#Supplementary Material for Dalton Transactions #This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_email 'smitra 2002@yahoo.com' _publ_section_title ; Isolation of Four New CoII/CoIII and NiII Complexes with a Pentadentate Schiff Base Ligand: Syntheses, Structural Descriptions and Magnetic Studies ; _publ_contact_author_name 'Prof. Samiran Mitra' loop_ _publ_author_name S.Mitra S.Banerjee M.Nandy S.Sen G.Rosair A.Slawin C.G.Garcia ; E.Zangrando ; data_687036 _database_code_depnum_ccdc_archive 'CCDC 687036' #TrackingRef 'complex-1-CCDC-687036-.cif.cif' # start Validation Reply Form _vrf_PLAT029_687036 ; PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.93 RESPONSE: Poor quality crystals - several tried - best result presented. ; _vrf_PLAT601_687036 ; PROBLEM: Structure Contains Solvent Accessible VOIDS of . 227.00 A**3 RESPONSE: no ordered solvent discernible. ; _vrf_PLAT731_687036 ; PROBLEM: Bond Calc 0.98(5), Rep 0.9800(11) ...... 9.90 su-Ra RESPONSE: DFIX instruction in SHELXL. ; _vrf_PLAT735_687036 ; PROBLEM: D-H Calc 0.98(5), Rep 0.9800(11) ...... 9.90 su-Ra RESPONSE: DFIX instruction in SHELXL. ; # end Validation _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H38 Co2 N4 O6.H2 O' _chemical_formula_sum 'C38 H40 Co2 N4 O7' _chemical_formula_weight 782.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.035(3) _cell_length_b 13.078(4) _cell_length_c 14.492(5) _cell_angle_alpha 90.443(14) _cell_angle_beta 100.661(12) _cell_angle_gamma 105.340(11) _cell_volume 1799.2(10) _cell_formula_units_Z 2 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 2255 _cell_measurement_theta_min 1.42 _cell_measurement_theta_max 20.85 _exptl_crystal_description platelet _exptl_crystal_colour orange _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.010 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.445 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 812 _exptl_absorpt_coefficient_mu 0.977 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8693 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type CCD _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9415 _diffrn_reflns_av_R_equivalents 0.0798 _diffrn_reflns_av_sigmaI/netI 0.1186 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 4.75 _diffrn_reflns_theta_max 25.35 _reflns_number_total 6006 _reflns_number_gt 4231 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2004)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2004)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The hydrogen atoms on the water molecule were refined with riding thermal parameters and a distance constraint.Poor quality crystals - several tried - best result presented. The poor quality of crystal leads to a poor Rint and a low completeness due to poor diffraction. ; _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^)+(0.0184P)^2^+9.8071P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6006 _refine_ls_number_parameters 471 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1533 _refine_ls_R_factor_gt 0.1032 _refine_ls_wR_factor_ref 0.1650 _refine_ls_wR_factor_gt 0.1486 _refine_ls_goodness_of_fit_ref 1.159 _refine_ls_restrained_S_all 1.159 _refine_ls_shift/su_max 0.013 _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 0.27233(11) 0.34767(7) 0.11971(7) 0.0184(3) Uani 1 1 d . . . Co2 Co 0.41369(11) 0.14239(7) 0.22312(7) 0.0187(3) Uani 1 1 d . . . C1 C 0.0978(8) 0.3048(6) -0.0572(5) 0.0217(17) Uani 1 1 d . . . C2 C 0.0864(8) 0.4100(6) -0.0611(5) 0.0236(17) Uani 1 1 d . . . C3 C -0.0210(8) 0.4322(6) -0.1263(6) 0.0281(19) Uani 1 1 d . . . H3A H -0.0272 0.5033 -0.1299 0.034 Uiso 1 1 calc R . . C4 C -0.1200(9) 0.3528(6) -0.1865(6) 0.032(2) Uani 1 1 d . . . H4A H -0.1958 0.3685 -0.2284 0.038 Uiso 1 1 calc R . . C5 C -0.1047(8) 0.2507(6) -0.1837(5) 0.0289(19) Uani 1 1 d . . . H5A H -0.1696 0.1957 -0.2251 0.035 Uiso 1 1 calc R . . C6 C 0.0024(8) 0.2284(6) -0.1220(5) 0.0270(19) Uani 1 1 d . . . H6A H 0.0126 0.1583 -0.1233 0.032 Uiso 1 1 calc R . . C7 C 0.1996(8) 0.4967(5) -0.0097(5) 0.0215(17) Uani 1 1 d . . . N8 N 0.2858(6) 0.4781(4) 0.0611(4) 0.0221(14) Uani 1 1 d . . . C9 C 0.4268(8) 0.5511(5) 0.0953(5) 0.0225(17) Uani 1 1 d . . . H9A H 0.4215 0.6075 0.1394 0.027 Uiso 1 1 calc R . . H9B H 0.4672 0.5848 0.0421 0.027 Uiso 1 1 calc R . . C10 C 0.5176(8) 0.4823(5) 0.1458(5) 0.0213(17) Uani 1 1 d . . . H10A H 0.6187 0.5119 0.1415 0.026 Uiso 1 1 calc R . . O10 O 0.4629(5) 0.3782(4) 0.1014(3) 0.0207(11) Uani 1 1 d . . . O1 O 0.1969(5) 0.2772(4) 0.0014(3) 0.0222(12) Uani 1 1 d . . . C11 C 0.5013(8) 0.4742(6) 0.2470(6) 0.0255(18) Uani 1 1 d . . . H11A H 0.5649 0.4351 0.2818 0.031 Uiso 1 1 calc R . . H11B H 0.5218 0.5455 0.2787 0.031 Uiso 1 1 calc R . . N12 N 0.3526(6) 0.4153(4) 0.2411(4) 0.0204(14) Uani 1 1 d . . . C13 C 0.2986(8) 0.4035(6) 0.3156(5) 0.0229(17) Uani 1 1 d . . . C14 C 0.1519(8) 0.3397(6) 0.3105(5) 0.0250(18) Uani 1 1 d . . . C15 C 0.0583(8) 0.3102(5) 0.2226(5) 0.0196(17) Uani 1 1 d . . . O15 O 0.0871(5) 0.3301(4) 0.1407(3) 0.0204(11) Uani 1 1 d . . . C16 C -0.0828(8) 0.2545(5) 0.2264(5) 0.0197(16) Uani 1 1 d . . . H16A H -0.1495 0.2349 0.1691 0.024 Uiso 1 1 calc R . . C17 C -0.1258(9) 0.2281(6) 0.3086(6) 0.0280(19) Uani 1 1 d . . . H17A H -0.2211 0.1907 0.3077 0.034 Uiso 1 1 calc R . . C18 C -0.0320(10) 0.2552(7) 0.3938(6) 0.038(2) Uani 1 1 d . . . H18A H -0.0622 0.2366 0.4513 0.046 Uiso 1 1 calc R . . C19 C 0.1052(9) 0.3093(6) 0.3935(6) 0.0298(19) Uani 1 1 d . . . H19A H 0.1703 0.3267 0.4516 0.036 Uiso 1 1 calc R . . C20 C 0.2206(9) 0.6058(6) -0.0459(6) 0.0281(19) Uani 1 1 d . . . H20A H 0.3031 0.6546 -0.0063 0.042 Uiso 1 1 calc R . . H20B H 0.1369 0.6306 -0.0442 0.042 Uiso 1 1 calc R . . H20C H 0.2354 0.6037 -0.1108 0.042 Uiso 1 1 calc R . . C21 C 0.3832(9) 0.4517(7) 0.4081(5) 0.032(2) Uani 1 1 d . . . H21A H 0.4268 0.4001 0.4410 0.048 Uiso 1 1 calc R . . H21B H 0.3219 0.4723 0.4458 0.048 Uiso 1 1 calc R . . H21C H 0.4568 0.5147 0.3986 0.048 Uiso 1 1 calc R . . O31 O 0.5050(5) 0.2462(4) 0.3201(3) 0.0224(12) Uani 1 1 d . . . C31 C 0.5284(8) 0.2168(6) 0.4071(5) 0.0250(18) Uani 1 1 d . . . C32 C 0.4356(8) 0.1316(6) 0.4417(6) 0.0274(19) Uani 1 1 d . . . C33 C 0.4725(9) 0.1079(7) 0.5355(6) 0.035(2) Uani 1 1 d . . . H33A H 0.4127 0.0493 0.5593 0.042 Uiso 1 1 calc R . . C34 C 0.5921(10) 0.1665(7) 0.5938(6) 0.038(2) Uani 1 1 d . . . H34A H 0.6145 0.1493 0.6574 0.045 Uiso 1 1 calc R . . C35 C 0.6794(9) 0.2508(7) 0.5593(6) 0.040(2) Uani 1 1 d . . . H35A H 0.7619 0.2921 0.5999 0.048 Uiso 1 1 calc R . . C36 C 0.6505(9) 0.2764(7) 0.4684(6) 0.0302(19) Uani 1 1 d . . . H36A H 0.7130 0.3346 0.4462 0.036 Uiso 1 1 calc R . . C37 C 0.2998(8) 0.0799(6) 0.3842(5) 0.0220(17) Uani 1 1 d . . . N38 N 0.2779(6) 0.0824(4) 0.2946(4) 0.0205(14) Uani 1 1 d . . . C39 C 0.1357(8) 0.0652(6) 0.2360(5) 0.0216(17) Uani 1 1 d . . . H39A H 0.0749 0.0939 0.2697 0.026 Uiso 1 1 calc R . . H39B H 0.0913 -0.0116 0.2204 0.026 Uiso 1 1 calc R . . C40 C 0.1563(7) 0.1235(5) 0.1472(5) 0.0207(17) Uani 1 1 d . . . H40A H 0.0706 0.1467 0.1202 0.025 Uiso 1 1 calc R . . O40 O 0.2728(5) 0.2121(4) 0.1745(3) 0.0225(12) Uani 1 1 d . . . C41 C 0.1910(8) 0.0570(5) 0.0751(5) 0.0215(17) Uani 1 1 d . . . H41A H 0.1171 -0.0111 0.0592 0.026 Uiso 1 1 calc R . . H41B H 0.2012 0.0951 0.0170 0.026 Uiso 1 1 calc R . . N42 N 0.3243(6) 0.0394(4) 0.1212(4) 0.0193(14) Uani 1 1 d . . . C43 C 0.3720(8) -0.0349(5) 0.0885(5) 0.0232(17) Uani 1 1 d . . . C44 C 0.4972(8) -0.0597(5) 0.1389(5) 0.0207(17) Uani 1 1 d . . . C45 C 0.5721(8) -0.0069(5) 0.2269(5) 0.0209(17) Uani 1 1 d . . . O45 O 0.5414(5) 0.0669(4) 0.2723(3) 0.0229(12) Uani 1 1 d . . . C46 C 0.6925(8) -0.0383(6) 0.2702(6) 0.0271(18) Uani 1 1 d . . . H46A H 0.7454 -0.0034 0.3284 0.033 Uiso 1 1 calc R . . C47 C 0.7358(9) -0.1171(6) 0.2315(6) 0.0299(19) Uani 1 1 d . . . H47A H 0.8160 -0.1368 0.2636 0.036 Uiso 1 1 calc R . . C48 C 0.6631(9) -0.1680(6) 0.1458(6) 0.032(2) Uani 1 1 d . . . H48A H 0.6931 -0.2221 0.1182 0.038 Uiso 1 1 calc R . . C49 C 0.5466(9) -0.1388(6) 0.1012(6) 0.0286(19) Uani 1 1 d . . . H49A H 0.4973 -0.1736 0.0421 0.034 Uiso 1 1 calc R . . C50 C 0.1807(9) 0.0285(7) 0.4330(6) 0.035(2) Uani 1 1 d . . . H50A H 0.1566 0.0833 0.4680 0.052 Uiso 1 1 calc R . . H50B H 0.2098 -0.0220 0.4765 0.052 Uiso 1 1 calc R . . H50C H 0.0983 -0.0091 0.3860 0.052 Uiso 1 1 calc R . . C51 C 0.2887(8) -0.0982(5) -0.0002(5) 0.0243(18) Uani 1 1 d . . . H51A H 0.2116 -0.1550 0.0149 0.036 Uiso 1 1 calc R . . H51B H 0.3504 -0.1293 -0.0298 0.036 Uiso 1 1 calc R . . H51C H 0.2499 -0.0516 -0.0436 0.036 Uiso 1 1 calc R . . O61 O 0.5486(5) 0.2211(4) 0.1505(3) 0.0212(12) Uani 1 1 d D . . H61A H 0.518(8) 0.286(3) 0.140(5) 0.032 Uiso 1 1 d D . . H61B H 0.487(6) 0.163(4) 0.107(4) 0.032 Uiso 1 1 d 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 0.0173(6) 0.0128(5) 0.0253(6) 0.0015(4) 0.0040(4) 0.0046(4) Co2 0.0174(6) 0.0143(5) 0.0243(6) 0.0010(4) 0.0031(4) 0.0045(4) C1 0.025(5) 0.025(4) 0.023(4) 0.007(3) 0.012(3) 0.013(3) C2 0.021(5) 0.025(4) 0.027(4) 0.001(3) 0.007(3) 0.007(3) C3 0.028(5) 0.023(4) 0.038(5) 0.008(4) 0.011(4) 0.012(4) C4 0.030(5) 0.030(5) 0.033(5) 0.000(4) 0.002(4) 0.008(4) C5 0.025(5) 0.032(4) 0.026(5) -0.001(3) -0.002(4) 0.007(4) C6 0.029(5) 0.028(4) 0.022(4) -0.003(3) -0.003(4) 0.011(4) C7 0.023(5) 0.014(4) 0.032(5) 0.001(3) 0.007(3) 0.012(3) N8 0.025(4) 0.009(3) 0.031(4) 0.003(3) 0.008(3) 0.002(3) C9 0.021(5) 0.013(4) 0.032(5) -0.001(3) 0.004(3) 0.002(3) C10 0.015(4) 0.017(4) 0.029(4) -0.002(3) -0.002(3) 0.003(3) O10 0.016(3) 0.015(2) 0.032(3) 0.002(2) 0.008(2) 0.006(2) O1 0.021(3) 0.020(3) 0.026(3) 0.002(2) 0.005(2) 0.008(2) C11 