? H40A C40 H40B 109(3) . . ? C41 C40 H40C 113(2) . . ? H40A C40 H40C 103(3) . . ? H40B C40 H40C 107(3) . . ? O7 C41 C40 109.3(4) . . ? O7 C41 H41A 107(2) . . ? C40 C41 H41A 111(2) . . ? O7 C41 H41B 109(2) . . ? C40 C41 H41B 111(2) . . ? H41A C41 H41B 109(3) . . ? O7 C42 C43 108.8(3) . . ? O7 C42 H42A 110(2) . . ? C43 C42 H42A 109(2) . . ? O7 C42 H42B 110(2) . . ? C43 C42 H42B 110(2) . . ? H42A C42 H42B 109(3) . . ? C42 C43 H43A 112(3) . . ? C42 C43 H43B 113(2) . . ? H43A C43 H43B 107(3) . . ? C42 C43 H43C 111(2) . . ? H43A C43 H43C 109(3) . . ? H43B C43 H43C 105(3) . . ? C5 N1 C1 117.9(3) . . ? C5 N1 Ni1 113.7(2) . . ? C1 N1 Ni1 126.6(2) . . ? C13 N2 C7 112.2(3) . . ? C13 N2 C6 110.7(3) . . ? C7 N2 C6 112.1(3) . . ? C13 N2 Ni1 106.4(2) . . ? C7 N2 Ni1 105.66(19) . . ? C6 N2 Ni1 109.5(2) . . ? C12 N3 C8 118.2(3) . . ? C12 N3 Ni1 127.6(2) . . ? C8 N3 Ni1 112.8(2) . . ? C18 N4 C14 118.6(3) . . ? C18 N4 Ni1 130.4(2) . . ? C14 N4 Ni1 110.5(2) . . ? C25 O1 Ni1 126.0(2) . . ? C33 O2 Ni1 125.6(2) . . ? C42 O7 C41 113.0(3) . . ? O4 Cl1 O5 110.60(18) . . ? O4 Cl1 O3 109.54(17) . . ? O5 Cl1 O3 109.91(16) . . ? O4 Cl1 O6 108.75(19) . . ? O5 Cl1 O6 109.29(16) . . ? O3 Cl1 O6 108.72(17) . . ? O2 Ni1 O1 91.77(9) . . ? O2 Ni1 N1 94.96(9) . . ? O1 Ni1 N1 172.53(10) . . ? O2 Ni1 N2 172.17(9) . . ? O1 Ni1 N2 90.38(9) . . ? N1 Ni1 N2 82.53(10) . . ? O2 Ni1 N3 91.69(9) . . ? O1 Ni1 N3 91.33(9) . . ? N1 Ni1 N3 85.24(10) . . ? N2 Ni1 N3 80.73(10) . . ? O2 Ni1 N4 106.72(9) . . ? O1 Ni1 N4 85.18(9) . . ? N1 Ni1 N4 95.97(10) . . ? N2 Ni1 N4 80.97(10) . . ? N3 Ni1 N4 161.33(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 1.4(5) . . . . ? C1 C2 C3 C4 -1.5(5) . . . . ? C2 C3 C4 C5 0.9(5) . . . . ? C3 C4 C5 N1 -0.2(5) . . . . ? C3 C4 C5 C6 -175.5(3) . . . . ? N1 C5 C6 N2 24.0(4) . . . . ? C4 C5 C6 N2 -160.4(3) . . . . ? N2 C7 C8 N3 -39.4(4) . . . . ? N2 C7 C8 C9 142.4(3) . . . . ? N3 C8 C9 C10 0.9(5) . . . . ? C7 C8 C9 C10 179.0(3) . . . . ? C8 C9 C10 C11 -1.3(6) . . . . ? C9 C10 C11 C12 1.2(6) . . . . ? C10 C11 C12 N3 -0.6(6) . . . . ? N2 C13 C14 N4 27.1(4) . . . . ? N2 C13 C14 C15 -158.4(3) . . . . ? N4 C14 C15 C16 3.5(6) . . . . ? C13 C14 C15 C16 -170.8(3) . . . . ? C14 C15 C16 C17 -1.1(6) . . . . ? C15 C16 C17 C18 -1.6(6) . . . . ? C16 C17 C18 N4 2.0(6) . . . . ? C16 C17 C18 C19 -177.5(3) . . . . ? N4 C18 C19 C20 113.6(4) . . . . ? C17 C18 C19 C20 -66.9(5) . . . . ? N4 C18 C19 C24 -70.6(4) . . . . ? C17 C18 C19 C24 108.9(4) . . . . ? C24 C19 C20 C21 -0.1(5) . . . . ? C18 C19 C20 C21 175.8(3) . . . . ? C19 C20 C21 C22 -0.7(6) . . . . ? C20 C21 C22 C23 0.4(6) . . . . ? C21 C22 C23 C24 0.6(6) . . . . ? C22 C23 C24 C19 -1.4(6) . . . . ? C20 C19 C24 C23 1.1(5) . . . . ? C18 C19 C24 C23 -174.7(3) . . . . ? O1 C25 C26 C31 -161.0(3) . . . . ? C32 C25 C26 C31 19.0(5) . . . . ? O1 C25 C26 C27 20.1(4) . . . . ? C32 C25 C26 C27 -160.0(3) . . . . ? C31 C26 C27 C28 -0.7(5) . . . . ? C25 C26 C27 C28 178.3(3) . . . . ? C26 C27 C28 C29 0.6(5) . . . . ? C27 C28 C29 C30 0.6(5) . . . . ? C28 C29 C30 C31 -1.7(5) . . . . ? C29 C30 C31 C26 1.6(5) . . . . ? C27 C26 C31 C30 -0.4(5) . . . . ? C25 C26 C31 C30 -179.4(3) . . . . ? O1 C25 C32 C33 -1.9(5) . . . . ? C26 C25 C32 C33 178.2(3) . . . . ? C25 C32 C33 O2 -1.7(5) . . . . ? C25 C32 C33 C34 175.1(3) . . . . ? O2 C33 C34 C39 -165.4(3) . . . . ? C32 C33 C34 C39 17.5(4) . . . . ? O2 C33 C34 C35 16.8(4) . . . . ? C32 C33 C34 C35 -160.3(3) . . . . ? C39 C34 C35 C36 -1.2(5) . . . . ? C33 C34 C35 C36 176.8(3) . . . . ? C34 C35 C36 C37 0.5(5) . . . . ? C35 C36 C37 C38 0.0(5) . . . . ? C36 C37 C38 C39 0.3(5) . . . . ? C37 C38 C39 C34 -1.0(5) . . . . ? C35 C34 C39 C38 1.4(5) . . . . ? C33 C34 C39 C38 -176.5(3) . . . . ? C4 C5 N1 C1 0.1(5) . . . . ? C6 C5 N1 C1 175.7(3) . . . . ? C4 C5 N1 Ni1 166.2(2) . . . . ? C6 C5 N1 Ni1 -18.2(3) . . . . ? C2 C1 N1 C5 -0.7(5) . . . . ? C2 C1 N1 Ni1 -164.9(2) . . . . ? C14 C13 N2 C7 -152.6(3) . . . . ? C14 C13 N2 C6 81.3(4) . . . . ? C14 C13 N2 Ni1 -37.5(3) . . . . ? C8 C7 N2 C13 158.8(3) . . . . ? C8 C7 N2 C6 -75.9(3) . . . . ? C8 C7 N2 Ni1 43.2(3) . . . . ? C5 C6 N2 C13 -134.0(3) . . . . ? C5 C6 N2 C7 99.9(3) . . . . ? C5 C6 N2 Ni1 -17.0(3) . . . . ? C11 C12 N3 C8 0.1(5) . . . . ? C11 C12 N3 Ni1 165.5(3) . . . . ? C9 C8 N3 C12 -0.2(5) . . . . ? C7 C8 N3 C12 -178.5(3) . . . . ? C9 C8 N3 Ni1 -167.8(3) . . . . ? C7 C8 N3 Ni1 14.0(3) . . . . ? C17 C18 N4 C14 0.3(5) . . . . ? C19 C18 N4 C14 179.9(3) . . . . ? C17 C18 N4 Ni1 171.4(3) . . . . ? C19 C18 N4 Ni1 -9.0(4) . . . . ? C15 C14 N4 C18 -3.1(5) . . . . ? C13 C14 N4 C18 171.3(3) . . . . ? C15 C14 N4 Ni1 -175.9(3) . . . . ? C13 C14 N4 Ni1 -1.5(4) . . . . ? C32 C25 O1 Ni1 -0.6(4) . . . . ? C26 C25 O1 Ni1 179.26(19) . . . . ? C32 C33 O2 Ni1 7.1(4) . . . . ? C34 C33 O2 Ni1 -169.76(18) . . . . ? C43 C42 O7 C41 -174.9(4) . . . . ? C40 C41 O7 C42 176.3(4) . . . . ? C33 O2 Ni1 O1 -7.2(2) . . . . ? C33 O2 Ni1 N1 169.6(2) . . . . ? C33 O2 Ni1 N2 98.7(7) . . . . ? C33 O2 Ni1 N3 84.2(2) . . . . ? C33 O2 Ni1 N4 -92.7(2) . . . . ? C25 O1 Ni1 O2 4.0(2) . . . . ? C25 O1 Ni1 N1 -150.2(7) . . . . ? C25 O1 Ni1 N2 -168.4(2) . . . . ? C25 O1 Ni1 N3 -87.7(2) . . . . ? C25 O1 Ni1 N4 110.7(2) . . . . ? C5 N1 Ni1 O2 -166.1(2) . . . . ? C1 N1 Ni1 O2 -1.4(3) . . . . ? C5 N1 Ni1 O1 -12.0(8) . . . . ? C1 N1 Ni1 O1 152.7(6) . . . . ? C5 N1 Ni1 N2 6.5(2) . . . . ? C1 N1 Ni1 N2 171.2(3) . . . . ? C5 N1 Ni1 N3 -74.8(2) . . . . ? C1 N1 Ni1 N3 89.9(3) . . . . ? C5 N1 Ni1 N4 86.5(2) . . . . ? C1 N1 Ni1 N4 -108.8(3) . . . . ? C13 N2 Ni1 O2 -162.4(6) . . . . ? C7 N2 Ni1 O2 -43.0(8) . . . . ? C6 N2 Ni1 O2 78.0(8) . . . . ? C13 N2 Ni1 O1 -56.5(2) . . . . ? C7 N2 Ni1 O1 63.0(2) . . . . ? C6 N2 Ni1 O1 -176.1(2) . . . . ? C13 N2 Ni1 N1 125.9(2) . . . . ? C7 N2 Ni1 N1 -114.7(2) . . . . ? C6 N2 Ni1 N1 6.3(2) . . . . ? C13 N2 Ni1 N3 -147.7(2) . . . . ? C7 N2 Ni1 N3 -28.3(2) . . . . ? C6 N2 Ni1 N3 92.6(2) . . . . ? C13 N2 Ni1 N4 28.6(2) . . . . ? C7 N2 Ni1 N4 148.0(2) . . . . ? C6 N2 Ni1 N4 -91.0(2) . . . . ? C12 N3 Ni1 O2 20.5(3) . . . . ? C8 N3 Ni1 O2 -173.4(2) . . . . ? C12 N3 Ni1 O1 112.3(3) . . . . ? C8 N3 Ni1 O1 -81.6(2) . . . . ? C12 N3 Ni1 N1 -74.4(3) . . . . ? C8 N3 Ni1 N1 91.7(2) . . . . ? C12 N3 Ni1 N2 -157.5(3) . . . . ? C8 N3 Ni1 N2 8.5(2) . . . . ? C12 N3 Ni1 N4 -168.9(3) . . . . ? C8 N3 Ni1 N4 -2.8(4) . . . . ? C18 N4 Ni1 O2 -5.8(3) . . . . ? C14 N4 Ni1 O2 165.9(2) . . . . ? C18 N4 Ni1 O1 -96.2(3) . . . . ? C14 N4 Ni1 O1 75.5(2) . . . . ? C18 N4 Ni1 N1 91.2(3) . . . . ? C14 N4 Ni1 N1 -97.1(2) . . . . ? C18 N4 Ni1 N2 172.7(3) . . . . ? C14 N4 Ni1 N2 -15.7(2) . . . . ? C18 N4 Ni1 N3 -176.0(3) . . . . ? C14 N4 Ni1 N3 -4.3(4) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.452 _refine_diff_density_min -0.465 _refine_diff_density_rms 0.082 #===END data_usu160 #(Compound 5) _database_code_depnum_ccdc_archive 'CCDC 821107' #TrackingRef '- Revised_cifs.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H29 N5 Ni O1,2(Cl O4)' _chemical_formula_sum 'C27 H29 Cl2 N5 Ni O9' _chemical_formula_weight 697.16 _chemical_absolute_configuration ad 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P212121 _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 9.8884(2) _cell_length_b 10.8891(2) _cell_length_c 28.1201(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3027.85(9) _cell_formula_units_Z 4 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 27839 _cell_measurement_theta_min 1.018 _cell_measurement_theta_max 27.485 _exptl_crystal_description prism _exptl_crystal_colour purple _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.529 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1440 _exptl_absorpt_coefficient_mu 0.878 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7605 _exptl_absorpt_correction_T_max 0.8440 _exptl_absorpt_process_details 'DENZO-SMN (Otwinowski & Minor, 1997)' _exptl_special_details ; The program Denzo-SMN (Otwinowski & Minor, 1997) uses a scaling algorithm (Fox & Holmes, 1966) which effectively corrects for absorption effects. High redundancy data were used in the scaling program hence the 'multi-scan' code word was used. No transmission coefficients are available from the program (only scale factors for each frame). The scale factors in the experimental table are calculated from the 'size' command in the SHELXL-97 input file. ; _diffrn_ambient_temperature 150(1) _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 'Nonius KappaCCD Diffractometer' _diffrn_measurement_method 'Phi and Omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6591 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0625 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6591 _reflns_number_gt 5067 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'WinGx, Ortep3' _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 Rfactors 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^)+(0.0485P)^2^+11.9366P] 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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0074(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(3) _refine_ls_number_reflns 6591 _refine_ls_number_parameters 400 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1016 _refine_ls_R_factor_gt 0.0654 _refine_ls_wR_factor_ref 0.1667 _refine_ls_wR_factor_gt 0.1377 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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 Ni1 Ni 0.42906(7) 0.41727(7) 0.11460(2) 0.0298(2) Uani 1 1 d . . . Cl1 Cl -0.04482(19) 0.3987(2) 0.02928(8) 0.0621(5) Uani 1 1 d . . . Cl2 Cl 0.10110(14) 0.91762(15) 0.16304(5) 0.0367(3) Uani 1 1 d . . . O1 O 0.2745(5) 0.3128(4) 0.08521(16) 0.0404(11) Uani 1 1 d . . . H1A H 0.2388 0.3325 0.0592 0.049 Uiso 1 1 calc R . . O2 O 0.0875(6) 0.3642(8) 0.01367(19) 0.098(3) Uani 1 1 d . . . O3 O -0.0525(7) 0.3743(9) 0.0806(2) 0.102(3) Uani 1 1 d . . . O4 O -0.1420(8) 0.3233(8) 0.0084(3) 0.109(3) Uani 1 1 d . . . O5 O -0.0644(16) 0.5176(8) 0.0239(6) 0.220(7) Uani 1 1 d . . . O6 O 0.0645(5) 0.7895(4) 0.16453(19) 0.0509(12) Uani 1 1 d . . . O7 O 0.1144(6) 0.9645(5) 0.21037(17) 0.0599(15) Uani 1 1 d . . . O8 O -0.0026(5) 0.9856(5) 0.13873(19) 0.0571(14) Uani 1 1 d . . . O9 O 0.2269(5) 0.9299(5) 0.1375(2) 0.0587(14) Uani 1 1 d . . . N1 N 0.5751(5) 0.5427(4) 0.13746(16) 0.0310(11) Uani 1 1 d . . . N2 N 0.2977(5) 0.5648(5) 0.12752(16) 0.0313(11) Uani 1 1 d . . . N3 N 0.4493(6) 0.5057(5) 0.04901(17) 0.0355(12) Uani 1 1 d . . . N4 N 0.3395(5) 0.3614(4) 0.18168(16) 0.0296(11) Uani 1 1 d . . . N5 N 0.5651(6) 0.2789(5) 0.10112(17) 0.0364(11) Uani 1 1 d . . . C1 C 0.7090(6) 0.5375(6) 0.1287(2) 0.0340(14) Uani 1 1 d . . . H1 H 0.7488 0.4598 0.1223 0.041 Uiso 1 1 calc R . . C2 C 0.7906(7) 0.6402(6) 0.1285(2) 0.0396(15) Uani 1 1 d . . . H2 H 0.8850 0.6330 0.1229 0.048 Uiso 1 1 calc R . . C3 C 0.7332(7) 0.7534(6) 0.1366(2) 0.0412(16) Uani 1 1 d . . . H3 H 0.7869 0.8257 0.1359 0.049 Uiso 1 1 calc R . . C4 C 0.5949(7) 0.7603(6) 0.1458(2) 0.0380(14) Uani 1 1 d . . . H4 H 0.5530 0.8375 0.1513 0.046 Uiso 1 1 calc R . . C5 C 0.5203(6) 0.6542(6) 0.1468(2) 0.0314(13) Uani 1 1 d . . . C6 C 0.3727(6) 0.6500(6) 0.1595(2) 0.0323(13) Uani 1 1 d . . . H6A H 0.3625 0.6224 0.1929 0.039 Uiso 1 1 calc R . . H6B H 0.3337 0.7334 0.1569 0.039 Uiso 1 1 calc R . . C7 C 0.2622(7) 0.6231(6) 0.0815(2) 0.0396(15) Uani 1 1 d . . . H7A H 0.2463 0.7119 0.0867 0.047 Uiso 1 1 calc R . . H7B H 0.1771 0.5866 0.0695 0.047 Uiso 1 1 calc R . . C8 C 0.3724(6) 0.6067(6) 0.0446(2) 0.0347(14) Uani 1 1 d . . . C9 C 0.3872(7) 0.6877(6) 0.0069(2) 0.0425(16) Uani 1 1 d . . . H9 H 0.3322 0.7591 0.0047 0.051 Uiso 1 1 calc R . . C10 C 0.4829(8) 0.6629(7) -0.0271(3) 0.0530(19) Uani 1 1 d . . . H10 H 0.4944 0.7170 -0.0533 0.064 Uiso 1 1 calc R . . C11 C 0.5622(8) 0.5596(6) -0.0233(2) 0.0481(17) Uani 1 1 d . . . H11 H 0.6283 0.5410 -0.0467 0.058 Uiso 1 1 calc R . . C12 C 0.5434(8) 0.4831(6) 0.0157(2) 0.0428(16) Uani 1 1 d . . . H12 H 0.5990 0.4124 0.0189 0.051 Uiso 1 1 calc R . . C13 C 0.1770(6) 0.5143(6) 0.1520(2) 0.0349(14) Uani 1 1 d . . . H13A H 0.1117 0.4843 0.1280 0.042 Uiso 1 1 calc R . . H13B H 0.1326 0.5803 0.1705 0.042 Uiso 1 1 calc R . . C14 C 0.2149(6) 0.4103(6) 0.18492(19) 0.0312(12) Uani 1 1 d . . . C15 C 0.1178(7) 0.3657(6) 0.2158(2) 0.0382(15) Uani 1 1 d . . . H15 H 0.0328 0.4058 0.2186 0.046 Uiso 1 1 calc R . . C16 C 0.1454(7) 0.2631(6) 0.2424(2) 0.0404(15) Uani 1 1 d . . . H16 H 0.0784 0.2280 0.2624 0.048 Uiso 1 1 calc R . . C17 C 0.2728(7) 0.2122(6) 0.2393(2) 0.0387(15) Uani 1 1 d . . . H17 H 0.2939 0.1411 0.2574 0.046 