Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Linpei Jin' _publ_contact_author_address ; School of Chemistry, Beijing Normal University Beijing 100875 CHINA ; _publ_contact_author_email LPJIN@BNU.EDU.CN _publ_section_title ; Structural diversity and properties of M(II) 4-carboxyl phenoxyacetate complexes with 0D-, 1D-, 2D- and 3D M-cpoa framework ; loop_ _publ_author_name 'Linpei Jin.' 'Licun Li.' 'Dai-Zheng Liao.' 'Hui Ma.' 'Xiangjun Zheng.' ; Wen-Juan Zhuang ; data_complex1 _database_code_depnum_ccdc_archive 'CCDC 637132' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H42 Co N4 O12' _chemical_formula_sum 'C42 H42 Co N4 O12' _chemical_formula_weight 853.73 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 41.574(8) _cell_length_b 5.7944(11) _cell_length_c 16.876(3) _cell_angle_alpha 90.00 _cell_angle_beta 109.095(3) _cell_angle_gamma 90.00 _cell_volume 3841.8(13) _cell_formula_units_Z 4 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 1687 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 23.14 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 1.476 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1780 _exptl_absorpt_coefficient_mu 0.519 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9215 _exptl_absorpt_correction_T_max 0.9596 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10304 _diffrn_reflns_av_R_equivalents 0.0644 _diffrn_reflns_av_sigmaI/netI 0.0858 _diffrn_reflns_limit_h_min -51 _diffrn_reflns_limit_h_max 51 _diffrn_reflns_limit_k_min -3 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.04 _diffrn_reflns_theta_max 26.36 _reflns_number_total 3914 _reflns_number_gt 2135 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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^)+(0.0789P)^2^+15.0494P] 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 contra _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3914 _refine_ls_number_parameters 348 _refine_ls_number_restraints 629 _refine_ls_R_factor_all 0.1319 _refine_ls_R_factor_gt 0.0634 _refine_ls_wR_factor_ref 0.1945 _refine_ls_wR_factor_gt 0.1524 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 0.983 _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 0.2500 0.7500 0.5000 0.0302(3) Uani 1 2 d S . . O1 O 0.22401(7) 0.9559(6) 0.39715(19) 0.0348(8) Uani 1 1 d . A . O2 O 0.22801(9) 0.7356(6) 0.2914(2) 0.0494(9) Uani 1 1 d . A . O3 O 0.18267(7) 1.2589(6) 0.2883(2) 0.0398(8) Uani 1 1 d . . . O4 O 0.05081(13) 1.0800(9) 0.3878(4) 0.106(2) Uani 1 1 d . . . O5 O 0.05317(10) 0.7552(8) 0.3222(3) 0.0684(12) Uani 1 1 d . . . H5A H 0.0375 0.7195 0.3392 0.103 Uiso 1 1 calc R . . O6 O 0.24482(8) 0.4570(6) 0.4212(2) 0.0426(9) Uani 1 1 d D A . H6A H 0.2293 0.3570 0.4131 0.051 Uiso 1 1 d RD . . H6B H 0.2653 0.4135 0.4472 0.051 Uiso 1 1 d RD . . C1 C 0.21941(10) 0.9135(9) 0.3197(3) 0.0338(11) Uani 1 1 d . . . C2 C 0.20273(12) 1.1043(9) 0.2579(3) 0.0411(12) Uani 1 1 d . A . H2A H 0.2203 1.1917 0.2451 0.049 Uiso 1 1 calc R . . H2B H 0.1884 1.0348 0.2061 0.049 Uiso 1 1 calc R . . C3 C 0.15406(11) 1.1718(8) 0.3006(3) 0.0326(11) Uani 1 1 d . . . C4 C 0.14006(11) 0.9573(9) 0.2728(3) 0.0385(12) Uani 1 1 d . . . H4 H 0.1504 0.8594 0.2448 0.046 Uiso 1 1 calc R . . C5 C 0.11033(11) 0.8903(9) 0.2871(3) 0.0393(12) Uani 1 1 d . . . H5 H 0.1010 0.7459 0.2691 0.047 Uiso 1 1 calc R . . C6 C 0.09448(11) 1.0356(9) 0.3278(3) 0.0385(12) Uani 1 1 d . . . C7 C 0.10898(12) 1.2510(9) 0.3551(3) 0.0439(12) Uani 1 1 d . . . H7 H 0.0986 1.3495 0.3830 0.053 Uiso 1 1 calc R . . C8 C 0.13837(13) 1.3191(9) 0.3412(3) 0.0439(13) Uani 1 1 d . . . H8 H 0.1477 1.4637 0.3590 0.053 Uiso 1 1 calc R . . C9 C 0.06406(13) 0.9618(11) 0.3492(4) 0.0511(14) Uani 1 1 d . . . N1 N 0.2991(2) 0.810(2) 0.4822(7) 0.032(2) Uani 0.488(9) 1 d PGDU A 1 C10 C 0.3049(2) 1.0086(19) 0.4428(7) 0.032(2) Uani 0.488(9) 1 d PGDU A 1 H10A H 0.2896 1.1310 0.4332 0.039 Uiso 0.488(9) 1 calc PR A 1 C11 C 0.3335(2) 1.0243(15) 0.4178(6) 0.039(2) Uani 0.488(9) 1 d PGDU A 1 H11A H 0.3374 1.1573 0.3915 0.047 Uiso 0.488(9) 1 calc PR A 1 C12 C 0.35633(17) 0.8413(15) 0.4322(5) 0.038(2) Uani 0.488(9) 1 d PGDU A 1 C13 C 0.3505(2) 0.6425(14) 0.4716(7) 0.034(2) Uani 0.488(9) 1 d PGDU A 1 H13A H 0.3658 0.5201 0.4812 0.041 Uiso 0.488(9) 1 calc PR A 1 C14 C 0.3219(3) 0.6268(18) 0.4966(8) 0.040(2) Uani 0.488(9) 1 d PGDU A 1 H14A H 0.3180 0.4938 0.5229 0.048 Uiso 0.488(9) 1 calc PR A 1 C15 C 0.3879(2) 0.852(2) 0.4050(7) 0.049(2) Uani 0.488(9) 1 d PDU A 1 H15A H 0.3989 0.7029 0.4149 0.058 Uiso 0.488(9) 1 calc PR A 1 H15B H 0.3806 0.8809 0.3451 0.058 Uiso 0.488(9) 1 calc PR A 1 C17 C 0.44301(18) 1.0675(16) 0.4150(5) 0.050(2) Uani 0.488(9) 1 d PGDU A 1 C18 C 0.4526(2) 0.9011(15) 0.3677(7) 0.056(2) Uani 0.488(9) 1 d PGDU A 1 H18A H 0.4408 0.7623 0.3553 0.067 Uiso 0.488(9) 1 calc PR A 1 C19 C 0.4799(3) 0.9423(19) 0.3391(8) 0.051(2) Uani 0.488(9) 1 d PGDU A 1 H19A H 0.4863 0.8310 0.3075 0.061 Uiso 0.488(9) 1 calc PR A 1 N2 N 0.4975(2) 1.150(2) 0.3577(8) 0.049(2) Uani 0.488(9) 1 d PGDU A 1 C20 C 0.4879(2) 1.3162(17) 0.4049(7) 0.056(3) Uani 0.488(9) 1 d PGDU A 1 H20A H 0.4997 1.4550 0.4174 0.068 Uiso 0.488(9) 1 calc PR A 1 C21 C 0.4607(2) 1.2750(16) 0.4336(6) 0.056(3) Uani 0.488(9) 1 d PGDU A 1 H21A H 0.4542 1.3863 0.4652 0.068 Uiso 0.488(9) 1 calc PR A 1 C16 C 0.4135(2) 1.033(2) 0.4480(7) 