0.017(5) 0.020(4) 0.040(5) -0.004(3) 0.006(4) 0.005(3) N12 0.019(4) 0.016(3) 0.026(4) -0.002(3) 0.003(3) 0.005(3) C13 0.028(5) 0.023(4) 0.018(4) -0.004(3) 0.000(3) 0.011(4) C14 0.028(5) 0.022(4) 0.029(5) -0.003(3) 0.006(4) 0.013(4) C15 0.022(5) 0.011(3) 0.023(4) -0.002(3) -0.002(3) 0.006(3) O15 0.018(3) 0.020(3) 0.023(3) 0.002(2) 0.004(2) 0.005(2) C16 0.013(4) 0.018(4) 0.027(4) 0.002(3) 0.004(3) 0.003(3) C17 0.027(5) 0.023(4) 0.034(5) 0.006(3) 0.006(4) 0.006(3) C18 0.045(6) 0.040(5) 0.037(5) 0.011(4) 0.013(4) 0.019(5) C19 0.020(5) 0.038(5) 0.027(5) 0.001(4) 0.000(3) 0.005(4) C20 0.026(5) 0.019(4) 0.041(5) 0.010(3) 0.008(4) 0.009(3) C21 0.033(5) 0.037(5) 0.020(4) -0.011(4) -0.001(4) 0.002(4) O31 0.024(3) 0.015(3) 0.026(3) -0.001(2) 0.003(2) 0.005(2) C31 0.027(5) 0.026(4) 0.026(5) -0.007(3) 0.001(4) 0.018(4) C32 0.022(5) 0.031(5) 0.033(5) 0.003(4) 0.004(4) 0.012(4) C33 0.026(5) 0.045(5) 0.032(5) 0.007(4) 0.005(4) 0.007(4) C34 0.038(6) 0.059(6) 0.017(4) 0.012(4) 0.004(4) 0.014(5) C35 0.027(6) 0.054(6) 0.034(5) -0.004(4) -0.003(4) 0.009(4) C36 0.024(5) 0.036(5) 0.031(5) -0.002(4) 0.003(4) 0.010(4) C37 0.021(5) 0.021(4) 0.025(5) 0.012(3) 0.008(3) 0.007(3) N38 0.015(4) 0.018(3) 0.029(4) 0.002(3) 0.004(3) 0.003(3) C39 0.014(4) 0.018(4) 0.031(4) -0.003(3) 0.007(3) -0.001(3) C40 0.010(4) 0.010(3) 0.036(5) -0.002(3) -0.003(3) -0.002(3) O40 0.023(3) 0.013(2) 0.028(3) -0.001(2) 0.002(2) 0.001(2) C41 0.022(5) 0.011(4) 0.024(4) -0.005(3) -0.004(3) -0.001(3) N42 0.021(4) 0.010(3) 0.026(4) 0.001(3) 0.006(3) 0.003(3) C43 0.032(5) 0.009(3) 0.028(4) 0.004(3) 0.008(3) 0.003(3) C44 0.016(4) 0.014(4) 0.036(5) 0.004(3) 0.012(3) 0.005(3) C45 0.024(5) 0.014(4) 0.026(4) 0.003(3) 0.009(3) 0.004(3) O45 0.022(3) 0.018(3) 0.029(3) -0.001(2) 0.005(2) 0.005(2) C46 0.019(5) 0.024(4) 0.039(5) 0.000(4) 0.010(4) 0.005(3) C47 0.024(5) 0.031(4) 0.042(5) 0.008(4) 0.016(4) 0.014(4) C48 0.030(5) 0.022(4) 0.051(6) 0.006(4) 0.015(4) 0.015(4) C49 0.033(5) 0.021(4) 0.034(5) -0.004(3) 0.019(4) 0.004(4) C50 0.029(5) 0.041(5) 0.035(5) 0.007(4) 0.011(4) 0.007(4) C51 0.029(5) 0.014(4) 0.029(4) -0.004(3) 0.005(3) 0.006(3) O61 0.021(3) 0.016(3) 0.027(3) -0.002(2) 0.004(2) 0.006(2) _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 1.868(5) . ? Co1 O15 1.893(5) . ? Co1 N8 1.895(6) . ? Co1 N12 1.898(6) . ? Co1 O10 1.917(5) . ? Co1 O40 1.949(5) . ? Co2 O45 1.862(5) . ? Co2 O31 1.870(5) . ? Co2 N38 1.875(6) . ? Co2 N42 1.908(6) . ? Co2 O40 1.910(5) . ? Co2 O61 1.952(5) . ? C1 O1 1.312(8) . ? C1 C6 1.394(10) . ? C1 C2 1.411(10) . ? C2 C3 1.390(10) . ? C2 C7 1.457(10) . ? C3 C4 1.395(11) . ? C3 H3A 0.9500 . ? C4 C5 1.384(10) . ? C4 H4A 0.9500 . ? C5 C6 1.361(10) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C7 N8 1.284(9) . ? C7 C20 1.500(10) . ? N8 C9 1.475(9) . ? C9 C10 1.540(10) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 O10 1.424(8) . ? C10 C11 1.507(11) . ? C10 H10A 1.0000 . ? C11 N12 1.473(10) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? N12 C13 1.287(9) . ? C13 C14 1.476(11) . ? C13 C21 1.482(10) . ? C14 C19 1.394(11) . ? C14 C15 1.418(10) . ? C15 O15 1.286(8) . ? C15 C16 1.421(10) . ? C16 C17 1.357(10) . ? C16 H16A 0.9500 . ? C17 C18 1.387(11) . ? C17 H17A 0.9500 . ? C18 C19 1.373(12) . ? C18 H18A 0.9500 . ? C19 H19A 0.9500 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? O31 C31 1.319(9) . ? C31 C36 1.407(11) . ? C31 C32 1.411(11) . ? C32 C33 1.401(11) . ? C32 C37 1.447(11) . ? C33 C34 1.368(12) . ? C33 H33A 0.9500 . ? C34 C35 1.376(12) . ? C34 H34A 0.9500 . ? C35 C36 1.359(11) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? C37 N38 1.278(9) . ? C37 C50 1.507(11) . ? N38 C39 1.478(9) . ? C39 C40 1.521(10) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 O40 1.404(8) . ? C40 C41 1.500(10) . ? C40 H40A 1.0000 . ? C41 N42 1.457(9) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? N42 C43 1.312(9) . ? C43 C44 1.448(10) . ? C43 C51 1.502(10) . ? C44 C49 1.405(9) . ? C44 C45 1.424(10) . ? C45 O45 1.296(8) . ? C45 C46 1.416(10) . ? C46 C47 1.373(10) . ? C46 H46A 0.9500 . ? C47 C48 1.383(11) . ? C47 H47A 0.9500 . ? C48 C49 1.375(11) . ? C48 H48A 0.9500 . ? C49 H49A 0.9500 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? O61 H61A 0.9800(11) . ? O61 H61B 0.9800(11) . ? 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 O15 89.2(2) . . ? O1 Co1 N8 88.4(2) . . ? O15 Co1 N8 95.7(2) . . ? O1 Co1 N12 177.9(2) . . ? O15 Co1 N12 91.9(2) . . ? N8 Co1 N12 93.3(3) . . ? O1 Co1 O10 93.8(2) . . ? O15 Co1 O10 175.1(2) . . ? N8 Co1 O10 80.5(2) . . ? N12 Co1 O10 85.2(2) . . ? O1 Co1 O40 89.9(2) . . ? O15 Co1 O40 89.3(2) . . ? N8 Co1 O40 174.7(2) . . ? N12 Co1 O40 88.3(2) . . ? O10 Co1 O40 94.6(2) . . ? O45 Co2 O31 87.3(2) . . ? O45 Co2 N38 96.2(2) . . ? O31 Co2 N38 90.0(2) . . ? O45 Co2 N42 93.0(2) . . ? O31 Co2 N42 178.0(2) . . ? N38 Co2 N42 92.0(3) . . ? O45 Co2 O40 176.2(2) . . ? O31 Co2 O40 94.4(2) . . ? N38 Co2 O40 80.4(2) . . ? N42 Co2 O40 85.4(2) . . ? O45 Co2 O61 89.5(2) . . ? O31 Co2 O61 86.1(2) . . ? N38 Co2 O61 172.9(2) . . ? N42 Co2 O61 91.9(2) . . ? O40 Co2 O61 94.0(2) . . ? O1 C1 C6 119.1(6) . . ? O1 C1 C2 123.1(7) . . ? C6 C1 C2 117.7(7) . . ? C3 C2 C1 119.2(7) . . ? C3 C2 C7 119.9(7) . . ? C1 C2 C7 120.0(7) . . ? C2 C3 C4 121.8(7) . . ? C2 C3 H3A 119.1 . . ? C4 C3 H3A 119.1 . . ? C5 C4 C3 118.2(7) . . ? C5 C4 H4A 120.9 . . ? C3 C4 H4A 120.9 . . ? C6 C5 C4 120.6(7) . . ? C6 C5 H5A 119.7 . . ? C4 C5 H5A 119.7 . . ? C5 C6 C1 122.4(7) . . ? C5 C6 H6A 118.8 . . ? C1 C6 H6A 118.8 . . ? N8 C7 C2 120.3(6) . . ? N8 C7 C20 120.7(7) . . ? C2 C7 C20 118.8(7) . . ? C7 N8 C9 122.5(6) . . ? C7 N8 Co1 126.7(5) . . ? C9 N8 Co1 109.5(5) . . ? N8 C9 C10 105.9(5) . . ? N8 C9 H9A 110.6 . . ? C10 C9 H9A 110.6 . . ? N8 C9 H9B 110.6 . . ? C10 C9 H9B 110.6 . . ? H9A C9 H9B 108.7 . . ? O10 C10 C11 107.4(6) . . ? O10 C10 C9 106.9(5) . . ? C11 C10 C9 109.9(6) . . ? O10 C10 H10A 110.8 . . ? C11 C10 H10A 110.8 . . ? C9 C10 H10A 110.8 . . ? C10 O10 Co1 100.0(4) . . ? C1 O1 Co1 121.2(4) . . ? N12 C11 C10 104.0(6) . . ? N12 C11 H11A 111.0 . . ? C10 C11 H11A 111.0 . . ? N12 C11 H11B 111.0 . . ? C10 C11 H11B 111.0 . . ? H11A C11 H11B 109.0 . . ? C13 N12 C11 120.4(6) . . ? C13 N12 Co1 127.8(5) . . ? C11 N12 Co1 111.2(5) . . ? N12 C13 C14 120.3(7) . . ? N12 C13 C21 120.8(7) . . ? C14 C13 C21 118.9(7) . . ? C19 C14 C15 119.9(7) . . ? C19 C14 C13 119.2(7) . . ? C15 C14 C13 120.9(7) . . ? O15 C15 C16 117.0(6) . . ? O15 C15 C14 126.9(7) . . ? C16 C15 C14 116.1(7) . . ? C15 O15 Co1 120.6(5) . . ? C17 C16 C15 122.5(7) . . ? C17 C16 H16A 118.7 . . ? C15 C16 H16A 118.7 . . ? C16 C17 C18 120.7(8) . . ? C16 C17 H17A 119.6 . . ? C18 C17 H17A 119.6 . . ? C19 C18 C17 118.7(8) . . ? C19 C18 H18A 120.7 . . ? C17 C18 H18A 120.7 . . ? C18 C19 C14 122.0(8) . . ? C18 C19 H19A 119.0 . . ? C14 C19 H19A 119.0 . . ? C7 C20 H20A 109.5 . . ? C7 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C7 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C13 C21 H21A 109.5 . . ? C13 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C13 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C31 O31 Co2 118.9(4) . . ? O31 C31 C36 117.4(7) . . ? O31 C31 C32 123.4(7) . . ? C36 C31 C32 119.2(7) . . ? C33 C32 C31 118.0(7) . . ? C33 C32 C37 121.8(7) . . ? C31 C32 C37 119.8(7) . . ? C34 C33 C32 122.0(8) . . ? C34 C33 H33A 119.0 . . ? C32 C33 H33A 119.0 . . ? C33 C34 C35 119.1(8) . . ? C33 C34 H34A 120.5 . . ? C35 C34 H34A 120.5 . . ? C36 C35 C34 121.6(8) . . ? C36 C35 H35A 119.2 . . ? C34 C35 H35A 119.2 . . ? C35 C36 C31 120.1(8) . . ? C35 C36 H36A 119.9 . . ? C31 C36 H36A 119.9 . . ? N38 C37 C32 121.4(7) . . ? N38 C37 C50 120.3(7) . . ? C32 C37 C50 118.3(7) . . ? C37 N38 C39 123.0(6) . . ? C37 N38 Co2 125.7(5) . . ? C39 N38 Co2 109.4(5) . . ? N38 C39 C40 106.1(6) . . ? N38 C39 H39A 110.5 . . ? C40 C39 H39A 110.5 . . ? N38 C39 H39B 110.5 . . ? C40 C39 H39B 110.5 . . ? H39A C39 H39B 108.7 . . ? O40 C40 C41 107.7(6) . . ? O40 C40 C39 106.0(6) . . ? C41 C40 C39 111.9(6) . . ? O40 C40 H40A 110.4 . . ? C41 C40 H40A 110.4 . . ? C39 C40 H40A 110.4 . . ? C40 O40 Co2 100.0(4) . . ? C40 O40 Co1 119.8(4) . . ? Co2 O40 Co1 135.5(3) . . ? N42 C41 C40 103.7(5) . . ? N42 C41 H41A 111.0 . . ? C40 C41 H41A 111.0 . . ? N42 C41 H41B 111.0 . . ? C40 C41 H41B 111.0 . . ? H41A C41 H41B 109.0 . . ? C43 N42 C41 121.0(6) . . ? C43 N42 Co2 128.4(5) . . ? C41 N42 Co2 110.5(4) . . ? N42 C43 C44 121.3(7) . . ? N42 C43 C51 118.2(7) . . ? C44 C43 C51 120.5(6) . . ? C49 C44 C45 118.4(7) . . ? C49 C44 C43 119.8(7) . . ? C45 C44 C43 121.8(6) . . ? O45 C45 C46 116.3(7) . . ? O45 C45 C44 126.8(7) . . ? C46 C45 C44 116.9(6) . . ? C45 O45 Co2 125.6(5) . . ? C47 C46 C45 122.7(8) . . ? C47 C46 H46A 118.6 . . ? C45 C46 H46A 118.6 . . ? C46 C47 C48 120.2(8) . . ? C46 C47 H47A 119.9 . . ? C48 C47 H47A 119.9 . . ? C49 C48 C47 118.7(7) . . ? C49 C48 H48A 120.6 . . ? C47 C48 H48A 120.6 . . ? C48 C49 C44 123.1(8) . . ? C48 C49 H49A 118.5 . . ? C44 C49 H49A 118.5 . . ? C37 C50 H50A 109.5 . . ? C37 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C37 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C43 C51 H51A 109.5 . . ? C43 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C43 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? Co2 O61 H61A 102(5) . . ? Co2 O61 H61B 76(5) . . ? H61A O61 H61B 110(6) . . ? 