Uiso 1 1 calc R . . C18 C 0.3697(6) 0.2633(5) 0.2102(2) 0.0287(13) Uani 1 1 d . . . C19 C 0.5103(6) 0.2174(6) 0.2104(2) 0.0298(12) Uani 1 1 d . . . C20 C 0.6176(6) 0.2968(6) 0.2156(2) 0.0341(14) Uani 1 1 d . . . H20 H 0.6014 0.3825 0.2181 0.041 Uiso 1 1 calc R . . C21 C 0.7493(7) 0.2529(6) 0.2173(2) 0.0399(15) Uani 1 1 d . . . H21 H 0.8226 0.3088 0.2203 0.048 Uiso 1 1 calc R . . C22 C 0.7742(7) 0.1274(6) 0.2144(2) 0.0414(16) Uani 1 1 d . . . H22 H 0.8641 0.0968 0.2156 0.050 Uiso 1 1 calc R . . C23 C 0.6653(7) 0.0474(6) 0.2098(2) 0.0439(17) Uani 1 1 d . . . H23 H 0.6815 -0.0385 0.2082 0.053 Uiso 1 1 calc R . . C24 C 0.5344(6) 0.0903(6) 0.20746(19) 0.0340(12) Uani 1 1 d . . . H24 H 0.4612 0.0347 0.2039 0.041 Uiso 1 1 calc R . . C25 C 0.6423(7) 0.2056(6) 0.0922(2) 0.0389(15) Uani 1 1 d . . . C26 C 0.7391(8) 0.1103(7) 0.0813(3) 0.054(2) Uani 1 1 d . . . H26A H 0.7958 0.0947 0.1092 0.080 Uiso 1 1 calc R . . H26B H 0.7962 0.1366 0.0547 0.080 Uiso 1 1 calc R . . H26C H 0.6910 0.0349 0.0726 0.080 Uiso 1 1 calc R . . C27 C 0.2353(9) 0.1905(6) 0.0975(3) 0.052(2) Uani 1 1 d . . . H27A H 0.2898 0.1317 0.0793 0.077 Uiso 1 1 calc R . . H27B H 0.1394 0.1786 0.0899 0.077 Uiso 1 1 calc R . . H27C H 0.2498 0.1772 0.1316 0.077 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 Ni1 0.0293(4) 0.0279(4) 0.0323(3) -0.0017(3) 0.0006(3) 0.0012(3) Cl1 0.0391(10) 0.0657(13) 0.0814(13) -0.0153(11) -0.0102(9) 0.0037(9) Cl2 0.0342(8) 0.0333(7) 0.0427(7) 0.0042(7) 0.0029(6) 0.0024(7) O1 0.047(3) 0.034(2) 0.040(2) 0.0010(19) -0.008(2) -0.002(2) O2 0.050(4) 0.195(8) 0.049(3) 0.005(4) 0.005(3) 0.041(5) O3 0.068(4) 0.184(8) 0.054(3) -0.042(4) -0.002(3) 0.015(5) O4 0.095(6) 0.150(8) 0.082(5) -0.009(5) -0.024(4) -0.058(5) O5 0.208(13) 0.060(5) 0.39(2) 0.072(9) 0.019(15) 0.024(8) O6 0.039(3) 0.027(2) 0.087(3) 0.001(2) 0.011(3) -0.009(2) O7 0.075(4) 0.059(3) 0.046(3) -0.008(2) -0.007(3) -0.011(3) O8 0.051(3) 0.057(3) 0.063(3) 0.013(3) -0.002(3) 0.024(3) O9 0.042(3) 0.045(3) 0.089(4) 0.018(3) 0.031(3) 0.007(3) N1 0.028(3) 0.032(3) 0.032(2) -0.0034(19) 0.000(2) 0.002(2) N2 0.029(2) 0.029(3) 0.036(2) 0.001(2) -0.002(2) -0.005(2) N3 0.040(3) 0.031(3) 0.036(2) -0.002(2) 0.000(2) 0.005(2) N4 0.026(3) 0.031(3) 0.032(2) -0.002(2) -0.001(2) -0.003(2) N5 0.039(3) 0.033(3) 0.037(3) 0.000(2) 0.004(3) 0.004(3) C1 0.030(3) 0.035(3) 0.037(3) 0.002(3) 0.001(3) 0.006(3) C2 0.032(3) 0.046(4) 0.041(3) -0.001(3) 0.002(3) 0.000(3) C3 0.036(4) 0.032(3) 0.056(4) 0.000(3) 0.005(3) -0.008(3) C4 0.038(4) 0.031(3) 0.045(3) -0.004(3) 0.004(3) -0.002(3) C5 0.027(3) 0.034(3) 0.033(3) -0.002(3) 0.002(2) 0.000(3) C6 0.029(3) 0.032(3) 0.036(3) -0.005(3) 0.000(3) 0.002(3) C7 0.032(3) 0.045(4) 0.042(3) 0.003(3) 0.000(3) 0.004(3) C8 0.031(3) 0.034(4) 0.039(3) 0.000(3) -0.008(3) -0.001(3) C9 0.044(4) 0.035(3) 0.048(4) 0.011(3) -0.003(3) 0.008(3) C10 0.068(5) 0.044(4) 0.047(4) 0.006(3) 0.005(4) -0.001(4) C11 0.062(5) 0.045(4) 0.037(3) 0.004(3) 0.005(3) 0.011(4) C12 0.058(5) 0.034(3) 0.036(3) 0.001(3) 0.004(3) 0.004(3) C13 0.030(3) 0.031(3) 0.043(3) -0.001(3) 0.001(3) 0.002(3) C14 0.027(3) 0.033(3) 0.033(3) -0.007(3) -0.005(2) -0.003(3) C15 0.029(3) 0.038(3) 0.047(3) 0.000(3) 0.005(3) 0.003(3) C16 0.039(4) 0.038(4) 0.044(4) 0.001(3) 0.009(3) -0.005(3) C17 0.034(3) 0.042(4) 0.040(3) 0.000(3) 0.005(3) -0.001(3) C18 0.029(3) 0.029(3) 0.028(3) -0.006(2) 0.004(2) -0.001(2) C19 0.026(3) 0.032(3) 0.031(3) -0.002(3) -0.004(2) 0.002(2) C20 0.027(3) 0.032(3) 0.043(3) -0.003(3) 0.001(3) 0.001(3) C21 0.028(3) 0.045(4) 0.047(4) 0.002(3) 0.001(3) -0.001(3) C22 0.042(4) 0.045(4) 0.037(3) -0.003(3) -0.003(3) 0.010(3) C23 0.054(4) 0.036(4) 0.042(3) -0.004(3) -0.008(3) 0.014(3) C24 0.036(3) 0.030(3) 0.036(3) -0.002(3) -0.005(2) 0.005(3) C25 0.038(4) 0.042(4) 0.037(3) 0.005(3) -0.005(3) 0.007(3) C26 0.057(5) 0.052(5) 0.052(4) -0.004(3) -0.001(4) 0.021(4) C27 0.071(5) 0.038(4) 0.046(4) -0.001(3) 0.000(4) -0.026(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 Ni1 N5 2.055(5) . ? Ni1 O1 2.077(5) . ? Ni1 N1 2.089(5) . ? Ni1 N3 2.090(5) . ? Ni1 N2 2.097(5) . ? Ni1 N4 2.170(5) . ? Cl1 O5 1.318(9) . ? Cl1 O4 1.393(7) . ? Cl1 O2 1.430(6) . ? Cl1 O3 1.470(7) . ? Cl2 O7 1.432(5) . ? Cl2 O8 1.438(5) . ? Cl2 O6 1.442(4) . ? Cl2 O9 1.442(5) . ? O1 C27 1.430(8) . ? O1 H1A 0.8400 . ? N1 C1 1.348(8) . ? N1 C5 1.355(8) . ? N2 C7 1.483(7) . ? N2 C13 1.483(8) . ? N2 C6 1.489(7) . ? N3 C12 1.343(8) . ? N3 C8 1.343(8) . ? N4 C14 1.345(7) . ? N4 C18 1.368(8) . ? N5 C25 1.133(8) . ? C1 C2 1.380(9) . ? C1 H1 0.9500 . ? C2 C3 1.376(9) . ? C2 H2 0.9500 . ? C3 C4 1.393(9) . ? C3 H3 0.9500 . ? C4 C5 1.372(9) . ? C4 H4 0.9500 . ? C5 C6 1.503(8) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.516(9) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.386(9) . ? C9 C10 1.373(10) . ? C9 H9 0.9500 . ? C10 C11 1.376(10) . ? C10 H10 0.9500 . ? C11 C12 1.389(9) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.511(9) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.384(8) . ? C15 C16 1.371(9) . ? C15 H15 0.9500 . ? C16 C17 1.380(9) . ? C16 H16 0.9500 . ? C17 C18 1.378(9) . ? C17 H17 0.9500 . ? C18 C19 1.478(8) . ? C19 C20 1.377(8) . ? C19 C24 1.406(9) . ? C20 C21 1.388(9) . ? C20 H20 0.9500 . ? C21 C22 1.391(10) . ? C21 H21 0.9500 . ? C22 C23 1.392(10) . ? C22 H22 0.9500 . ? C23 C24 1.377(9) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.445(10) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Ni1 O1 90.4(2) . . ? N5 Ni1 N1 94.8(2) . . ? O1 Ni1 N1 171.61(18) . . ? N5 Ni1 N3 96.43(19) . . ? O1 Ni1 N3 88.37(19) . . ? N1 Ni1 N3 84.5(2) . . ? N5 Ni1 N2 177.2(2) . . ? O1 Ni1 N2 91.86(18) . . ? N1 Ni1 N2 82.77(18) . . ? N3 Ni1 N2 81.92(19) . . ? N5 Ni1 N4 102.82(19) . . ? O1 Ni1 N4 83.81(18) . . ? N1 Ni1 N4 101.40(18) . . ? N3 Ni1 N4 159.22(19) . . ? N2 Ni1 N4 79.13(19) . . ? O5 Cl1 O4 115.4(9) . . ? O5 Cl1 O2 110.9(8) . . ? O4 Cl1 O2 110.3(5) . . ? O5 Cl1 O3 106.5(9) . . ? O4 Cl1 O3 105.8(5) . . ? O2 Cl1 O3 107.5(4) . . ? O7 Cl2 O8 108.9(3) . . ? O7 Cl2 O6 110.0(3) . . ? O8 Cl2 O6 109.5(3) . . ? O7 Cl2 O9 110.5(4) . . ? O8 Cl2 O9 109.3(3) . . ? O6 Cl2 O9 108.7(3) . . ? C27 O1 Ni1 127.9(4) . . ? C27 O1 H1A 109.5 . . ? Ni1 O1 H1A 121.1 . . ? C1 N1 C5 117.8(5) . . ? C1 N1 Ni1 126.5(4) . . ? C5 N1 Ni1 111.6(4) . . ? C7 N2 C13 111.8(5) . . ? C7 N2 C6 112.2(5) . . ? C13 N2 C6 110.6(5) . . ? C7 N2 Ni1 108.9(4) . . ? C13 N2 Ni1 107.2(4) . . ? C6 N2 Ni1 105.9(3) . . ? C12 N3 C8 118.5(5) . . ? C12 N3 Ni1 126.7(4) . . ? C8 N3 Ni1 113.9(4) . . ? C14 N4 C18 118.0(5) . . ? C14 N4 Ni1 108.8(4) . . ? C18 N4 Ni1 129.7(4) . . ? C25 N5 Ni1 177.1(5) . . ? N1 C1 C2 122.7(6) . . ? N1 C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? C3 C2 C1 119.0(6) . . ? C3 C2 H2 120.5 . . ? C1 C2 H2 120.5 . . ? C2 C3 C4 118.9(6) . . ? C2 C3 H3 120.5 . . ? C4 C3 H3 120.5 . . ? C5 C4 C3 119.1(6) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? N1 C5 C4 122.3(5) . . ? N1 C5 C6 114.0(5) . . ? C4 C5 C6 123.6(6) . . ? N2 C6 C5 111.0(5) . . ? N2 C6 H6A 109.4 . . ? C5 C6 H6A 109.4 . . ? N2 C6 H6B 109.4 . . ? C5 C6 H6B 109.4 . . ? H6A C6 H6B 108.0 . . ? N2 C7 C8 112.1(5) . . ? N2 C7 H7A 109.2 . . ? C8 C7 H7A 109.2 . . ? N2 C7 H7B 109.2 . . ? C8 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? N3 C8 C9 122.2(6) . . ? N3 C8 C7 116.1(5) . . ? C9 C8 C7 121.6(6) . . ? C10 C9 C8 118.7(6) . . ? C10 C9 H9 120.7 . . ? C8 C9 H9 120.7 . . ? C9 C10 C11 119.9(7) . . ? C9 C10 H10 120.0 . . ? C11 C10 H10 120.0 . . ? C10 C11 C12 118.4(7) . . ? C10 C11 H11 120.8 . . ? C12 C11 H11 120.8 . . ? N3 C12 C11 122.2(6) . . ? N3 C12 H12 118.9 . . ? C11 C12 H12 118.9 . . ? N2 C13 C14 111.2(5) . . ? N2 C13 H13A 109.4 . . ? C14 C13 H13A 109.4 . . ? N2 C13 H13B 109.4 . . ? C14 C13 H13B 109.4 . . ? H13A C13 H13B 108.0 . . ? N4 C14 C15 122.7(6) . . ? N4 C14 C13 118.8(5) . . ? C15 C14 C13 118.4(5) . . ? C16 C15 C14 119.3(6) . . ? C16 C15 H15 120.3 . . ? C14 C15 H15 120.3 . . ? C15 C16 C17 118.4(6) . . ? C15 C16 H16 120.8 . . ? C17 C16 H16 120.8 . . ? C18 C17 C16 120.7(6) . . ? C18 C17 H17 119.7 . . ? C16 C17 H17 119.7 . . ? N4 C18 C17 120.8(6) . . ? N4 C18 C19 118.2(5) . . ? C17 C18 C19 120.9(6) . . ? C20 C19 C24 119.6(6) . . ? C20 C19 C18 120.9(5) . . ? C24 C19 C18 119.5(5) . . ? C19 C20 C21 120.7(6) . . ? C19 C20 H20 119.7 . . ? C21 C20 H20 119.7 . . ? C20 C21 C22 120.2(7) . . ? C20 C21 H21 119.9 . . ? C22 C21 H21 119.9 . . ? C21 C22 C23 118.9(6) . . ? C21 C22 H22 120.5 . . ? C23 C22 H22 120.5 . . ? C24 C23 C22 121.3(6) . . ? C24 C23 H23 119.4 . . ? C22 C23 H23 119.4 . . ? C23 C24 C19 119.4(6) . . ? C23 C24 H24 120.3 . . ? C19 C24 H24 120.3 . . ? N5 C25 C26 178.8(8) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O1 C27 H27A 109.5 . . ? O1 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? O1 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N5 Ni1 O1 C27 53.9(6) . . . . ? N1 Ni1 O1 C27 -177.8(12) . . . . ? N3 Ni1 O1 C27 150.3(6) . . . . ? N2 Ni1 O1 C27 -127.9(5) . . . . ? N4 Ni1 O1 C27 -49.0(5) . . . . ? N5 Ni1 N1 C1 19.0(5) . . . . ? O1 Ni1 N1 C1 -109.1(13) . . . . ? N3 Ni1 N1 C1 -77.1(5) . . . . ? N2 Ni1 N1 C1 -159.6(5) . . . . ? N4 Ni1 N1 C1 123.1(5) . . . . ? N5 Ni1 N1 C5 175.6(4) . . . . ? O1 Ni1 N1 C5 47.5(15) . . . . ? N3 Ni1 N1 C5 79.6(4) . . . . ? N2 Ni1 N1 C5 -3.0(4) . . . . ? N4 Ni1 N1 C5 -80.3(4) . . . . ? N5 Ni1 N2 C7 71(4) . . . . ? O1 Ni1 N2 C7 -71.7(4) . . . . ? N1 Ni1 N2 C7 101.9(4) . . . . ? N3 Ni1 N2 C7 16.4(4) . . . . ? N4 Ni1 N2 C7 -155.0(4) . . . . ? N5 Ni1 N2 C13 -168(4) . . . . ? O1 Ni1 N2 C13 49.5(4) . . . . ? N1 Ni1 N2 C13 -137.0(4) . . . . ? N3 Ni1 N2 C13 137.6(4) . . . . ? N4 Ni1 N2 C13 -33.9(4) . . . . ? N5 Ni1 N2 C6 -50(4) . . . . ? O1 Ni1 N2 C6 167.5(4) . . . . ? N1 Ni1 N2 C6 -18.9(4) . . . . ? N3 Ni1 N2 C6 -104.4(4) . . . . ? N4 Ni1 N2 C6 84.2(4) . . . . ? N5 Ni1 N3 C12 -10.5(6) . . . . ? O1 Ni1 N3 C12 -100.7(6) . . . . ? N1 Ni1 N3 C12 83.7(6) . . . . ? N2 Ni1 N3 C12 167.1(6) . . . . ? N4 Ni1 N3 C12 -168.5(5) . . . . ? N5 Ni1 N3 C8 -179.4(4) . . . . ? O1 Ni1 N3 C8 90.4(4) . . . . ? N1 Ni1 N3 C8 -85.2(4) . . . . ? N2 Ni1 N3 C8 -1.7(4) . . . . ? N4 Ni1 N3 C8 22.6(8) . . . . ? N5 Ni1 N4 C14 -154.1(4) . . . . ? O1 Ni1 N4 C14 -65.1(4) . . . . ? N1 Ni1 N4 C14 108.2(4) . . . . ? N3 Ni1 N4 C14 3.4(8) . . . . ? N2 Ni1 N4 C14 28.0(4) . . . . ? N5 Ni1 N4 C18 3.6(5) . . . . ? O1 Ni1 N4 C18 92.6(5) . . . . ? N1 Ni1 N4 C18 -94.1(5) . . . . ? N3 Ni1 N4 C18 161.1(5) . . . . ? N2 Ni1 N4 C18 -174.3(5) . . . . ? O1 Ni1 N5 C25 107(11) . . . . ? N1 Ni1 N5 C25 -66(11) . . . . ? N3 Ni1 N5 C25 19(11) . . . . ? N2 Ni1 N5 C25 -36(14) . . . . ? N4 Ni1 N5 C25 -169(11) . . . . ? C5 N1 C1 C2 -0.5(9) . . . . ? Ni1 N1 C1 C2 154.8(5) . . . . ? N1 C1 C2 C3 -1.4(10) . . . . ? C1 C2 C3 C4 1.5(10) . . . . ? C2 C3 C4 C5 0.4(10) . . . . ? C1 N1 C5 C4 2.5(9) . . . . ? Ni1 N1 C5 C4 -156.4(5) . . . . ? C1 N1 C5 C6 -176.0(5) . . . . ? Ni1 N1 C5 C6 25.2(6) . . . . ? C3 C4 C5 N1 -2.4(10) . . . . ? C3 C4 C5 C6 175.9(6) . . . . ? C7 N2 C6 C5 -81.7(6) . . . . ? C13 N2 C6 C5 152.7(5) . . . . ? Ni1 N2 C6 C5 37.0(6) . . . . ? N1 C5 C6 N2 -43.1(7) . . . . ? C4 C5 C6 N2 138.4(6) . . . . ? C13 N2 C7 C8 -146.0(5) . . . . ? C6 N2 C7 C8 89.1(6) . . . . ? Ni1 N2 C7 C8 -27.7(6) . . . . ? C12 N3 C8 C9 0.0(9) . . . . ? Ni1 N3 C8 C9 169.8(5) . . . . ? C12 N3 C8 C7 176.3(6) . . . . ? Ni1 N3 C8 C7 -13.8(7) . . . . ? N2 C7 C8 N3 28.4(8) . . . . ? N2 C7 C8 C9 -155.2(6) . . . . ? N3 C8 C9 C10 0.6(10) . . . . ? C7 C8 C9 C10 -175.5(6) . . . . ? C8 C9 C10 C11 -0.4(11) . . . . ? C9 C10 C11 C12 -0.5(12) . . . . ? C8 N3 C12 C11 -0.9(10) . . . . ? Ni1 N3 C12 C11 -169.3(5) . . . . ? C10 C11 C12 N3 1.2(11) . . . . ? C7 N2 C13 C14 154.4(5) . . . . ? C6 N2 C13 C14 -79.8(6) . . . . ? Ni1 N2 C13 C14 35.1(6) . . . . ? C18 N4 C14 C15 0.3(8) . . . . ? Ni1 N4 C14 C15 161.0(5) . . . . ? C18 N4 C14 C13 -176.8(5) . . . . ? Ni1 N4 C14 C13 -16.1(6) . . . . ? N2 C13 C14 N4 -12.6(8) . . . . ? N2 C13 C14 C15 170.2(5) . . . . ? N4 C14 C15 C16 -4.0(9) . . . . ? C13 C14 C15 C16 173.1(6) . . . . ? C14 C15 C16 C17 3.8(10) . . . . ? C15 C16 C17 C18 0.0(10) . . . . ? C14 N4 C18 C17 3.5(8) . . . . ? Ni1 N4 C18 C17 -152.5(5) . . . . ? C14 N4 C18 C19 -173.8(5) . . . . ? Ni1 N4 C18 C19 30.2(7) . . . . ? C16 C17 C18 N4 -3.7(10) . . . . ? C16 C17 C18 C19 173.5(6) . . . . ? N4 C18 C19 C20 48.4(8) . . . . ? C17 C18 C19 C20 -129.0(6) . . . . ? N4 C18 C19 C24 -134.5(6) . . . . ? C17 C18 C19 C24 48.2(8) . . . . ? C24 C19 C20 C21 1.0(9) . . . . ? C18 C19 C20 C21 178.1(6) . . . . ? C19 C20 C21 C22 -1.1(10) . . . . ? C20 C21 C22 C23 0.2(10) . . . . ? C21 C22 C23 C24 0.7(10) . . . . ? C22 C23 C24 C19 -0.9(10) . . . . ? C20 C19 C24 C23 0.0(9) . . . . ? C18 C19 C24 C23 -177.2(6) . . . . ? Ni1 N5 C25 C26 -162(31) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1A O2 0.84 2.00 2.789(7) 156.4 . _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.699 _refine_diff_density_min -0.976 _refine_diff_density_rms 0.107 #===END data_usu162 #(Compound 8.0.5CH3CN) _database_code_depnum_ccdc_archive 'CCDC 821108' #TrackingRef '- Revised_cifs.