0.052(2) Uani 0.488(9) 1 d PDU A 1 H16A H 0.4228 0.9929 0.5069 0.063 Uiso 0.488(9) 1 calc PR A 1 H16B H 0.4017 1.1788 0.4442 0.063 Uiso 0.488(9) 1 calc PR A 1 N1' N 0.29623(19) 0.824(2) 0.4687(7) 0.031(2) Uani 0.512(9) 1 d PGU A 2 C10' C 0.29785(19) 1.0192(19) 0.4224(7) 0.042(2) Uani 0.512(9) 1 d PGU A 2 H10B H 0.2793 1.1182 0.4042 0.050 Uiso 0.512(9) 1 calc PR A 2 C11' C 0.3273(2) 1.0667(15) 0.4033(6) 0.047(2) Uani 0.512(9) 1 d PGDU A 2 H11B H 0.3283 1.1974 0.3723 0.057 Uiso 0.512(9) 1 calc PR A 2 C12' C 0.35503(16) 0.9187(16) 0.4304(6) 0.040(2) Uani 0.512(9) 1 d PGDU A 2 C13' C 0.3534(2) 0.7232(15) 0.4767(6) 0.034(2) Uani 0.512(9) 1 d PGDU A 2 H13B H 0.3720 0.6242 0.4949 0.040 Uiso 0.512(9) 1 calc PR A 2 C14' C 0.3240(2) 0.6757(16) 0.4958(7) 0.0283(19) Uani 0.512(9) 1 d PGU A 2 H14B H 0.3229 0.5450 0.5268 0.034 Uiso 0.512(9) 1 calc PR A 2 C15' C 0.38463(19) 0.971(2) 0.3995(7) 0.051(2) Uani 0.512(9) 1 d PDU A 2 H15C H 0.3798 0.9023 0.3445 0.061 Uiso 0.512(9) 1 calc PR A 2 H15D H 0.3857 1.1369 0.3928 0.061 Uiso 0.512(9) 1 calc PR A 2 C16' C 0.41939(19) 0.889(2) 0.4544(7) 0.055(2) Uani 0.512(9) 1 d PDU A 2 H16C H 0.4195 0.7219 0.4572 0.066 Uiso 0.512(9) 1 calc PR A 2 H16D H 0.4240 0.9483 0.5107 0.066 Uiso 0.512(9) 1 calc PR A 2 C17' C 0.44739(18) 0.9689(17) 0.4206(6) 0.053(2) Uani 0.512(9) 1 d PGDU A 2 C18' C 0.4638(2) 1.1775(16) 0.4479(6) 0.055(2) Uani 0.512(9) 1 d PGDU A 2 H18B H 0.4566 1.2723 0.4833 0.066 Uiso 0.512(9) 1 calc PR A 2 C19' C 0.4910(2) 1.2444(16) 0.4223(7) 0.052(2) Uani 0.512(9) 1 d PGU A 2 H19B H 0.5019 1.3839 0.4405 0.063 Uiso 0.512(9) 1 calc PR A 2 N2' N 0.5017(2) 1.103(2) 0.3694(7) 0.046(2) Uani 0.512(9) 1 d PGU A 2 C20' C 0.4853(3) 0.894(2) 0.3421(8) 0.063(3) Uani 0.512(9) 1 d PGU A 2 H20B H 0.4925 0.7994 0.3067 0.075 Uiso 0.512(9) 1 calc PR A 2 C21' C 0.4582(2) 0.8273(16) 0.3677(7) 0.063(2) Uani 0.512(9) 1 d PGDU A 2 H21B H 0.4472 0.6878 0.3494 0.075 Uiso 0.512(9) 1 calc PRU A 2 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 0.0226(4) 0.0291(5) 0.0419(5) -0.0027(5) 0.0146(4) -0.0019(4) O1 0.0307(16) 0.040(2) 0.0368(19) -0.0045(15) 0.0146(14) -0.0005(14) O2 0.058(2) 0.045(2) 0.052(2) -0.0052(19) 0.0291(18) 0.0033(19) O3 0.0339(16) 0.0351(19) 0.053(2) 0.0003(17) 0.0186(15) -0.0057(16) O4 0.096(4) 0.086(4) 0.183(6) -0.044(4) 0.110(4) -0.024(3) O5 0.052(2) 0.083(3) 0.087(3) -0.020(3) 0.046(2) -0.026(2) O6 0.0312(17) 0.038(2) 0.058(2) -0.0108(17) 0.0143(16) -0.0039(15) C1 0.024(2) 0.038(3) 0.045(3) -0.005(2) 0.019(2) -0.006(2) C2 0.037(3) 0.048(3) 0.042(3) 0.004(2) 0.019(2) -0.001(2) C3 0.026(2) 0.032(3) 0.041(3) 0.002(2) 0.012(2) -0.0005(19) C4 0.033(2) 0.038(3) 0.051(3) -0.007(2) 0.022(2) -0.002(2) C5 0.032(2) 0.039(3) 0.047(3) -0.005(2) 0.014(2) -0.007(2) C6 0.030(2) 0.043(3) 0.046(3) 0.000(2) 0.016(2) 0.004(2) C7 0.048(3) 0.038(3) 0.054(3) -0.005(3) 0.027(2) 0.008(3) C8 0.044(3) 0.033(3) 0.057(3) -0.002(2) 0.020(3) 0.001(2) C9 0.037(3) 0.058(4) 0.065(4) -0.002(3) 0.026(3) -0.001(3) N1 0.026(3) 0.034(4) 0.037(4) 0.005(3) 0.010(3) -0.006(3) C10 0.018(3) 0.032(4) 0.041(4) 0.017(3) 0.002(3) 0.006(3) C11 0.027(4) 0.041(4) 0.049(4) 0.019(3) 0.011(3) -0.004(3) C12 0.030(3) 0.037(4) 0.049(3) -0.002(4) 0.017(3) -0.001(3) C13 0.030(3) 0.027(4) 0.046(4) -0.005(4) 0.014(3) -0.006(4) C14 0.030(3) 0.039(4) 0.048(4) -0.001(4) 0.010(3) 0.000(3) C15 0.039(3) 0.051(4) 0.061(4) 0.001(4) 0.023(3) -0.005(4) C17 0.040(4) 0.055(4) 0.065(4) -0.005(4) 0.031(3) -0.003(4) C18 0.046(4) 0.061(4) 0.069(4) -0.004(4) 0.032(3) -0.005(4) C19 0.044(4) 0.058(4) 0.061(4) -0.007(4) 0.033(3) 0.003(4) N2 0.037(4) 0.058(4) 0.057(4) 0.008(4) 0.022(3) -0.001(3) C20 0.050(4) 0.065(5) 0.062(4) 0.003(4) 0.029(3) -0.001(4) C21 0.050(4) 0.058(5) 0.070(4) -0.003(4) 0.033(4) -0.004(4) C16 0.043(4) 0.056(4) 0.065(4) -0.006(4) 0.028(3) -0.004(4) N1' 0.022(3) 0.035(3) 0.034(4) -0.001(3) 0.007(3) 0.001(3) C10' 0.028(4) 0.041(4) 0.050(4) 0.005(4) 0.004(4) -0.009(3) C11' 0.031(4) 0.048(4) 0.057(4) 0.015(4) 0.007(4) -0.001(3) C12' 0.033(3) 0.041(4) 0.049(3) 0.011(3) 0.018(3) -0.008(3) C13' 0.028(3) 0.029(4) 0.045(3) -0.002(4) 0.013(3) 0.004(3) C14' 0.024(3) 0.023(4) 0.039(3) 0.008(3) 0.013(3) 0.000(3) C15' 0.041(3) 0.053(4) 0.061(4) 0.011(4) 0.019(3) -0.001(4) C16' 0.042(4) 0.063(5) 0.064(4) 0.012(4) 0.021(3) -0.002(4) C17' 0.040(3) 0.061(4) 0.065(4) 0.003(4) 0.025(3) -0.003(3) C18' 0.048(4) 0.057(5) 0.067(4) -0.003(4) 0.030(3) 0.002(4) C19' 0.046(4) 0.051(4) 0.068(4) 0.004(4) 0.029(3) -0.004(4) N2' 0.034(3) 0.060(4) 0.053(4) 0.009(3) 0.025(3) 0.002(3) C20' 0.051(4) 0.073(5) 0.069(4) 0.001(4) 0.026(4) -0.007(4) C21' 0.052(4) 0.069(4) 0.072(4) -0.002(4) 0.028(3) -0.008(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 O1 2.092(3) . ? Co1 O1 2.092(3) 7_566 ? Co1 O6 2.123(3) . ? Co1 O6 2.123(3) 7_566 ? Co1 N1 2.184(7) . ? Co1 N1 2.185(7) 7_566 ? Co1 N1' 2.195(7) . ? Co1 N1' 2.196(7) 7_566 ? O1 C1 1.281(5) . ? O2 C1 1.237(5) . ? O3 C3 1.370(5) . ? O3 C2 1.429(6) . ? O4 C9 1.196(7) . ? O5 C9 1.308(7) . ? O5 H5A 0.8200 . ? O6 H6A 0.8450 . ? O6 H6B 0.8565 . ? C1 C2 1.523(7) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C8 1.384(7) . ? C3 C4 1.388(7) . ? C4 C5 1.391(6) . ? C4 H4 0.9300 . ? C5 C6 1.382(7) . ? C5 H5 0.9300 . ? C6 C7 1.397(7) . ? C6 C9 1.487(7) . ? C7 C8 1.376(7) . ? C7 H7 0.9300 . ? C8 H8 0.9300 . ? N1 C10 1.3900 . ? N1 C14 1.3900 . ? C10 C11 1.3900 . ? C10 H10A 0.9300 . ? C11 C12 1.3900 . ? C11 H11A 0.9300 . ? C12 C13 1.3900 . ? C12 C15 1.526(7) . ? C13 C14 1.3900 . ? C13 H13A 0.9300 . ? C14 H14A 0.9300 . ? C15 C16 1.500(8) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C17 C18 1.3900 . ? C17 C21 1.3900 . ? C17 C16 1.517(7) . ? C18 C19 1.3900 . ? C18 H18A 0.9300 . ? C19 N2 1.3900 . ? C19 H19A 0.9300 . ? N2 C20 1.3900 . ? C20 C21 1.3900 . ? C20 H20A 0.9300 . ? C21 H21A 0.9300 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? N1' C10' 1.3900 . ? N1' C14' 1.3900 . ? C10' C11' 1.3900 . ? C10' H10B 0.9300 . ? C11' C12' 1.3900 . ? C11' H11B 0.9300 . ? C12' C13' 1.3900 . ? C12' C15' 1.516(7) . ? C13' C14' 1.3900 . ? C13' H13B 0.9300 . ? C14' H14B 0.9300 . ? C15' C16' 1.515(8) . ? C15' H15C 0.9700 . ? C15' H15D 0.9700 . ? C16' C17' 1.526(7) . ? C16' H16C 0.9700 . ? C16' H16D 0.9700 . ? C17' C18' 1.3900 . ? C17' C21' 1.3900 . ? C18' C19' 1.3900 . ? C18' H18B 0.9300 . ? C19' N2' 1.3900 . ? C19' H19B 0.9300 . ? N2' C20' 1.3900 . ? C20' C21' 1.3900 . ? C20' H20B 0.9300 . ? C21' H21B 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 O1 179.998(2) . 7_566 ? O1 Co1 O6 91.01(13) . . ? O1 Co1 O6 88.99(13) 7_566 . ? O1 Co1 O6 89.00(13) . 7_566 ? O1 Co1 O6 91.00(13) 7_566 7_566 ? O6 Co1 O6 179.998(1) . 7_566 ? O1 Co1 N1 92.7(3) . . ? O1 Co1 N1 87.3(3) 7_566 . ? O6 Co1 N1 87.1(3) . . ? O6 Co1 N1 92.9(3) 7_566 . ? O1 Co1 N1 87.3(3) . 7_566 ? O1 Co1 N1 92.7(3) 7_566 7_566 ? O6 Co1 N1 92.9(3) . 7_566 ? O6 Co1 N1 87.1(3) 7_566 7_566 ? N1 Co1 N1 180.0(6) . 7_566 ? O1 Co1 N1' 86.8(3) . . ? O1 Co1 N1' 93.2(3) 7_566 . ? O6 Co1 N1' 85.5(3) . . ? O6 Co1 N1' 94.5(3) 7_566 . ? N1 Co1 N1' 6.1(6) . . ? N1 Co1 N1' 173.9(6) 7_566 . ? O1 Co1 N1' 93.2(3) . 7_566 ? O1 Co1 N1' 86.8(3) 7_566 7_566 ? O6 Co1 N1' 94.5(3) . 7_566 ? O6 Co1 N1' 85.5(3) 7_566 7_566 ? N1 Co1 N1' 173.9(6) . 7_566 ? N1 Co1 N1' 6.1(6) 7_566 7_566 ? N1' Co1 N1' 180.0 . 7_566 ? C1 O1 Co1 126.9(3) . . ? C3 O3 C2 117.5(4) . . ? C9 O5 H5A 109.5 . . ? Co1 O6 H6A 124.4 . . ? Co1 O6 H6B 92.0 . . ? H6A O6 H6B 117.3 . . ? O2 C1 O1 126.0(5) . . ? O2 C1 C2 117.7(4) . . ? O1 C1 C2 116.2(4) . . ? O3 C2 C1 113.4(4) . . ? O3 C2 H2A 108.9 . . ? C1 C2 H2A 108.9 . . ? O3 C2 H2B 108.9 . . ? C1 C2 H2B 108.9 . . ? H2A C2 H2B 107.7 . . ? O3 C3 C8 114.9(4) . . ? O3 C3 C4 124.6(4) . . ? C8 C3 C4 120.5(4) . . ? C3 C4 C5 119.3(4) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? C6 C5 C4 120.8(5) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? C5 C6 C7 118.9(4) . . ? C5 C6 C9 121.8(5) . . ? C7 C6 C9 119.1(5) . . ? C8 C7 C6 120.8(5) . . ? C8 C7 H7 119.6 . . ? C6 C7 H7 119.6 . . ? C7 C8 C3 119.7(5) . . ? C7 C8 H8 120.1 . . ? C3 C8 H8 120.1 . . ? O4 C9 O5 123.0(5) . . ? O4 C9 C6 123.2(6) . . ? O5 C9 C6 113.8(5) . . ? C10 N1 C14 120.0 . . ? C10 N1 Co1 120.9(6) . . ? C14 N1 Co1 118.0(6) . . ? N1 C10 C11 120.0 . . ? N1 C10 H10A 120.0 . . ? C11 C10 H10A 120.0 . . ? C12 C11 C10 120.0 . . ? C12 C11 H11A 120.0 . . ? C10 C11 H11A 120.0 . . ? C13 C12 C11 120.0 . . ? C13 C12 C15 118.7(5) . . ? C11 C12 C15 121.3(5) . . ? C12 C13 C14 120.0 . . ? C12 C13 H13A 120.0 . . ? C14 C13 H13A 120.0 . . ? C13 C14 N1 120.0 . . ? C13 C14 H14A 120.0 . . ? N1 C14 H14A 120.0 . . ? C16 C15 C12 115.4(6) . . ? C16 C15 H15A 108.4 . . ? C12 C15 H15A 108.4 . . ? C16 C15 H15B 108.4 . . ? C12 C15 H15B 108.4 . . ? H15A C15 H15B 107.5 . . ? C18 C17 C21 120.0 . . ? C18 C17 C16 122.5(5) . . ? C21 C17 C16 117.5(5) . . ? C17 C18 C19 120.0 . . ? C17 C18 H18A 120.0 . . ? C19 C18 H18A 120.0 . . ? N2 C19 C18 120.0 . . ? N2 C19 H19A 120.0 . . ? C18 C19 H19A 120.0 . . ? C19 N2 C20 120.0 . . ? N2 C20 C21 120.0 . . ? N2 C20 H20A 120.0 . . ? C21 C20 H20A 120.0 . . ? C20 C21 C17 120.0 . . ? C20 C21 H21A 120.0 . . ? C17 C21 H21A 120.0 . . ? C15 C16 C17 116.6(7) . . ? C15 C16 H16A 108.1 . . ? C17 C16 H16A 108.1 . . ? C15 C16 H16B 108.1 . . ? C17 C16 H16B 108.1 . . ? H16A C16 H16B 107.3 . . ? C10' N1' C14' 120.0 . . ? C10' N1' Co1 120.1(5) . . ? C14' N1' Co1 119.9(5) . . ? C11' C10' N1' 120.0 . . ? C11' C10' H10B 120.0 . . ? N1' C10' H10B 120.0 . . ? C10' C11' C12' 120.0 . . ? C10' C11' H11B 120.0 . . ? C12' C11' H11B 120.0 . . ? C13' C12' C11' 120.0 . . ? C13' C12' C15' 123.4(5) . . ? C11' C12' C15' 116.3(5) . . ? C14' C13' C12' 120.0 . . ? C14' C13' H13B 120.0 . . ? C12' C13' H13B 120.0 . . ? C13' C14' N1' 120.0 . . ? C13' C14' H14B 120.0 . . ? N1' C14' H14B 120.0 . . ? C16' C15' C12' 116.5(7) . . ? C16' C15' H15C 108.2 . . ? C12' C15' H15C 108.2 . . ? C16' C15' H15D 108.2 . . ? C12' C15' H15D 108.2 . . ? H15C C15' H15D 107.3 . . ? C15' C16' C17' 111.6(7) . . ? C15' C16' H16C 109.3 . . ? C17' C16' H16C 109.3 . . ? C15' C16' H16D 109.3 . . ? C17' C16' H16D 109.3 . . ? H16C C16' H16D 108.0 . . ? C18' C17' C21' 120.0 . . ? C18' C17' C16' 119.4(6) . . ? C21' C17' C16' 120.4(6) . . ? C19' C18' C17' 120.0 . . ? C19' C18' H18B 120.0 . . ? C17' C18' H18B 120.0 . . ? C18' C19' N2' 120.0 . . ? C18' C19' H19B 120.0 . . ? N2' C19' H19B 120.0 . . ? C20' N2' C19' 120.0 . . ? C21' C20' N2' 120.0 . . ? C21' C20' H20B 120.0 . . ? N2' C20' H20B 120.0 . . ? C20' C21' C17' 120.0 . . ? C20' C21' H21B 120.0 . . ? C17' C21' H21B 120.0 . . ? 