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 O1 C1 C2 C3 179.2(7) . . . . ? C6 C1 C2 C3 2.3(11) . . . . ? O1 C1 C2 C7 10.0(11) . . . . ? C6 C1 C2 C7 -166.8(7) . . . . ? C1 C2 C3 C4 1.5(12) . . . . ? C7 C2 C3 C4 170.6(7) . . . . ? C2 C3 C4 C5 -3.4(12) . . . . ? C3 C4 C5 C6 1.4(12) . . . . ? C4 C5 C6 C1 2.5(12) . . . . ? O1 C1 C6 C5 178.7(7) . . . . ? C2 C1 C6 C5 -4.3(12) . . . . ? C3 C2 C7 N8 168.4(7) . . . . ? C1 C2 C7 N8 -22.6(11) . . . . ? C3 C2 C7 C20 -16.6(11) . . . . ? C1 C2 C7 C20 152.4(7) . . . . ? C2 C7 N8 C9 158.4(7) . . . . ? C20 C7 N8 C9 -16.5(11) . . . . ? C2 C7 N8 Co1 -7.9(10) . . . . ? C20 C7 N8 Co1 177.2(5) . . . . ? O1 Co1 N8 C7 35.3(6) . . . . ? O15 Co1 N8 C7 -53.7(6) . . . . ? N12 Co1 N8 C7 -146.0(6) . . . . ? O10 Co1 N8 C7 129.4(6) . . . . ? O1 Co1 N8 C9 -132.5(5) . . . . ? O15 Co1 N8 C9 138.4(5) . . . . ? N12 Co1 N8 C9 46.2(5) . . . . ? O10 Co1 N8 C9 -38.4(4) . . . . ? C7 N8 C9 C10 -154.7(7) . . . . ? Co1 N8 C9 C10 13.7(7) . . . . ? N8 C9 C10 O10 29.4(7) . . . . ? N8 C9 C10 C11 -86.8(7) . . . . ? C11 C10 O10 Co1 60.0(5) . . . . ? C9 C10 O10 Co1 -57.9(6) . . . . ? O1 Co1 O10 C10 141.6(4) . . . . ? N8 Co1 O10 C10 53.9(4) . . . . ? N12 Co1 O10 C10 -40.3(4) . . . . ? O40 Co1 O10 C10 -128.2(4) . . . . ? C6 C1 O1 Co1 -151.6(6) . . . . ? C2 C1 O1 Co1 31.6(9) . . . . ? O15 Co1 O1 C1 49.9(5) . . . . ? N8 Co1 O1 C1 -45.9(5) . . . . ? O10 Co1 O1 C1 -126.2(5) . . . . ? O40 Co1 O1 C1 139.2(5) . . . . ? O10 C10 C11 N12 -50.6(7) . . . . ? C9 C10 C11 N12 65.3(7) . . . . ? C10 C11 N12 C13 -173.0(6) . . . . ? C10 C11 N12 Co1 15.7(6) . . . . ? O15 Co1 N12 C13 27.0(6) . . . . ? N8 Co1 N12 C13 122.9(6) . . . . ? O10 Co1 N12 C13 -157.0(6) . . . . ? O40 Co1 N12 C13 -62.2(6) . . . . ? O15 Co1 N12 C11 -162.4(5) . . . . ? N8 Co1 N12 C11 -66.5(5) . . . . ? O10 Co1 N12 C11 13.6(4) . . . . ? O40 Co1 N12 C11 108.4(5) . . . . ? C11 N12 C13 C14 -176.7(6) . . . . ? Co1 N12 C13 C14 -6.9(10) . . . . ? C11 N12 C13 C21 2.1(10) . . . . ? Co1 N12 C13 C21 171.9(5) . . . . ? N12 C13 C14 C19 166.6(7) . . . . ? C21 C13 C14 C19 -12.2(10) . . . . ? N12 C13 C14 C15 -14.1(10) . . . . ? C21 C13 C14 C15 167.0(7) . . . . ? C19 C14 C15 O15 -178.2(7) . . . . ? C13 C14 C15 O15 2.5(11) . . . . ? C19 C14 C15 C16 3.0(10) . . . . ? C13 C14 C15 C16 -176.2(6) . . . . ? C16 C15 O15 Co1 -153.6(5) . . . . ? C14 C15 O15 Co1 27.7(9) . . . . ? O1 Co1 O15 C15 142.4(5) . . . . ? N8 Co1 O15 C15 -129.2(5) . . . . ? N12 Co1 O15 C15 -35.7(5) . . . . ? O40 Co1 O15 C15 52.5(5) . . . . ? O15 C15 C16 C17 179.5(6) . . . . ? C14 C15 C16 C17 -1.7(10) . . . . ? C15 C16 C17 C18 0.1(11) . . . . ? C16 C17 C18 C19 0.1(12) . . . . ? C17 C18 C19 C14 1.4(12) . . . . ? C15 C14 C19 C18 -3.0(11) . . . . ? C13 C14 C19 C18 176.3(7) . . . . ? O45 Co2 O31 C31 -49.5(5) . . . . ? N38 Co2 O31 C31 46.8(5) . . . . ? O40 Co2 O31 C31 127.1(5) . . . . ? O61 Co2 O31 C31 -139.2(5) . . . . ? Co2 O31 C31 C36 147.7(5) . . . . ? Co2 O31 C31 C32 -34.1(9) . . . . ? O31 C31 C32 C33 179.8(7) . . . . ? C36 C31 C32 C33 -2.1(11) . . . . ? O31 C31 C32 C37 -7.5(11) . . . . ? C36 C31 C32 C37 170.7(7) . . . . ? C31 C32 C33 C34 1.9(12) . . . . ? C37 C32 C33 C34 -170.7(8) . . . . ? C32 C33 C34 C35 -0.5(13) . . . . ? C33 C34 C35 C36 -0.7(14) . . . . ? C34 C35 C36 C31 0.5(13) . . . . ? O31 C31 C36 C35 179.2(7) . . . . ? C32 C31 C36 C35 1.0(11) . . . . ? C33 C32 C37 N38 -163.5(7) . . . . ? C31 C32 C37 N38 24.0(11) . . . . ? C33 C32 C37 C50 20.4(11) . . . . ? C31 C32 C37 C50 -152.1(7) . . . . ? C32 C37 N38 C39 -158.2(7) . . . . ? C50 C37 N38 C39 17.7(10) . . . . ? C32 C37 N38 Co2 4.3(10) . . . . ? C50 C37 N38 Co2 -179.7(5) . . . . ? O45 Co2 N38 C37 53.9(6) . . . . ? O31 Co2 N38 C37 -33.4(6) . . . . ? N42 Co2 N38 C37 147.1(6) . . . . ? O40 Co2 N38 C37 -127.9(6) . . . . ? O45 Co2 N38 C39 -141.6(4) . . . . ? O31 Co2 N38 C39 131.1(4) . . . . ? N42 Co2 N38 C39 -48.3(4) . . . . ? O40 Co2 N38 C39 36.6(4) . . . . ? C37 N38 C39 C40 153.9(6) . . . . ? Co2 N38 C39 C40 -11.2(6) . . . . ? N38 C39 C40 O40 -32.3(7) . . . . ? N38 C39 C40 C41 84.9(7) . . . . ? C41 C40 O40 Co2 -60.2(6) . . . . ? C39 C40 O40 Co2 59.7(5) . . . . ? C41 C40 O40 Co1 99.0(6) . . . . ? C39 C40 O40 Co1 -141.1(4) . . . . ? O31 Co2 O40 C40 -143.7(4) . . . . ? N38 Co2 O40 C40 -54.4(4) . . . . ? N42 Co2 O40 C40 38.3(4) . . . . ? O61 Co2 O40 C40 129.9(4) . . . . ? O31 Co2 O40 Co1 62.3(4) . . . . ? N38 Co2 O40 Co1 151.6(4) . . . . ? N42 Co2 O40 Co1 -115.7(4) . . . . ? O61 Co2 O40 Co1 -24.1(4) . . . . ? O1 Co1 O40 C40 -42.9(5) . . . . ? O15 Co1 O40 C40 46.3(5) . . . . ? N12 Co1 O40 C40 138.2(5) . . . . ? O10 Co1 O40 C40 -136.8(5) . . . . ? O1 Co1 O40 Co2 107.2(4) . . . . ? O15 Co1 O40 Co2 -163.6(4) . . . . ? N12 Co1 O40 Co2 -71.6(4) . . . . ? O10 Co1 O40 Co2 13.4(4) . . . . ? O40 C40 C41 N42 53.7(7) . . . . ? C39 C40 C41 N42 -62.4(7) . . . . ? C40 C41 N42 C43 164.4(6) . . . . ? C40 C41 N42 Co2 -19.4(6) . . . . ? O45 Co2 N42 C43 -17.8(6) . . . . ? N38 Co2 N42 C43 -114.1(6) . . . . ? O40 Co2 N42 C43 165.7(6) . . . . ? O61 Co2 N42 C43 71.9(6) . . . . ? O45 Co2 N42 C41 166.4(5) . . . . ? N38 Co2 N42 C41 70.1(5) . . . . ? O40 Co2 N42 C41 -10.1(5) . . . . ? O61 Co2 N42 C41 -104.0(5) . . . . ? C41 N42 C43 C44 -173.9(7) . . . . ? Co2 N42 C43 C44 10.6(10) . . . . ? C41 N42 C43 C51 2.7(10) . . . . ? Co2 N42 C43 C51 -172.8(5) . . . . ? N42 C43 C44 C49 -179.1(7) . . . . ? C51 C43 C44 C49 4.4(10) . . . . ? N42 C43 C44 C45 1.6(11) . . . . ? C51 C43 C44 C45 -174.9(7) . . . . ? C49 C44 C45 O45 -179.5(7) . . . . ? C43 C44 C45 O45 -0.2(11) . . . . ? C49 C44 C45 C46 0.2(10) . . . . ? C43 C44 C45 C46 179.5(7) . . . . ? C46 C45 O45 Co2 167.0(5) . . . . ? C44 C45 O45 Co2 -13.3(10) . . . . ? O31 Co2 O45 C45 -159.6(6) . . . . ? N38 Co2 O45 C45 110.7(6) . . . . ? N42 Co2 O45 C45 18.4(6) . . . . ? O61 Co2 O45 C45 -73.5(5) . . . . ? O45 C45 C46 C47 178.5(7) . . . . ? C44 C45 C46 C47 -1.2(11) . . . . ? C45 C46 C47 C48 1.5(12) . . . . ? C46 C47 C48 C49 -0.6(12) . . . . ? C47 C48 C49 C44 -0.4(12) . . . . ? C45 C44 C49 C48 0.6(11) . . . . ? C43 C44 C49 C48 -178.7(7) . . . . ? 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 O61 H61A O10 0.9800(11) 1.523(16) 2.490(7) 168(7) . O61 H61B N42 0.9800(11) 2.02(6) 2.774(7) 132(6) . _diffrn_measured_fraction_theta_max 0.912 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.930 _refine_diff_density_max 0.633 _refine_diff_density_min -0.516 _refine_diff_density_rms 0.106 # Attachment 'complex-4-CCDC-720540.cif' data_x82660_0m _database_code_depnum_ccdc_archive 'CCDC 720540' #TrackingRef 'complex-4-CCDC-720540.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 2009-02-12 # Formatted by publCIF ; _chemical_name_common 2009-02-12 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H52 N4 Ni4 O12' _chemical_formula_weight 1015.70 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' 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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.347(5) _cell_length_b 9.598(4) _cell_length_c 22.172(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.676(15) _cell_angle_gamma 90.00 _cell_volume 2201.9(18) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5891 _cell_measurement_theta_min 2.68 _cell_measurement_theta_max 24.47 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.532 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1056 _exptl_absorpt_coefficient_mu 1.748 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5273 _exptl_absorpt_correction_T_max 0.7438 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; 2009-02-12 # Formatted by publCIF ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33350 _diffrn_reflns_av_R_equivalents 0.0853 _diffrn_reflns_av_sigmaI/netI 0.0639 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 25.80 _reflns_number_total 4222 _reflns_number_gt 2744 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0700P)^2^+6.3030P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4222 _refine_ls_number_parameters 286 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0995 _refine_ls_R_factor_gt 0.0441 _refine_ls_wR_factor_ref 0.1452 _refine_ls_wR_factor_gt 0.1064 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _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 0.07362(6) 0.38873(7) 0.46337(3) 0.01695(19) Uani 1 1 d . . . Ni2 Ni 0.00867(6) 0.34247(7) 0.59810(3) 0.0181(2) Uani 1 1 d . . . O1 O 0.1569(3) 0.5520(4) 0.42201(15) 0.0183(8) Uani 1 1 d . . . O2 O -0.0876(3) 0.5085(4) 0.45334(16) 0.0172(8) Uani 1 1 d . . . C1 C 0.2669(5) 0.5465(5) 0.3917(2) 0.0189(12) Uani 1 1 d . . . C2 C 0.2901(5) 0.6432(6) 0.3462(2) 0.0210(12) Uani 1 1 d . . . H2 H 0.2248 0.7098 0.3370 0.025 Uiso 1 1 calc R . . C3 C 0.4037(5) 0.6470(6) 0.3135(3) 0.0260(13) Uani 1 1 d . . . H3 H 0.4159 0.7157 0.2832 0.031 Uiso 1 1 calc R . . O3 O 0.0275(4) 0.3034(4) 0.37576(17) 0.0231(9) Uani 1 1 d D . . H31 H 0.094(4) 0.263(5) 0.360(2) 0.028 Uiso 1 1 d D . . H32 H 0.007(5) 0.378(4) 0.351(2) 0.028 Uiso 1 1 d D . . C4 C 0.4997(5) 0.5489(6) 0.3256(2) 0.0243(13) Uani 1 1 d . . . H4 H 0.5771 0.5485 0.3030 0.029 Uiso 1 1 calc R . . O4 O 0.0253(3) 0.4376(4) 0.67634(16) 0.0216(8) Uani 1 1 d . . . C5 C 0.4812(5) 0.4520(6) 0.3709(2) 0.0226(12) Uani 1 1 d . . . H5 H 0.5475 0.3861 0.3792 0.027 Uiso 1 1 calc R . . O5 O 0.0070(3) 0.2351(4) 0.51851(16) 0.0186(8) Uani 1 1 d . . . C6 C 0.3665(5) 0.4474(6) 0.4055(2) 0.0191(11) Uani 1 1 d . . . O6 O 0.2455(4) 0.8628(4) 0.4672(2) 0.0354(11) Uani 1 1 d D . . H61W H 0.287(5) 0.802(6) 0.444(3) 0.043 Uiso 1 1 d D . . H62W H 0.166(4) 0.837(6) 0.478(3) 0.043 Uiso 1 1 d D . . C7 C 0.3573(5) 0.3403(5) 0.4532(2) 0.0187(11) Uani 1 1 d . . . N8 N 0.2468(4) 0.2954(4) 0.47170(19) 0.0177(9) Uani 1 1 d . . . C9 C 0.2418(5) 0.1880(6) 0.5184(2) 0.0197(12) Uani 1 1 d . . . H9A H 0.2705 0.2280 0.5575 0.024 Uiso 1 1 calc R . . H9B H 0.3014 0.1112 0.5081 0.024 Uiso 1 1 calc R . . C10 C 0.1033(5) 0.1303(5) 0.5243(2) 0.0180(11) Uani 1 