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C45 H37 Co N4 O2,Cl O4,0.5(C2 H3 N)' _chemical_formula_sum 'C46 H38.50 Cl Co N4.50 O6' _chemical_formula_weight 844.69 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 Tetragonal _symmetry_space_group_name_H-M I-4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 34.4730(5) _cell_length_b 34.4730(5) _cell_length_c 13.5221(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 16069.5(5) _cell_formula_units_Z 16 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 27554 _cell_measurement_theta_min 1.018 _cell_measurement_theta_max 27.485 _exptl_crystal_description plate _exptl_crystal_colour red-brown _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.397 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7008 _exptl_absorpt_coefficient_mu 0.550 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8308 _exptl_absorpt_correction_T_max 0.9319 _exptl_absorpt_process_details 'DENZO-SMN (Otwinowski & Minor, 1997)' _exptl_special_details ; The program Denzo-SMN (Otwinowski & Minor, 1997) uses a scaling algorithm (Fox & Holmes, 1966) which effectively corrects for absorption effects. High redundancy data were used in the scaling program hence the 'multi-scan' code word was used. No transmission coefficients are available from the program (only scale factors for each frame). The scale factors in the experimental table are calculated from the 'size' command in the SHELXL-97 input file. ; _diffrn_ambient_temperature 150(1) _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 'Nonius KappaCCD Diffractometer' _diffrn_measurement_method 'Phi and Omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15365 _diffrn_reflns_av_R_equivalents 0.0395 _diffrn_reflns_av_sigmaI/netI 0.0963 _diffrn_reflns_limit_h_min -44 _diffrn_reflns_limit_h_max 44 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 27.48 _reflns_number_total 15360 _reflns_number_gt 10548 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NOnius COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'WinGX, Ortep3' _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 Rfactors 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^)+(0.0438P)^2^+47.0229P] 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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00084(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.371(16) _refine_ls_number_reflns 15360 _refine_ls_number_parameters 1060 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1206 _refine_ls_R_factor_gt 0.0638 _refine_ls_wR_factor_ref 0.1558 _refine_ls_wR_factor_gt 0.1236 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _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 0.35571(2) 0.08419(2) 0.39190(5) 0.02878(19) Uani 1 1 d . . . Co2 Co 0.07156(2) 0.15555(2) 0.59451(6) 0.03035(19) Uani 1 1 d . . . Cl1 Cl 0.24001(5) 0.06582(6) 0.93202(11) 0.0502(4) Uani 1 1 d . . . Cl2 Cl 0.5000 0.0000 0.7500 0.0503(8) Uani 1 4 d S . . Cl3 Cl 0.5000 0.0000 0.2500 0.0384(7) Uani 1 4 d S . . Cl4 Cl 0.0000 0.0000 0.0000 0.0769(13) Uani 1 4 d S . . Cl5 Cl 0.0000 0.0000 0.5000 0.0316(6) Uani 1 4 d S . . O1 O 0.38271(11) 0.08886(11) 0.2591(3) 0.0281(9) Uani 1 1 d . . . O1A O 0.08283(11) 0.12608(11) 0.4706(3) 0.0306(9) Uani 1 1 d . . . O2 O 0.31534(11) 0.12165(11) 0.3480(3) 0.0297(9) Uani 1 1 d . . . O2A O 0.11014(11) 0.19571(12) 0.5581(3) 0.0330(9) Uani 1 1 d . . . O3 O 0.20630(16) 0.0652(2) 0.9924(4) 0.100(3) Uani 1 1 d . A . O4 O 0.2311(2) 0.0562(3) 0.8358(4) 0.135(4) Uani 1 1 d . A . O5 O 0.2695(4) 0.0958(4) 0.9461(10) 0.090(4) Uiso 0.50 1 d P A 1 O6 O 0.2617(4) 0.0313(4) 0.9626(10) 0.090(4) Uiso 0.50 1 d P A 1 O5A O 0.2460(4) 0.1068(4) 0.9083(10) 0.090(4) Uiso 0.50 1 d P A 2 O6A O 0.2732(4) 0.0575(4) 0.9875(9) 0.077(3) Uiso 0.50 1 d P A 2 O7 O 0.4679(2) 0.01059(18) 0.6932(5) 0.114(3) Uani 1 1 d . . . O8 O 0.49079(16) 0.03311(17) 0.3088(4) 0.0768(19) Uani 1 1 d . . . O9 O 0.02803(12) -0.01890(14) 0.5613(3) 0.0487(12) Uani 1 1 d . . . O13 O 0.0460(3) -0.0029(4) 0.0135(11) 0.086(4) Uani 0.50 1 d P . . O13A O 0.0000 0.0000 0.1048(17) 0.100(6) Uiso 0.50 2 d SP . 2 O13B O -0.0229(8) 0.0092(7) 0.0706(16) 0.063(6) Uiso 0.25 1 d P . 2 N1 N 0.33156(14) 0.07753(14) 0.5362(3) 0.0303(11) Uani 1 1 d . . . N1A N 0.05875(14) 0.18037(14) 0.7327(3) 0.0308(11) Uani 1 1 d . . . N2 N 0.39192(14) 0.03893(14) 0.4475(3) 0.0308(11) Uani 1 1 d . . . N2A N 0.02366(14) 0.12032(13) 0.6342(3) 0.0306(11) Uani 1 1 d . . . N3 N 0.33212(14) 0.02852(13) 0.3216(3) 0.0320(11) Uani 1 1 d . . . N3A N 0.01893(13) 0.18183(14) 0.5079(4) 0.0329(11) Uani 1 1 d . . . N4 N 0.39940(13) 0.11989(14) 0.4806(3) 0.0300(11) Uani 1 1 d . . . N4A N 0.10182(15) 0.11193(14) 0.6940(4) 0.0340(12) Uani 1 1 d . . . N5 N 0.0789(3) 0.2307(3) 0.1659(6) 0.098(3) Uani 1 1 d . . . C1 C 0.30710(17) 0.10236(19) 0.5817(5) 0.0396(15) Uani 1 1 d . . . H1 H 0.2960 0.1230 0.5446 0.048 Uiso 1 1 calc R . . C1A C 0.08104(19) 0.20634(18) 0.7820(4) 0.0367(14) Uani 1 1 d . . . H1A H 0.1044 0.2153 0.7525 0.044 Uiso 1 1 calc R . . C2 C 0.2976(2) 0.0987(2) 0.6815(5) 0.0471(17) Uani 1 1 d . . . H2 H 0.2801 0.1163 0.7124 0.057 Uiso 1 1 calc R . . C2A C 0.07066(19) 0.22014(19) 0.8742(4) 0.0421(15) Uani 1 1 d . . . H2A H 0.0866 0.2385 0.9076 0.050 Uiso 1 1 calc R . . C3 C 0.31461(19) 0.0684(2) 0.7344(5) 0.0474(17) Uani 1 1 d . . . H3 H 0.3090 0.0651 0.8027 0.057 Uiso 1 1 calc R . . C3A C 0.03689(19) 0.20695(19) 0.9171(4) 0.0423(15) Uani 1 1 d . . . H3A H 0.0292 0.2163 0.9803 0.051 Uiso 1 1 calc R . . C4 C 0.33938(19) 0.0434(2) 0.6877(5) 0.0432(16) Uani 1 1 d . . . H4 H 0.3512 0.0229 0.7233 0.052 Uiso 1 1 calc R . . C4A C 0.01413(19) 0.18002(19) 0.8681(4) 0.0391(15) Uani 1 1 d . . . H4A H -0.0092 0.1707 0.8969 0.047 Uiso 1 1 calc R . . C5 C 0.34709(17) 0.04841(17) 0.5882(4) 0.0344(13) Uani 1 1 d . . . C5A C 0.02629(17) 0.16685(17) 0.7752(4) 0.0321(13) Uani 1 1 d . . . C6 C 0.37111(19) 0.02001(18) 0.5299(4) 0.0388(15) Uani 1 1 d . . . H6A H 0.3902 0.0075 0.5745 0.047 Uiso 1 1 calc R . . H6B H 0.3540 -0.0005 0.5031 0.047 Uiso 1 1 calc R . . C6A C 0.00173(18) 0.14036(18) 0.7139(4) 0.0367(14) Uani 1 1 d . . . H6A1 H -0.0102 0.1206 0.7576 0.044 Uiso 1 1 calc R . . H6A2 H -0.0195 0.1556 0.6836 0.044 Uiso 1 1 calc R . . C7 C 0.39869(18) 0.01094(18) 0.3665(4) 0.0365(14) Uani 1 1 d . . . H7A H 0.4061 -0.0144 0.3951 0.044 Uiso 1 1 calc R . . H7B H 0.4205 0.0202 0.3252 0.044 Uiso 1 1 calc R . . C7A C -0.00136(18) 0.11520(18) 0.5462(4) 0.0375(15) Uani 1 1 d . . . H7A1 H -0.0273 0.1061 0.5677 0.045 Uiso 1 1 calc R . . H7A2 H 0.0100 0.0949 0.5031 0.045 Uiso 1 1 calc R . . C8 C 0.36356(17) 0.00572(17) 0.3027(4) 0.0329(13) Uani 1 1 d . . . C8A C -0.00589(18) 0.15215(17) 0.4875(4) 0.0337(14) Uani 1 1 d . . . C9 C 0.36472(19) -0.02044(18) 0.2243(4) 0.0389(15) Uani 1 1 d . . . H9 H 0.3863 -0.0371 0.2152 0.047 Uiso 1 1 calc R . . C9A C -0.03335(18) 0.15369(19) 0.4139(5) 0.0416(15) Uani 1 1 d . . . H9A H -0.0503 0.1324 0.4029 0.050 Uiso 1 1 calc R . . C10 C 0.33328(18) -0.02145(19) 0.1597(5) 0.0410(16) Uani 1 1 d . . . H10 H 0.3341 -0.0374 0.1024 0.049 Uiso 1 1 calc R . . C10A C -0.0359(2) 0.1866(2) 0.3560(5) 0.0461(17) Uani 1 1 d . . . H10A H -0.0539 0.1879 0.3029 0.055 Uiso 1 1 calc R . . C11 C 0.30113(19) 0.00076(19) 0.1793(5) 0.0384(14) Uani 1 1 d . . . H11 H 0.2794 0.0000 0.1362 0.046 Uiso 1 1 calc R . . C11A C -0.01180(19) 0.2177(2) 0.3768(4) 0.0421(16) Uani 1 1 d . . . H11A H -0.0132 0.2408 0.3385 0.051 Uiso 1 1 calc R . . C12 C 0.30045(17) 0.02451(17) 0.2629(4) 0.0322(13) Uani 1 1 d . . . C12A C 0.01436(17) 0.21468(18) 0.4539(4) 0.0330(14) Uani 1 1 d . . . C13 C 0.26501(16) 0.04592(16) 0.2917(4) 0.0310(13) Uani 1 1 d . . . C13A C 0.03723(17) 0.24938(17) 0.4852(4) 0.0330(14) Uani 1 1 d . . . C14 C 0.23774(18) 0.05744(17) 0.2214(4) 0.0342(14) Uani 1 1 d . . . H14 H 0.2420 0.0516 0.1536 0.041 Uiso 1 1 calc R . . C14A C 0.04977(18) 0.27660(19) 0.4155(5) 0.0427(15) Uani 1 1 d . . . H14A H 0.0449 0.2723 0.3472 0.051 Uiso 1 1 calc R . . C15 C 0.20457(18) 0.07720(17) 0.2491(5) 0.0373(14) Uani 1 1 d . . . H15 H 0.1862 0.0849 0.2004 0.045 Uiso 1 1 calc R . . C15A C 0.0692(2) 0.30974(19) 0.4456(5) 0.0448(16) Uani 1 1 d . . . H15A H 0.0782 0.3278 0.3977 0.054 Uiso 1 1 calc R . . C16 C 0.19818(17) 0.08568(19) 0.3470(5) 0.0397(15) Uani 1 1 d . . . H16 H 0.1756 0.0997 0.3657 0.048 Uiso 1 1 calc R . . C16A C 0.0755(2) 0.31655(19) 0.5440(5) 0.0454(17) Uani 1 1 d . . . H16A H 0.0884 0.3396 0.5643 0.054 Uiso 1 1 calc R . . C17 C 0.22422(18) 0.07393(18) 0.4182(5) 0.0382(14) Uani 1 1 d . . . H17 H 0.2195 0.0794 0.4860 0.046 Uiso 1 1 calc R . . C17A C 0.06324(17) 0.28992(18) 0.6143(5) 0.0384(14) Uani 1 1 d . . . H17A H 0.0680 0.2945 0.6825 0.046 Uiso 1 1 calc R . . C18 C 0.25722(16) 0.05412(16) 0.3901(4) 0.0334(13) Uani 1 1 d . . . H18 H 0.2750 0.0459 0.4394 0.040 Uiso 1 1 calc R . . C18A C 0.04380(17) 0.25639(17) 0.5840(4) 0.0328(13) Uani 1 1 d . . . H18A H 0.0350 0.2383 0.6321 0.039 Uiso 1 1 calc R . . C19 C 0.42903(17) 0.05604(17) 0.4824(4) 0.0337(13) Uani 1 1 d . . . H19A H 0.4468 0.0592 0.4255 0.040 Uiso 1 1 calc R . . H19B H 0.4414 0.0381 0.5302 0.040 Uiso 1 1 calc R . . C19A C 0.03920(19) 0.08248(18) 0.6673(5) 0.0406(15) Uani 1 1 d . . . H19C H 0.0454 0.0664 0.6087 0.049 Uiso 1 1 calc R . . H19D H 0.0191 0.0687 0.7061 0.049 Uiso 1 1 calc R . . C20 C 0.42286(17) 0.09480(18) 0.5310(4) 0.0328(13) Uani 1 1 d . . . C20A C 0.07504(19) 0.08707(17) 0.7296(4) 0.0376(15) Uani 1 1 d . . . C21 C 0.44199(19) 0.1050(2) 0.6163(5) 0.0441(16) Uani 1 1 d . . . H21 H 0.4585 0.0870 0.6488 0.053 Uiso 1 1 calc R . . C21A C 0.0802(2) 0.0660(2) 0.8160(5) 0.0476(17) Uani 1 1 d . . . H21A H 0.0610 0.0484 0.8390 0.057 Uiso 1 1 calc R . . C22 C 0.4369(2) 0.1421(2) 0.6542(5) 0.0525(19) Uani 1 1 d . . . H22 H 0.4491 0.1495 0.7142 0.063 Uiso 1 1 calc R . . C22A C 0.1147(2) 0.0717(2) 0.8678(5) 0.054(2) Uani 1 1 d . . . H22A H 0.1190 0.0583 0.9282 0.065 Uiso 1 1 calc R . . C23 C 0.4137(2) 0.1680(2) 0.6038(5) 0.0474(16) Uani 1 1 d . . . H23 H 0.4102 0.1936 0.6282 0.057 Uiso 1 1 calc R . . C23A C 0.1423(2) 0.0963(2) 0.8324(5) 0.0457(17) Uani 1 1 d . . . H23A H 0.1660 0.0998 0.8671 0.055 Uiso 1 1 calc R . . C24 C 0.39550(17) 0.15638(17) 0.5170(4) 0.0329(13) Uani 1 1 d . . . C24A C 0.13531(18) 0.11613(18) 0.7447(4) 0.0368(15) Uani 1 1 d . . . C25 C 0.37190(18) 0.18405(17) 0.4577(5) 0.0360(14) Uani 1 1 d . . . C25A C 0.16717(18) 0.14003(18) 0.7004(5) 0.0375(14) Uani 1 1 d . . . C26 C 0.37426(18) 0.18342(18) 0.3555(4) 0.0362(14) Uani 1 1 d . . . H26 H 0.3897 0.1644 0.3234 0.043 Uiso 1 1 calc R . . C26A C 0.17323(18) 0.13970(17) 0.5993(5) 0.0400(14) Uani 1 1 d . . . H26A H 0.1561 0.1258 0.5573 0.048 Uiso 1 1 calc R . . C27 C 0.35372(19) 0.21095(19) 0.2988(5) 0.0444(17) Uani 1 1 d . . . H27 H 0.3552 0.2104 0.2287 0.053 Uiso 1 1 calc R . . C27A C 0.20449(19) 0.15969(19) 0.5594(6) 0.0491(17) Uani 1 1 d . . . H27A H 0.2086 0.1592 0.4900 0.059 Uiso 1 1 calc R . . C28 C 0.3316(2) 0.2386(2) 0.3452(6) 0.056(2) Uani 1 1 d . . . H28 H 0.3176 0.2571 0.3073 0.067 Uiso 1 1 calc R . . C28A C 0.2297(2) 0.1804(2) 0.6190(7) 0.0548(19) Uani 1 1 d . . . H28A H 0.2510 0.1940 0.5910 0.066 Uiso 1 1 calc R . . C29 C 0.3295(2) 0.2392(2) 0.4478(6) 0.055(2) Uani 1 1 d . . . H29 H 0.3145 0.2586 0.4796 0.066 Uiso 1 1 calc R . . C29A C 0.2235(2) 0.1810(2) 0.7193(7) 0.060(2) Uani 1 1 d . . . H29A H 0.2406 0.1953 0.7605 0.072 Uiso 1 1 calc R . . C30 C 0.3491(2) 0.21224(19) 0.5041(5) 0.0466(16) Uani 1 1 d . . . H30 H 0.3470 0.2128 0.5742 0.056 Uiso 1 1 calc R . . C30A C 0.1927(2) 0.1612(2) 0.7615(6) 0.0523(19) Uani 1 1 d . . . H30A H 0.1887 0.1619 0.8310 0.063 Uiso 1 1 calc R . . C31 C 0.36368(17) 0.09619(16) 0.1798(4) 0.0287(13) Uani 1 1 d . . . C31A C 0.09643(16) 0.14131(16) 0.3924(4) 0.0299(12) Uani 1 1 d . . . C32 C 0.38337(16) 0.08379(16) 0.0839(4) 0.0311(13) Uani 1 1 d . . . C32A C 0.09184(17) 0.11822(17) 0.2988(4) 0.0298(13) Uani 1 1 d . . . C33 C 0.41347(16) 0.05721(17) 0.0883(4) 0.0337(13) Uani 1 1 d . . . H33 H 0.4214 0.0472 