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 O6 Co1 O1 C1 -19.5(3) . . . . ? O6 Co1 O1 C1 160.5(3) 7_566 . . . ? N1 Co1 O1 C1 67.6(5) . . . . ? N1 Co1 O1 C1 -112.4(5) 7_566 . . . ? N1' Co1 O1 C1 66.0(4) . . . . ? N1' Co1 O1 C1 -114.0(4) 7_566 . . . ? Co1 O1 C1 O2 4.2(6) . . . . ? Co1 O1 C1 C2 -173.8(3) . . . . ? C3 O3 C2 C1 -65.9(5) . . . . ? O2 C1 C2 O3 157.9(4) . . . . ? O1 C1 C2 O3 -23.9(6) . . . . ? C2 O3 C3 C8 171.2(4) . . . . ? C2 O3 C3 C4 -11.5(7) . . . . ? O3 C3 C4 C5 -178.2(4) . . . . ? C8 C3 C4 C5 -1.0(8) . . . . ? C3 C4 C5 C6 0.8(8) . . . . ? C4 C5 C6 C7 -0.5(8) . . . . ? C4 C5 C6 C9 -175.7(5) . . . . ? C5 C6 C7 C8 0.6(8) . . . . ? C9 C6 C7 C8 175.8(5) . . . . ? C6 C7 C8 C3 -0.8(8) . . . . ? O3 C3 C8 C7 178.5(4) . . . . ? C4 C3 C8 C7 1.0(8) . . . . ? C5 C6 C9 O4 176.4(6) . . . . ? C7 C6 C9 O4 1.3(9) . . . . ? C5 C6 C9 O5 -3.3(8) . . . . ? C7 C6 C9 O5 -178.4(5) . . . . ? O1 Co1 N1 C10 26.0(5) . . . . ? O1 Co1 N1 C10 -154.0(5) 7_566 . . . ? O6 Co1 N1 C10 116.9(5) . . . . ? O6 Co1 N1 C10 -63.1(5) 7_566 . . . ? N1' Co1 N1 C10 41(6) . . . . ? O1 Co1 N1 C14 -142.0(4) . . . . ? O1 Co1 N1 C14 38.0(4) 7_566 . . . ? O6 Co1 N1 C14 -51.2(4) . . . . ? O6 Co1 N1 C14 128.8(4) 7_566 . . . ? N1' Co1 N1 C14 -127(6) . . . . ? C14 N1 C10 C11 0.0 . . . . ? Co1 N1 C10 C11 -167.8(6) . . . . ? N1 C10 C11 C12 0.0 . . . . ? C10 C11 C12 C13 0.0 . . . . ? C10 C11 C12 C15 179.6(3) . . . . ? C11 C12 C13 C14 0.0 . . . . ? C15 C12 C13 C14 -179.6(3) . . . . ? C12 C13 C14 N1 0.0 . . . . ? C10 N1 C14 C13 0.0 . . . . ? Co1 N1 C14 C13 168.2(6) . . . . ? C13 C12 C15 C16 -116.0(11) . . . . ? C11 C12 C15 C16 64.4(12) . . . . ? C21 C17 C18 C19 0.0 . . . . ? C16 C17 C18 C19 -179.99(7) . . . . ? C17 C18 C19 N2 0.0 . . . . ? C18 C19 N2 C20 0.0 . . . . ? C19 N2 C20 C21 0.0 . . . . ? N2 C20 C21 C17 0.0 . . . . ? C18 C17 C21 C20 0.0 . . . . ? C16 C17 C21 C20 179.99(7) . . . . ? C12 C15 C16 C17 -172.9(6) . . . . ? C18 C17 C16 C15 -20.2(10) . . . . ? C21 C17 C16 C15 159.8(10) . . . . ? O1 Co1 N1' C10' 22.8(5) . . . . ? O1 Co1 N1' C10' -157.2(5) 7_566 . . . ? O6 Co1 N1' C10' 114.1(5) . . . . ? O6 Co1 N1' C10' -65.9(5) 7_566 . . . ? N1 Co1 N1' C10' -142(6) . . . . ? O1 Co1 N1' C14' -157.8(5) . . . . ? O1 Co1 N1' C14' 22.3(5) 7_566 . . . ? O6 Co1 N1' C14' -66.5(5) . . . . ? O6 Co1 N1' C14' 113.5(5) 7_566 . . . ? N1 Co1 N1' C14' 38(6) . . . . ? C14' N1' C10' C11' 0.0 . . . . ? Co1 N1' C10' C11' 179.4(7) . . . . ? N1' C10' C11' C12' 0.0 . . . . ? C10' C11' C12' C13' 0.0 . . . . ? C10' C11' C12' C15' 174.2(8) . . . . ? C11' C12' C13' C14' 0.0 . . . . ? C15' C12' C13' C14' -173.8(8) . . . . ? C12' C13' C14' N1' 0.0 . . . . ? C10' N1' C14' C13' 0.0 . . . . ? Co1 N1' C14' C13' -179.4(7) . . . . ? C13' C12' C15' C16' -32.1(15) . . . . ? C11' C12' C15' C16' 153.9(11) . . . . ? C12' C15' C16' C17' -175.3(8) . . . . ? C15' C16' C17' C18' 91.1(11) . . . . ? C15' C16' C17' C21' -93.5(11) . . . . ? C21' C17' C18' C19' 0.0 . . . . ? C16' C17' C18' C19' 175.4(8) . . . . ? C17' C18' C19' N2' 0.0 . . . . ? C18' C19' N2' C20' 0.0 . . . . ? C19' N2' C20' C21' 0.0 . . . . ? N2' C20' C21' C17' 0.0 . . . . ? C18' C17' C21' C20' 0.0 . . . . ? C16' C17' C21' C20' -175.3(8) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.36 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.515 _refine_diff_density_min -0.800 _refine_diff_density_rms 0.083 #===END data_complex2 _database_code_depnum_ccdc_archive 'CCDC 637133' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H28 Co N3 O7' _chemical_formula_sum 'C27 H28 Co N3 O7' _chemical_formula_weight 565.46 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 orthorhombic _symmetry_space_group_name_H-M 'F d d d' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/4, z+1/4' 'x+1/4, -y, z+1/4' '-x+1/4, -y+3/4, z+1/2' 'x, y+1/2, z+1/2' '-x, y+3/4, z+3/4' 'x+1/4, -y+1/2, z+3/4' '-x+1/4, -y+5/4, z+1' 'x+1/2, y, z+1/2' '-x+1/2, y+1/4, z+3/4' 'x+3/4, -y, z+3/4' '-x+3/4, -y+3/4, z+1' 'x+1/2, y+1/2, z' '-x+1/2, y+3/4, z+1/4' 'x+3/4, -y+1/2, z+1/4' '-x+3/4, -y+5/4, z+1/2' '-x, -y, -z' 'x, -y-1/4, -z-1/4' '-x-1/4, y, -z-1/4' 'x-1/4, y-3/4, -z-1/2' '-x, -y+1/2, -z+1/2' 'x, -y+1/4, -z+1/4' '-x-1/4, y+1/2, -z+1/4' 'x-1/4, y-1/4, -z' '-x+1/2, -y, -z+1/2' 'x+1/2, -y-1/4, -z+1/4' '-x+1/4, y, -z+1/4' 'x+1/4, y-3/4, -z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/4, -z-1/4' '-x+1/4, y+1/2, -z-1/4' 'x+1/4, y-1/4, -z-1/2' _cell_length_a 13.931(2) _cell_length_b 21.777(2) _cell_length_c 35.140(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 10661(3) _cell_formula_units_Z 16 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 5092 _cell_measurement_theta_min 1.8 _cell_measurement_theta_max 27.8 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.409 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4704 _exptl_absorpt_coefficient_mu 0.694 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9091 _exptl_absorpt_correction_T_max 0.9338 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15772 _diffrn_reflns_av_R_equivalents 0.0519 _diffrn_reflns_av_sigmaI/netI 0.0282 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 24.99 _reflns_number_total 2367 _reflns_number_gt 2217 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.7.0' _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^)+(0.0000P)^2^+109.8133P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00021(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2367 _refine_ls_number_parameters 260 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.0764 _refine_ls_R_factor_gt 0.0721 _refine_ls_wR_factor_ref 0.1386 _refine_ls_wR_factor_gt 0.1370 _refine_ls_goodness_of_fit_ref 1.307 _refine_ls_restrained_S_all 1.310 _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 0.6250 0.43926(4) 0.6250 0.0442(3) Uani 1 2 d S . . N1 N 0.5510(3) 0.43479(19) 0.57156(11) 0.0496(10) Uani 1 1 d . . . C1 C 0.4661(4) 0.4609(2) 0.56567(15) 0.0530(13) Uani 1 1 d . . . H1A H 0.4398 0.4845 0.5851 0.064 Uiso 1 1 calc R . . C2 C 0.4157(4) 0.4550(3) 0.53258(16) 0.0625(15) Uani 1 1 d . . . H2A H 0.3566 0.4744 0.5298 0.075 Uiso 1 1 calc R . . C3 C 0.4531(5) 0.4195(3) 0.50271(15) 0.0681(17) Uani 1 1 d . . . C4 C 0.5414(5) 0.3938(3) 0.50866(17) 0.078(2) Uani 1 1 d . . . H4A H 0.5702 0.3708 0.4895 0.094 Uiso 1 1 calc R . . C5 C 0.5874(4) 0.4019(3) 0.54279(16) 0.0646(15) Uani 1 1 d . . . H5A H 0.6471 0.3835 0.5461 0.077 Uiso 1 1 calc R . . C6 C 0.3960(6) 0.4076(3) 0.46684(16) 0.099(3) Uani 1 1 d . . . H6A H 0.4373 0.4128 0.4448 0.119 Uiso 1 1 calc R . . H6B H 0.3443 0.4373 0.4650 0.119 Uiso 1 1 calc R . . O1 O 0.7679(14) 0.4419(8) 0.5955(7) 0.042(4) Uani 0.50 1 d PD . . O2 O 0.8049(14) 0.5380(8) 0.6012(5) 0.080(5) Uani 0.50 1 d PD . . O3 O 1.2225(14) 0.4580(7) 0.4149(6) 0.106(7) Uani 0.50 1 d PD . . O4 O 1.2552(13) 0.5548(9) 0.4102(8) 0.049(5) Uani 0.50 1 d PD . . C7 C 0.8038(15) 0.4897(9) 0.5822(6) 0.093(13) Uani 0.50 1 d PD . . C8 C 0.8749(8) 0.4928(5) 0.5496(3) 0.047(4) Uani 0.50 1 d PGD . . C9 C 0.9425(10) 0.5394(5) 0.5458(3) 0.078(7) Uani 0.50 1 d PG . . H9A H 0.9432 0.5729 0.5635 0.094 Uiso 0.50 1 d PR . . C10 C 1.0091(10) 0.5373(5) 0.5164(4) 0.064(5) Uani 0.50 1 d PG . . H10A H 1.0558 0.5695 0.5138 0.077 Uiso 0.50 1 d PR . . C11 C 1.0081(8) 0.4887(5) 0.4908(3) 0.050(4) Uani 0.50 1 d PGD . . C12 C 0.9405(7) 0.4422(4) 0.4945(3) 0.116(7) Uani 0.50 1 d PG . . H12A H 0.9398 0.4086 0.4768 0.140 Uiso 0.50 1 d PR . . C13 C 0.8739(7) 0.4442(4) 0.5240(3) 0.080(4) Uani 0.50 1 d PG . . H13A H 0.8272 0.4121 0.5266 0.097 Uiso 0.50 1 d PR . . O5 O 1.0745(8) 0.4814(6) 0.4614(3) 0.068(3) Uani 0.50 1 d PD . . C14 C 1.1336(11) 0.5334(6) 0.4518(4) 0.050(4) Uani 0.50 1 d PD . . H14A H 1.1690 0.5475 0.4736 0.060 Uiso 0.50 1 d PR . . H14B H 1.0942 0.5664 0.4427 0.060 Uiso 0.50 1 d PR . . C15 C 1.2000(13) 0.5127(6) 0.4202(5) 0.043(7) Uani 0.50 1 d PD . . O6 O 0.6250 0.5355(3) 0.6250 0.0640(15) Uani 1 2 d SD . . H6C H 0.571(3) 0.551(3) 0.631(2) 0.12(3) Uiso 1 1 d D . . N2 N 0.6366(15) 0.3390(2) 0.6252(8) 0.048(4) Uani 0.50 1 d PG . . C16 C 0.7195(12) 0.3060(5) 0.6333(7) 0.101(10) Uani 0.50 1 d PG . . H16A H 0.7801 0.3268 0.6349 0.121 Uiso 0.50 1 d PR . . C17 C 0.7145(8) 0.2430(5) 0.6393(4) 0.077(5) Uani 0.50 1 d PGD . . H17A H 0.7717 0.2202 0.6449 0.092 Uiso 0.50 1 d PR . . C18 C 0.6266(8) 0.2130(2) 0.6371(2) 0.057(3) Uani 0.50 1 d PGD . . C19 C 0.5437(8) 0.2460(5) 0.6289(3) 0.068(5) Uani 0.50 1 d PGD . . H19A H 0.4830 0.2252 0.6274 0.082 Uiso 0.50 1 d PR . . C20 C 0.5487(12) 0.3090(5) 0.6229(5) 0.043(3) Uani 0.50 1 d PG . . H20A H 0.4914 0.3318 0.6173 0.052 Uiso 0.50 1 d PR . . C21 C 0.6223(12) 0.1439(3) 0.6433(3) 0.080(4) Uani 0.50 1 d PD . . H21A H 0.5658 0.1340 0.6577 0.096 Uiso 0.50 1 d PR . . H21B H 0.6773 0.1326 0.6582 0.096 Uiso 0.50 1 d PR . . O7 O 0.8839(12) 0.6439(6) 0.5950(5) 0.169(7) Uani 0.50 1 d PD . . H7A H 0.88(2) 0.642(12) 0.6190(12) 0.254 Uiso 0.50 1 d PD . . H7B H 0.86(2) 0.611(7) 0.584(6) 0.254 Uiso 0.50 1 d PD . . 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 0.0391(5) 0.0479(6) 0.0455(5) 0.000 0.0113(4) 0.000 N1 0.054(2) 0.053(3) 0.042(2) -0.005(2) 0.0125(19) -0.005(2) C1 0.057(3) 0.054(3) 0.048(3) -0.004(2) 0.004(2) -0.009(3) C2 0.070(4) 0.064(4) 0.054(3) 0.010(3) -0.005(3) -0.021(3) C3 0.102(5) 0.067(4) 0.036(3) 0.011(3) 0.002(3) -0.039(4) C4 0.106(5) 0.079(5) 0.049(3) -0.013(3) 0.023(4) -0.026(4) C5 0.069(4) 0.071(4) 0.054(3) -0.012(3) 0.017(3) -0.006(3) C6 0.144(7) 0.116(6) 0.038(3) 0.015(3) -0.009(4) -0.065(5) O1 0.012(7) 0.070(7) 0.044(8) 0.002(5) 0.007(6) 0.002(5) O2 0.069(9) 0.101(10) 0.072(9) -0.020(7) 0.026(6) -0.031(7) O3 0.074(12) 0.106(12) 0.139(18) 0.007(11) 0.071(12) -0.015(8) O4 0.018(9) 0.077(8) 0.052(8) -0.002(5) 0.000(6) -0.001(6) C7 0.026(13) 0.21(3) 0.043(15) -0.025(18) 0.015(10) 0.003(15) C8 0.036(7) 0.057(10) 0.047(7) 0.002(7) 0.004(6) -0.022(8) C9 0.053(8) 0.103(15) 0.078(12) -0.036(9) 0.023(7) -0.041(9) C10 0.051(8) 0.080(14) 0.061(9) -0.016(8) 0.016(7) -0.022(8) C11 0.054(8) 0.057(12) 0.039(10) 0.005(7) 0.020(8) -0.013(7) C12 0.114(12) 0.111(12) 0.125(13) -0.066(10) 0.096(11) -0.068(10) C13 0.093(10) 0.079(9) 0.070(8) -0.018(7) 0.040(8) -0.036(8) O5 0.073(8) 0.073(7) 0.057(6) -0.014(5) 0.039(6) -0.034(6) C14 0.044(7) 0.058(10) 0.047(8) 0.003(7) 0.007(6) -0.026(7) C15 0.052(15) 0.030(7) 0.048(13) 0.007(7) 0.008(10) -0.010(7) O6 0.062(4) 0.062(4) 0.067(4) 0.000 0.026(3) 0.000 N2 0.029(10) 0.050(4) 0.066(4) -0.009(10) 0.011(7) -0.026(8) C16 0.072(16) 0.091(17) 0.14(2) 0.008(14) -0.003(13) 0.024(11) C17 0.082(11) 0.044(8) 0.105(14) 0.015(8) 0.004(9) -0.001(7) C18 0.075(7) 0.043(5) 0.052(7) -0.009(4) 0.003(8) -0.009(6) C19 0.045(7) 0.065(9) 0.095(13) -0.017(8) -0.003(7) -0.024(6) C20 0.009(4) 0.031(6) 0.089(9) 