1 d . . . H10 H 0.0885 0.0587 0.4922 0.022 Uiso 1 1 calc R . . C11 C 0.0934(5) 0.0598(6) 0.5860(2) 0.0212(12) Uani 1 1 d . . . H11A H 0.0105 0.0090 0.5894 0.025 Uiso 1 1 calc R . . H11B H 0.1653 -0.0070 0.5922 0.025 Uiso 1 1 calc R . . N12 N 0.1010(4) 0.1740(4) 0.63111(19) 0.0177(9) Uani 1 1 d . . . C13 C 0.1479(4) 0.1531(6) 0.6850(2) 0.0183(11) Uani 1 1 d . . . C14 C 0.1695(5) 0.2701(5) 0.7260(2) 0.0191(12) Uani 1 1 d . . . C15 C 0.2566(5) 0.2523(6) 0.7745(2) 0.0214(12) Uani 1 1 d . . . H15 H 0.2970 0.1640 0.7793 0.026 Uiso 1 1 calc R . . C16 C 0.2867(5) 0.3553(6) 0.8154(3) 0.0255(13) Uani 1 1 d . . . H16 H 0.3473 0.3385 0.8471 0.031 Uiso 1 1 calc R . . C17 C 0.2265(5) 0.4849(6) 0.8096(3) 0.0243(13) Uani 1 1 d . . . H17 H 0.2439 0.5567 0.8380 0.029 Uiso 1 1 calc R . . C18 C 0.1419(5) 0.5079(6) 0.7625(2) 0.0230(12) Uani 1 1 d . . . H18 H 0.1028 0.5971 0.7590 0.028 Uiso 1 1 calc R . . C19 C 0.1104(5) 0.4064(6) 0.7192(2) 0.0192(12) Uani 1 1 d . . . C20 C 0.1831(5) 0.0083(6) 0.7062(3) 0.0261(13) Uani 1 1 d . . . H20A H 0.1304 -0.0603 0.6843 0.039 Uiso 1 1 calc R . . H20B H 0.1671 0.0004 0.7495 0.039 Uiso 1 1 calc R . . H20C H 0.2748 -0.0091 0.6985 0.039 Uiso 1 1 calc R . . C21 C 0.4816(5) 0.2858(6) 0.4815(3) 0.0272(14) Uani 1 1 d . . . H21A H 0.4709 0.2767 0.5252 0.041 Uiso 1 1 calc R . . H21B H 0.5522 0.3510 0.4733 0.041 Uiso 1 1 calc R . . H21C H 0.5021 0.1945 0.4643 0.041 Uiso 1 1 calc R . . C22 C -0.2080(5) 0.4469(6) 0.4340(3) 0.0238(12) Uani 1 1 d . . . H22A H -0.2778 0.5151 0.4383 0.036 Uiso 1 1 calc R . . H22B H -0.2263 0.3651 0.4590 0.036 Uiso 1 1 calc R . . H22C H -0.2018 0.4185 0.3917 0.036 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 0.0066(3) 0.0198(4) 0.0244(4) 0.0007(3) -0.0003(3) -0.0009(3) Ni2 0.0093(3) 0.0194(4) 0.0257(4) 0.0020(3) 0.0002(3) 0.0005(3) O1 0.0079(17) 0.021(2) 0.026(2) 0.0013(16) 0.0020(15) -0.0009(14) O2 0.0040(16) 0.020(2) 0.028(2) 0.0010(16) -0.0010(14) -0.0006(14) C1 0.010(3) 0.020(3) 0.026(3) -0.004(2) -0.001(2) -0.002(2) C2 0.012(3) 0.023(3) 0.028(3) -0.001(2) -0.001(2) 0.003(2) C3 0.015(3) 0.033(3) 0.030(3) 0.005(3) 0.004(2) -0.005(2) O3 0.016(2) 0.023(2) 0.031(2) -0.0025(17) 0.0009(17) 0.0030(16) C4 0.012(3) 0.033(3) 0.028(3) -0.001(3) 0.005(2) -0.006(2) O4 0.0166(19) 0.024(2) 0.025(2) 0.0006(16) -0.0009(16) 0.0042(15) C5 0.007(2) 0.028(3) 0.033(3) -0.002(3) -0.002(2) -0.003(2) O5 0.0080(17) 0.018(2) 0.030(2) -0.0007(15) 0.0008(15) 0.0001(14) C6 0.006(2) 0.026(3) 0.026(3) 0.001(2) 0.000(2) -0.007(2) O6 0.018(2) 0.029(3) 0.060(3) -0.007(2) 0.006(2) 0.0016(18) C7 0.007(2) 0.023(3) 0.027(3) -0.004(2) -0.004(2) 0.000(2) N8 0.011(2) 0.019(2) 0.023(2) 0.0007(19) -0.0019(18) -0.0013(17) C9 0.008(2) 0.022(3) 0.029(3) -0.002(2) 0.003(2) -0.001(2) C10 0.015(3) 0.015(3) 0.024(3) 0.000(2) 0.001(2) -0.001(2) C11 0.018(3) 0.017(3) 0.029(3) -0.001(2) -0.003(2) -0.001(2) N12 0.013(2) 0.019(2) 0.021(2) 0.0019(19) 0.0038(18) -0.0036(18) C13 0.004(2) 0.026(3) 0.026(3) 0.004(2) 0.002(2) -0.001(2) C14 0.013(3) 0.017(3) 0.027(3) 0.003(2) 0.004(2) -0.004(2) C15 0.016(3) 0.021(3) 0.027(3) 0.005(2) 0.002(2) 0.002(2) C16 0.018(3) 0.032(3) 0.026(3) -0.001(3) -0.004(2) -0.003(2) C17 0.022(3) 0.021(3) 0.030(3) -0.004(2) -0.005(2) -0.005(2) C18 0.020(3) 0.015(3) 0.034(3) 0.002(2) 0.001(2) 0.005(2) C19 0.010(2) 0.023(3) 0.024(3) 0.006(2) 0.008(2) 0.001(2) C20 0.022(3) 0.023(3) 0.033(3) 0.002(3) -0.002(3) 0.005(2) C21 0.010(3) 0.029(3) 0.043(4) 0.013(3) -0.004(2) -0.002(2) C22 0.009(3) 0.028(3) 0.034(3) -0.002(3) -0.004(2) -0.003(2) _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 N8 2.010(4) . ? Ni1 O1 2.014(4) . ? Ni1 O2 2.036(3) . ? Ni1 O5 2.040(4) . ? Ni1 O2 2.097(4) 3_566 ? Ni1 O3 2.157(4) . ? Ni2 O4 1.966(4) . ? Ni2 O2 2.009(4) 3_566 ? Ni2 N12 2.012(4) . ? Ni2 O1 2.035(3) 3_566 ? Ni2 O5 2.043(4) . ? O1 C1 1.330(6) . ? O1 Ni2 2.035(3) 3_566 ? O2 C22 1.439(6) . ? O2 Ni2 2.009(4) 3_566 ? O2 Ni1 2.097(4) 3_566 ? C1 C2 1.395(7) . ? C1 C6 1.432(7) . ? C2 C3 1.389(7) . ? C2 H2 0.9500 . ? C3 C4 1.392(8) . ? C3 H3 0.9500 . ? O3 H31 0.87(3) . ? O3 H32 0.93(3) . ? C4 C5 1.384(8) . ? C4 H4 0.9500 . ? O4 C19 1.322(6) . ? C5 C6 1.420(7) . ? C5 H5 0.9500 . ? O5 C10 1.421(6) . ? C6 C7 1.480(7) . ? O6 H61W 0.90(3) . ? O6 H62W 0.89(3) . ? C7 N8 1.293(6) . ? C7 C21 1.517(7) . ? N8 C9 1.463(7) . ? C9 C10 1.544(7) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.531(7) . ? C10 H10 1.0000 . ? C11 N12 1.485(7) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? N12 C13 1.299(7) . ? C13 C14 1.462(7) . ? C13 C20 1.510(7) . ? C14 C15 1.405(7) . ? C14 C19 1.451(7) . ? C15 C16 1.375(8) . ? C15 H15 0.9500 . ? C16 C17 1.397(8) . ? C16 H16 0.9500 . ? C17 C18 1.372(7) . ? C17 H17 0.9500 . ? C18 C19 1.404(8) . ? C18 H18 0.9500 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 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 N8 Ni1 O1 90.17(16) . . ? N8 Ni1 O2 171.96(16) . . ? O1 Ni1 O2 82.27(14) . . ? N8 Ni1 O5 85.98(15) . . ? O1 Ni1 O5 169.81(14) . . ? O2 Ni1 O5 101.03(14) . . ? N8 Ni1 O2 94.40(15) . 3_566 ? O1 Ni1 O2 90.55(14) . 3_566 ? O2 Ni1 O2 83.02(14) . 3_566 ? O5 Ni1 O2 80.37(14) . 3_566 ? N8 Ni1 O3 95.81(16) . . ? O1 Ni1 O3 88.66(15) . . ? O2 Ni1 O3 86.77(14) . . ? O5 Ni1 O3 101.10(15) . . ? O2 Ni1 O3 169.76(14) 3_566 . ? O4 Ni2 O2 97.95(15) . 3_566 ? O4 Ni2 N12 90.93(16) . . ? O2 Ni2 N12 125.77(15) 3_566 . ? O4 Ni2 O1 91.52(14) . 3_566 ? O2 Ni2 O1 82.40(14) 3_566 3_566 ? N12 Ni2 O1 151.02(15) . 3_566 ? O4 Ni2 O5 174.84(14) . . ? O2 Ni2 O5 82.42(14) 3_566 . ? N12 Ni2 O5 84.72(16) . . ? O1 Ni2 O5 93.63(14) 3_566 . ? C1 O1 Ni1 124.9(3) . . ? C1 O1 Ni2 129.2(3) . 3_566 ? Ni1 O1 Ni2 97.10(14) . 3_566 ? C22 O2 Ni2 118.7(3) . 3_566 ? C22 O2 Ni1 120.4(3) . . ? Ni2 O2 Ni1 97.25(14) 3_566 . ? C22 O2 Ni1 120.4(3) . 3_566 ? Ni2 O2 Ni1 98.08(15) 3_566 3_566 ? Ni1 O2 Ni1 96.98(14) . 3_566 ? O1 C1 C2 119.7(5) . . ? O1 C1 C6 122.5(5) . . ? C2 C1 C6 117.8(5) . . ? C3 C2 C1 123.3(5) . . ? C3 C2 H2 118.4 . . ? C1 C2 H2 118.4 . . ? C2 C3 C4 119.2(5) . . ? C2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? Ni1 O3 H31 111(4) . . ? Ni1 O3 H32 107(4) . . ? H31 O3 H32 106(4) . . ? C5 C4 C3 119.4(5) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? C19 O4 Ni2 125.4(3) . . ? C4 C5 C6 122.4(5) . . ? C4 C5 H5 118.8 . . ? C6 C5 H5 118.8 . . ? C10 O5 Ni1 108.9(3) . . ? C10 O5 Ni2 106.3(3) . . ? Ni1 O5 Ni2 98.84(15) . . ? C5 C6 C1 117.9(5) . . ? C5 C6 C7 118.0(5) . . ? C1 C6 C7 124.2(4) . . ? H61W O6 H62W 114(5) . . ? N8 C7 C6 121.5(4) . . ? N8 C7 C21 120.2(5) . . ? C6 C7 C21 118.3(4) . . ? C7 N8 C9 119.9(4) . . ? C7 N8 Ni1 127.8(4) . . ? C9 N8 Ni1 109.9(3) . . ? N8 C9 C10 110.7(4) . . ? N8 C9 H9A 109.5 . . ? C10 C9 H9A 109.5 . . ? N8 C9 H9B 109.5 . . ? C10 C9 H9B 109.5 . . ? H9A C9 H9B 108.1 . . ? O5 C10 C11 109.9(4) . . ? O5 C10 C9 112.9(4) . . ? C11 C10 C9 107.8(4) . . ? O5 C10 H10 108.7 . . ? C11 C10 H10 108.7 . . ? C9 C10 H10 108.7 . . ? N12 C11 C10 105.8(4) . . ? N12 C11 H11A 110.6 . . ? C10 C11 H11A 110.6 . . ? N12 C11 H11B 110.6 . . ? C10 C11 H11B 110.6 . . ? H11A C11 H11B 108.7 . . ? C13 N12 C11 121.4(4) . . ? C13 N12 Ni2 129.0(4) . . ? C11 N12 Ni2 109.1(3) . . ? N12 C13 C14 120.4(5) . . ? N12 C13 C20 120.9(5) . . ? C14 C13 C20 118.6(5) . . ? C15 C14 C19 117.1(5) . . ? C15 C14 C13 118.3(5) . . ? C19 C14 C13 124.5(5) . . ? C16 C15 C14 123.7(5) . . ? C16 C15 H15 118.1 . . ? C14 C15 H15 118.1 . . ? C15 C16 C17 118.8(5) . . ? C15 C16 H16 120.6 . . ? C17 C16 H16 120.6 . . ? C18 C17 C16 119.6(5) . . ? C18 C17 H17 120.2 . . ? C16 C17 H17 120.2 . . ? C17 C18 C19 123.4(5) . . ? C17 C18 H18 118.3 . . ? C19 C18 H18 118.3 . . ? O4 C19 C18 118.8(5) . . ? O4 C19 C14 123.7(5) . . ? C18 C19 C14 117.4(5) . . ? C13 C20 H20A 109.5 . . ? C13 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C13 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C7 C21 H21A 109.5 . . ? C7 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C7 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O2 C22 H22A 109.5 . . ? O2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? O2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 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 N8 Ni1 O1 C1 25.4(4) . . . . ? O2 Ni1 O1 C1 -157.3(4) . . . . ? O5 Ni1 O1 C1 93.1(9) . . . . ? O2 Ni1 O1 C1 119.8(4) 3_566 . . . ? O3 Ni1 O1 C1 -70.4(4) . . . . ? N8 Ni1 O1 Ni2 175.22(16) . . . 3_566 ? O2 Ni1 O1 Ni2 -7.50(14) . . . 3_566 ? O5 Ni1 O1 Ni2 -117.1(7) . . . 3_566 ? O2 Ni1 O1 Ni2 -90.38(14) 3_566 . . 3_566 ? O3 Ni1 O1 Ni2 79.42(15) . . . 3_566 ? O1 Ni1 O2 C22 137.0(4) . . . . ? O5 Ni1 O2 C22 -52.8(4) . . . . ? O2 Ni1 O2 C22 -131.5(4) 3_566 . . . ? O3 Ni1 O2 C22 47.9(4) . . . . ? O1 Ni1 O2 Ni2 7.60(14) . . . 3_566 ? O5 Ni1 O2 Ni2 177.83(14) . . . 3_566 ? O2 Ni1 O2 Ni2 99.11(17) 3_566 . . 3_566 ? O3 Ni1 O2 Ni2 -81.48(16) . . . 3_566 ? O1 Ni1 O2 Ni1 -91.51(15) . . . 3_566 ? O5 Ni1 O2 Ni1 78.72(15) . . . 3_566 ? O2 Ni1 O2 Ni1 0.0 3_566 . . 3_566 ? O3 Ni1 O2 Ni1 179.41(15) . . . 