0.1505 0.040 Uiso 1 1 calc R . . C33A C 0.06330(17) 0.08930(16) 0.2961(4) 0.0304(13) Uani 1 1 d . . . H33A H 0.0485 0.0840 0.3538 0.036 Uiso 1 1 calc R . . C34 C 0.43221(18) 0.04501(19) 0.0022(5) 0.0401(15) Uani 1 1 d . . . H34 H 0.4526 0.0265 0.0057 0.048 Uiso 1 1 calc R . . C34A C 0.05639(18) 0.06843(18) 0.2106(4) 0.0374(15) Uani 1 1 d . . . H34A H 0.0366 0.0492 0.2096 0.045 Uiso 1 1 calc R . . C35 C 0.42080(19) 0.06009(19) -0.0893(5) 0.0455(16) Uani 1 1 d . . . H35 H 0.4335 0.0521 -0.1481 0.055 Uiso 1 1 calc R . . C35A C 0.07813(19) 0.0754(2) 0.1266(5) 0.0437(16) Uani 1 1 d . . . H35A H 0.0732 0.0612 0.0677 0.052 Uiso 1 1 calc R . . C36 C 0.39080(18) 0.0869(2) -0.0936(5) 0.0425(15) Uani 1 1 d . . . H36 H 0.3832 0.0974 -0.1556 0.051 Uiso 1 1 calc R . . C36A C 0.1072(2) 0.1033(2) 0.1289(5) 0.0444(16) Uani 1 1 d . . . H36A H 0.1226 0.1077 0.0717 0.053 Uiso 1 1 calc R . . C37 C 0.37162(18) 0.09844(19) -0.0077(4) 0.0373(14) Uani 1 1 d . . . H37 H 0.3506 0.1162 -0.0114 0.045 Uiso 1 1 calc R . . C37A C 0.11382(19) 0.12456(18) 0.2138(4) 0.0371(14) Uani 1 1 d . . . H37A H 0.1336 0.1438 0.2142 0.045 Uiso 1 1 calc R . . C38 C 0.32781(16) 0.11397(17) 0.1756(4) 0.0298(12) Uani 1 1 d . . . H38A H 0.3167 0.1176 0.1120 0.036 Uiso 1 1 calc R . . C38A C 0.11397(16) 0.17793(16) 0.3885(4) 0.0318(13) Uani 1 1 d . . . H38B H 0.1221 0.1869 0.3254 0.038 Uiso 1 1 calc R . . C39 C 0.30626(16) 0.12728(16) 0.2576(4) 0.0278(12) Uani 1 1 d . . . C39A C 0.12065(17) 0.20258(17) 0.4691(4) 0.0310(13) Uani 1 1 d . . . C40 C 0.27066(17) 0.15088(17) 0.2388(4) 0.0315(13) Uani 1 1 d . . . C40A C 0.14380(17) 0.23891(17) 0.4537(4) 0.0308(13) Uani 1 1 d . . . C41 C 0.25018(17) 0.14959(18) 0.1506(5) 0.0359(14) Uani 1 1 d . . . H41 H 0.2586 0.1328 0.0992 0.043 Uiso 1 1 calc R . . C41A C 0.14486(18) 0.25850(18) 0.3631(5) 0.0386(15) Uani 1 1 d . . . H41A H 0.1304 0.2490 0.3085 0.046 Uiso 1 1 calc R . . C42 C 0.21745(18) 0.17249(19) 0.1361(5) 0.0420(16) Uani 1 1 d . . . H42 H 0.2033 0.1707 0.0760 0.050 Uiso 1 1 calc R . . C42A C 0.1672(2) 0.29210(19) 0.3529(5) 0.0478(17) Uani 1 1 d . . . H42A H 0.1676 0.3057 0.2918 0.057 Uiso 1 1 calc R . . C43 C 0.2055(2) 0.1981(2) 0.2101(5) 0.0486(18) Uani 1 1 d . . . H43 H 0.1836 0.2144 0.2000 0.058 Uiso 1 1 calc R . . C43A C 0.1888(2) 0.3055(2) 0.4321(6) 0.053(2) Uani 1 1 d . . . H43A H 0.2043 0.3281 0.4252 0.064 Uiso 1 1 calc R . . C44 C 0.22577(19) 0.1995(2) 0.2980(5) 0.0469(17) Uani 1 1 d . . . H44 H 0.2176 0.2169 0.3484 0.056 Uiso 1 1 calc R . . C44A C 0.1877(2) 0.2858(2) 0.5217(6) 0.058(2) Uani 1 1 d . . . H44A H 0.2026 0.2951 0.5759 0.070 Uiso 1 1 calc R . . C45 C 0.25782(17) 0.17602(17) 0.3141(5) 0.0360(14) Uani 1 1 d . . . H45 H 0.2711 0.1769 0.3757 0.043 Uiso 1 1 calc R . . C45A C 0.16540(18) 0.25315(19) 0.5328(5) 0.0396(15) Uani 1 1 d . . . H45A H 0.1647 0.2402 0.5948 0.047 Uiso 1 1 calc R . . C46 C 0.0572(3) 0.2054(3) 0.1641(5) 0.062(2) Uani 1 1 d . . . C47 C 0.0283(2) 0.1747(2) 0.1597(6) 0.065(2) Uani 1 1 d . . . H47A H 0.0029 0.1860 0.1439 0.098 Uiso 1 1 calc R . . H47B H 0.0269 0.1616 0.2239 0.098 Uiso 1 1 calc R . . H47C H 0.0355 0.1560 0.1085 0.098 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 0.0303(4) 0.0286(4) 0.0274(4) 0.0013(3) 0.0017(3) 0.0027(3) Co2 0.0305(4) 0.0308(4) 0.0297(4) -0.0054(3) 0.0039(3) -0.0032(3) Cl1 0.0436(10) 0.0735(12) 0.0335(9) 0.0122(8) -0.0058(7) -0.0101(9) Cl2 0.0580(13) 0.0580(13) 0.0349(18) 0.000 0.000 0.000 Cl3 0.0389(10) 0.0389(10) 0.0374(17) 0.000 0.000 0.000 Cl4 0.096(2) 0.096(2) 0.039(2) 0.000 0.000 0.000 Cl5 0.0300(9) 0.0300(9) 0.0348(16) 0.000 0.000 0.000 O1 0.029(2) 0.030(2) 0.026(2) 0.0004(16) -0.0013(17) 0.0024(17) O1A 0.029(2) 0.032(2) 0.031(2) -0.0007(18) 0.0017(17) -0.0020(17) O2 0.032(2) 0.028(2) 0.029(2) 0.0010(16) 0.0009(17) 0.0016(17) O2A 0.030(2) 0.039(2) 0.030(2) -0.0059(18) 0.0037(17) -0.0029(18) O3 0.040(3) 0.220(8) 0.039(3) 0.033(4) 0.008(2) -0.005(4) O4 0.074(5) 0.282(11) 0.048(4) -0.061(5) 0.008(3) -0.044(6) O7 0.157(7) 0.067(5) 0.119(6) -0.015(4) -0.099(5) 0.027(4) O8 0.063(4) 0.079(4) 0.089(4) -0.060(3) 0.033(3) -0.030(3) O9 0.032(2) 0.060(3) 0.054(3) 0.012(2) -0.012(2) 0.008(2) O13 0.050(7) 0.065(8) 0.143(12) -0.032(8) -0.038(8) -0.002(6) N1 0.031(3) 0.035(3) 0.025(3) -0.001(2) 0.000(2) 0.001(2) N1A 0.031(3) 0.030(3) 0.032(3) -0.003(2) 0.003(2) -0.001(2) N2 0.032(3) 0.031(3) 0.029(3) -0.003(2) 0.000(2) -0.001(2) N2A 0.029(3) 0.027(3) 0.036(3) -0.008(2) 0.004(2) -0.001(2) N3 0.035(3) 0.029(3) 0.032(3) 0.001(2) 0.003(2) -0.003(2) N3A 0.024(2) 0.040(3) 0.034(3) -0.003(2) -0.002(2) -0.004(2) N4 0.028(3) 0.034(3) 0.028(3) 0.002(2) 0.002(2) -0.002(2) N4A 0.038(3) 0.030(3) 0.034(3) -0.006(2) 0.004(2) 0.005(2) N5 0.156(9) 0.072(6) 0.067(5) 0.007(4) -0.044(5) -0.020(6) C1 0.032(3) 0.045(4) 0.042(4) -0.001(3) 0.002(3) 0.000(3) C1A 0.037(3) 0.036(3) 0.037(4) -0.006(3) 0.000(3) -0.002(3) C2 0.044(4) 0.061(5) 0.037(4) -0.003(3) 0.007(3) 0.004(3) C2A 0.049(4) 0.045(4) 0.032(4) -0.005(3) 0.001(3) 0.000(3) C3 0.044(4) 0.063(5) 0.036(4) 0.003(3) 0.007(3) 0.001(3) C3A 0.051(4) 0.049(4) 0.027(3) -0.001(3) 0.006(3) 0.006(3) C4 0.046(4) 0.052(4) 0.032(4) 0.010(3) 0.006(3) 0.006(3) C4A 0.042(4) 0.044(4) 0.031(3) 0.001(3) 0.008(3) 0.003(3) C5 0.038(3) 0.030(3) 0.035(3) 0.007(3) -0.001(3) 0.001(3) C5A 0.035(3) 0.028(3) 0.033(3) -0.001(3) 0.001(3) 0.002(3) C6 0.049(4) 0.033(3) 0.034(3) 0.005(3) 0.005(3) 0.003(3) C6A 0.035(3) 0.041(4) 0.034(3) -0.005(3) 0.008(3) -0.005(3) C7 0.040(4) 0.034(3) 0.035(3) -0.003(3) 0.001(3) 0.007(3) C7A 0.036(4) 0.036(3) 0.040(4) -0.009(3) -0.002(3) -0.006(3) C8 0.034(3) 0.030(3) 0.034(3) 0.002(3) 0.004(3) 0.001(3) C8A 0.037(3) 0.033(3) 0.031(3) -0.010(3) 0.004(3) -0.003(3) C9 0.043(4) 0.031(3) 0.043(4) -0.006(3) 0.004(3) 0.002(3) C9A 0.038(3) 0.046(4) 0.041(4) -0.014(3) -0.005(3) -0.006(3) C10 0.038(4) 0.042(4) 0.042(4) -0.010(3) 0.006(3) -0.004(3) C10A 0.043(4) 0.055(4) 0.041(4) -0.005(3) -0.004(3) -0.007(3) C11 0.041(4) 0.041(4) 0.033(3) -0.005(3) 0.002(3) -0.006(3) C11A 0.046(4) 0.046(4) 0.035(4) -0.004(3) -0.002(3) -0.002(3) C12 0.035(3) 0.033(3) 0.029(3) -0.003(3) 0.000(3) -0.005(3) C12A 0.030(3) 0.042(4) 0.026(3) -0.006(3) 0.003(2) -0.004(3) C13 0.028(3) 0.026(3) 0.040(3) -0.003(2) 0.000(3) -0.004(2) C13A 0.028(3) 0.030(3) 0.041(4) -0.002(3) 0.000(3) 0.003(2) C14 0.034(3) 0.034(3) 0.034(3) 0.002(3) 0.002(3) -0.002(3) C14A 0.043(4) 0.044(4) 0.042(4) 0.003(3) -0.001(3) 0.002(3) C15 0.036(3) 0.033(3) 0.042(4) 0.007(3) -0.004(3) -0.006(3) C15A 0.044(4) 0.034(4) 0.056(5) -0.001(3) 0.003(3) 0.001(3) C16 0.026(3) 0.041(4) 0.052(4) 0.001(3) 0.006(3) 0.002(3) C16A 0.041(4) 0.032(3) 0.063(5) -0.010(3) 0.007(3) -0.005(3) C17 0.036(3) 0.041(4) 0.038(4) 0.002(3) 0.006(3) -0.004(3) C17A 0.035(3) 0.037(3) 0.043(4) -0.008(3) -0.006(3) 0.001(3) C18 0.030(3) 0.035(3) 0.036(3) -0.004(3) -0.001(3) -0.002(2) C18A 0.033(3) 0.035(3) 0.031(3) -0.001(3) -0.002(3) -0.003(2) C19 0.033(3) 0.038(3) 0.029(3) 0.005(3) -0.006(3) 0.009(3) C19A 0.047(4) 0.031(3) 0.044(4) 0.000(3) 0.006(3) -0.003(3) C20 0.032(3) 0.038(3) 0.029(3) 0.001(3) -0.003(3) 0.000(3) C20A 0.044(4) 0.030(3) 0.038(4) 0.002(3) 0.009(3) 0.003(3) C21 0.048(4) 0.045(4) 0.039(4) -0.004(3) -0.013(3) 0.009(3) C21A 0.061(5) 0.043(4) 0.039(4) 0.008(3) 0.009(3) 0.009(3) C22 0.059(5) 0.056(5) 0.042(4) -0.013(3) -0.013(3) 0.000(4) C22A 0.073(5) 0.057(5) 0.033(4) 0.004(3) 0.005(4) 0.027(4) C23 0.057(4) 0.042(4) 0.044(4) -0.009(3) -0.008(4) 0.001(3) C23A 0.047(4) 0.060(5) 0.030(3) -0.005(3) -0.002(3) 0.016(4) C24 0.034(3) 0.031(3) 0.033(3) -0.002(3) 0.003(3) -0.001(2) C24A 0.045(4) 0.038(3) 0.028(3) -0.013(3) -0.001(3) 0.011(3) C25 0.034(3) 0.030(3) 0.044(4) 0.001(3) 0.002(3) -0.002(3) C25A 0.031(3) 0.040(4) 0.042(4) -0.006(3) -0.002(3) 0.007(3) C26 0.035(3) 0.034(3) 0.040(4) 0.001(3) -0.003(3) -0.009(3) C26A 0.039(3) 0.033(3) 0.047(4) 0.001(3) 0.000(3) -0.002(3) C27 0.039(4) 0.041(4) 0.053(4) 0.018(3) -0.011(3) -0.004(3) C27A 0.039(4) 0.037(4) 0.071(5) 0.002(3) 0.004(3) 0.001(3) C28 0.056(5) 0.036(4) 0.075(6) 0.013(4) -0.014(4) -0.004(3) C28A 0.040(4) 0.040(4) 0.084(6) -0.004(4) 0.004(4) 0.005(3) C29 0.050(4) 0.032(4) 0.084(6) 0.004(4) -0.007(4) 0.007(3) C29A 0.034(4) 0.040(4) 0.106(7) -0.020(4) -0.017(4) 0.002(3) C30 0.049(4) 0.038(4) 0.054(4) -0.003(3) 0.005(3) -0.004(3) C30A 0.040(4) 0.062(5) 0.055(4) -0.019(4) -0.011(3) 0.014(4) C31 0.032(3) 0.026(3) 0.028(3) 0.004(2) 0.002(3) -0.003(2) C31A 0.031(3) 0.028(3) 0.030(3) -0.003(3) 0.000(3) 0.005(2) C32 0.033(3) 0.031(3) 0.029(3) -0.001(2) 0.001(3) -0.005(2) C32A 0.031(3) 0.032(3) 0.027(3) -0.008(2) -0.005(2) 0.003(3) C33 0.030(3) 0.039(3) 0.031(3) -0.003(3) 0.001(3) -0.001(3) C33A 0.029(3) 0.031(3) 0.031(3) 0.002(2) 0.001(2) -0.005(2) C34 0.038(4) 0.042(4) 0.040(4) -0.006(3) 0.007(3) 0.003(3) C34A 0.036(3) 0.037(3) 0.039(4) -0.005(3) -0.006(3) -0.006(3) C35 0.043(4) 0.051(4) 0.042(4) -0.012(3) 0.012(3) -0.004(3) C35A 0.044(4) 0.049(4) 0.038(4) -0.009(3) -0.005(3) -0.002(3) C36 0.037(3) 0.056(4) 0.034(4) -0.002(3) -0.001(3) 0.005(3) C36A 0.046(4) 0.050(4) 0.037(4) -0.012(3) 0.010(3) -0.007(3) C37 0.037(3) 0.044(4) 0.030(3) 0.000(3) -0.007(3) 0.000(3) C37A 0.041(4) 0.040(4) 0.030(3) -0.003(3) 0.003(3) -0.007(3) C38 0.030(3) 0.033(3) 0.026(3) 0.004(2) 0.003(2) 0.003(2) C38A 0.033(3) 0.032(3) 0.030(3) 0.000(3) 0.001(3) -0.004(2) C39 0.031(3) 0.021(3) 0.031(3) -0.001(2) 0.003(3) -0.002(2) C39A 0.030(3) 0.030(3) 0.033(3) -0.004(3) 0.002(3) 0.004(2) C40 0.032(3) 0.032(3) 0.031(3) 0.007(3) 0.003(3) -0.001(3) C40A 0.030(3) 0.030(3) 0.032(3) -0.005(2) 0.005(2) 0.002(2) C41 0.029(3) 0.036(3) 0.043(4) 0.005(3) 0.002(3) -0.002(3) C41A 0.038(4) 0.038(4) 0.040(4) -0.003(3) 0.003(3) -0.006(3) C42 0.032(3) 0.041(4) 0.053(4) 0.009(3) -0.008(3) 0.002(3) C42A 0.049(4) 0.035(4) 0.060(5) -0.003(3) 0.013(3) 0.001(3) C43 0.036(4) 0.047(4) 0.063(5) 0.015(4) 0.005(3) 0.008(3) C43A 0.046(4) 0.037(4) 0.077(6) -0.008(4) 0.016(4) -0.014(3) C44 0.040(4) 0.042(4) 0.058(5) 0.003(3) 0.010(3) 0.013(3) C44A 0.060(5) 0.049(4) 0.066(5) -0.017(4) 0.013(4) -0.016(4) C45 0.028(3) 0.039(4) 0.041(4) 0.002(3) 0.007(3) 0.000(3) C45A 0.035(3) 0.041(4) 0.042(4) -0.013(3) 0.013(3) -0.005(3) C46 0.096(7) 0.058(5) 0.031(4) -0.002(4) -0.014(4) 0.021(5) C47 0.070(6) 0.063(5) 0.063(5) 0.022(4) 0.009(4) 0.018(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 O2 1.989(4) . ? Co1 O1 2.029(4) . ? Co1 N1 2.134(5) . ? Co1 N2 2.135(5) . ? Co1 N4 2.285(5) . ? Co1 N3 2.291(5) . ? Co2 O2A 1.982(4) . ? Co2 O1A 1.998(4) . ? Co2 N1A 2.102(5) . ? Co2 N2A 2.119(5) . ? Co2 N4A 2.271(5) . ? Co2 N3A 2.342(5) . ? Cl1 O4 1.378(6) . ? Cl1 O6A 1.399(12) . ? Cl1 O3 1.420(5) . ? Cl1 O5 1.461(14) . ? Cl1 O5A 1.462(14) . ? Cl1 O6 1.466(14) . ? Cl2 O7 1.395(6) 7_556 ? Cl2 O7 1.395(6) . ? Cl2 O7 1.395(6) 8_546 ? Cl2 O7 1.395(6) 2_655 ? Cl3 O8 1.426(5) 8_545 ? Cl3 O8 1.426(5) . ? Cl3 O8 1.426(5) 7 ? Cl3 O8 1.426(5) 2_655 ? Cl4 O13B 1.28(2) . ? Cl4 O13B 1.28(2) 3 ? Cl4 O13B 1.28(2) 2 ? Cl4 O13B 1.28(2) 4 ? Cl4 O13A 1.42(2) 3 ? Cl4 O13A 1.42(2) . ? Cl4 O13 1.600(11) . ? Cl4 O13 1.600(11) 4 ? Cl4 O13 1.600(11) 2 ? Cl4 O13 1.600(11) 3 ? Cl5 O9 1.430(4) . ? Cl5 O9 1.430(4) 2 ? Cl5 O9 1.430(4) 4_556 ? Cl5 O9 1.430(4) 3_556 ? O1 C31 1.282(6) . ? O1A C31A 1.271(7) . ? O2 C39 1.278(6) . ? O2A C39A 1.279(7) . ? O5 O6A 1.439(17) . ? O13 O13B 1.13(2) 2 ? O13A O13B 0.97(2) . ? O13A O13B 0.97(2) 2 ? O13B O13 1.13(2) 2 ? O13B O13B 1.70(5) 2 ? N1 C5 1.337(7) . ? N1 C1 1.350(8) . ? N1A C5A 1.341(7) . ? N1A C1A 1.355(7) . ? N2 C6 1.477(7) . ? N2 C7 1.479(7) . ? N2 C19 1.486(7) . ? N2A C19A 1.480(8) . ? N2A C7A 1.481(7) . ? N2A C6A 1.486(7) . ? N3 C12 1.356(7) . ? N3 C8 1.363(7) . ? N3A C12A 1.357(8) . ? N3A C8A 1.362(7) . ? N4 C24 1.357(7) . ? N4 C20 1.366(7) . ? N4A C20A 1.348(8) . ? N4A C24A 1.350(8) . ? N5 C46 1.150(11) . ? C1 C2 1.394(9) . ? C1 H1 0.9500 . ? C1A C2A 1.382(8) . ? C1A H1A 0.9500 . ? C2 C3 1.398(10) . ? C2 H2 0.9500 . ? C2A C3A 1.378(9) . ? C2A H2A 0.9500 . ? C3 C4 1.366(9) . ? C3 H3 0.9500 . ? C3A C4A 1.385(9) . ? C3A H3A 0.9500 . ? C4 C5 1.383(8) . ? C4 H4 0.9500 . ? C4A C5A 1.400(8) . ? C4A H4A 0.9500 . ? C5 C6 1.505(8) . ? C5A C6A 1.496(8) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C6A H6A1 0.9900 . ? C6A H6A2 0.9900 . ? C7 C8 1.498(8) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C7A C8A 1.509(9) . ? C7A H7A1 0.9900 . ? C7A H7A2 0.9900 . ? C8 C9 1.392(8) . ? C8A C9A 1.375(8) . ? C9 C10 1.393(9) . ? C9 H9 0.9500 . ? C9A C10A 1.381(9) . ? C9A H9A 0.9500 . ? C10 C11 1.373(9) . ? C10 H10 0.9500 . ? C10A C11A 