0.001(7) 0.002(6) -0.009(4) C21 0.094(8) 0.056(9) 0.092(8) 0.008(5) 0.024(10) 0.010(10) O7 0.121(10) 0.075(8) 0.31(2) -0.031(10) -0.032(15) -0.029(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O4 2.08(2) 17_766 ? Co1 O4 2.08(2) 3_465 ? Co1 O6 2.095(6) . ? Co1 N1 2.145(4) . ? Co1 N1 2.145(4) 27_656 ? Co1 N2 2.189(5) . ? Co1 N2 2.189(5) 27_656 ? Co1 O1 2.24(2) . ? Co1 O1 2.24(2) 27_656 ? N1 C1 1.328(6) . ? N1 C5 1.339(6) . ? C1 C2 1.365(7) . ? C1 H1A 0.9300 . ? C2 C3 1.403(8) . ? C2 H2A 0.9300 . ? C3 C4 1.367(9) . ? C3 C6 1.513(8) . ? C4 C5 1.371(8) . ? C4 H4A 0.9300 . ? C5 H5A 0.9300 . ? C6 C6 1.537(12) 12_554 ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? O1 O4 0.39(4) 17_766 ? O1 C15 1.22(3) 17_766 ? O1 C7 1.247(9) . ? O2 O3 0.69(3) 17_766 ? O2 C7 1.245(10) . ? O2 C15 1.34(3) 17_766 ? O3 O2 0.69(3) 17_766 ? O3 C7 1.20(3) 17_766 ? O3 C15 1.246(10) . ? O4 O1 0.39(4) 17_766 ? O4 C15 1.246(9) . ? O4 C7 1.30(3) 17_766 ? O4 Co1 2.08(2) 17_766 ? C7 C15 0.11(4) 17_766 ? C7 O3 1.20(3) 17_766 ? C7 O4 1.30(3) 17_766 ? C7 C8 1.516(9) . ? C7 C14 1.56(2) 17_766 ? C8 C14 0.585(14) 17_766 ? C8 O5 0.980(15) 17_766 ? C8 C9 1.3900 . ? C8 C13 1.3900 . ? C8 C15 1.495(17) 17_766 ? C9 O5 0.570(11) 17_766 ? C9 C10 1.3900 . ? C9 C11 1.581(19) 17_766 ? C9 C14 1.908(14) 17_766 ? C9 H9A 0.9601 . ? C10 C11 0.666(11) 17_766 ? C10 C12 0.916(19) 17_766 ? C10 C11 1.3900 . ? C10 O5 1.461(17) 17_766 ? C10 C10 2.009(15) 17_766 ? C10 H10A 0.9600 . ? C11 C10 0.666(15) 17_766 ? C11 C11 0.845(18) 17_766 ? C11 C12 1.3900 . ? C11 O5 1.396(7) . ? C11 C9 1.581(17) 17_766 ? C11 C12 1.744(14) 17_766 ? C12 C10 0.916(15) 17_766 ? C12 C13 1.3900 . ? C12 C11 1.744(11) 17_766 ? C12 H12A 0.9600 . ? C13 C14 0.986(16) 17_766 ? C13 O5 1.845(11) 17_766 ? C13 H13A 0.9600 . ? O5 C9 0.57(2) 17_766 ? O5 C8 0.980(15) 17_766 ? O5 C14 1.438(9) . ? O5 C10 1.461(15) 17_766 ? O5 C13 1.85(2) 17_766 ? C14 C8 0.585(14) 17_766 ? C14 C13 0.99(2) 17_766 ? C14 C15 1.517(9) . ? C14 C7 1.56(2) 17_766 ? C14 C9 1.91(2) 17_766 ? C14 H14A 0.9599 . ? C14 H14B 0.9599 . ? C15 C7 0.11(4) 17_766 ? C15 O1 1.22(3) 17_766 ? C15 O2 1.34(3) 17_766 ? C15 C8 1.495(17) 17_766 ? O6 H6C 0.85(5) . ? N2 N2 0.32(4) 27_656 ? N2 C20 1.12(3) 27_656 ? N2 C16 1.3900 . ? N2 C20 1.3900 . ? N2 C16 1.67(3) 27_656 ? C16 C20 0.34(4) 27_656 ? C16 C19 1.389(9) 27_656 ? C16 C17 1.3900 . ? C16 N2 1.67(4) 27_656 ? C16 H16A 0.9598 . ? C17 C19 0.65(3) 27_656 ? C17 C18 1.3900 . ? C17 C20 1.511(14) 27_656 ? C17 C18 1.70(2) 27_656 ? C17 H17A 0.9597 . ? C18 C18 0.850(16) 27_656 ? C18 C19 1.3900 . ? C18 C19 1.436(18) 27_656 ? C18 C21 1.522(8) . ? C18 C17 1.702(18) 27_656 ? C18 C21 1.845(10) 27_656 ? C19 C17 0.653(18) 27_656 ? C19 C16 1.389(12) 27_656 ? C19 C20 1.3900 . ? C19 C18 1.44(2) 27_656 ? C19 H19A 0.9599 . ? C20 C16 0.34(3) 27_656 ? C20 N2 1.12(3) 27_656 ? C20 C17 1.511(5) 27_656 ? C20 H20A 0.9601 . ? C21 C21 0.825(15) 8_644 ? C21 C21 1.29(2) 27_656 ? C21 C21 1.53(2) 22_556 ? C21 C18 1.845(10) 27_656 ? C21 H21A 0.9601 . ? C21 H21B 0.9597 . ? O7 H7A 0.851(11) . ? O7 H7B 0.851(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 O4 Co1 O4 172.9(11) 17_766 3_465 ? O4 Co1 O6 86.5(5) 17_766 . ? O4 Co1 O6 86.5(5) 3_465 . ? O4 Co1 N1 82.4(6) 17_766 . ? O4 Co1 N1 97.9(6) 3_465 . ? O6 Co1 N1 92.60(11) . . ? O4 Co1 N1 97.9(6) 17_766 27_656 ? O4 Co1 N1 82.4(6) 3_465 27_656 ? O6 Co1 N1 92.61(12) . 27_656 ? N1 Co1 N1 174.8(2) . 27_656 ? O4 Co1 N2 90.2(8) 17_766 . ? O4 Co1 N2 96.8(8) 3_465 . ? O6 Co1 N2 175.8(5) . . ? N1 Co1 N2 89.6(7) . . ? N1 Co1 N2 85.2(7) 27_656 . ? O4 Co1 N2 96.8(8) 17_766 27_656 ? O4 Co1 N2 90.2(8) 3_465 27_656 ? O6 Co1 N2 175.8(5) . 27_656 ? N1 Co1 N2 85.2(7) . 27_656 ? N1 Co1 N2 89.6(7) 27_656 27_656 ? N2 Co1 N2 8.4(11) . 27_656 ? O4 Co1 O1 9.3(11) 17_766 . ? O4 Co1 O1 169.6(10) 3_465 . ? O6 Co1 O1 88.5(5) . . ? N1 Co1 O1 91.4(6) . . ? N1 Co1 O1 88.8(6) 27_656 . ? N2 Co1 O1 87.8(8) . . ? N2 Co1 O1 95.1(7) 27_656 . ? O4 Co1 O1 169.6(10) 17_766 27_656 ? O4 Co1 O1 9.3(11) 3_465 27_656 ? O6 Co1 O1 88.5(5) . 27_656 ? N1 Co1 O1 88.8(6) . 27_656 ? N1 Co1 O1 91.4(6) 27_656 27_656 ? N2 Co1 O1 95.1(8) . 27_656 ? N2 Co1 O1 87.8(8) 27_656 27_656 ? O1 Co1 O1 177.1(10) . 27_656 ? C1 N1 C5 116.7(5) . . ? C1 N1 Co1 123.0(3) . . ? C5 N1 Co1 120.2(4) . . ? N1 C1 C2 123.4(5) . . ? N1 C1 H1A 118.3 . . ? C2 C1 H1A 118.3 . . ? C1 C2 C3 119.9(6) . . ? C1 C2 H2A 120.1 . . ? C3 C2 H2A 120.1 . . ? C4 C3 C2 116.4(6) . . ? C4 C3 C6 122.0(7) . . ? C2 C3 C6 121.5(7) . . ? C3 C4 C5 120.1(6) . . ? C3 C4 H4A 119.9 . . ? C5 C4 H4A 119.9 . . ? N1 C5 C4 123.5(6) . . ? N1 C5 H5A 118.3 . . ? C4 C5 H5A 118.3 . . ? C3 C6 C6 111.0(5) . 12_554 ? C3 C6 H6A 109.4 . . ? C6 C6 H6A 109.4 12_554 . ? C3 C6 H6B 109.4 . . ? C6 C6 H6B 109.4 12_554 . ? H6A C6 H6B 108.0 . . ? O4 O1 C15 85(5) 17_766 17_766 ? O4 O1 C7 89(5) 17_766 . ? C15 O1 C7 5.0(19) 17_766 . ? O4 O1 Co1 61(7) 17_766 . ? C15 O1 Co1 123.8(17) 17_766 . ? C7 O1 Co1 123.4(14) . . ? O3 O2 C7 70(3) 17_766 . ? O3 O2 C15 67(2) 17_766 17_766 ? C7 O2 C15 3(2) . 17_766 ? O2 O3 C7 77(3) 17_766 17_766 ? O2 O3 C15 82(3) 17_766 . ? C7 O3 C15 5(2) 17_766 . ? O1 O4 C15 77(4) 17_766 . ? O1 O4 C7 74(4) 17_766 17_766 ? C15 O4 C7 4.5(17) . 17_766 ? O1 O4 Co1 110(8) 17_766 17_766 ? C15 O4 Co1 134.9(17) . 