3_566 ? Ni1 O1 C1 C2 154.3(4) . . . . ? Ni2 O1 C1 C2 14.4(7) 3_566 . . . ? Ni1 O1 C1 C6 -28.1(7) . . . . ? Ni2 O1 C1 C6 -168.0(4) 3_566 . . . ? O1 C1 C2 C3 178.2(5) . . . . ? C6 C1 C2 C3 0.5(8) . . . . ? C1 C2 C3 C4 1.0(8) . . . . ? C2 C3 C4 C5 -1.6(8) . . . . ? O2 Ni2 O4 C19 -105.6(4) 3_566 . . . ? N12 Ni2 O4 C19 20.7(4) . . . . ? O1 Ni2 O4 C19 171.8(4) 3_566 . . . ? C3 C4 C5 C6 0.7(8) . . . . ? N8 Ni1 O5 C10 -11.5(3) . . . . ? O1 Ni1 O5 C10 -79.5(8) . . . . ? O2 Ni1 O5 C10 172.5(3) . . . . ? O2 Ni1 O5 C10 -106.6(3) 3_566 . . . ? O3 Ni1 O5 C10 83.7(3) . . . . ? N8 Ni1 O5 Ni2 99.21(16) . . . . ? O1 Ni1 O5 Ni2 31.2(8) . . . . ? O2 Ni1 O5 Ni2 -76.82(15) . . . . ? O2 Ni1 O5 Ni2 4.05(13) 3_566 . . . ? O3 Ni1 O5 Ni2 -165.65(13) . . . . ? O2 Ni2 O5 C10 108.6(3) 3_566 . . . ? N12 Ni2 O5 C10 -18.6(3) . . . . ? O1 Ni2 O5 C10 -169.6(3) 3_566 . . . ? O2 Ni2 O5 Ni1 -4.20(13) 3_566 . . . ? N12 Ni2 O5 Ni1 -131.40(16) . . . . ? O1 Ni2 O5 Ni1 77.63(15) 3_566 . . . ? C4 C5 C6 C1 0.8(8) . . . . ? C4 C5 C6 C7 -179.4(5) . . . . ? O1 C1 C6 C5 -179.0(5) . . . . ? C2 C1 C6 C5 -1.4(7) . . . . ? O1 C1 C6 C7 1.2(8) . . . . ? C2 C1 C6 C7 178.9(5) . . . . ? C5 C6 C7 N8 -155.2(5) . . . . ? C1 C6 C7 N8 24.6(8) . . . . ? C5 C6 C7 C21 26.2(7) . . . . ? C1 C6 C7 C21 -154.0(5) . . . . ? C6 C7 N8 C9 179.2(5) . . . . ? C21 C7 N8 C9 -2.3(7) . . . . ? C6 C7 N8 Ni1 -20.4(7) . . . . ? C21 C7 N8 Ni1 158.2(4) . . . . ? O1 Ni1 N8 C7 -1.1(5) . . . . ? O2 Ni1 N8 C7 -20.8(14) . . . . ? O5 Ni1 N8 C7 -171.7(5) . . . . ? O2 Ni1 N8 C7 -91.7(5) 3_566 . . . ? O3 Ni1 N8 C7 87.5(5) . . . . ? O1 Ni1 N8 C9 160.9(3) . . . . ? O5 Ni1 N8 C9 -9.7(3) . . . . ? O2 Ni1 N8 C9 70.3(3) 3_566 . . . ? O3 Ni1 N8 C9 -110.4(3) . . . . ? C7 N8 C9 C10 -168.8(5) . . . . ? Ni1 N8 C9 C10 27.5(5) . . . . ? Ni1 O5 C10 C11 150.1(3) . . . . ? Ni2 O5 C10 C11 44.5(4) . . . . ? Ni1 O5 C10 C9 29.7(5) . . . . ? Ni2 O5 C10 C9 -75.9(4) . . . . ? N8 C9 C10 O5 -39.0(6) . . . . ? N8 C9 C10 C11 -160.5(4) . . . . ? O5 C10 C11 N12 -54.7(5) . . . . ? C9 C10 C11 N12 68.7(5) . . . . ? C10 C11 N12 C13 -151.2(4) . . . . ? C10 C11 N12 Ni2 36.3(4) . . . . ? O4 Ni2 N12 C13 -0.1(4) . . . . ? O2 Ni2 N12 C13 100.4(4) 3_566 . . . ? O1 Ni2 N12 C13 -94.9(5) 3_566 . . . ? O5 Ni2 N12 C13 177.1(4) . . . . ? O4 Ni2 N12 C11 171.7(3) . . . . ? O2 Ni2 N12 C11 -87.8(3) 3_566 . . . ? O1 Ni2 N12 C11 76.9(5) 3_566 . . . ? O5 Ni2 N12 C11 -11.1(3) . . . . ? C11 N12 C13 C14 172.3(4) . . . . ? Ni2 N12 C13 C14 -16.8(7) . . . . ? C11 N12 C13 C20 -6.8(7) . . . . ? Ni2 N12 C13 C20 164.1(4) . . . . ? N12 C13 C14 C15 -159.5(5) . . . . ? C20 C13 C14 C15 19.6(7) . . . . ? N12 C13 C14 C19 18.3(7) . . . . ? C20 C13 C14 C19 -162.6(5) . . . . ? C19 C14 C15 C16 0.8(8) . . . . ? C13 C14 C15 C16 178.8(5) . . . . ? C14 C15 C16 C17 1.0(8) . . . . ? C15 C16 C17 C18 -1.8(8) . . . . ? C16 C17 C18 C19 0.7(8) . . . . ? Ni2 O4 C19 C18 158.4(4) . . . . ? Ni2 O4 C19 C14 -24.7(7) . . . . ? C17 C18 C19 O4 178.3(5) . . . . ? C17 C18 C19 C14 1.1(8) . . . . ? C15 C14 C19 O4 -178.9(5) . . . . ? C13 C14 C19 O4 3.3(8) . . . . ? C15 C14 C19 C18 -1.9(7) . . . . ? C13 C14 C19 C18 -179.7(5) . . . . ? 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 H32 O4 0.93(3) 1.90(3) 2.792(5) 161(5) 3_566 O6 H61W O1 0.90(3) 2.79(6) 3.274(5) 115(4) . O6 H62W O5 0.89(3) 1.93(4) 2.798(5) 167(6) 3_566 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.582 _refine_diff_density_min -0.781 _refine_diff_density_rms 0.124 # Attachment 'complex-2-CCDC-750006.cif.cif' data_ju389 _database_code_depnum_ccdc_archive 'CCDC 750006' #TrackingRef 'complex-2-CCDC-750006.cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H48 Co4 N5 O13 1+, (N O3 1-), 2(H2 O)' _chemical_formula_sum 'C40 H52 Co4 N6 O18' _chemical_formula_weight 1140.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.983(3) _cell_length_b 13.084(3) _cell_length_c 16.634(4) _cell_angle_alpha 86.68(2) _cell_angle_beta 88.72(3) _cell_angle_gamma 65.55(2) _cell_volume 2370.1(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 250 _cell_measurement_theta_min 3.5 _cell_measurement_theta_max 24.0 _exptl_crystal_description needle _exptl_crystal_colour brown _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.598 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1172 _exptl_absorpt_coefficient_mu 1.454 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.4334 _exptl_absorpt_correction_T_max 0.7799 _exptl_absorpt_process_details ; Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56 Cubic fit to sin(theta)/lambda - 24 parameters ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius dip1030 image plate diffractometer' _diffrn_measurement_method '\f-scans with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31286 _diffrn_reflns_av_R_equivalents 0.0490 _diffrn_reflns_av_sigmaI/netI 0.0511 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.23 _diffrn_reflns_theta_max 27.88 _reflns_number_total 10208 _reflns_number_gt 6250 _reflns_threshold_expression >2\s(I) _computing_data_collection 'XPRESS (MacScience, 2002)' _computing_cell_refinement 'Denzo (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELX97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELX97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep3 for Windows (Farrugia,1997)' _computing_publication_material 'Wingx (Farrugia, 1999)' _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^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0987P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10208 _refine_ls_number_parameters 640 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0841 _refine_ls_R_factor_gt 0.0533 _refine_ls_wR_factor_ref 0.1574 _refine_ls_wR_factor_gt 0.1449 _refine_ls_goodness_of_fit_ref 0.926 _refine_ls_restrained_S_all 0.926 _refine_ls_shift/su_max 0.002 _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 0.77290(4) 0.09210(4) 0.25806(3) 0.05098(14) Uani 1 1 d . . . Co2 Co 0.70144(4) 0.51048(4) 0.19719(3) 0.05134(14) Uani 1 1 d . . . Co3 Co 0.59944(4) 0.34339(4) 0.26320(3) 0.05119(14) Uani 1 1 d . . . Co4 Co 0.85762(5) 0.26326(4) 0.17466(3) 0.05357(15) Uani 1 1 d . . . O1 O 0.6117(2) 0.18924(19) 0.21827(15) 0.0528(6) Uani 1 1 d . . . O2 O 0.8520(2) 0.11346(19) 0.16322(15) 0.0555(6) Uani 1 1 d . . . O3 O 0.6937(2) 0.0754(2) 0.35356(15) 0.0575(6) Uani 1 1 d . . . N1 N 0.7706(3) -0.0262(2) 0.19908(19) 0.0591(8) Uani 1 1 d . . . N2 N 0.9326(3) -0.0064(2) 0.2987(2) 0.0581(8) Uani 1 1 d . . . C1 C 0.5267(3) 0.1462(3) 0.2230(2) 0.0549(8) Uani 1 1 d . . . C2 C 0.4049(4) 0.2179(4) 0.2374(2) 0.0650(10) Uani 1 1 d . . . H2 H 0.3848 0.2937 0.2433 0.078 Uiso 1 1 calc R . . C3 C 0.3136(4) 0.1801(4) 0.2433(3) 0.0792(12) Uani 1 1 d . . . H3 H 0.2331 0.2301 0.2525 0.095 Uiso 1 1 calc R . . C4 C 0.3416(5) 0.0683(4) 0.2354(3) 0.0873(14) Uani 1 1 d . . . H4 H 0.2807 0.0417 0.2406 0.105 Uiso 1 1 calc R . . C5 C 0.4601(5) -0.0038(4) 0.2198(3) 0.0779(12) Uani 1 1 d . . . H5 H 0.4779 -0.0792 0.2137 0.093 Uiso 1 1 calc R . . C6 C 0.5551(4) 0.0318(3) 0.2128(2) 0.0598(9) Uani 1 1 d . . . C7 C 0.6758(4) -0.0429(3) 0.1837(2) 0.0610(10) Uani 1 1 d . . . C8 C 0.6849(5) -0.1359(4) 0.1299(3) 0.0849(14) Uani 1 1 d . . . H8A H 0.7697 -0.1839 0.1213 0.127 Uiso 1 1 calc R . . H8B H 0.6462 -0.1035 0.0792 0.127 Uiso 1 1 calc R . . H8C H 0.6447 -0.1792 0.1554 0.127 Uiso 1 1 calc R . . C9 C 0.8862(4) -0.0761(3) 0.1528(3) 0.0705(11) Uani 1 1 d . . . H9A H 0.8691 -0.0832 0.0972 0.085 Uiso 1 1 calc R . . H9B H 0.9383 -0.1499 0.1760 0.085 Uiso 1 1 calc R . . C10 C 0.9492(4) 0.0059(3) 0.1580(3) 0.0621(10) Uani 1 1 d . . . H10 H 1.0001 0.0031 0.1106 0.074 Uiso 1 1 calc R . . C11 C 1.0230(4) -0.0208(3) 0.2340(3) 0.0686(11) Uani 1 1 d . . . H11A H 1.0854 -0.0974 0.2356 0.082 Uiso 1 1 calc R . . H11B H 1.0622 0.0302 0.2387 0.082 Uiso 1 1 calc R . . C12 C 0.9617(4) -0.0566(3) 0.3691(3) 0.0608(10) Uani 1 1 d . . . C13 C 1.0960(4) -0.1147(4) 0.3916(3) 0.0812(13) Uani 1 1 d . . . H13A H 1.1279 -0.1917 0.3773 0.122 Uiso 1 1 calc R . . H13B H 1.1051 -0.1120 0.4485 0.122 Uiso 1 1 calc R . . H13C H 1.1404 -0.0774 0.3631 0.122 Uiso 1 1 calc R . . C14 C 0.8709(4) -0.0617(3) 0.4263(2) 0.0605(9) Uani 1 1 d . . . C15 C 0.9084(4) -0.1372(4) 0.4943(3) 0.0775(12) Uani 1 1 d . . . H15 H 0.9917 -0.1807 0.5021 0.093 Uiso 1 1 calc R . . C16 C 0.8277(5) -0.1492(4) 0.5493(3) 0.0882(15) Uani 1 1 d . . . H16 H 0.8559 -0.2004 0.5933 0.106 Uiso 1 1 calc R . . C17 C 0.7030(5) -0.0841(4) 0.5386(3) 0.0833(13) Uani 1 1 d . . . H17 H 0.6475 -0.0899 0.5766 0.100 Uiso 1 1 calc R . . C18 C 0.6608(4) -0.0108(3) 0.4718(2) 0.0670(10) Uani 1 1 d . . . H18 H 0.5770 0.0309 0.4647 0.080 Uiso 1 1 calc R . . C19 C 0.7425(3) 0.0015(3) 0.4148(2) 0.0545(8) Uani 1 1 d . . . O1W O 0.5425(3) 0.2938(2) 0.37125(17) 0.0644(7) Uani 1 1 d D . . H1A H 0.582(3) 0.2245(18) 0.380(3) 0.097 Uiso 1 1 d D . . H1B H 0.472(2) 0.304(3) 0.392(3) 0.097 Uiso 1 1 d D . . O2W O 0.4309(3) 0.4642(2) 0.21904(19) 0.0670(7) Uani 1 1 d D . . H2A H 0.448(4) 0.522(3) 0.211(3) 0.100 Uiso 1 1 d D . . H2B H 0.360(3) 0.495(4) 0.245(3) 0.100 Uiso 1 1 d D . . O4 O 0.7801(2) 0.23138(19) 0.28789(14) 0.0508(5) Uani 1 1 d . . . C20 C 0.8364(4) 0.2361(3) 0.3624(2) 0.0673(10) Uani 1 1 d . . . H20A H 0.7978 0.2129 0.4065 0.101 Uiso 1 1 calc R . . H20B H 0.8269 0.3117 0.3688 0.101 Uiso 1 1 calc R . . H20C H 0.9221 0.1870 0.3614 0.101 Uiso 1 1 calc R . . O8 O 0.6781(2) 0.38178(19) 0.15796(14) 0.0509(5) Uani 1 1 d . . . C40 C 0.6237(4) 0.3886(4) 0.0807(2) 0.0701(11) Uani 1 1 d . . . H40A H 0.5508 0.4571 0.0749 0.105 Uiso 1 1 calc R . . H40B H 0.6030 0.3256 0.0766 0.105 Uiso 1 1 calc R . . H40C H 0.6808 0.3876 0.0391 0.105 Uiso 1 1 calc R . . N3 N 0.7607(3) 0.6020(3) 0.2505(2) 0.0607(8) Uani 1 1 d . . . N4 N 0.7553(3) 0.5544(2) 0.09749(19) 0.0572(7) Uani 1 1 d . . . O5 O 0.6420(2) 0.47647(18) 0.29921(14) 0.0532(6) Uani 1 1 d . . . O6 O 0.5377(2) 0.6082(2) 0.17848(16) 0.0593(6) Uani 1 1 d . . . O7 O 0.8655(2) 0.4038(2) 0.21372(15) 0.0568(6) Uani 1 1 d . . . C21 C 0.5720(4) 0.5656(3) 0.3416(2) 0.0569(9) Uani 1 1 d . . . C22 C 0.4754(4) 0.5608(3) 0.3873(2) 0.0662(10) Uani 1 1 d . . . H37 H 0.4632 0.4950 0.3902 0.079 Uiso 1 1 calc R . . C23 C 0.3971(4) 0.6523(4) 0.4286(3) 0.0762(12) Uani 1 1 d . . . H36 H 0.3322 0.6477 0.4579 0.091 Uiso 1 1 calc R . . C24 C 0.4149(4) 0.7496(4) 0.4266(3) 