1.385(9) . ? C10A H10A 0.9500 . ? C11 C12 1.396(8) . ? C11 H11 0.9500 . ? C11A C12A 1.383(8) . ? C11A H11A 0.9500 . ? C12 C13 1.479(8) . ? C12A C13A 1.494(8) . ? C13 C18 1.387(8) . ? C13 C14 1.395(8) . ? C13A C18A 1.378(8) . ? C13A C14A 1.398(9) . ? C14 C15 1.383(9) . ? C14 H14 0.9500 . ? C14A C15A 1.385(9) . ? C14A H14A 0.9500 . ? C15 C16 1.374(9) . ? C15 H15 0.9500 . ? C15A C16A 1.369(9) . ? C15A H15A 0.9500 . ? C16 C17 1.377(9) . ? C16 H16 0.9500 . ? C16A C17A 1.388(9) . ? C16A H16A 0.9500 . ? C17 C18 1.380(8) . ? C17 H17 0.9500 . ? C17A C18A 1.398(8) . ? C17A H17A 0.9500 . ? C18 H18 0.9500 . ? C18A H18A 0.9500 . ? C19 C20 1.504(8) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C19A C20A 1.504(9) . ? C19A H19C 0.9900 . ? C19A H19D 0.9900 . ? C20 C21 1.375(8) . ? C20A C21A 1.387(9) . ? C21 C22 1.387(9) . ? C21 H21 0.9500 . ? C21A C22A 1.395(11) . ? C21A H21A 0.9500 . ? C22 C23 1.379(10) . ? C22 H22 0.9500 . ? C22A C23A 1.361(11) . ? C22A H22A 0.9500 . ? C23 C24 1.390(8) . ? C23 H23 0.9500 . ? C23A C24A 1.390(9) . ? C23A H23A 0.9500 . ? C24 C25 1.488(8) . ? C24A C25A 1.498(9) . ? C25 C26 1.386(8) . ? C25 C30 1.399(9) . ? C25A C26A 1.383(9) . ? C25A C30A 1.409(9) . ? C26 C27 1.410(9) . ? C26 H26 0.9500 . ? C26A C27A 1.388(9) . ? C26A H26A 0.9500 . ? C27 C28 1.372(10) . ? C27 H27 0.9500 . ? C27A C28A 1.384(10) . ? C27A H27A 0.9500 . ? C28 C29 1.389(10) . ? C28 H28 0.9500 . ? C28A C29A 1.372(11) . ? C28A H28A 0.9500 . ? C29 C30 1.378(10) . ? C29 H29 0.9500 . ? C29A C30A 1.386(11) . ? C29A H29A 0.9500 . ? C30 H30 0.9500 . ? C30A H30A 0.9500 . ? C31 C38 1.381(8) . ? C31 C32 1.524(8) . ? C31A C38A 1.401(8) . ? C31A C32A 1.503(8) . ? C32 C33 1.385(8) . ? C32 C37 1.398(8) . ? C32A C37A 1.394(8) . ? C32A C33A 1.401(8) . ? C33 C34 1.396(8) . ? C33 H33 0.9500 . ? C33A C34A 1.383(8) . ? C33A H33A 0.9500 . ? C34 C35 1.398(9) . ? C34 H34 0.9500 . ? C34A C35A 1.382(9) . ? C34A H34A 0.9500 . ? C35 C36 1.387(9) . ? C35 H35 0.9500 . ? C35A C36A 1.389(9) . ? C35A H35A 0.9500 . ? C36 C37 1.395(9) . ? C36 H36 0.9500 . ? C36A C37A 1.382(8) . ? C36A H36A 0.9500 . ? C37 H37 0.9500 . ? C37A H37A 0.9500 . ? C38 C39 1.411(8) . ? C38 H38A 0.9500 . ? C38A C39A 1.401(8) . ? C38A H38B 0.9500 . ? C39 C40 1.494(8) . ? C39A C40A 1.499(8) . ? C40 C41 1.387(8) . ? C40 C45 1.409(8) . ? C40A C45A 1.393(8) . ? C40A C41A 1.400(8) . ? C41 C42 1.391(9) . ? C41 H41 0.9500 . ? C41A C42A 1.398(9) . ? C41A H41A 0.9500 . ? C42 C43 1.398(10) . ? C42 H42 0.9500 . ? C42A C43A 1.382(10) . ? C42A H42A 0.9500 . ? C43 C44 1.380(10) . ? C43 H43 0.9500 . ? C43A C44A 1.388(10) . ? C43A H43A 0.9500 . ? C44 C45 1.388(9) . ? C44 H44 0.9500 . ? C44A C45A 1.373(9) . ? C44A H44A 0.9500 . ? C45 H45 0.9500 . ? C45A H45A 0.9500 . ? C46 C47 1.455(12) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? 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 O2 Co1 O1 90.30(15) . . ? O2 Co1 N1 93.99(17) . . ? O1 Co1 N1 175.44(17) . . ? O2 Co1 N2 171.34(17) . . ? O1 Co1 N2 95.84(16) . . ? N1 Co1 N2 80.06(18) . . ? O2 Co1 N4 105.54(16) . . ? O1 Co1 N4 96.88(16) . . ? N1 Co1 N4 80.50(17) . . ? N2 Co1 N4 79.83(18) . . ? O2 Co1 N3 99.88(17) . . ? O1 Co1 N3 82.06(16) . . ? N1 Co1 N3 98.68(18) . . ? N2 Co1 N3 75.03(18) . . ? N4 Co1 N3 154.56(17) . . ? O2A Co2 O1A 90.92(16) . . ? O2A Co2 N1A 94.46(17) . . ? O1A Co2 N1A 173.46(18) . . ? O2A Co2 N2A 170.49(18) . . ? O1A Co2 N2A 94.17(16) . . ? N1A Co2 N2A 81.04(18) . . ? O2A Co2 N4A 107.56(18) . . ? O1A Co2 N4A 94.06(17) . . ? N1A Co2 N4A 80.77(17) . . ? N2A Co2 N4A 80.11(19) . . ? O2A Co2 N3A 97.19(16) . . ? O1A Co2 N3A 85.87(16) . . ? N1A Co2 N3A 97.13(18) . . ? N2A Co2 N3A 75.21(18) . . ? N4A Co2 N3A 155.24(17) . . ? O4 Cl1 O6A 129.7(6) . . ? O4 Cl1 O3 110.9(4) . . ? O6A Cl1 O3 111.0(6) . . ? O4 Cl1 O5 116.6(6) . . ? O6A Cl1 O5 60.4(7) . . ? O3 Cl1 O5 120.4(6) . . ? O4 Cl1 O5A 93.3(7) . . ? O6A Cl1 O5A 101.5(8) . . ? O3 Cl1 O5A 105.0(7) . . ? O5 Cl1 O5A 41.2(7) . . ? O4 Cl1 O6 100.6(7) . . ? O6A Cl1 O6 42.6(7) . . ? O3 Cl1 O6 104.0(6) . . ? O5 Cl1 O6 100.5(8) . . ? O5A Cl1 O6 140.6(8) . . ? O7 Cl2 O7 107.7(4) 7_556 . ? O7 Cl2 O7 113.1(7) 7_556 8_546 ? O7 Cl2 O7 107.7(4) . 8_546 ? O7 Cl2 O7 107.7(4) 7_556 2_655 ? O7 Cl2 O7 113.1(7) . 2_655 ? O7 Cl2 O7 107.7(4) 8_546 2_655 ? O8 Cl3 O8 108.1(3) 8_545 . ? O8 Cl3 O8 112.3(6) 8_545 7 ? O8 Cl3 O8 108.1(3) . 7 ? O8 Cl3 O8 108.1(3) 8_545 2_655 ? O8 Cl3 O8 112.3(6) . 2_655 ? O8 Cl3 O8 108.1(3) 7 2_655 ? O13B Cl4 O13B 123.9(13) . 3 ? O13B Cl4 O13B 83(2) . 2 ? O13B Cl4 O13B 123.9(13) 3 2 ? O13B Cl4 O13B 123.9(13) . 4 ? O13B Cl4 O13B 83(2) 3 4 ? O13B Cl4 O13B 123.9(13) 2 4 ? O13B Cl4 O13A 138.3(11) . 3 ? O13B Cl4 O13A 41.7(11) 3 3 ? O13B Cl4 O13A 138.3(11) 2 3 ? O13B Cl4 O13A 41.7(11) 4 3 ? O13B Cl4 O13A 41.7(11) . . ? O13B Cl4 O13A 138.3(11) 3 . ? O13B Cl4 O13A 41.7(11) 2 . ? O13B Cl4 O13A 138.3(11) 4 . ? O13A Cl4 O13A 180.0 3 . ? O13B Cl4 O13 122.8(14) . . ? O13B Cl4 O13 82.9(11) 3 . ? O13B Cl4 O13 44.6(11) 2 . ? O13B Cl4 O13 107.1(12) 4 . ? O13A Cl4 O13 96.6(6) 3 . ? O13A Cl4 O13 83.4(6) . . ? O13B Cl4 O13 82.9(11) . 4 ? O13B Cl4 O13 44.6(11) 3 4 ? O13B Cl4 O13 107.1(12) 2 4 ? O13B Cl4 O13 122.8(14) 4 4 ? O13A Cl4 O13 83.4(6) 3 4 ? O13A Cl4 O13 96.6(6) . 4 ? O13 Cl4 O13 90.75(13) . 4 ? O13B Cl4 O13 44.6(11) . 2 ? O13B Cl4 O13 107.1(12) 3 2 ? O13B Cl4 O13 122.8(14) 2 2 ? O13B Cl4 O13 82.9(11) 4 2 ? O13A Cl4 O13 96.6(6) 3 2 ? O13A Cl4 O13 83.4(6) . 2 ? O13 Cl4 O13 166.9(11) . 2 ? O13 Cl4 O13 90.75(13) 4 2 ? O13B Cl4 O13 107.1(12) . 3 ? O13B Cl4 O13 122.8(14) 3 3 ? O13B Cl4 O13 82.9(11) 2 3 ? O13B Cl4 O13 44.6(11) 4 3 ? O13A Cl4 O13 83.4(6) 3 3 ? O13A Cl4 O13 96.6(6) . 3 ? O13 Cl4 O13 90.75(13) . 3 ? O13 Cl4 O13 166.9(11) 4 3 ? O13 Cl4 O13 90.75(13) 2 3 ? O9 Cl5 O9 109.2(4) . 2 ? O9 Cl5 O9 109.61(19) . 4_556 ? O9 Cl5 O9 109.62(19) 2 4_556 ? O9 Cl5 O9 109.61(19) . 3_556 ? O9 Cl5 O9 109.61(19) 2 3_556 ? O9 Cl5 O9 109.2(4) 4_556 3_556 ? C31 O1 Co1 121.4(4) . . ? C31A O1A Co2 124.1(4) . . ? C39 O2 Co1 123.8(3) . . ? C39A O2A Co2 123.6(4) . . ? O13B O13 Cl4 52.5(13) 2 . ? O13B O13A O13B 123(4) . 2 ? O13B O13A Cl4 62(2) . . ? O13B O13A Cl4 62(2) 2 . ? O13A O13B O13 147(3) . 2 ? O13A O13B Cl4 77(2) . . ? O13 O13B Cl4 82.9(15) 2 . ? O13A O13B O13B 28(2) . 2 ? O13 O13B O13B 125.5(18) 2 2 ? Cl4 O13B O13B 48.3(11) . 2 ? C5 N1 C1 119.1(5) . . ? C5 N1 Co1 113.9(4) . . ? C1 N1 Co1 126.3(4) . . ? C5A N1A C1A 119.5(5) . . ? C5A N1A Co2 114.5(4) . . ? C1A N1A Co2 126.0(4) . . ? C6 N2 C7 110.3(5) . . ? C6 N2 C19 110.7(5) . . ? C7 N2 C19 111.0(4) . . ? C6 N2 Co1 107.7(4) . . ? C7 N2 Co1 108.0(3) . . ? C19 N2 Co1 109.0(3) . . ? C19A N2A C7A 110.4(4) . . ? C19A N2A C6A 112.0(5) . . ? C7A N2A C6A 110.0(5) . . ? C19A N2A Co2 107.5(4) . . ? C7A N2A Co2 108.6(3) . . ? C6A N2A Co2 108.3(3) . . ? C12 N3 C8 118.1(5) . . ? C12 N3 Co1 127.9(4) . . ? C8 N3 Co1 106.2(4) . . ? C12A N3A C8A 116.4(5) . . ? C12A N3A Co2 133.0(4) . . ? C8A N3A Co2 107.3(4) . . ? C24 N4 C20 117.7(5) . . ? C24 N4 Co1 128.6(4) . . ? C20 N4 Co1 108.1(4) . . ? C20A N4A C24A 118.2(5) . . ? C20A N4A Co2 108.5(4) . . ? C24A N4A Co2 128.5(4) . . ? N1 C1 C2 122.1(6) . . ? N1 C1 H1 119.0 . . ? C2 C1 H1 119.0 . . ? N1A C1A C2A 121.7(6) . . ? N1A C1A H1A 119.2 . . ? C2A C1A H1A 119.2 . . ? C1 C2 C3 117.6(6) . . ? C1 C2 H2 121.2 . . ? C3 C2 H2 121.2 . . ? C3A C2A C1A 119.0(6) . . ? C3A C2A H2A 120.5 . . ? C1A C2A H2A 120.5 . . ? C4 C3 C2 119.8(6) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C2A C3A C4A 119.9(6) . . ? C2A C3A H3A 120.1 . . ? C4A C3A H3A 120.1 . . ? C3 C4 C5 119.5(6) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? C3A C4A C5A 118.5(6) . . ? C3A C4A H4A 120.7 . . ? C5A C4A H4A 120.7 . . ? N1 C5 C4 121.8(6) . . ? N1 C5 C6 115.7(5) . . ? C4 C5 C6 122.3(5) . . ? N1A C5A C4A 121.4(5) . . ? N1A C5A C6A 116.6(5) . . ? C4A C5A C6A 121.7(5) . . ? N2 C6 C5 112.0(5) . . ? N2 C6 H6A 109.2 . . ? C5 C6 H6A 109.2 . . ? N2 C6 H6B 109.2 . . ? C5 C6 H6B 109.2 . . ? H6A C6 H6B 107.9 . . ? N2A C6A C5A 113.4(5) . . ? N2A C6A H6A1 108.9 . . ? C5A C6A H6A1 108.9 . . ? N2A C6A H6A2 108.9 . . ? C5A C6A H6A2 108.9 . . ? H6A1 C6A H6A2 107.7 . . ? N2 C7 C8 112.2(5) . . ? N2 C7 H7A 109.2 . . ? C8 C7 H7A 109.2 . . ? N2 C7 H7B 109.2 . . ? C8 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? N2A C7A C8A 112.5(5) . . ? N2A C7A H7A1 109.1 . . ? C8A C7A H7A1 109.1 . . ? N2A C7A H7A2 109.1 . . ? C8A C7A H7A2 109.1 . . ? H7A1 C7A H7A2 107.8 . . ? N3 C8 C9 122.6(6) . . ? N3 C8 C7 117.8(5) . . ? C9 C8 C7 119.5(5) . . ? N3A C8A C9A 123.4(6) . . ? N3A C8A C7A 117.6(5) . . ? C9A C8A C7A 119.0(5) . . ? C8 C9 C10 118.1(6) . . ? C8 C9 H9 120.9 . . ? C10 C9 H9 120.9 . . ? C8A C9A C10A 119.1(6) . . ? C8A C9A H9A 120.4 . . ? C10A C9A H9A 120.4 . . ? C11 C10 C9 119.5(6) . . ? C11 C10 H10 120.2 . . ? C9 C10 H10 120.2 . . ? C9A C10A C11A 118.8(6) . . ? C9A C10A H10A 120.6 . . ? C11A C10A H10A 120.6 . . ? C10 C11 C12 119.8(6) . . ? C10 C11 H11 120.1 . . ? C12 C11 H11 120.1 . . ? C12A C11A C10A 119.1(6) . . ? C12A C11A H11A 120.5 . . ? C10A C11A H11A 120.5 . . ? N3 C12 C11 121.3(6) . . ? N3 C12 C13 117.4(5) . . ? C11 C12 C13 121.3(5) . . ? N3A C12A C11A 123.0(6) . . ? N3A C12A C13A 117.0(5) . . ? C11A C12A C13A 119.8(6) . . ? C18 C13 C14 117.7(5) . . ? C18 C13 C12 120.9(5) . . ? C14 C13 C12 121.3(5) . . ? C18A C13A C14A 119.1(6) . . ? C18A C13A C12A 120.1(5) . . ? C14A C13A C12A 120.7(6) . . ? C15 C14 C13 120.9(6) . . ? C15 C14 H14 119.6 . . ? C13 C14 H14 119.6 . . ? C15A C14A C13A 120.3(6) . . ? C15A C14A H14A 119.8 . . ? C13A C14A H14A 119.8 . . ? C16 C15 C14 119.9(6) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C16A C15A C14A 120.3(6) . . ? C16A C15A H15A 119.9 . . ? C14A C15A H15A 119.9 . . ? C15 C16 C17 120.4(6) . . ? C15 C16 H16 119.8 . . ? C17 C16 H16 119.8 . . ? C15A C16A C17A 120.3(6) . . ? C15A C16A H16A 119.9 . . ? C17A C16A H16A 119.9 . . ? C16 C17 C18 119.4(6) . . ? C16 C17 H17 120.3 . . ? C18 C17 H17 120.3 . . ? C16A C17A C18A 119.5(6) . . ? C16A C17A H17A 120.2 . . ? C18A C17A H17A 120.2 . . ? C17 C18 C13 121.6(6) . . ? C17 C18 H18 119.2 . . ? C13 C18 H18 119.2 . . ? C13A C18A C17A 120.5(6) . . ? C13A C18A H18A 119.7 . . ? C17A C18A H18A 119.7 . . ? N2 C19 C20 111.7(5) . . ? N2 C19 H19A 109.3 . . ? C20 C19 H19A 109.3 . . ? N2 C19 H19B 109.3 . . ? C20 C19 H19B 109.3 . . ? H19A C19 H19B 107.9 . . ? N2A C19A C20A 112.0(5) . . ? N2A C19A H19C 109.2 . . ? C20A C19A H19C 109.2 . . ? N2A C19A H19D 109.2 . . ? C20A C19A H19D 109.2 . . ? H19C C19A H19D 107.9 . . ? N4 C20 C21 122.7(6) . . ? N4 C20 C19 115.4(5) . . ? C21 C20 C19 121.7(5) . . ? N4A C20A C21A 123.1(6) . . ? N4A C20A C19A 115.4(5) . . ? C21A C20A C19A 121.5(6) . . ? C20 C21 C22 119.0(6) . . ? C20 C21 H21 120.5 . . ? C22 C21 H21 120.5 . . ? C20A C21A C22A 117.3(7) . . ? C20A C21A H21A 121.3 . . ? C22A C21A H21A 121.3 . . ? C23 C22 C21 119.2(6) . . ? C23 C22 H22 120.4 . . ? C21 C22 H22 120.4 . . ? C23A C22A C21A 120.4(6) . . ? C23A C22A H22A 119.8 . . ? C21A C22A H22A 119.8 . . ? C22 C23 C24 119.5(6) . . ? C22 C23 H23 120.2 . . ? C24 C23 H23 120.2 . . ? C22A C23A C24A 119.1(7) . . ? C22A C23A H23A 120.5 . . ? C24A C23A H23A 120.5 . . ? N4 C24 C23 121.9(6) . . ? N4 C24 C25 117.0(5) . . ? C23 C24 C25 121.1(6) . . ? N4A C24A C23A 121.9(6) . . ? N4A C24A C25A 118.9(5) . . ? C23A C24A C25A 119.0(6) . . ? C26 C25 C30 119.4(6) . . ? C26 C25 C24 119.7(6) . . ? C30 C25 C24 120.8(6) . . ? C26A C25A C30A 119.3(6) . . ? C26A C25A C24A 120.1(5) . . ? C30A C25A C24A 120.5(6) . . ? C25 C26 C27 120.1(6) . . ? C25 C26 H26 119.9 . . ? C27 C26 H26 119.9 . . ? C25A C26A C27A 119.9(6) . . ? C25A C26A H26A 120.1 . . ? C27A C26A H26A 120.1 . . ? C28 C27 C26 119.9(6) . . ? C28 C27 H27 120.1 . . ? C26 C27 H27 120.1 . . ? C28A C27A C26A 121.1(7) . . ? C28A C27A H27A 119.4 . . ? C26A C27A H27A 119.4 . . ? C27 C28 C29 119.7(7) . . ? C27 C28 H28 120.1 . . ? C29 C28 H28 120.1 . . ? C29A C28A C27A 119.0(7) . . ? C29A C28A H28A 120.5 . . ? C27A C28A H28A 120.5 . . ? C30 C29 C28 121.1(7) . . ? C30 C29 H29 119.5 . . ? C28 C29 H29 119.5 . . ? C28A C29A C30A 121.3(7) . . ? C28A C29A H29A 119.3 . . ? C30A C29A H29A 119.3 . . ? C29 C30 C25 119.7(7) . . ? C29 C30 H30 120.1 . . ? C25 C30 H30 120.1 . . ? C29A C30A C25A 119.4(7) . . ? C29A C30A H30A 120.3 . . ? C25A C30A H30A 120.3 . . ? O1 C31 C38 125.4(5) . . ? O1 C31 C32 115.3(5) . . ? C38 C31 C32 119.2(5) . . ? O1A C31A C38A 124.2(5) . . ? O1A C31A C32A 116.3(5) . . ? C38A C31A C32A 119.4(5) . . ? C33 C32 C37 119.6(5) . . ? C33 C32 C31 118.9(5) . . ? C37 C32 C31 121.6(5) . . ? C37A C32A C33A 