17_766 ? C7 O4 Co1 132(2) 17_766 17_766 ? C15 C7 O3 112(10) 17_766 17_766 ? C15 C7 O2 144(10) 17_766 . ? O3 C7 O2 32.6(14) 17_766 . ? C15 C7 O1 72(10) 17_766 . ? O3 C7 O1 129.7(19) 17_766 . ? O2 C7 O1 120.6(12) . . ? C15 C7 O4 60(10) 17_766 17_766 ? O3 C7 O4 119.9(19) 17_766 17_766 ? O2 C7 O4 122(2) . 17_766 ? O1 C7 O4 17.3(17) . 17_766 ? C15 C7 C8 77(10) 17_766 . ? O3 C7 C8 102.8(17) 17_766 . ? O2 C7 C8 111.0(15) . . ? O1 C7 C8 125.7(16) . . ? O4 C7 C8 127(2) 17_766 . ? C15 C7 C14 63(10) 17_766 17_766 ? O3 C7 C14 122.7(19) 17_766 17_766 ? O2 C7 C14 132.4(16) . 17_766 ? O1 C7 C14 104.1(16) . 17_766 ? O4 C7 C14 105.6(19) 17_766 17_766 ? C8 C7 C14 21.8(5) . 17_766 ? C14 C8 O5 132(2) 17_766 17_766 ? C14 C8 C9 147(2) 17_766 . ? O5 C8 C9 19.5(8) 17_766 . ? C14 C8 C13 36.8(19) 17_766 . ? O5 C8 C13 100.9(8) 17_766 . ? C9 C8 C13 120.0 . . ? C14 C8 C15 80.9(17) 17_766 17_766 ? O5 C8 C15 145.9(11) 17_766 17_766 ? C9 C8 C15 126.9(9) . 17_766 ? C13 C8 C15 113.1(9) . 17_766 ? C14 C8 C7 83.7(19) 17_766 . ? O5 C8 C7 142.4(12) 17_766 . ? C9 C8 C7 123.2(11) . . ? C13 C8 C7 116.7(10) . . ? C15 C8 C7 4.2(16) 17_766 . ? O5 C9 C10 85.6(17) 17_766 . ? O5 C9 C8 35.0(17) 17_766 . ? C10 C9 C8 120.0 . . ? O5 C9 C11 60.9(16) 17_766 17_766 ? C10 C9 C11 24.8(4) . 17_766 ? C8 C9 C11 95.2(4) . 17_766 ? O5 C9 C14 29.3(16) 17_766 17_766 ? C10 C9 C14 112.1(5) . 17_766 ? C8 C9 C14 9.6(7) . 17_766 ? C11 C9 C14 87.4(6) 17_766 17_766 ? O5 C9 H9A 153.6 17_766 . ? C10 C9 H9A 120.0 . . ? C8 C9 H9A 120.0 . . ? C11 C9 H9A 144.8 17_766 . ? C14 C9 H9A 127.6 17_766 . ? C11 C10 C12 122(3) 17_766 17_766 ? C11 C10 C9 93.9(16) 17_766 . ? C12 C10 C9 143.9(16) 17_766 . ? C11 C10 C11 26.1(16) 17_766 . ? C12 C10 C11 96.1(16) 17_766 . ? C9 C10 C11 120.0 . . ? C11 C10 O5 71.1(15) 17_766 17_766 ? C12 C10 O5 166(2) 17_766 17_766 ? C9 C10 O5 22.9(5) . 17_766 ? C11 C10 O5 97.3(5) . 17_766 ? C11 C10 C10 17.8(14) 17_766 17_766 ? C12 C10 C10 104.5(16) 17_766 17_766 ? C9 C10 C10 111.6(4) . 17_766 ? C11 C10 C10 8.4(4) . 17_766 ? O5 C10 C10 88.9(5) 17_766 17_766 ? C11 C10 H10A 146.1 17_766 . ? C12 C10 H10A 23.9 17_766 . ? C9 C10 H10A 120.0 . . ? C11 C10 H10A 120.0 . . ? O5 C10 H10A 142.7 17_766 . ? C10 C10 H10A 128.4 17_766 . ? C10 C11 C11 134(2) 17_766 17_766 ? C10 C11 C12 33.9(13) 17_766 . ? C11 C11 C12 99.7(9) 17_766 . ? C10 C11 C10 153.8(13) 17_766 . ? C11 C11 C10 20.3(9) 17_766 . ? C12 C11 C10 120.0 . . ? C10 C11 O5 82.1(15) 17_766 . ? C11 C11 O5 144.4(11) 17_766 . ? C12 C11 O5 115.9(6) . . ? C10 C11 O5 124.1(6) . . ? C10 C11 C9 61.3(13) 17_766 17_766 ? C11 C11 C9 165.1(14) 17_766 17_766 ? C12 C11 C9 95.2(9) . 17_766 ? C10 C11 C9 144.8(9) . 17_766 ? O5 C11 C9 20.9(7) . 17_766 ? C10 C11 C12 175(2) 17_766 17_766 ? C11 C11 C12 51.8(7) 17_766 17_766 ? C12 C11 C12 151.5(9) . 17_766 ? C10 C11 C12 31.5(9) . 17_766 ? O5 C11 C12 92.7(8) . 17_766 ? C9 C11 C12 113.4(8) 17_766 17_766 ? C10 C12 C13 143.9(9) 17_766 . ? C10 C12 C11 23.9(9) 17_766 . ? C13 C12 C11 120.0 . . ? C10 C12 C11 52.4(6) 17_766 17_766 ? C13 C12 C11 91.5(6) . 17_766 ? C11 C12 C11 28.5(6) . 17_766 ? C10 C12 H12A 96.1 17_766 . ? C13 C12 H12A 120.0 . . ? C11 C12 H12A 120.0 . . ? C11 C12 H12A 148.5 17_766 . ? C14 C13 C12 136.7(10) 17_766 . ? C14 C13 C8 20.8(10) 17_766 . ? C12 C13 C8 120.0 . . ? C14 C13 O5 50.6(6) 17_766 17_766 ? C12 C13 O5 88.6(5) . 17_766 ? C8 C13 O5 31.4(5) . 17_766 ? C14 C13 H13A 101.9 17_766 . ? C12 C13 H13A 120.0 . . ? C8 C13 H13A 120.0 . . ? O5 C13 H13A 151.3 17_766 . ? C9 O5 C8 125(2) 17_766 17_766 ? C9 O5 C11 98.2(17) 17_766 . ? C8 O5 C11 134.6(10) 17_766 . ? C9 O5 C14 139(2) 17_766 . ? C8 O5 C14 17.6(8) 17_766 . ? C11 O5 C14 117.4(9) . . ? C9 O5 C10 71.5(14) 17_766 17_766 ? C8 O5 C10 160.7(14) 17_766 17_766 ? C11 O5 C10 26.8(6) . 17_766 ? C14 O5 C10 143.1(10) . 17_766 ? C9 O5 C13 169(3) 17_766 17_766 ? C8 O5 C13 47.7(7) 17_766 17_766 ? C11 O5 C13 87.2(8) . 17_766 ? C14 O5 C13 32.0(8) . 17_766 ? C10 O5 C13 114.0(11) 17_766 17_766 ? C8 C14 C13 122(3) 17_766 17_766 ? C8 C14 O5 30.4(16) 17_766 . ? C13 C14 O5 97.4(11) 17_766 . ? C8 C14 C15 76.7(17) 17_766 . ? C13 C14 C15 147.6(18) 17_766 . ? O5 C14 C15 106.6(9) . . ? C8 C14 C7 74.5(17) 17_766 17_766 ? C13 C14 C7 151.4(19) 17_766 17_766 ? O5 C14 C7 104.1(10) . 17_766 ? C15 C14 C7 3.8(16) . 17_766 ? C8 C14 C9 23.3(19) 17_766 17_766 ? C13 C14 C9 108.4(12) 17_766 17_766 ? O5 C14 C9 11.2(6) . 17_766 ? C15 C14 C9 97.2(9) . 17_766 ? C7 C14 C9 94.4(10) 17_766 17_766 ? C8 C14 H14A 119.0 17_766 . ? C13 C14 H14A 37.8 17_766 . ? O5 C14 H14A 111.1 . . ? C15 C14 H14A 111.4 . . ? C7 C14 H14A 115.1 17_766 . ? C9 C14 H14A 121.1 17_766 . ? C8 C14 H14B 125.9 17_766 . ? C13 C14 H14B 81.9 17_766 . ? O5 C14 H14B 109.9 . . ? C15 C14 H14B 108.9 . . ? C7 C14 H14B 107.6 17_766 . ? C9 C14 H14B 108.6 17_766 . ? H14A C14 H14B 108.8 . . ? C7 C15 O1 103(10) 17_766 17_766 ? C7 C15 O3 64(10) 17_766 . ? O1 C15 O3 128(2) 17_766 . ? C7 C15 O4 116(10) 17_766 . ? O1 C15 O4 18.0(17) 17_766 . ? O3 C15 O4 120.5(12) . . ? C7 C15 O2 34(10) 17_766 17_766 ? O1 C15 O2 115.8(18) 17_766 17_766 ? O3 C15 O2 30.6(13) . 17_766 ? O4 C15 O2 119(2) . 17_766 ? C7 C15 C8 99(10) 17_766 17_766 ? O1 C15 C8 130.1(18) 17_766 17_766 ? O3 C15 C8 101.8(12) . 17_766 ? O4 C15 C8 133.5(16) . 