0.0753(12) Uani 1 1 d . . . H35 H 0.3605 0.8120 0.4525 0.090 Uiso 1 1 calc R . . C25 C 0.5125(4) 0.7535(3) 0.3865(3) 0.0718(11) Uani 1 1 d . . . H34 H 0.5260 0.8184 0.3876 0.086 Uiso 1 1 calc R . . C26 C 0.5957(4) 0.6621(3) 0.3425(2) 0.0603(9) Uani 1 1 d . . . C27 C 0.7079(4) 0.6629(3) 0.3095(3) 0.0665(10) Uani 1 1 d . . . C28 C 0.7683(5) 0.7286(4) 0.3499(3) 0.0890(14) Uani 1 1 d . . . H32A H 0.8011 0.6922 0.4012 0.133 Uiso 1 1 calc R . . H32B H 0.7086 0.8037 0.3576 0.133 Uiso 1 1 calc R . . H32C H 0.8334 0.7315 0.3164 0.133 Uiso 1 1 calc R . . C29 C 0.8927(4) 0.5691(4) 0.2303(3) 0.0731(11) Uani 1 1 d . . . H30A H 0.9418 0.5513 0.2790 0.088 Uiso 1 1 calc R . . H30B H 0.9035 0.6297 0.1996 0.088 Uiso 1 1 calc R . . C30 C 0.9302(4) 0.4662(3) 0.1806(3) 0.0641(10) Uani 1 1 d . . . H29 H 1.0189 0.4213 0.1839 0.077 Uiso 1 1 calc R . . C31 C 0.8894(4) 0.5003(3) 0.0932(3) 0.0668(10) Uani 1 1 d . . . H31A H 0.9218 0.5523 0.0702 0.080 Uiso 1 1 calc R . . H31B H 0.9165 0.4350 0.0609 0.080 Uiso 1 1 calc R . . C32 C 0.6896(4) 0.6265(3) 0.0410(2) 0.0621(10) Uani 1 1 d . . . C33 C 0.7504(5) 0.6373(4) -0.0379(3) 0.0861(14) Uani 1 1 d . . . H33A H 0.7520 0.7102 -0.0435 0.129 Uiso 1 1 calc R . . H33B H 0.7051 0.6284 -0.0817 0.129 Uiso 1 1 calc R . . H33C H 0.8328 0.5803 -0.0384 0.129 Uiso 1 1 calc R . . C34 C 0.5608(4) 0.6998(3) 0.0530(2) 0.0606(9) Uani 1 1 d . . . C35 C 0.5008(5) 0.7905(4) -0.0034(3) 0.0762(12) Uani 1 1 d . . . H24 H 0.5430 0.7995 -0.0490 0.091 Uiso 1 1 calc R . . C36 C 0.3824(5) 0.8652(4) 0.0076(4) 0.0954(16) Uani 1 1 d . . . H23 H 0.3451 0.9240 -0.0305 0.115 Uiso 1 1 calc R . . C37 C 0.3175(5) 0.8543(4) 0.0745(3) 0.0939(16) Uani 1 1 d . . . H37A H 0.2370 0.9056 0.0819 0.113 Uiso 1 1 calc R . . C38 C 0.3731(4) 0.7673(4) 0.1297(3) 0.0772(12) Uani 1 1 d . . . H38 H 0.3288 0.7598 0.1745 0.093 Uiso 1 1 calc R . . C39 C 0.4936(4) 0.6896(3) 0.1212(2) 0.0574(9) Uani 1 1 d . . . N5 N 1.0491(4) 0.1945(3) 0.0835(3) 0.0781(10) Uani 1 1 d . . . O9 O 1.0583(3) 0.1883(3) 0.1592(2) 0.0768(8) Uani 1 1 d . . . O10 O 0.9398(3) 0.2449(3) 0.05522(18) 0.0780(8) Uani 1 1 d . . . O11 O 1.1384(4) 0.1552(3) 0.0403(3) 0.1151(13) Uani 1 1 d . . . N6 N 0.1484(5) 0.6125(6) 0.2987(4) 0.1137(17) Uani 1 1 d . . . O12 O 0.2050(4) 0.5113(4) 0.2885(3) 0.1322(16) Uani 1 1 d . . . O13 O 0.1497(7) 0.6836(5) 0.2507(4) 0.185(3) Uani 1 1 d . . . O14 O 0.0799(6) 0.6457(6) 0.3555(5) 0.218(4) Uani 1 1 d . . . O3W O 0.3160(5) 0.3664(4) 0.4329(4) 0.162(2) Uani 1 1 d D . . H3A H 0.2852 0.3976 0.4763 0.243 Uiso 1 1 d RD . . H3B H 0.292(9) 0.415(4) 0.3947(16) 0.243 Uiso 1 1 d D . . O4W O 0.9199(6) 0.3642(5) -0.0981(3) 0.157(2) Uani 1 1 d D . . H4A H 0.870(7) 0.354(9) -0.062(4) 0.236 Uiso 1 1 d D . . H4B H 0.886(8) 0.358(9) -0.143(3) 0.236 Uiso 1 1 d 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 0.0499(3) 0.0471(3) 0.0526(3) 0.00116(19) -0.0039(2) -0.0170(2) Co2 0.0536(3) 0.0494(3) 0.0516(3) -0.00094(19) 0.0001(2) -0.0219(2) Co3 0.0496(3) 0.0489(3) 0.0527(3) 0.00105(19) -0.0007(2) -0.0184(2) Co4 0.0516(3) 0.0522(3) 0.0555(3) -0.0024(2) 0.0022(2) -0.0203(2) O1 0.0507(14) 0.0548(13) 0.0540(14) 0.0042(10) -0.0056(11) -0.0233(11) O2 0.0524(14) 0.0479(13) 0.0599(15) -0.0022(10) 0.0020(12) -0.0145(11) O3 0.0510(14) 0.0555(13) 0.0583(15) 0.0104(11) -0.0045(12) -0.0157(11) N1 0.063(2) 0.0516(16) 0.0589(19) 0.0005(13) -0.0010(15) -0.0201(15) N2 0.0517(18) 0.0517(16) 0.065(2) 0.0034(14) -0.0038(15) -0.0159(13) C1 0.060(2) 0.060(2) 0.049(2) 0.0061(15) -0.0087(16) -0.0296(18) C2 0.058(2) 0.072(2) 0.067(2) 0.0076(19) -0.0101(19) -0.031(2) C3 0.060(3) 0.094(3) 0.087(3) 0.012(2) -0.011(2) -0.038(2) C4 0.078(3) 0.097(3) 0.107(4) 0.009(3) -0.013(3) -0.058(3) C5 0.080(3) 0.072(3) 0.094(3) 0.007(2) -0.014(3) -0.045(2) C6 0.063(2) 0.067(2) 0.058(2) 0.0055(17) -0.0099(18) -0.0354(19) C7 0.074(3) 0.049(2) 0.063(2) 0.0008(16) -0.007(2) -0.0279(18) C8 0.112(4) 0.076(3) 0.083(3) -0.009(2) -0.006(3) -0.054(3) C9 0.071(3) 0.056(2) 0.077(3) -0.0105(19) 0.009(2) -0.0189(19) C10 0.064(2) 0.048(2) 0.067(2) -0.0069(16) 0.0112(19) -0.0174(17) C11 0.053(2) 0.057(2) 0.082(3) 0.0037(19) 0.002(2) -0.0094(17) C12 0.058(2) 0.0472(19) 0.069(3) 0.0037(17) -0.0130(19) -0.0138(16) C13 0.058(3) 0.088(3) 0.089(3) 0.014(2) -0.018(2) -0.023(2) C14 0.064(2) 0.057(2) 0.059(2) 0.0041(17) -0.0142(19) -0.0237(18) C15 0.076(3) 0.074(3) 0.072(3) 0.017(2) -0.019(2) -0.022(2) C16 0.088(4) 0.096(3) 0.069(3) 0.028(2) -0.018(3) -0.030(3) C17 0.093(4) 0.096(3) 0.065(3) 0.018(2) -0.003(3) -0.047(3) C18 0.071(3) 0.068(2) 0.064(3) 0.0056(19) -0.005(2) -0.031(2) C19 0.060(2) 0.0488(19) 0.054(2) -0.0004(15) -0.0070(17) -0.0214(16) O1W 0.0688(18) 0.0597(15) 0.0594(16) 0.0028(12) 0.0079(14) -0.0223(13) O2W 0.0521(15) 0.0611(15) 0.081(2) 0.0113(14) -0.0053(14) -0.0186(13) O4 0.0517(14) 0.0484(12) 0.0508(13) -0.0013(10) -0.0054(11) -0.0191(10) C20 0.070(3) 0.070(2) 0.062(2) -0.0003(18) -0.016(2) -0.028(2) O8 0.0540(14) 0.0509(13) 0.0499(13) 0.0004(10) -0.0034(11) -0.0240(11) C40 0.076(3) 0.080(3) 0.060(2) -0.0006(19) -0.014(2) -0.038(2) N3 0.063(2) 0.0609(19) 0.061(2) -0.0078(14) 0.0025(16) -0.0277(15) N4 0.0617(19) 0.0554(17) 0.0580(19) -0.0059(14) 0.0051(15) -0.0274(15) O5 0.0583(15) 0.0457(13) 0.0527(14) -0.0027(10) 0.0029(11) -0.0186(11) O6 0.0560(15) 0.0544(14) 0.0599(15) 0.0083(11) -0.0008(12) -0.0166(11) O7 0.0546(15) 0.0567(14) 0.0615(16) -0.0018(11) 0.0001(12) -0.0258(12) C21 0.065(2) 0.052(2) 0.050(2) -0.0008(15) -0.0068(17) -0.0195(17) C22 0.066(3) 0.059(2) 0.068(3) -0.0081(18) 0.011(2) -0.0193(19) C23 0.072(3) 0.088(3) 0.065(3) -0.009(2) 0.011(2) -0.030(2) C24 0.079(3) 0.064(3) 0.073(3) -0.015(2) 0.003(2) -0.018(2) C25 0.086(3) 0.056(2) 0.070(3) -0.0067(19) -0.003(2) -0.026(2) C26 0.071(3) 0.054(2) 0.052(2) -0.0020(15) -0.0007(18) -0.0223(18) C27 0.075(3) 0.065(2) 0.064(3) -0.0044(18) -0.003(2) -0.034(2) C28 0.109(4) 0.091(3) 0.086(3) -0.024(3) 0.009(3) -0.058(3) C29 0.072(3) 0.082(3) 0.078(3) -0.010(2) 0.002(2) -0.043(2) C30 0.058(2) 0.062(2) 0.078(3) -0.0018(19) -0.003(2) -0.0311(19) C31 0.069(3) 0.066(2) 0.070(3) -0.0010(19) 0.012(2) -0.034(2) C32 0.078(3) 0.059(2) 0.055(2) 0.0029(17) -0.001(2) -0.035(2) C33 0.095(4) 0.085(3) 0.070(3) 0.008(2) 0.015(3) -0.031(3) C34 0.073(3) 0.058(2) 0.056(2) 0.0044(16) -0.0091(19) -0.0324(19) C35 0.093(3) 0.069(3) 0.066(3) 0.012(2) -0.009(2) -0.034(2) C36 0.104(4) 0.072(3) 0.100(4) 0.024(3) -0.028(3) -0.028(3) C37 0.082(3) 0.080(3) 0.092(4) 0.020(3) -0.008(3) -0.008(2) C38 0.069(3) 0.069(3) 0.079(3) 0.010(2) -0.004(2) -0.016(2) C39 0.064(2) 0.052(2) 0.058(2) 0.0009(16) -0.0074(18) -0.0258(17) N5 0.080(3) 0.074(2) 0.086(3) -0.016(2) 0.022(2) -0.037(2) O9 0.0611(18) 0.087(2) 0.084(2) -0.0109(16) 0.0041(16) -0.0318(15) O10 0.088(2) 0.0795(19) 0.0659(19) -0.0016(14) 0.0079(16) -0.0346(17) O11 0.096(3) 0.126(3) 0.122(3) -0.041(2) 0.057(2) -0.043(2) N6 0.080(3) 0.111(4) 0.144(5) -0.027(4) -0.004(3) -0.031(3) O12 0.099(3) 0.093(3) 0.186(5) -0.012(3) 0.037(3) -0.022(2) O13 0.282(8) 0.109(4) 0.162(5) 0.019(4) -0.052(5) -0.079(5) O14 0.171(6) 0.254(7) 0.286(9) -0.149(7) 0.126(6) -0.134(6) O3W 0.107(4) 0.157(4) 0.194(6) 0.022(4) 0.048(4) -0.034(3) O4W 0.235(7) 0.150(4) 0.116(4) -0.006(4) 0.014(4) -0.111(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O3 1.881(3) . ? Co1 O2 1.889(3) . ? Co1 N1 1.889(3) . ? Co1 N2 1.923(3) . ? Co1 O1 1.926(2) . ? Co1 O4 1.952(2) . ? Co2 O6 1.867(3) . ? Co2 N3 1.892(3) . ? Co2 O7 1.897(3) . ? Co2 N4 1.909(3) . ? Co2 O5 1.925(2) . ? Co2 O8 1.966(2) . ? Co3 O1W 2.072(3) . ? Co3 O4 2.085(2) . ? Co3 O2W 2.099(3) . ? Co3 O8 2.103(3) . ? Co3 O5 2.126(2) . ? Co3 O1 2.138(2) . ? Co4 O2 2.009(2) . ? Co4 O7 2.025(2) . ? Co4 O8 2.080(3) . ? Co4 O4 2.176(3) . ? Co4 O10 2.179(3) . ? Co4 O9 2.205(3) . ? O1 C1 1.352(4) . ? O2 C10 1.413(4) . ? O3 C19 1.326(4) . ? N1 C7 1.276(5) . ? N1 C9 1.484(5) . ? N2 C12 1.290(5) . ? N2 C11 1.473(5) . ? C1 C2 1.395(5) . ? C1 C6 1.411(5) . ? C2 C3 1.374(6) . ? C2 H2 0.9300 . ? C3 C4 1.372(7) . ? C3 H3 0.9300 . ? C4 C5 1.369(7) . ? C4 H4 0.9300 . ? C5 C6 1.398(6) . ? C5 H5 0.9300 . ? C6 C7 1.461(6) . ? C7 C8 1.518(5) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 C10 1.553(6) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.498(6) . ? C10 H10 0.9800 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C14 1.449(6) . ? C12 C13 1.513(5) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C15 1.408(5) . ? C14 C19 1.424(5) . ? C15 C16 1.366(7) . ? C15 H15 0.9300 . ? C16 C17 1.390(7) . ? C16 H16 0.9300 . ? C17 C18 1.382(6) . ? C17 H17 0.9300 . ? C18 C19 1.398(5) . ? C18 H18 0.9300 . ? O1W H1A 0.838(18) . ? O1W H1B 0.860(18) . ? O2W H2A 0.865(19) . ? O2W H2B 0.887(18) . ? O4 C20 1.440(4) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? O8 C40 1.435(5) . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? N3 C27 1.282(5) . ? N3 C29 1.494(5) . ? N4 C32 1.307(5) . ? N4 C31 1.466(5) . ? O5 C21 1.348(4) . ? O6 C39 1.326(4) . ? O7 C30 1.422(4) . ? C21 C22 1.392(5) . ? C21 C26 1.406(5) . ? C22 C23 1.387(5) . ? C22 H37 0.9300 . ? C23 C24 1.374(6) . ? C23 H36 0.9300 . ? C24 C25 1.351(6) . ? C24 H35 0.9300 . ? C25 C26 1.429(5) . ? C25 H34 0.9300 . ? C26 C27 1.445(6) . ? C27 C28 1.522(6) . ? C28 H32A 0.9600 . ? C28 H32B 0.9600 . ? C28 H32C 0.9600 . ? C29 C30 1.519(6) . ? C29 H30A 0.9700 . ? C29 H30B 0.9700 . ? C30 C31 1.526(6) . ? C30 H29 0.9800 . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 C34 1.458(6) . ? C32 C33 1.514(6) . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 C39 1.409(5) . ? C34 C35 1.414(5) . ? C35 C36 1.365(7) . ? C35 H24 0.9300 . ? C36 C37 1.378(7) . ? C36 H23 0.9300 . ? C37 C38 1.364(6) . ? C37 H37A 0.9300 . ? C38 C39 1.390(6) . ? C38 H38 0.9300 . ? N5 O11 1.217(5) . ? N5 O9 1.261(5) . ? N5 O10 1.284(5) . ? N6 O13 1.196(7) . ? N6 O14 1.213(7) . ? N6 O12 1.233(6) . ? O3W H3A 0.8500 . ? O3W H3B 0.84(2) . ? O4W H4A 0.88(2) . ? O4W H4B 0.88(2) . ? 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 O3 Co1 O2 178.14(10) . . ? O3 Co1 N1 101.24(13) . . ? O2 Co1 N1 80.58(13) . . ? O3 Co1 N2 93.19(13) . . ? O2 Co1 N2 87.17(13) . . ? N1 Co1 N2 89.44(14) . . ? O3 Co1 O1 86.03(11) . . ? O2 Co1 O1 93.62(11) . . ? N1 Co1 O1 90.18(13) . . ? N2 Co1 O1 179.05(12) . . ? O3 Co1 O4 94.11(11) . . ? O2 Co1 O4 84.04(11) . . ? N1 Co1 O4 163.41(12) . . ? N2 Co1 O4 95.99(12) . . ? O1 Co1 O4 84.61(10) . . ? O6 Co2 N3 102.00(13) . . ? O6 Co2 O7 176.36(11) . . ? N3 Co2 O7 81.61(13) . . ? O6 Co2 N4 93.31(13) . . ? N3 Co2 N4 88.97(14) . . ? O7 Co2 N4 87.14(13) . . ? O6 Co2 O5 84.40(11) . . ? N3 Co2 O5 88.58(13) . . ? O7 Co2 O5 95.33(11) . . ? N4 Co2 O5 176.24(11) . . ? O6 Co2 O8 92.63(11) . . ? N3 Co2 O8 163.98(12) . . ? O7 Co2 O8 83.73(10) . . ? N4 Co2 O8 96.74(12) . . ? O5 Co2 O8 86.36(10) . . ? O1W Co3 O4 90.57(11) . . ? O1W Co3 O2W 99.93(12) . . ? O4 Co3 O2W 169.49(11) . . ? O1W Co3 O8 173.34(11) . . ? O4 Co3 O8 82.80(10) . . ? O2W Co3 O8 86.69(11) . . ? O1W Co3 O5 101.23(11) . . ? O4 Co3 O5 89.06(9) . . ? O2W Co3 O5 88.63(10) . . ? O8 Co3 O5 78.05(9) . . ? O1W Co3 O1 87.04(10) . . ? O4 Co3 O1 76.36(9) . . ? O2W Co3 O1 104.26(11) . . ? O8 Co3 O1 92.05(9) . . ? O5 Co3 O1 163.38(10) . . ? O2 Co4 O7 166.72(11) . . ? O2 Co4 O8 105.51(10) . . ? O7 Co4 O8 77.82(10) . . ? O2 Co4 O4 75.73(10) . . ? O7 Co4 O4 92.33(10) . . ? O8 Co4 O4 81.18(10) . . ? O2 Co4 O10 87.14(11) . . ? O7 Co4 O10 104.58(11) . . ? O8 Co4 O10 105.07(12) . . ? O4 Co4 O10 162.82(10) . . ? O2 Co4 O9 91.08(11) . . ? O7 Co4 O9 89.75(11) . . ? O8 Co4 O9 156.85(11) . . ? O4 Co4 O9 119.20(12) . . ? O10 Co4 O9 58.92(13) . . ? C1 O1 Co1 116.3(2) . . ? C1 O1 Co3 127.9(2) . . ? Co1 O1 Co3 98.53(11) . . ? C10 O2 Co1 101.1(2) . . ? C10 O2 Co4 129.7(2) . . ? Co1 O2 Co4 103.93(11) . . ? C19 O3 Co1 126.9(2) . . ? C7 N1 C9 122.6(3) . . ? C7 N1 Co1 125.9(3) . . ? C9 N1 Co1 109.3(3) . . ? C12 N2 C11 122.9(3) . . ? C12 N2 Co1 128.4(3) . . ? C11 N2 Co1 108.6(2) . . ? O1 C1 C2 118.9(3) . . ? O1 C1 C6 122.9(3) . . ? C2 C1 C6 118.1(4) . . ? C3 C2 C1 122.2(4) . . ? C3 C2 H2 118.9 . . ? C1 C2 H2 118.9 . . ? C4 C3 C2 119.8(5) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C5 C4 C3 119.4(4) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? C4 C5 C6 122.4(4) . . ? C4 C5 H5 118.8 . . ? C6 C5 H5 118.8 . . ? C5 C6 C1 118.1(4) . . ? C5 C6 C7 120.8(4) . . ? C1 C6 C7 120.5(3) . . ? N1 C7 C6 120.7(3) . . ? N1 C7 C8 120.6(4) . . ? C6 C7 C8 118.6(4) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N1 C9 C10 105.8(3) . . ? N1 C9 H9A 110.6 . . ? C10 C9 H9A 110.6 . . ? N1 C9 H9B 110.6 . . ? C10 C9 H9B 110.6 . . ? H9A C9 H9B 108.7 . . ? O2 C10 C11 108.1(3) . . ? O2 C10 C9 105.1(3) . . ? C11 C10 C9 109.7(3) . . ? O2 C10 H10 111.2 . . ? C11 C10 H10 111.2 . . ? C9 C10 H10 111.2 . . ? N2 C11 C10 104.3(3) . . ? N2 C11 H11A 110.9 . . ? C10 C11 H11A 110.9 . . ? N2 C11 H11B 110.9 . . ? C10 C11 H11B 110.9 . . ? H11A C11 H11B 108.9 . . ? N2 C12 C14 122.4(4) . . ? N2 C12 C13 118.4(4) . . ? C14 C12 C13 119.1(4) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 C19 117.2(4) . . ? C15 C14 C12 119.6(4) . . ? C19 C14 C12 123.1(3) . . ? C16 C15 C14 122.9(4) . . ? C16 C15 H15 118.6 . . ? C14 C15 H15 118.6 . . ? C15 C16 C17 119.2(4) . . ? C15 C16 H16 120.4 . . ? C17 C16 H16 120.4 . . ? C18 C17 C16 120.4(5) . . ? C18 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? C17 C18 C19 120.9(4) . . ? C17 C18 H18 119.6 . . ? C19 C18 H18 119.6 . . ? O3 C19 C18 116.6(3) . . ? O3 C19 C14 124.0(4) . . ? C18 C19 C14 119.4(3) . . ? Co3 O1W H1A 109(3) . . ? Co3 O1W H1B 135(3) . . ? H1A O1W H1B 102(3) . . ? Co3 O2W H2A 101(3) . . ? Co3 O2W H2B 128(3) . . ? H2A O2W H2B 100(2) . . ? C20 O4 Co1 120.8(2) . . ? C20 O4 Co3 119.7(2) . . ? Co1 O4 Co3 99.51(11) . . ? C20 O4 Co4 119.0(2) . . ? Co1 O4 Co4 95.96(10) . . ? Co3 O4 Co4 96.63(10) . . ? O4 C20 H20A 109.5 . . ? O4 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? O4 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C40 O8 Co2 121.0(2) . . ? C40 O8 Co4 116.9(2) . . ? Co2 O8 Co4 97.13(10) . . ? C40 O8 Co3 120.5(2) . . ? Co2 O8 Co3 97.41(10) . . ? Co4 O8 Co3 99.10(10) . . ? O8 C40 H40A 109.5 . . ? O8 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? O8 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C27 N3 C29 122.8(4) . . ? C27 N3 Co2 125.5(3) . . ? C29 N3 Co2 109.6(2) . . ? C32 N4 C31 121.6(3) . . ? C32 N4 Co2 128.5(3) . . ? C31 N4 Co2 109.8(2) . . ? C21 O5 Co2 116.0(2) . . ? C21 O5 Co3 128.3(2) . . ? Co2 O5 Co3 97.91(10) . . ? C39 O6 Co2 127.4(3) . . ? C30 O7 Co2 100.4(2) . . ? C30 O7 Co4 129.2(2) . . ? Co2 O7 Co4 101.31(11) . . ? O5 C21 C22 119.1(3) . . ? O5 C21 C26 121.9(4) . . ? C22 C21 C26 119.0(3) . . ? C23 C22 C21 121.2(4) . . ? C23 C22 H37 119.4 . . ? C21 C22 H37 119.4 . . ? C24 C23 C22 120.4(4) . . ? C24 C23 H36 119.8 . . ? C22 C23 H36 119.8 . . ? C25 C24 C23 119.1(4) . . ? C25 C24 H35 120.4 . . ? C23 C24 H35 120.4 . . ? C24 C25 C26 122.8(4) . . ? C24 C25 H34 118.6 . . ? C26 C25 H34 118.6 . . ? C21 C26 C25 117.2(4) . . ? C21 C26 C27 121.0(3) . . ? C25 C26 C27 121.3(4) . . ? N3 C27 C26 120.0(4) . . ? N3 C27 C28 120.4(4) . . ? C26 C27 C28 119.4(4) . . ? C27 C28 H32A 109.5 . . ? C27 C28 H32B 109.5 . . ? H32A C28 H32B 109.5 . . ? C27 C28 H32C 109.5 . . ? H32A C28 H32C 109.5 . . ? H32B C28 H32C 109.5 . . ? N3 C29 C30 105.9(3) . . ? N3 C29 H30A 110.6 . . ? C30 C29 H30A 110.6 . . ? N3 C29 H30B 110.6 . . ? C30 C29 H30B 110.6 . . ? H30A C29 H30B 108.7 . . ? O7 C30 C29 105.9(3) . . ? O7 C30 C31 107.8(3) . . ? C29 C30 C31 110.8(3) . . ? O7 C30 H29 110.7 . . ? C29 C30 H29 110.7 . . ? C31 C30 H29 110.7 . . ? N4 C31 C30 104.2(3) . . ? N4 C31 H31A 110.9 . . ? C30 C31 H31A 110.9 . . ? N4 C31 H31B 110.9 . . ? C30 C31 H31B 110.9 . . ? H31A C31 H31B 108.9 . . ? N4 C32 C34 121.8(4) . . ? N4 C32 C33 119.0(4) . . ? C34 C32 C33 119.2(4) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C39 C34 C35 117.4(4) . . ? C39 C34 C32 123.2(3) . . ? C35 C34 C32 119.2(4) . . ? C36 C35 C34 121.4(5) . . ? C36 C35 H24 119.3 . . ? C34 C35 H24 119.3 . . ? C35 C36 C37 120.7(4) . . ? C35 C36 H23 119.7 . . ? C37 C36 H23 119.7 . . ? C38 C37 C36 119.1(5) . . ? C38 C37 H37A 120.5 . . ? C36 C37 H37A 120.5 . . ? C37 C38 C39 122.3(5) . . ? C37 C38 H38 118.9 . . ? C39 C38 H38 118.9 . . ? O6 C39 C38 116.9(4) . . ? O6 C39 C34 123.9(3) . . ? C38 C39 C34 119.1(4) . . ? O11 N5 O9 121.8(5) . . ? O11 N5 O10 122.4(5) . . ? O9 N5 O10 115.8(4) . . ? N5 O9 Co4 92.2(3) . . ? N5 O10 Co4 92.8(2) . . ? O13 N6 O14 115.7(7) . . ? O13 N6 O12 122.6(7) . . ? O14 N6 O12 121.4(8) . . ? H3A O3W H3B 108.4 . . ? H4A O4W H4B 100(3) . . ? 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 O3 Co1 O1 C1 -53.2(2) . . . . ? O2 Co1 O1 C1 128.6(2) . . . . ? N1 Co1 O1 C1 48.0(3) . . . . ? N2 Co1 O1 C1 -18(8) . . . . ? O4 Co1 O1 C1 -147.7(3) . . . . ? O3 Co1 O1 Co3 86.82(11) . . . . ? O2 Co1 O1 Co3 -91.35(11) . . . . ? N1 Co1 O1 Co3 -171.92(12) . . . . ? N2 Co1 O1 Co3 122(8) . . . . ? O4 Co1 O1 Co3 -7.69(10) . . . . ? O1W Co3 O1 C1 49.2(3) . . . . ? O4 Co3 O1 C1 140.5(3) . . . . ? O2W Co3 O1 C1 -50.3(3) . . . . ? O8 Co3 O1 C1 -137.4(3) . . . . ? O5 Co3 O1 C1 169.8(3) . . . . ? O1W Co3 O1 Co1 -83.93(12) . . . . ? O4 Co3 O1 Co1 7.38(10) . . . . ? O2W Co3 O1 Co1 176.57(11) . . . . ? O8 Co3 O1 Co1 89.46(11) . . . . ? O5 Co3 O1 Co1 36.6(4) . . . . ? O3 Co1 O2 C10 136(3) . . . . ? N1 Co1 O2 C10 -55.1(2) . . . . ? N2 Co1 O2 C10 34.8(2) . . . . ? O1 Co1 O2 C10 -144.7(2) . . . . ? O4 Co1 O2 C10 131.1(2) . . . . ? O3 Co1 O2 Co4 0(3) . . . . ? N1 Co1 O2 Co4 168.92(14) . . . . ? N2 Co1 O2 Co4 -101.18(13) . . . . ? O1 Co1 O2 Co4 79.34(12) . . . . ? O4 Co1 O2 Co4 -4.85(11) . . . . ? O7 Co4 O2 C10 -86.7(5) . . . . ? O8 Co4 O2 C10 170.4(3) . . . . ? O4 Co4 O2 C10 -113.2(3) . . . . ? O10 Co4 O2 C10 65.6(3) . . . . ? O9 Co4 O2 C10 6.8(3) . . . . ? O7 Co4 O2 Co1 30.9(5) . . . . ? O8 Co4 O2 Co1 -71.96(13) . . . . ? O4 Co4 O2 Co1 4.46(10) . . . . ? O10 Co4 O2 Co1 -176.81(13) . . . . ? O9 Co4 O2 Co1 124.38(14) . . . . ? O2 Co1 O3 C19 -112(3) . . . . ? N1 Co1 O3 C19 79.4(3) . . . . ? N2 Co1 O3 C19 -10.6(3) . . . . ? O1 Co1 O3 C19 168.8(3) . . . . ? O4 Co1 O3 C19 -106.9(3) . . . . ? O3 Co1 N1 C7 53.7(3) . . . . ? O2 Co1 N1 C7 -125.9(3) . . . . ? N2 Co1 N1 C7 146.8(3) . . . . ? O1 Co1 N1 C7 -32.3(3) . . . . ? O4 Co1 N1 C7 -103.7(5) . . . . ? O3 Co1 N1 C9 -143.3(3) . . . . ? O2 Co1 N1 C9 37.1(3) . . . . ? N2 Co1 N1 C9 -50.1(3) . . . . ? O1 Co1 N1 C9 130.8(3) . . . . ? O4 Co1 N1 C9 59.3(5) . . . . ? O3 Co1 N2 C12 -2.4(3) . . . . ? O2 Co1 N2 C12 175.8(3) . . . . ? N1 Co1 N2 C12 -103.6(3) . . . . ? O1 Co1 N2 C12 -37(8) . . . . ? O4 Co1 N2 C12 92.1(3) . . . . ? O3 Co1 N2 C11 175.8(3) . . . . ? O2 Co1 N2 C11 -6.1(3) . . . . ? N1 Co1 N2 C11 74.5(3) . . . . ? O1 Co1 N2 C11 141(8) . . . . ? O4 Co1 N2 C11 -89.8(3) . . . . ? Co1 O1 C1 C2 146.2(3) . . . . ? Co3 O1 C1 C2 19.8(5) . . . . ? Co1 O1 C1 C6 -34.9(4) . . . . ? Co3 O1 C1 C6 -161.3(3) . . . . ? O1 C1 C2 C3 -179.8(4) . . . . ? C6 C1 C2 C3 1.2(6) . . . . ? C1 C2 C3 C4 0.5(7) . . . . ? C2 C3 C4 C5 -1.6(8) . . . . ? C3 C4 C5 C6 1.1(8) . . . . ? C4 C5 C6 C1 0.6(7) . . . . ? C4 C5 C6 C7 -170.2(4) . . . . ? O1 C1 C6 C5 179.3(4) . . . . ? C2 C1 C6 C5 -1.7(6) . . . . ? O1 C1 C6 C7 -9.8(6) . . . . ? C2 C1 C6 C7 169.1(4) . . . . ? C9 N1 C7 C6 -161.6(4) . . . . ? Co1 N1 C7 