118.2(5) . . ? C37A C32A C31A 123.6(5) . . ? C33A C32A C31A 118.2(5) . . ? C32 C33 C34 120.7(6) . . ? C32 C33 H33 119.7 . . ? C34 C33 H33 119.7 . . ? C34A C33A C32A 120.8(5) . . ? C34A C33A H33A 119.6 . . ? C32A C33A H33A 119.6 . . ? C33 C34 C35 119.7(6) . . ? C33 C34 H34 120.2 . . ? C35 C34 H34 120.2 . . ? C35A C34A C33A 120.3(6) . . ? C35A C34A H34A 119.9 . . ? C33A C34A H34A 119.9 . . ? C36 C35 C34 119.6(6) . . ? C36 C35 H35 120.2 . . ? C34 C35 H35 120.2 . . ? C34A C35A C36A 119.5(6) . . ? C34A C35A H35A 120.2 . . ? C36A C35A H35A 120.2 . . ? C35 C36 C37 120.6(6) . . ? C35 C36 H36 119.7 . . ? C37 C36 H36 119.7 . . ? C37A C36A C35A 120.4(6) . . ? C37A C36A H36A 119.8 . . ? C35A C36A H36A 119.8 . . ? C36 C37 C32 119.8(6) . . ? C36 C37 H37 120.1 . . ? C32 C37 H37 120.1 . . ? C36A C37A C32A 120.8(6) . . ? C36A C37A H37A 119.6 . . ? C32A C37A H37A 119.6 . . ? C31 C38 C39 125.7(5) . . ? C31 C38 H38A 117.2 . . ? C39 C38 H38A 117.2 . . ? C31A C38A C39A 126.1(6) . . ? C31A C38A H38B 117.0 . . ? C39A C38A H38B 117.0 . . ? O2 C39 C38 125.0(5) . . ? O2 C39 C40 116.5(5) . . ? C38 C39 C40 118.4(5) . . ? O2A C39A C38A 125.0(5) . . ? O2A C39A C40A 115.8(5) . . ? C38A C39A C40A 119.1(5) . . ? C41 C40 C45 118.8(6) . . ? C41 C40 C39 123.2(5) . . ? C45 C40 C39 118.0(5) . . ? C45A C40A C41A 119.2(6) . . ? C45A C40A C39A 118.2(5) . . ? C41A C40A C39A 122.6(5) . . ? C40 C41 C42 121.1(6) . . ? C40 C41 H41 119.5 . . ? C42 C41 H41 119.5 . . ? C42A C41A C40A 120.0(6) . . ? C42A C41A H41A 120.0 . . ? C40A C41A H41A 120.0 . . ? C41 C42 C43 119.8(6) . . ? C41 C42 H42 120.1 . . ? C43 C42 H42 120.1 . . ? C43A C42A C41A 119.8(7) . . ? C43A C42A H42A 120.1 . . ? C41A C42A H42A 120.1 . . ? C44 C43 C42 119.3(6) . . ? C44 C43 H43 120.3 . . ? C42 C43 H43 120.3 . . ? C42A C43A C44A 119.9(6) . . ? C42A C43A H43A 120.1 . . ? C44A C43A H43A 120.1 . . ? C43 C44 C45 121.2(7) . . ? C43 C44 H44 119.4 . . ? C45 C44 H44 119.4 . . ? C45A C44A C43A 120.8(7) . . ? C45A C44A H44A 119.6 . . ? C43A C44A H44A 119.6 . . ? C44 C45 C40 119.7(6) . . ? C44 C45 H45 120.1 . . ? C40 C45 H45 120.1 . . ? C44A C45A C40A 120.3(7) . . ? C44A C45A H45A 119.9 . . ? C40A C45A H45A 119.9 . . ? N5 C46 C47 177.0(10) . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Co1 O1 C31 -30.1(4) . . . . ? N1 Co1 O1 C31 170(2) . . . . ? N2 Co1 O1 C31 143.8(4) . . . . ? N4 Co1 O1 C31 -135.8(4) . . . . ? N3 Co1 O1 C31 69.8(4) . . . . ? O2A Co2 O1A C31A -24.7(4) . . . . ? N1A Co2 O1A C31A -170.1(14) . . . . ? N2A Co2 O1A C31A 147.2(4) . . . . ? N4A Co2 O1A C31A -132.4(4) . . . . ? N3A Co2 O1A C31A 72.4(4) . . . . ? O1 Co1 O2 C39 25.5(4) . . . . ? N1 Co1 O2 C39 -156.0(4) . . . . ? N2 Co1 O2 C39 -109.7(11) . . . . ? N4 Co1 O2 C39 122.8(4) . . . . ? N3 Co1 O2 C39 -56.5(4) . . . . ? O1A Co2 O2A C39A 24.3(4) . . . . ? N1A Co2 O2A C39A -159.5(4) . . . . ? N2A Co2 O2A C39A -98.2(11) . . . . ? N4A Co2 O2A C39A 118.8(4) . . . . ? N3A Co2 O2A C39A -61.7(4) . . . . ? O13B Cl4 O13 O13B 32(3) . . . 2 ? O13B Cl4 O13 O13B 157.9(18) 3 . . 2 ? O13B Cl4 O13 O13B -121(2) 4 . . 2 ? O13A Cl4 O13 O13B -162.6(15) 3 . . 2 ? O13A Cl4 O13 O13B 17.4(15) . . . 2 ? O13 Cl4 O13 O13B 113.9(17) 4 . . 2 ? O13 Cl4 O13 O13B 17.4(15) 2 . . 2 ? O13 Cl4 O13 O13B -79.1(15) 3 . . 2 ? O13B Cl4 O13A O13B 90.0 3 . . . ? O13B Cl4 O13A O13B -180.0 2 . . . ? O13B Cl4 O13A O13B -89.999(1) 4 . . . ? O13A Cl4 O13A O13B -139(9) 3 . . . ? O13 Cl4 O13A O13B 161.6(16) . . . . ? O13 Cl4 O13A O13B 71.6(16) 4 . . . ? O13 Cl4 O13A O13B -18.4(16) 2 . . . ? O13 Cl4 O13A O13B -108.4(16) 3 . . . ? O13B Cl4 O13A O13B 180.0 . . . 2 ? O13B Cl4 O13A O13B -90.0 3 . . 2 ? O13B Cl4 O13A O13B 90.0 4 . . 2 ? O13A Cl4 O13A O13B 41(9) 3 . . 2 ? O13 Cl4 O13A O13B -18.4(16) . . . 2 ? O13 Cl4 O13A O13B -108.4(16) 4 . . 2 ? O13 Cl4 O13A O13B 161.6(16) 2 . . 2 ? O13 Cl4 O13A O13B 71.6(16) 3 . . 2 ? O13B O13A O13B O13 54(5) 2 . . 2 ? Cl4 O13A O13B O13 54(5) . . . 2 ? O13B O13A O13B Cl4 -0.008(3) 2 . . . ? Cl4 O13A O13B O13B 0.008(3) . . . 2 ? O13B Cl4 O13B O13A -126.7(5) 3 . . . ? O13B Cl4 O13B O13A 0.005(3) 2 . . . ? O13B Cl4 O13B O13A 126.7(5) 4 . . . ? O13A Cl4 O13B O13A 179.997(1) 3 . . . ? O13 Cl4 O13B O13A -21.9(18) . . . . ? O13 Cl4 O13B O13A -108.2(14) 4 . . . ? O13 Cl4 O13B O13A 153(2) 2 . . . ? O13 Cl4 O13B O13A 80.5(13) 3 . . . ? O13B Cl4 O13B O13 80(2) 3 . . 2 ? O13B Cl4 O13B O13 -153(2) 2 . . 2 ? O13B Cl4 O13B O13 -27(2) 4 . . 2 ? O13A Cl4 O13B O13 27(2) 3 . . 2 ? O13A Cl4 O13B O13 -153(2) . . . 2 ? O13 Cl4 O13B O13 -175.4(6) . . . 2 ? O13 Cl4 O13B O13 98.3(11) 4 . . 2 ? O13 Cl4 O13B O13 -73.0(13) 3 . . 2 ? O13B Cl4 O13B O13B -126.7(5) 3 . . 2 ? O13B Cl4 O13B O13B 126.7(5) 4 . . 2 ? O13A Cl4 O13B O13B 179.992(3) 3 . . 2 ? O13A Cl4 O13B O13B -0.005(4) . . . 2 ? O13 Cl4 O13B O13B -21.9(18) . . . 2 ? O13 Cl4 O13B O13B -108.2(14) 4 . . 2 ? O13 Cl4 O13B O13B 153(2) 2 . . 2 ? O13 Cl4 O13B O13B 80.5(13) 3 . . 2 ? O2 Co1 N1 C5 169.3(4) . . . . ? O1 Co1 N1 C5 -30(2) . . . . ? N2 Co1 N1 C5 -4.4(4) . . . . ? N4 Co1 N1 C5 -85.6(4) . . . . ? N3 Co1 N1 C5 68.6(4) . . . . ? O2 Co1 N1 C1 -20.3(5) . . . . ? O1 Co1 N1 C1 140(2) . . . . ? N2 Co1 N1 C1 166.1(5) . . . . ? N4 Co1 N1 C1 84.8(5) . . . . ? N3 Co1 N1 C1 -120.9(5) . . . . ? O2A Co2 N1A C5A 165.1(4) . . . . ? O1A Co2 N1A C5A -49.7(17) . . . . ? N2A Co2 N1A C5A -6.5(4) . . . . ? N4A Co2 N1A C5A -87.8(4) . . . . ? N3A Co2 N1A C5A 67.2(4) . . . . ? O2A Co2 N1A C1A -18.5(5) . . . . ? O1A Co2 N1A C1A 126.7(15) . . . . ? N2A Co2 N1A C1A 169.9(5) . . . . ? N4A Co2 N1A C1A 88.5(5) . . . . ? N3A Co2 N1A C1A -116.4(5) . . . . ? O2 Co1 N2 C6 -25.7(13) . . . . ? O1 Co1 N2 C6 -160.7(4) . . . . ? N1 Co1 N2 C6 21.3(4) . . . . ? N4 Co1 N2 C6 103.3(4) . . . . ? N3 Co1 N2 C6 -80.6(4) . . . . ? O2 Co1 N2 C7 93.4(12) . . . . ? O1 Co1 N2 C7 -41.6(4) . . . . ? N1 Co1 N2 C7 140.4(4) . . . . ? N4 Co1 N2 C7 -137.6(4) . . . . ? N3 Co1 N2 C7 38.6(4) . . . . ? O2 Co1 N2 C19 -145.9(10) . . . . ? O1 Co1 N2 C19 79.1(4) . . . . ? N1 Co1 N2 C19 -98.9(4) . . . . ? N4 Co1 N2 C19 -16.9(3) . . . . ? N3 Co1 N2 C19 159.2(4) . . . . ? O2A Co2 N2A C19A -165.4(9) . . . . ? O1A Co2 N2A C19A 72.5(4) . . . . ? N1A Co2 N2A C19A -103.1(4) . . . . ? N4A Co2 N2A C19A -21.0(4) . . . . ? N3A Co2 N2A C19A 157.1(4) . . . . ? O2A Co2 N2A C7A 75.2(11) . . . . ? O1A Co2 N2A C7A -47.0(4) . . . . ? N1A Co2 N2A C7A 137.5(4) . . . . ? N4A Co2 N2A C7A -140.4(4) . . . . ? N3A Co2 N2A C7A 37.6(3) . . . . ? O2A Co2 N2A C6A -44.2(12) . . . . ? O1A Co2 N2A C6A -166.4(4) . . . . ? N1A Co2 N2A C6A 18.1(4) . . . . ? N4A Co2 N2A C6A 100.2(4) . . . . ? N3A Co2 N2A C6A -81.8(4) . . . . ? O2 Co1 N3 C12 3.0(5) . . . . ? O1 Co1 N3 C12 -85.9(5) . . . . ? N1 Co1 N3 C12 98.6(5) . . . . ? N2 Co1 N3 C12 175.8(5) . . . . ? N4 Co1 N3 C12 -175.3(4) . . . . ? O2 Co1 N3 C8 150.9(4) . . . . ? O1 Co1 N3 C8 62.0(4) . . . . ? N1 Co1 N3 C8 -113.4(4) . . . . ? N2 Co1 N3 C8 -36.2(4) . . . . ? N4 Co1 N3 C8 -27.3(6) . . . . ? O2A Co2 N3A C12A -3.1(5) . . . . ? O1A Co2 N3A C12A -93.5(5) . . . . ? N1A Co2 N3A C12A 92.4(5) . . . . ? N2A Co2 N3A C12A 171.1(5) . . . . ? N4A Co2 N3A C12A 175.8(4) . . . . ? O2A Co2 N3A C8A 155.0(4) . . . . ? O1A Co2 N3A C8A 64.6(4) . . . . ? N1A Co2 N3A C8A -109.5(4) . . . . ? N2A Co2 N3A C8A -30.8(4) . . . . ? N4A Co2 N3A C8A -26.1(6) . . . . ? O2 Co1 N4 C24 14.1(5) . . . . ? O1 Co1 N4 C24 106.3(5) . . . . ? N1 Co1 N4 C24 -77.5(5) . . . . ? N2 Co1 N4 C24 -159.0(5) . . . . ? N3 Co1 N4 C24 -167.7(4) . . . . ? O2 Co1 N4 C20 166.6(3) . . . . ? O1 Co1 N4 C20 -101.2(4) . . . . ? N1 Co1 N4 C20 75.1(4) . . . . ? N2 Co1 N4 C20 -6.4(4) . . . . ? N3 Co1 N4 C20 -15.2(6) . . . . ? O2A Co2 N4A C20A 172.5(4) . . . . ? O1A Co2 N4A C20A -95.3(4) . . . . ? N1A Co2 N4A C20A 80.7(4) . . . . ? N2A Co2 N4A C20A -1.8(4) . . . . ? N3A Co2 N4A C20A -6.3(6) . . . . ? O2A Co2 N4A C24A 18.0(5) . . . . ? O1A Co2 N4A C24A 110.2(5) . . . . ? N1A Co2 N4A C24A -73.8(5) . . . . ? N2A Co2 N4A C24A -156.2(5) . . . . ? N3A Co2 N4A C24A -160.8(4) . . . . ? C5 N1 C1 C2 0.3(9) . . . . ? Co1 N1 C1 C2 -169.8(5) . . . . ? C5A N1A C1A C2A -1.8(9) . . . . ? Co2 N1A C1A C2A -178.0(5) . . . . ? N1 C1 C2 C3 0.6(10) . . . . ? N1A C1A C2A C3A 0.4(10) . . . . ? C1 C2 C3 C4 -0.4(10) . . . . ? C1A C2A C3A C4A 0.5(10) . . . . ? C2 C3 C4 C5 -0.5(11) . . . . ? C2A C3A C4A C5A 0.0(9) . . . . ? C1 N1 C5 C4 -1.2(9) . . . . ? Co1 N1 C5 C4 170.0(5) . . . . ? C1 N1 C5 C6 174.7(5) . . . . ? Co1 N1 C5 C6 -14.1(7) . . . . ? C3 C4 C5 N1 1.4(10) . . . . ? C3 C4 C5 C6 -174.3(6) . . . . ? C1A N1A C5A C4A 2.3(9) . . . . ? Co2 N1A C5A C4A 178.9(5) . . . . ? C1A N1A C5A C6A 176.0(5) . . . . ? Co2 N1A C5A C6A -7.4(7) . . . . ? C3A C4A C5A N1A -1.4(9) . . . . ? C3A C4A C5A C6A -174.8(6) . . . . ? C7 N2 C6 C5 -152.2(5) . . . . ? C19 N2 C6 C5 84.5(6) . . . . ? Co1 N2 C6 C5 -34.6(6) . . . . ? N1 C5 C6 N2 33.6(8) . . . . ? C4 C5 C6 N2 -150.5(6) . . . . ? C19A N2A C6A C5A 91.1(6) . . . . ? C7A N2A C6A C5A -145.7(5) . . . . ? Co2 N2A C6A C5A -27.2(6) . . . . ? N1A C5A C6A N2A 23.8(8) . . . . ? C4A C5A C6A N2A -162.5(5) . . . . ? C6 N2 C7 C8 80.6(6) . . . . ? C19 N2 C7 C8 -156.3(5) . . . . ? Co1 N2 C7 C8 -36.9(6) . . . . ? C19A N2A C7A C8A -158.8(5) . . . . ? C6A N2A C7A C8A 77.0(6) . . . . ? Co2 N2A C7A C8A -41.3(6) . . . . ? C12 N3 C8 C9 2.0(8) . . . . ? Co1 N3 C8 C9 -149.7(5) . . . . ? C12 N3 C8 C7 178.8(5) . . . . ? Co1 N3 C8 C7 27.1(6) . . . . ? N2 C7 C8 N3 4.7(7) . . . . ? N2 C7 C8 C9 -178.4(5) . . . . ? C12A N3A C8A C9A 2.7(8) . . . . ? Co2 N3A C8A C9A -159.5(5) . . . . ? C12A N3A C8A C7A 179.7(5) . . . . ? Co2 N3A C8A C7A 17.5(6) . . . . ? N2A C7A C8A N3A 13.9(8) . . . . ? N2A C7A C8A C9A -169.0(5) . . . . ? N3 C8 C9 C10 3.9(9) . . . . ? C7 C8 C9 C10 -172.8(6) . . . . ? N3A C8A C9A C10A 0.9(9) . . . . ? C7A C8A C9A C10A -176.0(6) . . . . ? C8 C9 C10 C11 -5.2(9) . . . . ? C8A C9A C10A C11A -2.7(9) . . . . ? C9 C10 C11 C12 0.9(10) . . . . ? C9A C10A C11A C12A 0.7(10) . . . . ? C8 N3 C12 C11 -6.6(8) . . . . ? Co1 N3 C12 C11 138.1(5) . . . . ? C8 N3 C12 C13 172.7(5) . . . . ? Co1 N3 C12 C13 -42.5(7) . . . . ? C10 C11 C12 N3 5.2(9) . . . . ? C10 C11 C12 C13 -174.1(6) . . . . ? C8A N3A C12A C11A -4.8(8) . . . . ? Co2 N3A C12A C11A 151.7(5) . . . . ? C8A N3A C12A C13A 171.2(5) . . . . ? Co2 N3A C12A C13A -32.3(8) . . . . ? C10A C11A C12A N3A 3.2(9) . . . . ? C10A C11A C12A C13A -172.7(6) . . . . ? N3 C12 C13 C18 -29.6(8) . . . . ? C11 C12 C13 C18 149.7(6) . . . . ? N3 C12 C13 C14 152.5(5) . . . . ? C11 C12 C13 C14 -28.2(9) . . . . ? N3A C12A C13A C18A -35.9(8) . . . . ? C11A C12A C13A C18A 140.2(6) . . . . ? N3A C12A C13A C14A 148.8(6) . . . . ? C11A C12A C13A C14A -35.1(8) . . . . ? C18 C13 C14 C15 1.6(9) . . . . ? C12 C13 C14 C15 179.5(5) . . . . ? C18A C13A C14A C15A 1.3(9) . . . . ? C12A C13A C14A C15A 176.6(6) . . . . ? C13 C14 C15 C16 0.0(9) . . . . ? C13A C14A C15A C16A -1.5(10) . . . . ? C14 C15 C16 C17 -1.3(9) . . . . ? C14A C15A C16A C17A 1.4(10) . . . . ? C15 C16 C17 C18 1.2(9) . . . . ? C15A C16A C17A C18A -1.1(10) . . . . ? C16 C17 C18 C13 0.4(9) . . . . ? C14 C13 C18 C17 -1.8(8) . . . . ? C12 C13 C18 C17 -179.7(5) . . . . ? C14A C13A C18A C17A -1.0(9) . . . . ? C12A C13A C18A C17A -176.3(5) . . . . ? C16A C17A C18A C13A 0.9(9) . . . . ? C6 N2 C19 C20 -81.0(6) . . . . ? C7 N2 C19 C20 156.1(5) . . . . ? Co1 N2 C19 C20 37.3(5) . . . . ? C7A N2A C19A C20A 158.9(5) . . . . ? C6A N2A C19A C20A -78.1(6) . . . . ? Co2 N2A C19A C20A 40.7(6) . . . . ? C24 N4 C20 C21 0.6(9) . . . . ? Co1 N4 C20 C21 -155.3(5) . . . . ? C24 N4 C20 C19 -174.6(5) . . . . ? Co1 N4 C20 C19 29.4(6) . . . . ? N2 C19 C20 N4 -46.7(7) . . . . ? N2 C19 C20 C21 138.0(6) . . . . ? C24A N4A C20A C21A 0.6(9) . . . . ? Co2 N4A C20A C21A -156.9(5) . . . . ? C24A N4A C20A C19A -177.5(5) . . . . ? Co2 N4A C20A C19A 25.0(6) . . . . ? N2A C19A C20A N4A -46.1(7) . . . . ? N2A C19A C20A C21A 135.9(6) . . . . ? N4 C20 C21 C22 1.2(10) . . . . ? C19 C20 C21 C22 176.1(6) . . . . ? N4A C20A C21A C22A 0.9(10) . . . . ? C19A C20A C21A C22A 178.8(6) . . . . ? C20 C21 C22 C23 -2.0(11) . . . . ? C20A C21A C22A C23A -1.7(10) . . . . ? C21 C22 C23 C24 0.9(11) . . . . ? C21A C22A C23A C24A 1.0(10) . . . . ? C20 N4 C24 C23 -1.7(8) . . . . ? Co1 N4 C24 C23 148.6(5) . . . . ? C20 N4 C24 C25 176.2(5) . . . . ? Co1 N4 C24 C25 -33.5(7) . . . . ? C22 C23 C24 N4 1.0(10) . . . . ? C22 C23 C24 C25 -176.9(6) . . . . ? C20A N4A C24A C23A -1.3(8) . . . . ? Co2 N4A C24A C23A 151.1(5) . . . . ? C20A N4A C24A C25A 173.1(5) . . . . ? Co2 N4A C24A C25A -34.5(7) . . . . ? C22A C23A C24A N4A 0.5(10) . . . . ? C22A C23A C24A C25A -173.9(6) . . . . ? N4 C24 C25 C26 -38.4(8) . . . . ? C23 C24 C25 C26 139.5(6) . . . . ? N4 C24 C25 C30 145.3(6) . . . . ? C23 C24 C25 C30 -36.7(9) . . . . ? N4A C24A C25A C26A -35.7(8) . . . . ? C23A C24A C25A C26A 138.9(6) . . . . ? N4A C24A C25A C30A 148.1(6) . . . . ? C23A C24A C25A C30A -37.4(9) . . . . ? C30 C25 C26 C27 -0.1(9) . . . . ? C24 C25 C26 C27 -176.4(6) . . . . ? C30A C25A C26A C27A 0.8(9) . . . . ? C24A C25A C26A C27A -175.4(6) . . . . ? C25 C26 C27 C28 0.4(10) . . . . ? C25A C26A C27A C28A -0.6(10) . . . . ? C26 C27 C28 C29 0.1(10) . . . . ? C26A C27A C28A C29A 0.0(10) . . . . ? C27 C28 C29 C30 -0.9(11) . . . . ? C27A C28A C29A C30A 0.3(11) . . . . ? C28 C29 C30 C25 1.2(11) . . . . ? C26 C25 C30 C29 -0.6(10) . . . . ? C24 C25 C30 C29 175.6(6) . . . . ? C28A C29A C30A C25A -0.1(11) . . . . ? C26A C25A C30A C29A -0.5(10) . . . . ? C24A C25A C30A C29A 175.7(6) . . . . ? Co1 O1 C31 C38 22.8(7) . . . . ? Co1 O1 C31 C32 -157.3(4) . . . . ? Co2 O1A C31A C38A 16.0(8) . . . . ? Co2 O1A C31A C32A -162.1(4) . . . . ? O1 C31 C32 C33 17.3(8) . . . . ? C38 C31 C32 C33 -162.8(5) . . . . ? O1 C31 C32 C37 -163.0(5) . . . . ? C38 C31 C32 C37 16.9(8) . . . . ? O1A C31A C32A C37A -161.2(6) . . . . ? C38A C31A C32A C37A 20.6(8) . . . . ? O1A C31A C32A C33A 20.3(8) . . . . ? C38A C31A C32A C33A -157.9(5) . . . . ? C37 C32 C33 C34 0.2(9) . . . . ? C31 C32 C33 C34 179.8(5) . . . . ? C37A C32A C33A C34A -1.9(9) . . . . ? C31A C32A C33A C34A 176.7(5) . . . . ? C32 C33 C34 C35 0.7(9) . . . . ? C32A C33A C34A C35A 1.2(9) . . . . ? C33 C34 C35 C36 -0.4(10) . . . . ? C33A C34A C35A C36A 0.5(10) . . . . ? C34 C35 C36 C37 -0.8(10) . . . . ? C34A C35A C36A C37A -1.4(10) . . . . ? C35 C36 C37 C32 1.7(10) . . . . ? C33 C32 C37 C36 -1.4(9) . . . . ? C31 C32 C37 C36 179.0(6) . . . . ? C35A C36A C37A C32A 0.7(10) . . . . ? C33A C32A C37A C36A 0.9(9) . . . . ? C31A C32A C37A C36A -177.6(6) . . . . ? O1 C31 C38 C39 0.5(9) . . . . ? C32 C31 C38 C39 -179.4(5) . . . . ? O1A C31A C38A C39A 2.6(9) . . . . ? C32A C31A C38A C39A -179.3(5) . . . . ? Co1 O2 C39 C38 -12.8(8) . . . . ? Co1 O2 C39 C40 169.2(3) . . . . ? C31 C38 C39 O2 -6.6(9) . . . . ? C31 C38 C39 C40 171.4(5) . . . . ? Co2 O2A C39A C38A -15.5(8) . . . . ? Co2 O2A C39A C40A 168.2(4) . . . . ? C31A C38A C39A O2A -3.0(10) . . . . ? C31A C38A C39A C40A 173.2(5) . . . . ? O2 C39 C40 C41 -159.0(5) . . . . ? C38 C39 C40 C41 22.9(8) . . . . ? O2 C39 C40 C45 22.0(7) . . . . ? C38 C39 C40 C45 -156.1(5) . . . . ? O2A C39A C40A C45A 26.2(8) . . . . ? C38A C39A C40A C45A -150.4(6) . . . . ? O2A C39A C40A C41A -154.7(5) . . . . ? C38A C39A C40A C41A 28.7(8) . . . . ? C45 C40 C41 C42 -0.2(9) . . . . ? C39 C40 C41 C42 -179.2(5) . . . . ? C45A C40A C41A C42A -0.4(9) . . . . ? C39A C40A C41A C42A -179.5(6) . . . . ? C40 C41 C42 C43 1.9(9) . . . . ? C40A C41A C42A C43A 1.1(10) . . . . ? C41 C42 C43 C44 -1.9(10) . . . . ? C41A C42A C43A C44A -0.9(11) . . . . ? C42 C43 C44 C45 0.1(10) . . . . ? C42A C43A C44A C45A 0.0(11) . . . . ? C43 C44 C45 C40 1.6(10) . . . . ? C41 C40 C45 C44 -1.6(9) . . . . ? C39 C40 C45 C44 177.5(6) . . . . ? C43A C44A C45A C40A 0.8(11) . . . . ? C41A C40A C45A C44A -0.6(9) . . . . ? C39A C40A C45A C44A 178.6(6) . . . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 0.475 _refine_diff_density_min -0.586 _refine_diff_density_rms 0.076 #===END data_usu161 #(Compound 10) _database_code_depnum_ccdc_archive 'CCDC 821109' #TrackingRef '- Revised_cifs.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C37 H31 Co N4 O2,Cl O4' _chemical_formula_sum 'C37 H31 Cl Co N4 O6' _chemical_formula_weight 722.04 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 P21/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 11.0736(2) _cell_length_b 24.5657(5) _cell_length_c 12.18640(10) _cell_angle_alpha 90.00 _cell_angle_beta 100.8097(10) _cell_angle_gamma 90.00 _cell_volume 3256.25(9) _cell_formula_units_Z 4 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 39950 _cell_measurement_theta_min 1.018 _cell_measurement_theta_max 27.485 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.473 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1492 _exptl_absorpt_coefficient_mu 0.664 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8008 _exptl_absorpt_correction_T_max 0.9366 _exptl_absorpt_process_details 'DENZO-SMN (Otwinowski & Minor, 1997)' _exptl_special_details ; The program Denzo-SMN (Otwinowski & Minor, 1997) uses a scaling algorithm (Fox & Holmes, 1966) which effectively corrects for absorption effects. High redundancy data were used in the scaling program hence the 'multi-scan' code word was used. No transmission coefficients are available from the program (only scale factors for each frame). The scale factors in the experimental table are calculated from the 'size' command in the SHELXL-97 input file. ; _diffrn_ambient_temperature 150(1) _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 'Nonius KappaCCD Diffractometer' _diffrn_measurement_method 'Phi and Omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14646 _diffrn_reflns_av_R_equivalents 0.0374 _diffrn_reflns_av_sigmaI/netI 0.0503 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 27.48 _reflns_number_total 7451 _reflns_number_gt 5409 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'WinGX, Ortep3' _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 Rfactors 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^)+(0.0362P)^2^+1.7972P] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7451 _refine_ls_number_parameters 566 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0675 _refine_ls_R_factor_gt 0.0385 _refine_ls_wR_factor_ref 0.0924 _refine_ls_wR_factor_gt 0.0811 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _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 0.59581(2) 0.384756(11) 0.22191(2) 0.01980(8) Uani 1 1 d . . . Cl1 Cl 0.92505(5) 0.42836(2) 0.66758(4) 0.02543(13) Uani 1 1 d . . . O1 O 0.42736(13) 0.35559(6) 0.18582(12) 0.0247(3) Uani 1 1 d . . . O2 O 0.52497(13) 0.27659(6) 0.21980(12) 0.0291(4) Uani 1 1 d . . . O3 O 0.79543(14) 0.42822(7) 0.62241(15) 0.0418(4) Uani 1 1 d . . . O4 O 0.95258(16) 0.38593(7) 0.74934(14) 0.0419(4) Uani 1 1 d . . . O5 O 0.95965(15) 0.47986(7) 0.72062(15) 0.0430(4) Uani 1 1 d . . . O6 O 0.99272(16) 0.41919(8) 0.57984(14) 0.0442(5) Uani 1 1 d . . . N1 N 0.66171(16) 0.36249(7) 0.07645(14) 0.0233(4) Uani 1 1 d . . . N2 N 0.78884(15) 0.40797(7) 0.26175(14) 0.0233(4) Uani 1 1 d . . . N3 N 0.58651(15) 0.47081(7) 0.22934(13) 0.0206(4) Uani 1 1 d . . . N4 N 0.65852(16) 0.35587(7) 0.38887(14) 0.0221(4) Uani 1 1 d . . . C1 C 0.6000(2) 0.33088(9) -0.00550(18) 0.0264(5) Uani 1 1 d . . . C2 C 0.6455(2) 0.31756(10) -0.10004(19) 0.0297(5) Uani 1 1 d . . . C3 C 0.7591(2) 0.33810(10) -0.1109(2) 0.0321(5) Uani 1 1 d . . . C4 C 0.8234(2) 0.37032(10) -0.02772(19) 0.0300(5) Uani 1 1 d . . . C5 C 0.77248(19) 0.38213(9) 0.06545(18) 0.0241(5) Uani 1 1 d . . . C6 C 0.8336(2) 0.41934(10) 0.15733(19) 0.0284(5) Uani 1 1 d . . . C7 C 0.7955(2) 0.45707(10) 0.33280(19) 0.0268(5) Uani 1 1 d . . . C8 C 0.68775(19) 0.49372(9) 0.29194(16) 0.0235(5) Uani 1 1 d . . . C9 C 0.6922(2) 0.54766(10) 0.32395(19) 0.0310(5) Uani 1 1 d . . . C10 C 0.5868(2) 0.57870(10) 0.2984(2) 0.0341(6) Uani 1 1 d . . . C11 C 0.4831(2) 0.55596(10) 0.2348(2) 0.0304(5) Uani 1 1 d . . . C12 C 0.48518(19) 0.50254(9) 0.19779(17) 0.0230(5) Uani 1 1 d . . . C13 C 0.37795(19) 0.47945(9) 0.12033(17) 0.0236(5) Uani 1 1 d . . . C14 C 0.2583(2) 0.49057(10) 0.1356(2) 0.0296(5) Uani 1 1 d . . . C15 C 0.1589(2) 0.47005(11) 0.0624(2) 0.0362(6) Uani 1 1 d . . . C16 C 0.1755(2) 0.43832(11) -0.0271(2) 0.0366(6) Uani 1 1 d . . . C17 C 0.2938(2) 0.42703(10) -0.04338(19) 0.0311(5) Uani 1 1 d . . . C18 C 0.3945(2) 0.44781(9) 0.02973(17) 0.0242(5) Uani 1 1 d . . . C19 C 0.8513(2) 0.36117(11) 0.3227(2) 0.0294(5) Uani 1 1 d . . . C20 C 0.77689(19) 0.34016(9) 0.40607(17) 0.0249(5) Uani 1 1 d . . . C21 C 0.8286(2) 0.30667(10) 0.49332(19) 0.0312(5) Uani 1 1 d . . . C22 C 0.7550(2) 0.28887(10) 0.5658(2) 0.0332(6) Uani 1 1 d . . . C23 C 0.6354(2) 0.30602(9) 0.55187(19) 0.0292(5) Uani 1 1 d . . . C24 C 0.58855(19) 0.34031(9) 0.46303(17) 0.0238(5) Uani 1 1 d . . . C25 C 0.4621(2) 0.36228(10) 0.44788(17) 0.0270(5) Uani 1 1 d . . . C26 C 0.4403(2) 0.41693(11) 0.42282(19) 0.0332(6) Uani 1 1 d . . . C27 C 0.3216(3) 0.43793(13) 0.4071(2) 0.0430(7) Uani 1 1 d . . . C28 C 0.2244(3) 0.40408(15) 0.4174(2) 0.0488(8) Uani 1 1 d . . . C29 C 0.2449(3) 0.35065(15) 0.4447(2) 0.0489(8) Uani 1 1 d . . . C30 C 0.3633(2) 0.32890(12) 0.46125(19) 0.0354(6) Uani 1 1 d . . . C31 C 0.42935(19) 0.30410(9) 0.20129(16) 0.0215(4) Uani 1 1 d . . . C32 C 0.30584(19) 0.27771(9) 0.19890(17) 0.0232(5) Uani 1 1 d . . . C33 C 0.1981(2) 0.30623(10) 0.1598(2) 0.0322(5) Uani 1 1 d . . . C34 C 0.0853(2) 0.28221(11) 0.1631(2) 0.0399(6) Uani 1 1 d . . . C35 C 0.0803(2) 0.23032(11) 0.2059(2) 0.0398(6) Uani 1 1 d . . . C36 C 0.1870(2) 0.20159(11) 0.2440(2) 0.0417(7) Uani 1 1 d . . . C37 C 0.3000(2) 0.22517(10) 0.2399(2) 0.0343(6) Uani 1 1 d . . . H1 H 0.519(2) 0.3189(9) 0.0055(18) 0.029(6) Uiso 1 1 d . . . H2 H 0.601(2) 0.2942(9) -0.1531(18) 0.024(6) Uiso 1 1 d . . . H3 H 0.792(2) 0.3300(10) -0.176(2) 0.043(7) Uiso 1 1 d . . . H4 H 0.899(2) 0.3859(9) -0.0333(19) 0.030(6) Uiso 1 1 d . . . H6A H 0.922(2) 0.4157(10) 0.1695(19) 0.035(7) Uiso 1 1 d . . . H6B H 0.810(2) 0.4585(10) 0.1357(18) 0.029(6) Uiso 1 1 d . . . H7A H 0.792(2) 0.4443(9) 0.410(2) 0.028(6) Uiso 1 1 d . . . H7B H 0.875(2) 0.4769(10) 0.3350(19) 0.034(7) Uiso 1 1 d . . . H8 H 0.761(2) 0.5617(10) 0.365(2) 0.031(7) Uiso 1 1 d . . . H9 H 0.588(2) 0.6156(10) 0.322(2) 0.036(7) Uiso 1 1 d . . . H11 H 0.414(2) 0.5756(10) 0.214(2) 0.032(7) Uiso 1 1 d . . . H14 H 0.249(2) 0.5139(10) 0.196(2) 0.037(7) Uiso 1 1 d . . . H15 H 0.075(2) 0.4782(10) 0.073(2) 0.040(7) Uiso 1 1 d . . . H16 H 0.112(2) 0.4236(10) -0.078(2) 0.043(8) Uiso 1 1 d . . . H17 H 0.311(2) 0.4065(11) -0.103(2) 0.040(7) Uiso 1 1 d . . . H18 H 0.478(2) 0.4397(9) 0.018(2) 0.035(7) Uiso 1 1 d . . . H19A H 0.858(2) 0.3304(10) 0.2691(19) 0.032(6) Uiso 1 1 d . . . H19B H 0.931(2) 0.3714(9) 0.3604(19) 0.030(6) Uiso 1 1 d . . . H21 H 0.910(2) 0.2967(9) 0.5009(18) 0.028(6) Uiso 1 1 d . . . H22 H 0.787(2) 0.2645(9) 0.625(2) 0.030(6) Uiso 1 1 d . . . H23 H 0.584(2) 0.2961(9) 0.5990(19) 0.027(6) Uiso 1 1 d . . . H26 H 0.505(2) 0.4409(10) 0.4155(19) 0.032(7) Uiso 1 1 d . . . H27 H 0.308(2) 0.4743(11) 0.392(2) 0.040(8) Uiso 1 1 d . . . H28 H 0.142(3) 0.4211(12) 0.406(3) 0.065(9) Uiso 1 1 d . . . H29 H 0.184(3) 0.3276(11) 0.455(2) 0.049(8) Uiso 1 1 d . . . H30 H 0.379(2) 0.2903(11) 0.4794(19) 0.033(7) Uiso 1 1 d . . . H33 H 0.200(2) 0.3438(10) 0.132(2) 0.037(7) Uiso 1 1 d . . . H34 H 0.012(3) 0.3015(12) 0.137(2) 0.060(9) Uiso 1 1 d . . . H35 H 0.003(3) 0.2153(11) 0.211(2) 0.050(8) Uiso 1 1 d . . . H36 H 0.183(3) 0.1648(13) 0.273(2) 0.065(9) Uiso 1 1 d . . . H37 H 0.378(3) 0.2057(12) 0.265(2) 0.056(8) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.01650(14) 0.02295(16) 0.02008(15) 0.00074(12) 0.00381(10) -0.00210(12) Cl1 0.0204(3) 0.0294(3) 0.0275(3) -0.0027(2) 0.0070(2) -0.0012(2) O1 0.0222(8) 0.0251(8) 0.0268(8) 0.0031(6) 0.0043(6) -0.0043(6) O2 0.0227(8) 0.0332(9) 0.0321(9) 0.0005(7) 0.0069(7) 0.0040(7) O3 0.0189(8) 0.0459(11) 0.0577(11) -0.0104(9) 0.0000(8) 0.0030(8) O4 0.0467(11) 0.0422(11) 0.0371(10) 0.0106(8) 0.0084(8) 0.0045(9) O5 0.0369(10) 0.0361(10) 0.0588(12) -0.0164(9) 0.0159(9) -0.0118(8) O6 0.0377(10) 0.0685(13) 0.0308(9) -0.0089(9) 0.0176(8) -0.0056(9) N1 0.0213(9) 0.0244(10) 0.0248(9) 0.0026(8) 0.0060(7) 0.0003(8) N2 0.0190(9) 0.0294(10) 0.0215(9) 0.0022(8) 0.0037(7) -0.0046(8) N3 0.0218(9) 0.0231(9) 0.0175(8) 0.0011(7) 0.0052(7) -0.0031(8) N4 0.0210(9) 0.0253(10) 0.0193(9) -0.0006(7) 0.0015(7) -0.0039(8) C1 0.0267(12) 0.0247(12) 0.0286(12) 0.0014(9) 0.0071(10) 0.0007(10) C2 0.0376(14) 0.0275(13) 0.0241(12) -0.0017(10) 0.0062(10) 0.0024(11) C3 0.0365(14) 0.0345(14) 0.0284(13) 0.0011(10) 0.0143(10) 0.0062(11) C4 0.0273(13) 0.0348(14) 0.0311(13) 0.0056(10) 0.0134(10) 0.0007(10) C5 0.0216(11) 0.0255(12) 0.0262(11) 0.0054(9) 0.0070(9) 0.0008(9) C6 0.0220(12) 0.0369(15) 0.0278(12) 0.0036(10) 0.0089(9) -0.0044(10) C7 0.0216(12) 0.0344(13) 0.0234(12) -0.0011(10) 0.0016(9) -0.0099(10) C8 0.0273(12) 0.0283(12) 0.0164(10) -0.0013(9) 0.0081(9) -0.0087(9) C9 0.0374(14) 0.0338(14) 0.0221(11) -0.0053(10) 0.0063(10) -0.0116(11) C10 0.0520(16) 0.0250(13) 0.0287(12) -0.0064(10) 