C6 -0.6(5) . . . . ? C9 N1 C7 C8 14.2(6) . . . . ? Co1 N1 C7 C8 175.2(3) . . . . ? C5 C6 C7 N1 -159.0(4) . . . . ? C1 C6 C7 N1 30.4(6) . . . . ? C5 C6 C7 C8 25.2(6) . . . . ? C1 C6 C7 C8 -145.5(4) . . . . ? C7 N1 C9 C10 152.1(4) . . . . ? Co1 N1 C9 C10 -11.6(4) . . . . ? Co1 O2 C10 C11 -57.7(3) . . . . ? Co4 O2 C10 C11 61.1(4) . . . . ? Co1 O2 C10 C9 59.4(3) . . . . ? Co4 O2 C10 C9 178.2(2) . . . . ? N1 C9 C10 O2 -31.0(4) . . . . ? N1 C9 C10 C11 85.1(4) . . . . ? C12 N2 C11 C10 155.4(3) . . . . ? Co1 N2 C11 C10 -22.9(3) . . . . ? O2 C10 C11 N2 54.4(4) . . . . ? C9 C10 C11 N2 -59.8(4) . . . . ? C11 N2 C12 C14 -166.3(3) . . . . ? Co1 N2 C12 C14 11.6(5) . . . . ? C11 N2 C12 C13 12.0(6) . . . . ? Co1 N2 C12 C13 -170.1(3) . . . . ? N2 C12 C14 C15 166.3(4) . . . . ? C13 C12 C14 C15 -12.0(6) . . . . ? N2 C12 C14 C19 -9.7(6) . . . . ? C13 C12 C14 C19 172.1(4) . . . . ? C19 C14 C15 C16 -1.7(7) . . . . ? C12 C14 C15 C16 -177.8(4) . . . . ? C14 C15 C16 C17 -0.5(8) . . . . ? C15 C16 C17 C18 2.1(8) . . . . ? C16 C17 C18 C19 -1.6(7) . . . . ? Co1 O3 C19 C18 -167.4(2) . . . . ? Co1 O3 C19 C14 14.5(5) . . . . ? C17 C18 C19 O3 -178.8(4) . . . . ? C17 C18 C19 C14 -0.6(6) . . . . ? C15 C14 C19 O3 -179.9(3) . . . . ? C12 C14 C19 O3 -3.8(6) . . . . ? C15 C14 C19 C18 2.2(5) . . . . ? C12 C14 C19 C18 178.2(3) . . . . ? O3 Co1 O4 C20 55.5(3) . . . . ? O2 Co1 O4 C20 -124.7(3) . . . . ? N1 Co1 O4 C20 -146.7(4) . . . . ? N2 Co1 O4 C20 -38.2(3) . . . . ? O1 Co1 O4 C20 141.1(3) . . . . ? O3 Co1 O4 Co3 -77.70(11) . . . . ? O2 Co1 O4 Co3 102.13(11) . . . . ? N1 Co1 O4 Co3 80.1(4) . . . . ? N2 Co1 O4 Co3 -171.35(12) . . . . ? O1 Co1 O4 Co3 7.91(10) . . . . ? O3 Co1 O4 Co4 -175.47(9) . . . . ? O2 Co1 O4 Co4 4.37(9) . . . . ? N1 Co1 O4 Co4 -17.7(5) . . . . ? N2 Co1 O4 Co4 90.88(13) . . . . ? O1 Co1 O4 Co4 -89.86(11) . . . . ? O1W Co3 O4 C20 -54.4(3) . . . . ? O2W Co3 O4 C20 124.2(6) . . . . ? O8 Co3 O4 C20 124.9(3) . . . . ? O5 Co3 O4 C20 46.9(3) . . . . ? O1 Co3 O4 C20 -141.2(3) . . . . ? O1W Co3 O4 Co1 79.51(12) . . . . ? O2W Co3 O4 Co1 -102.0(6) . . . . ? O8 Co3 O4 Co1 -101.18(11) . . . . ? O5 Co3 O4 Co1 -179.26(10) . . . . ? O1 Co3 O4 Co1 -7.30(10) . . . . ? O1W Co3 O4 Co4 176.72(10) . . . . ? O2W Co3 O4 Co4 -4.8(6) . . . . ? O8 Co3 O4 Co4 -3.98(8) . . . . ? O5 Co3 O4 Co4 -82.06(10) . . . . ? O1 Co3 O4 Co4 89.91(10) . . . . ? O2 Co4 O4 C20 126.1(3) . . . . ? O7 Co4 O4 C20 -48.0(3) . . . . ? O8 Co4 O4 C20 -125.3(3) . . . . ? O10 Co4 O4 C20 121.8(4) . . . . ? O9 Co4 O4 C20 43.0(3) . . . . ? O2 Co4 O4 Co1 -4.21(9) . . . . ? O7 Co4 O4 Co1 -178.34(10) . . . . ? O8 Co4 O4 Co1 104.37(10) . . . . ? O10 Co4 O4 Co1 -8.5(4) . . . . ? O9 Co4 O4 Co1 -87.33(13) . . . . ? O2 Co4 O4 Co3 -104.54(11) . . . . ? O7 Co4 O4 Co3 81.33(10) . . . . ? O8 Co4 O4 Co3 4.04(8) . . . . ? O10 Co4 O4 Co3 -108.9(4) . . . . ? O9 Co4 O4 Co3 172.34(10) . . . . ? O6 Co2 O8 C40 52.3(3) . . . . ? N3 Co2 O8 C40 -151.6(4) . . . . ? O7 Co2 O8 C40 -127.7(3) . . . . ? N4 Co2 O8 C40 -41.4(3) . . . . ? O5 Co2 O8 C40 136.5(3) . . . . ? O6 Co2 O8 Co4 179.63(10) . . . . ? N3 Co2 O8 Co4 -24.3(5) . . . . ? O7 Co2 O8 Co4 -0.38(10) . . . . ? N4 Co2 O8 Co4 85.99(13) . . . . ? O5 Co2 O8 Co4 -96.15(11) . . . . ? O6 Co2 O8 Co3 -80.17(11) . . . . ? N3 Co2 O8 Co3 75.9(5) . . . . ? O7 Co2 O8 Co3 99.82(11) . . . . ? N4 Co2 O8 Co3 -173.82(11) . . . . ? O5 Co2 O8 Co3 4.05(10) . . . . ? O2 Co4 O8 C40 -62.6(3) . . . . ? O7 Co4 O8 C40 130.6(3) . . . . ? O4 Co4 O8 C40 -135.1(3) . . . . ? O10 Co4 O8 C40 28.6(3) . . . . ? O9 Co4 O8 C40 71.7(4) . . . . ? O2 Co4 O8 Co2 167.11(9) . . . . ? O7 Co4 O8 Co2 0.36(10) . . . . ? O4 Co4 O8 Co2 94.69(11) . . . . ? O10 Co4 O8 Co2 -101.68(12) . . . . ? O9 Co4 O8 Co2 -58.5(3) . . . . ? O2 Co4 O8 Co3 68.39(12) . . . . ? O7 Co4 O8 Co3 -98.36(11) . . . . ? O4 Co4 O8 Co3 -4.03(8) . . . . ? O10 Co4 O8 Co3 159.60(11) . . . . ? O9 Co4 O8 Co3 -157.3(2) . . . . ? O1W Co3 O8 C40 138.9(8) . . . . ? O4 Co3 O8 C40 132.9(3) . . . . ? O2W Co3 O8 C40 -47.3(3) . . . . ? O5 Co3 O8 C40 -136.6(3) . . . . ? O1 Co3 O8 C40 56.9(3) . . . . ? O1W Co3 O8 Co2 -88.3(9) . . . . ? O4 Co3 O8 Co2 -94.30(11) . . . . ? O2W Co3 O8 Co2 85.55(11) . . . . ? O5 Co3 O8 Co2 -3.74(9) . . . . ? O1 Co3 O8 Co2 -170.28(10) . . . . ? O1W Co3 O8 Co4 10.2(9) . . . . ? O4 Co3 O8 Co4 4.19(8) . . . . ? O2W Co3 O8 Co4 -175.95(11) . . . . ? O5 Co3 O8 Co4 94.75(10) . . . . ? O1 Co3 O8 Co4 -71.78(10) . . . . ? O6 Co2 N3 C27 47.8(4) . . . . ? O7 Co2 N3 C27 -131.8(4) . . . . ? N4 Co2 N3 C27 140.9(3) . . . . ? O5 Co2 N3 C27 -36.2(3) . . . . ? O8 Co2 N3 C27 -107.8(5) . . . . ? O6 Co2 N3 C29 -148.1(3) . . . . ? O7 Co2 N3 C29 32.3(3) . . . . ? N4 Co2 N3 C29 -55.0(3) . . . . ? O5 Co2 N3 C29 127.9(3) . . . . ? O8 Co2 N3 C29 56.3(6) . . . . ? O6 Co2 N4 C32 -1.4(3) . . . . ? N3 Co2 N4 C32 -103.4(3) . . . . ? O7 Co2 N4 C32 175.0(3) . . . . ? O5 Co2 N4 C32 -54(2) . . . . ? O8 Co2 N4 C32 91.6(3) . . . . ? O6 Co2 N4 C31 174.3(2) . . . . ? N3 Co2 N4 C31 72.3(3) . . . . ? O7 Co2 N4 C31 -9.3(2) . . . . ? O5 Co2 N4 C31 121.9(18) . . . . ? O8 Co2 N4 C31 -92.6(2) . . . . ? O6 Co2 O5 C21 -50.8(3) . . . . ? N3 Co2 O5 C21 51.4(3) . . . . ? O7 Co2 O5 C21 132.8(2) . . . . ? N4 Co2 O5 C21 2(2) . . . . ? O8 Co2 O5 C21 -143.8(3) . . . . ? O6 Co2 O5 Co3 88.99(11) . . . . ? N3 Co2 O5 Co3 -168.80(12) . . . . ? O7 Co2 O5 Co3 -87.37(11) . . . . ? N4 Co2 O5 Co3 141.7(18) . . . . ? O8 Co2 O5 Co3 -4.01(10) . . . . ? O1W Co3 O5 C21 -50.6(3) . . . . ? O4 Co3 O5 C21 -141.0(3) . . . . ? O2W Co3 O5 C21 49.3(3) . . . . ? O8 Co3 O5 C21 136.2(3) . . . . ? O1 Co3 O5 C21 -169.4(3) . . . . ? O1W Co3 O5 Co2 177.07(10) . . . . ? O4 Co3 O5 Co2 86.67(11) . . . . ? O2W Co3 O5 Co2 -83.08(12) . . . . ? O8 Co3 O5 Co2 3.83(9) . . . . ? O1 Co3 O5 Co2 58.3(4) . . . . ? N3 Co2 O6 C39 78.5(3) . . . . ? O7 Co2 O6 C39 -108.2(17) . . . . ? N4 Co2 O6 C39 -11.1(3) . . . . ? O5 Co2 O6 C39 165.9(3) . . . . ? O8 Co2 O6 C39 -108.1(3) . . . . ? O6 Co2 O7 C30 134.4(17) . . . . ? N3 Co2 O7 C30 -52.3(2) . . . . ? N4 Co2 O7 C30 37.1(2) . . . . ? O5 Co2 O7 C30 -140.0(2) . . . . ? O8 Co2 O7 C30 134.2(2) . . . . ? O6 Co2 O7 Co4 0.5(18) . . . . ? N3 Co2 O7 Co4 173.90(14) . . . . ? N4 Co2 O7 Co4 -96.71(13) . . . . ? O5 Co2 O7 Co4 86.13(12) . . . . ? O8 Co2 O7 Co4 0.39(10) . . . . ? O2 Co4 O7 C30 139.9(4) . . . . ? O8 Co4 O7 C30 -114.1(3) . . . . ? O4 Co4 O7 C30 165.5(3) . . . . ? O10 Co4 O7 C30 -11.4(3) . . . . ? O9 Co4 O7 C30 46.3(3) . . . . ? O2 Co4 O7 Co2 -106.4(4) . . . . ? O8 Co4 O7 Co2 -0.38(10) . . . . ? O4 Co4 O7 Co2 -80.83(12) . . . . ? O10 Co4 O7 Co2 102.26(14) . . . . ? O9 Co4 O7 Co2 159.95(14) . . . . ? Co2 O5 C21 C22 144.9(3) . . . . ? Co3 O5 C21 C22 19.5(5) . . . . ? Co2 O5 C21 C26 -36.7(4) . . . . ? Co3 O5 C21 C26 -162.2(3) . . . . ? O5 C21 C22 C23 -176.7(4) . . . . ? C26 C21 C22 C23 4.9(6) . . . . ? C21 C22 C23 C24 -1.3(7) . . . . ? C22 C23 C24 C25 -2.6(7) . . . . ? C23 C24 C25 C26 3.0(7) . . . . ? O5 C21 C26 C25 177.3(3) . . . . ? C22 C21 C26 C25 -4.4(5) . . . . ? O5 C21 C26 C27 -10.7(6) . . . . ? C22 C21 C26 C27 167.7(4) . . . . ? C24 C25 C26 C21 0.5(6) . . . . ? C24 C25 C26 C27 -171.5(4) . . . . ? C29 N3 C27 C26 -159.8(4) . . . . ? Co2 N3 C27 C26 2.3(6) . . . . ? C29 N3 C27 C28 15.0(6) . . . . ? Co2 N3 C27 C28 177.0(3) . . . . ? C21 C26 C27 N3 30.7(6) . . . . ? C25 C26 C27 N3 -157.6(4) . . . . ? C21 C26 C27 C28 -144.1(4) . . . . ? C25 C26 C27 C28 27.6(6) . . . . ? C27 N3 C29 C30 159.2(4) . . . . ? Co2 N3 C29 C30 -5.4(4) . . . . ? Co2 O7 C30 C29 60.7(3) . . . . ? Co4 O7 C30 C29 174.8(2) . . . . ? Co2 O7 C30 C31 -57.9(3) . . . . ? Co4 O7 C30 C31 56.1(4) . . . . ? N3 C29 C30 O7 -36.1(4) . . . . ? N3 C29 C30 C31 80.5(4) . . . . ? C32 N4 C31 C30 156.6(3) . . . . ? Co2 N4 C31 C30 -19.5(3) . . . . ? O7 C30 C31 N4 52.2(4) . . . . ? C29 C30 C31 N4 -63.2(4) . . . . ? C31 N4 C32 C34 -165.4(3) . . . . ? Co2 N4 C32 C34 9.9(5) . . . . ? C31 N4 C32 C33 12.3(6) . . . . ? Co2 N4 C32 C33 -172.4(3) . . . . ? N4 C32 C34 C39 -8.0(6) . . . . ? C33 C32 C34 C39 174.4(4) . . . . ? N4 C32 C34 C35 167.7(4) . . . . ? C33 C32 C34 C35 -9.9(6) . . . . ? C39 C34 C35 C36 -0.3(6) . . . . ? C32 C34 C35 C36 -176.2(4) . . . . ? C34 C35 C36 C37 0.2(8) . . . . ? C35 C36 C37 C38 -0.3(8) . . . . ? C36 C37 C38 C39 0.6(8) . . . . ? Co2 O6 C39 C38 -165.9(3) . . . . ? Co2 O6 C39 C34 15.3(5) . . . . ? C37 C38 C39 O6 -179.6(5) . . . . ? C37 C38 C39 C34 -0.7(7) . . . . ? C35 C34 C39 O6 179.3(4) . . . . ? C32 C34 C39 O6 -4.9(6) . . . . ? C35 C34 C39 C38 0.5(6) . . . . ? C32 C34 C39 C38 176.3(4) . . . . ? O11 N5 O9 Co4 -174.8(4) . . . . ? O10 N5 O9 Co4 5.4(4) . . . . ? O2 Co4 O9 N5 82.7(2) . . . . ? O7 Co4 O9 N5 -110.6(2) . . . . ? O8 Co4 O9 N5 -53.8(4) . . . . ? O4 Co4 O9 N5 156.9(2) . . . . ? O10 Co4 O9 N5 -3.3(2) . . . . ? O11 N5 O10 Co4 174.7(4) . . . . ? O9 N5 O10 Co4 -5.5(4) . . . . ? O2 Co4 O10 N5 -89.7(2) . . . . ? O7 Co4 O10 N5 84.0(2) . . . . ? O8 Co4 O10 N5 165.0(2) . . . . ? O4 Co4 O10 N5 -85.5(4) . . . . ? O9 Co4 O10 N5 3.3(2) . . . . ? 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 O1W H1A O3 0.838(18) 1.92(2) 2.707(4) 155(5) . O1W H1B O3W 0.860(18) 1.84(2) 2.679(6) 165(4) . O2W H2A O6 0.865(19) 1.90(2) 2.729(4) 159(4) . O2W H2B O12 0.887(18) 1.91(2) 2.759(5) 158(4) . O2W H2B N6 0.887(18) 2.54(2) 3.412(7) 169(4) . O3W H3B O12 0.84(2) 2.13(3) 2.942(8) 164(11) . O4W H4A O10 0.88(2) 2.31(8) 2.873(6) 122(8) . O4W H4B O13 0.88(2) 2.01(3) 2.871(8) 166(9) 2_665 O4W H4B N6 0.88(2) 2.62(4) 3.420(9) 152(8) 2_665 _diffrn_measured_fraction_theta_max 0.904 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.904 _refine_diff_density_max 0.639 _refine_diff_density_min -0.458 _refine_diff_density_rms 0.082