0.0164(11) -0.0077(12) C11 0.0355(14) 0.0278(13) 0.0302(13) 0.0007(10) 0.0120(10) 0.0038(11) C12 0.0264(12) 0.0255(11) 0.0190(10) 0.0019(9) 0.0090(9) -0.0025(9) C13 0.0238(11) 0.0246(12) 0.0222(11) 0.0068(9) 0.0037(9) 0.0022(9) C14 0.0272(12) 0.0334(13) 0.0286(12) 0.0078(10) 0.0067(10) 0.0068(10) C15 0.0232(13) 0.0480(16) 0.0370(14) 0.0160(12) 0.0046(11) 0.0045(11) C16 0.0278(13) 0.0514(17) 0.0269(13) 0.0131(12) -0.0044(10) -0.0105(12) C17 0.0351(14) 0.0358(14) 0.0215(12) 0.0045(10) 0.0029(10) -0.0044(11) C18 0.0240(12) 0.0271(12) 0.0213(11) 0.0060(9) 0.0039(9) -0.0003(9) C19 0.0160(11) 0.0369(14) 0.0338(13) 0.0037(11) 0.0006(10) 0.0009(10) C20 0.0223(11) 0.0274(12) 0.0232(11) -0.0025(9) -0.0001(9) -0.0026(9) C21 0.0261(13) 0.0310(13) 0.0330(13) 0.0003(10) -0.0035(10) 0.0020(10) C22 0.0403(15) 0.0279(13) 0.0277(13) 0.0070(10) -0.0032(11) -0.0031(11) C23 0.0369(14) 0.0260(12) 0.0243(12) 0.0004(9) 0.0042(10) -0.0099(10) C24 0.0270(12) 0.0224(11) 0.0216(11) -0.0019(9) 0.0038(9) -0.0066(9) C25 0.0278(12) 0.0390(13) 0.0151(10) 0.0000(9) 0.0066(9) -0.0026(10) C26 0.0348(14) 0.0460(16) 0.0218(12) 0.0063(11) 0.0131(10) 0.0070(12) C27 0.0454(17) 0.061(2) 0.0251(13) 0.0063(13) 0.0120(11) 0.0209(15) C28 0.0314(15) 0.084(2) 0.0296(14) -0.0112(15) 0.0035(11) 0.0109(16) C29 0.0282(15) 0.082(2) 0.0385(15) -0.0205(15) 0.0114(12) -0.0165(16) C30 0.0315(14) 0.0497(17) 0.0263(12) -0.0081(12) 0.0086(10) -0.0112(12) C31 0.0220(11) 0.0261(12) 0.0157(10) -0.0017(8) 0.0022(8) -0.0003(9) C32 0.0234(11) 0.0229(11) 0.0229(11) -0.0041(9) 0.0030(9) -0.0028(9) C33 0.0261(12) 0.0293(14) 0.0396(14) 0.0057(11) 0.0023(10) -0.0013(10) C34 0.0210(13) 0.0436(16) 0.0523(16) 0.0085(13) -0.0005(11) -0.0004(11) C35 0.0251(14) 0.0461(16) 0.0461(15) 0.0090(12) 0.0014(11) -0.0133(12) C36 0.0318(14) 0.0345(15) 0.0558(17) 0.0126(13) 0.0003(12) -0.0106(12) C37 0.0274(13) 0.0296(13) 0.0435(14) 0.0053(11) 0.0003(11) -0.0019(11) _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 1.9695(14) . ? Co1 N1 2.1117(17) . ? Co1 N3 2.1192(18) . ? Co1 N4 2.1437(17) . ? Co1 N2 2.1773(17) . ? Cl1 O6 1.4339(16) . ? Cl1 O4 1.4346(17) . ? Cl1 O3 1.4376(16) . ? Cl1 O5 1.4396(17) . ? O1 C31 1.278(3) . ? O2 C31 1.241(2) . ? N1 C1 1.346(3) . ? N1 C5 1.348(3) . ? N2 C19 1.469(3) . ? N2 C6 1.476(3) . ? N2 C7 1.478(3) . ? N3 C8 1.355(3) . ? N3 C12 1.361(3) . ? N4 C20 1.345(3) . ? N4 C24 1.351(3) . ? C1 C2 1.381(3) . ? C1 H1 0.98(2) . ? C2 C3 1.384(3) . ? C2 H2 0.93(2) . ? C3 C4 1.375(3) . ? C3 H3 0.96(3) . ? C4 C5 1.390(3) . ? C4 H4 0.94(2) . ? C5 C6 1.504(3) . ? C6 H6A 0.97(2) . ? C6 H6B 1.02(2) . ? C7 C8 1.504(3) . ? C7 H7A 1.00(2) . ? C7 H7B 1.00(2) . ? C8 C9 1.380(3) . ? C9 C10 1.380(4) . ? C9 H8 0.90(2) . ? C10 C11 1.378(4) . ? C10 H9 0.95(2) . ? C11 C12 1.389(3) . ? C11 H11 0.90(2) . ? C12 C13 1.484(3) . ? C13 C18 1.390(3) . ? C13 C14 1.399(3) . ? C14 C15 1.376(3) . ? C14 H14 0.95(2) . ? C15 C16 1.381(4) . ? C15 H15 0.98(2) . ? C16 C17 1.390(3) . ? C16 H16 0.92(3) . ? C17 C18 1.388(3) . ? C17 H17 0.93(3) . ? C18 H18 0.99(2) . ? C19 C20 1.514(3) . ? C19 H19A 1.01(2) . ? C19 H19B 0.95(2) . ? C20 C21 1.381(3) . ? C21 C22 1.381(3) . ? C21 H21 0.92(2) . ? C22 C23 1.370(3) . ? C22 H22 0.95(2) . ? C23 C24 1.393(3) . ? C23 H23 0.92(2) . ? C24 C25 1.480(3) . ? C25 C26 1.388(3) . ? C25 C30 1.401(3) . ? C26 C27 1.392(4) . ? C26 H26 0.95(2) . ? C27 C28 1.384(4) . ? C27 H27 0.92(3) . ? C28 C29 1.362(5) . ? C28 H28 0.99(3) . ? C29 C30 1.396(4) . ? C29 H29 0.91(3) . ? C30 H30 0.98(2) . ? C31 C32 1.509(3) . ? C32 C33 1.388(3) . ? C32 C37 1.390(3) . ? C33 C34 1.389(3) . ? C33 H33 0.99(3) . ? C34 C35 1.382(4) . ? C34 H34 0.94(3) . ? C35 C36 1.380(4) . ? C35 H35 0.95(3) . ? C36 C37 1.388(3) . ? C36 H36 0.97(3) . ? C37 H37 0.98(3) . ? 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 100.38(6) . . ? O1 Co1 N3 108.72(6) . . ? N1 Co1 N3 108.75(6) . . ? O1 Co1 N4 102.48(6) . . ? N1 Co1 N4 127.56(7) . . ? N3 Co1 N4 107.42(6) . . ? O1 Co1 N2 173.83(7) . . ? N1 Co1 N2 77.04(7) . . ? N3 Co1 N2 77.45(7) . . ? N4 Co1 N2 75.25(6) . . ? O6 Cl1 O4 109.33(11) . . ? O6 Cl1 O3 109.76(11) . . ? O4 Cl1 O3 109.33(11) . . ? O6 Cl1 O5 109.91(11) . . ? O4 Cl1 O5 108.82(11) . . ? O3 Cl1 O5 109.66(10) . . ? C31 O1 Co1 109.73(13) . . ? C1 N1 C5 118.51(18) . . ? C1 N1 Co1 124.42(14) . . ? C5 N1 Co1 117.06(14) . . ? C19 N2 C6 112.42(18) . . ? C19 N2 C7 112.03(17) . . ? C6 N2 C7 111.25(18) . . ? C19 N2 Co1 104.91(13) . . ? C6 N2 Co1 109.36(13) . . ? C7 N2 Co1 106.47(13) . . ? C8 N3 C12 118.19(19) . . ? C8 N3 Co1 113.38(14) . . ? C12 N3 Co1 127.11(14) . . ? C20 N4 C24 118.62(18) . . ? C20 N4 Co1 112.07(13) . . ? C24 N4 Co1 127.16(14) . . ? N1 C1 C2 122.8(2) . . ? N1 C1 H1 115.0(13) . . ? C2 C1 H1 122.1(13) . . ? C1 C2 C3 118.3(2) . . ? C1 C2 H2 119.9(14) . . ? C3 C2 H2 121.8(13) . . ? C4 C3 C2 119.6(2) . . ? C4 C3 H3 120.4(15) . . ? C2 C3 H3 120.0(15) . . ? C3 C4 C5 119.3(2) . . ? C3 C4 H4 122.0(14) . . ? C5 C4 H4 118.7(14) . . ? N1 C5 C4 121.5(2) . . ? N1 C5 C6 115.73(18) . . ? C4 C5 C6 122.7(2) . . ? N2 C6 C5 110.48(18) . . ? N2 C6 H6A 110.2(14) . . ? C5 C6 H6A 111.1(14) . . ? N2 C6 H6B 106.8(12) . . ? C5 C6 H6B 108.8(13) . . ? H6A C6 H6B 109.4(19) . . ? N2 C7 C8 110.19(17) . . ? N2 C7 H7A 106.9(13) . . ? C8 C7 H7A 109.2(13) . . ? N2 C7 H7B 111.2(13) . . ? C8 C7 H7B 110.8(14) . . ? H7A C7 H7B 108.4(18) . . ? N3 C8 C9 122.7(2) . . ? N3 C8 C7 117.35(19) . . ? C9 C8 C7 119.8(2) . . ? C8 C9 C10 118.9(2) . . ? C8 C9 H8 120.6(16) . . ? C10 C9 H8 120.4(15) . . ? C11 C10 C9 118.9(2) . . ? C11 C10 H9 121.5(15) . . ? C9 C10 H9 119.6(15) . . ? C10 C11 C12 120.2(2) . . ? C10 C11 H11 121.0(16) . . ? C12 C11 H11 118.8(16) . . ? N3 C12 C11 120.8(2) . . ? N3 C12 C13 118.65(19) . . ? C11 C12 C13 120.5(2) . . ? C18 C13 C14 119.0(2) . . ? C18 C13 C12 120.65(19) . . ? C14 C13 C12 120.4(2) . . ? C15 C14 C13 120.3(2) . . ? C15 C14 H14 122.3(15) . . ? C13 C14 H14 117.4(15) . . ? C14 C15 C16 120.7(2) . . ? C14 C15 H15 120.0(14) . . ? C16 C15 H15 119.3(14) . . ? C15 C16 C17 119.6(2) . . ? C15 C16 H16 123.6(16) . . ? C17 C16 H16 116.8(16) . . ? C18 C17 C16 120.0(2) . . ? C18 C17 H17 116.5(16) . . ? C16 C17 H17 123.4(16) . . ? C17 C18 C13 120.4(2) . . ? C17 C18 H18 119.9(14) . . ? C13 C18 H18 119.7(14) . . ? N2 C19 C20 110.00(18) . . ? N2 C19 H19A 110.1(13) . . ? C20 C19 H19A 107.1(13) . . ? N2 C19 H19B 110.2(14) . . ? C20 C19 H19B 109.9(14) . . ? H19A C19 H19B 109.5(19) . . ? N4 C20 C21 122.9(2) . . ? N4 C20 C19 115.78(18) . . ? C21 C20 C19 121.4(2) . . ? C22 C21 C20 118.2(2) . . ? C22 C21 H21 122.4(14) . . ? C20 C21 H21 119.4(14) . . ? C23 C22 C21 119.8(2) . . ? C23 C22 H22 120.3(14) . . ? C21 C22 H22 119.9(14) . . ? C22 C23 C24 119.5(2) . . ? C22 C23 H23 122.9(14) . . ? C24 C23 H23 117.6(14) . . ? N4 C24 C23 121.0(2) . . ? N4 C24 C25 117.48(18) . . ? C23 C24 C25 121.55(19) . . ? C26 C25 C30 119.0(2) . . ? C26 C25 C24 120.1(2) . . ? C30 C25 C24 120.9(2) . . ? C25 C26 C27 120.6(3) . . ? C25 C26 H26 121.3(15) . . ? C27 C26 H26 118.1(15) . . ? C28 C27 C26 119.7(3) . . ? C28 C27 H27 120.2(17) . . ? C26 C27 H27 120.1(17) . . ? C29 C28 C27 120.3(3) . . ? C29 C28 H28 123.1(18) . . ? C27 C28 H28 116.6(18) . . ? C28 C29 C30 120.8(3) . . ? C28 C29 H29 122.6(18) . . ? C30 C29 H29 116.5(18) . . ? C29 C30 C25 119.5(3) . . ? C29 C30 H30 121.9(14) . . ? C25 C30 H30 118.5(14) . . ? O2 C31 O1 123.8(2) . . ? O2 C31 C32 120.60(19) . . ? O1 C31 C32 115.58(18) . . ? C33 C32 C37 119.8(2) . . ? C33 C32 C31 120.5(2) . . ? C37 C32 C31 119.7(2) . . ? C32 C33 C34 119.7(2) . . ? C32 C33 H33 121.5(14) . . ? C34 C33 H33 118.8(14) . . ? C35 C34 C33 120.2(2) . . ? C35 C34 H34 120.1(18) . . ? C33 C34 H34 119.7(18) . . ? C36 C35 C34 120.4(2) . . ? C36 C35 H35 120.6(17) . . ? C34 C35 H35 119.0(17) . . ? C35 C36 C37 119.7(2) . . ? C35 C36 H36 120.4(18) . . ? C37 C36 H36 119.9(18) . . ? C36 C37 C32 120.3(2) . . ? C36 C37 H37 121.7(17) . . ? C32 C37 H37 118.0(17) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Co1 O1 C31 78.00(13) . . . . ? N3 Co1 O1 C31 -167.97(12) . . . . ? N4 Co1 O1 C31 -54.48(14) . . . . ? N2 Co1 O1 C31 13.3(6) . . . . ? O1 Co1 N1 C1 -7.12(18) . . . . ? N3 Co1 N1 C1 -121.11(17) . . . . ? N4 Co1 N1 C1 107.60(18) . . . . ? N2 Co1 N1 C1 167.16(18) . . . . ? O1 Co1 N1 C5 172.02(15) . . . . ? N3 Co1 N1 C5 58.02(16) . . . . ? N4 Co1 N1 C5 -73.27(17) . . . . ? N2 Co1 N1 C5 -13.71(15) . . . . ? O1 Co1 N2 C19 -28.7(6) . . . . ? N1 Co1 N2 C19 -94.59(14) . . . . ? N3 Co1 N2 C19 152.51(14) . . . . ? N4 Co1 N2 C19 40.44(13) . . . . ? O1 Co1 N2 C6 92.1(6) . . . . ? N1 Co1 N2 C6 26.20(15) . . . . ? N3 Co1 N2 C6 -86.70(15) . . . . ? N4 Co1 N2 C6 161.23(16) . . . . ? O1 Co1 N2 C7 -147.6(5) . . . . ? N1 Co1 N2 C7 146.50(14) . . . . ? N3 Co1 N2 C7 33.60(13) . . . . ? N4 Co1 N2 C7 -78.47(13) . . . . ? O1 Co1 N3 C8 156.76(13) . . . . ? N1 Co1 N3 C8 -94.82(14) . . . . ? N4 Co1 N3 C8 46.55(14) . . . . ? N2 Co1 N3 C8 -23.38(13) . . . . ? O1 Co1 N3 C12 -9.76(17) . . . . ? N1 Co1 N3 C12 98.66(16) . . . . ? N4 Co1 N3 C12 -119.98(15) . . . . ? N2 Co1 N3 C12 170.10(16) . . . . ? O1 Co1 N4 C20 141.08(14) . . . . ? N1 Co1 N4 C20 27.31(18) . . . . ? N3 Co1 N4 C20 -104.47(15) . . . . ? N2 Co1 N4 C20 -33.02(14) . . . . ? O1 Co1 N4 C24 -21.88(18) . . . . ? N1 Co1 N4 C24 -135.65(17) . . . . ? N3 Co1 N4 C24 92.57(18) . . . . ? N2 Co1 N4 C24 164.02(19) . . . . ? C5 N1 C1 C2 0.3(3) . . . . ? Co1 N1 C1 C2 179.38(16) . . . . ? N1 C1 C2 C3 -0.5(3) . . . . ? C1 C2 C3 C4 0.8(4) . . . . ? C2 C3 C4 C5 -0.7(4) . . . . ? C1 N1 C5 C4 -0.2(3) . . . . ? Co1 N1 C5 C4 -179.35(16) . . . . ? C1 N1 C5 C6 177.15(19) . . . . ? Co1 N1 C5 C6 -2.0(2) . . . . ? C3 C4 C5 N1 0.4(3) . . . . ? C3 C4 C5 C6 -176.7(2) . . . . ? C19 N2 C6 C5 81.4(2) . . . . ? C7 N2 C6 C5 -152.01(19) . . . . ? Co1 N2 C6 C5 -34.7(2) . . . . ? N1 C5 C6 N2 25.1(3) . . . . ? C4 C5 C6 N2 -157.6(2) . . . . ? C19 N2 C7 C8 -153.08(17) . . . . ? C6 N2 C7 C8 80.1(2) . . . . ? Co1 N2 C7 C8 -38.94(19) . . . . ? C12 N3 C8 C9 -0.5(3) . . . . ? Co1 N3 C8 C9 -168.29(16) . . . . ? C12 N3 C8 C7 175.74(17) . . . . ? Co1 N3 C8 C7 7.9(2) . . . . ? N2 C7 C8 N3 22.0(3) . . . . ? N2 C7 C8 C9 -161.64(19) . . . . ? N3 C8 C9 C10 4.9(3) . . . . ? C7 C8 C9 C10 -171.3(2) . . . . ? C8 C9 C10 C11 -4.6(3) . . . . ? C9 C10 C11 C12 0.3(3) . . . . ? C8 N3 C12 C11 -4.1(3) . . . . ? Co1 N3 C12 C11 161.88(16) . . . . ? C8 N3 C12 C13 174.23(18) . . . . ? Co1 N3 C12 C13 -19.8(2) . . . . ? C10 C11 C12 N3 4.2(3) . . . . ? C10 C11 C12 C13 -174.1(2) . . . . ? N3 C12 C13 C18 -41.6(3) . . . . ? C11 C12 C13 C18 136.7(2) . . . . ? N3 C12 C13 C14 140.3(2) . . . . ? C11 C12 C13 C14 -41.4(3) . . . . ? C18 C13 C14 C15 0.5(3) . . . . ? C12 C13 C14 C15 178.7(2) . . . . ? C13 C14 C15 C16 -0.1(4) . . . . ? C14 C15 C16 C17 -0.1(4) . . . . ? C15 C16 C17 C18 -0.3(4) . . . . ? C16 C17 C18 C13 0.8(3) . . . . ? C14 C13 C18 C17 -0.9(3) . . . . ? C12 C13 C18 C17 -179.0(2) . . . . ? C6 N2 C19 C20 -161.86(18) . . . . ? C7 N2 C19 C20 72.0(2) . . . . ? Co1 N2 C19 C20 -43.1(2) . . . . ? C24 N4 C20 C21 3.2(3) . . . . ? Co1 N4 C20 C21 -161.42(18) . . . . ? C24 N4 C20 C19 -177.30(19) . . . . ? Co1 N4 C20 C19 18.1(2) . . . . ? N2 C19 C20 N4 18.0(3) . . . . ? N2 C19 C20 C21 -162.5(2) . . . . ? N4 C20 C21 C22 -0.2(3) . . . . ? C19 C20 C21 C22 -179.7(2) . . . . ? C20 C21 C22 C23 -2.1(4) . . . . ? C21 C22 C23 C24 1.5(3) . . . . ? C20 N4 C24 C23 -3.8(3) . . . . ? Co1 N4 C24 C23 158.15(16) . . . . ? C20 N4 C24 C25 174.54(19) . . . . ? Co1 N4 C24 C25 -23.5(3) . . . . ? C22 C23 C24 N4 1.6(3) . . . . ? C22 C23 C24 C25 -176.7(2) . . . . ? N4 C24 C25 C26 -43.8(3) . . . . ? C23 C24 C25 C26 134.6(2) . . . . ? N4 C24 C25 C30 137.9(2) . . . . ? C23 C24 C25 C30 -43.8(3) . . . . ? C30 C25 C26 C27 -2.4(3) . . . . ? C24 C25 C26 C27 179.3(2) . . . . ? C25 C26 C27 C28 0.5(4) . . . . ? C26 C27 C28 C29 1.1(4) . . . . ? C27 C28 C29 C30 -0.9(4) . . . . ? C28 C29 C30 C25 -1.0(4) . . . . ? C26 C25 C30 C29 2.6(3) . . . . ? C24 C25 C30 C29 -179.0(2) . . . . ? Co1 O1 C31 O2 -9.9(2) . . . . ? Co1 O1 C31 C32 168.50(13) . . . . ? O2 C31 C32 C33 -169.0(2) . . . . ? O1 C31 C32 C33 12.6(3) . . . . ? O2 C31 C32 C37 13.4(3) . . . . ? O1 C31 C32 C37 -165.1(2) . . . . ? C37 C32 C33 C34 0.7(4) . . . . ? C31 C32 C33 C34 -176.9(2) . . . . ? C32 C33 C34 C35 0.5(4) . . . . ? C33 C34 C35 C36 -1.0(4) . . . . ? C34 C35 C36 C37 0.4(4) . . . . ? C35 C36 C37 C32 0.8(4) . . . . ? C33 C32 C37 C36 -1.3(4) . . . . ? C31 C32 C37 C36 176.3(2) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.337 _refine_diff_density_min -0.512 _refine_diff_density_rms 0.062