17_766 ? O2 C15 C8 107.2(14) 17_766 17_766 ? C7 C15 C14 113(10) 17_766 . ? O1 C15 C14 108.4(17) 17_766 . ? O3 C15 C14 123.1(13) . . ? O4 C15 C14 111.3(15) . . ? O2 C15 C14 128.7(15) 17_766 . ? C8 C15 C14 22.4(5) 17_766 . ? Co1 O6 H6C 114(5) . . ? N2 N2 C20 144.1(17) 27_656 27_656 ? N2 N2 C16 147(3) 27_656 . ? C20 N2 C16 9(2) 27_656 . ? N2 N2 C20 28.1(8) 27_656 . ? C20 N2 C20 116.0(10) 27_656 . ? C16 N2 C20 120.0 . . ? N2 N2 C16 27(3) 27_656 27_656 ? C20 N2 C16 118.3(6) 27_656 27_656 ? C16 N2 C16 123.3(5) . 27_656 ? C20 N2 C16 7.4(11) . 27_656 ? N2 N2 Co1 85.8(6) 27_656 . ? C20 N2 Co1 130.1(19) 27_656 . ? C16 N2 Co1 125.2(10) . . ? C20 N2 Co1 113.8(10) . . ? C16 N2 Co1 111.3(14) 27_656 . ? C20 C16 C19 83(3) 27_656 27_656 ? C20 C16 N2 32(6) 27_656 . ? C19 C16 N2 108.2(9) 27_656 . ? C20 C16 C17 104.2(13) 27_656 . ? C19 C16 C17 27.2(10) 27_656 . ? N2 C16 C17 120.0 . . ? C20 C16 N2 32(5) 27_656 27_656 ? C19 C16 N2 103.5(16) 27_656 27_656 ? N2 C16 N2 6.1(9) . 27_656 ? C17 C16 N2 114.1(7) . 27_656 ? C20 C16 H16A 126.9 27_656 . ? C19 C16 H16A 125.2 27_656 . ? N2 C16 H16A 120.0 . . ? C17 C16 H16A 120.0 . . ? N2 C16 H16A 125.9 27_656 . ? C19 C17 C18 80.6(16) 27_656 . ? C19 C17 C16 76.4(3) 27_656 . ? C18 C17 C16 120.0 . . ? C19 C17 C20 66.8(15) 27_656 27_656 ? C18 C17 C20 108.9(12) . 27_656 ? C16 C17 C20 12.7(14) . 27_656 ? C19 C17 C18 51.2(13) 27_656 27_656 ? C18 C17 C18 29.8(6) . 27_656 ? C16 C17 C18 109.5(2) . 27_656 ? C20 C17 C18 96.9(14) 27_656 27_656 ? C19 C17 H17A 113.5 27_656 . ? C18 C17 H17A 120.0 . . ? C16 C17 H17A 120.0 . . ? C20 C17 H17A 130.6 27_656 . ? C18 C17 H17A 122.2 27_656 . ? C18 C18 C19 75.5(14) 27_656 . ? C18 C18 C17 95.9(14) 27_656 . ? C19 C18 C17 120.0 . . ? C18 C18 C19 69.6(12) 27_656 27_656 ? C19 C18 C19 107.6(7) . 27_656 ? C17 C18 C19 26.6(10) . 27_656 ? C18 C18 C21 98.1(9) 27_656 . ? C19 C18 C21 120.5(7) . . ? C17 C18 C21 119.5(7) . . ? C19 C18 C21 125.5(10) 27_656 . ? C18 C18 C17 54.3(11) 27_656 27_656 ? C19 C18 C17 21.5(6) . 27_656 ? C17 C18 C17 120.4(5) . 27_656 ? C19 C18 C17 99.9(7) 27_656 27_656 ? C21 C18 C17 115.4(8) . 27_656 ? C18 C18 C21 54.7(8) 27_656 27_656 ? C19 C18 C21 108.0(10) . 27_656 ? C17 C18 C21 114.2(10) . 27_656 ? C19 C18 C21 100.1(10) 27_656 27_656 ? C21 C18 C21 43.7(7) . 27_656 ? C17 C18 C21 90.3(10) 27_656 27_656 ? C17 C19 C16 76.5(15) 27_656 27_656 ? C17 C19 C18 107.3(16) 27_656 . ? C16 C19 C18 131.3(13) 27_656 . ? C17 C19 C20 87.6(2) 27_656 . ? C16 C19 C20 14.1(14) 27_656 . ? C18 C19 C20 120.0 . . ? C17 C19 C18 72.7(16) 27_656 27_656 ? C16 C19 C18 116.9(14) 27_656 27_656 ? C18 C19 C18 35.0(7) . 27_656 ? C20 C19 C18 113.4(5) . 27_656 ? C17 C19 H19A 75.1 27_656 . ? C16 C19 H19A 108.0 27_656 . ? C18 C19 H19A 120.0 . . ? C20 C19 H19A 120.0 . . ? C18 C19 H19A 115.0 27_656 . ? C16 C20 N2 138(6) 27_656 27_656 ? C16 C20 C19 82.8(14) 27_656 . ? N2 C20 C19 127.6(13) 27_656 . ? C16 C20 N2 141(5) 27_656 . ? N2 C20 N2 7.8(12) 27_656 . ? C19 C20 N2 120.0 . . ? C16 C20 C17 63.1(10) 27_656 27_656 ? N2 C20 C17 132.3(19) 27_656 27_656 ? C19 C20 C17 25.6(6) . 27_656 ? N2 C20 C17 124.8(9) . 27_656 ? C16 C20 H20A 49.4 27_656 . ? N2 C20 H20A 112.4 27_656 . ? C19 C20 H20A 120.0 . . ? N2 C20 H20A 120.0 . . ? C17 C20 H20A 109.4 27_656 . ? C21 C21 C21 89.7(3) 8_644 27_656 ? C21 C21 C18 168.9(19) 8_644 . ? C21 C21 C18 81.6(5) 27_656 . ? C21 C21 C21 57.6(6) 8_644 22_556 ? C21 C21 C21 32.8(7) 27_656 22_556 ? C18 C21 C21 114.3(10) . 22_556 ? C21 C21 C18 144.3(6) 8_644 27_656 ? C21 C21 C18 54.7(4) 27_656 27_656 ? C18 C21 C18 27.1(6) . 27_656 ? C21 C21 C18 87.3(8) 22_556 27_656 ? C21 C21 H21A 81.5 8_644 . ? C21 C21 H21A 125.0 27_656 . ? C18 C21 H21A 109.2 . . ? C21 C21 H21A 108.8 22_556 . ? C18 C21 H21A 119.5 27_656 . ? C21 C21 H21B 70.9 8_644 . ? C21 C21 H21B 119.9 27_656 . ? C18 C21 H21B 107.4 . . ? C21 C21 H21B 108.8 22_556 . ? C18 C21 H21B 121.2 27_656 . ? H21A C21 H21B 108.1 . . ? H7A O7 H7B 110.5(19) . . ? 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 O4 Co1 N1 C1 -143.3(7) 17_766 . . . ? O4 Co1 N1 C1 29.6(7) 3_465 . . . ? O6 Co1 N1 C1 -57.2(4) . . . . ? N1 Co1 N1 C1 122.8(4) 27_656 . . . ? N2 Co1 N1 C1 126.4(7) . . . . ? N2 Co1 N1 C1 119.1(7) 27_656 . . . ? O1 Co1 N1 C1 -145.8(6) . . . . ? O1 Co1 N1 C1 31.3(6) 27_656 . . . ? O4 Co1 N1 C5 40.3(7) 17_766 . . . ? O4 Co1 N1 C5 -146.8(7) 3_465 . . . ? O6 Co1 N1 C5 126.4(4) . . . . ? N1 Co1 N1 C5 -53.6(4) 27_656 . . . ? N2 Co1 N1 C5 -50.0(7) . . . . ? N2 Co1 N1 C5 -57.3(7) 27_656 . . . ? O1 Co1 N1 C5 37.8(6) . . . . ? O1 Co1 N1 C5 -145.2(6) 27_656 . . . ? C5 N1 C1 C2 0.9(8) . . . . ? Co1 N1 C1 C2 -175.6(4) . . . . ? N1 C1 C2 C3 0.3(8) . . . . ? C1 C2 C3 C4 -1.6(8) . . . . ? C1 C2 C3 C6 175.1(5) . . . . ? C2 C3 C4 C5 1.8(9) . . . . ? C6 C3 C4 C5 -174.9(5) . . . . ? C1 N1 C5 C4 -0.7(8) . . . . ? Co1 N1 C5 C4 175.9(4) . . . . ? C3 C4 C5 N1 -0.6(9) . . . . ? C4 C3 C6 C6 73.4(10) . . . 12_554 ? C2 C3 C6 C6 -103.1(9) . . . 12_554 ? O4 Co1 O1 O4 -138(9) 3_465 . . 17_766 ? O6 Co1 O1 O4 -77(6) . . . 17_766 ? N1 Co1 O1 O4 16(6) . . . 17_766 ? N1 Co1 O1 O4 -170(6) 27_656 . . 17_766 ? N2 Co1 O1 O4 105(7) . . . 17_766 ? N2 Co1 O1 O4 101(6) 27_656 . . 17_766 ? O1 Co1 O1 O4 -77(6) 27_656 . . 17_766 ? O4 Co1 O1 C15 61(5) 17_766 . . 17_766 ? O4 Co1 O1 C15 -77(5) 3_465 . . 17_766 ? O6 Co1 O1 C15 -16(2) . . . 17_766 ? N1 Co1 O1 C15 76(2) . . . 17_766 ? N1 Co1 O1 C15 -109(2) 27_656 . . 17_766 ? N2 Co1 O1 C15 166(2) . . . 17_766 ? N2 Co1 O1 C15 162(2) 27_656 . . 17_766 ? O1 Co1 O1 C15 -16(2) 27_656 . . 17_766 ? O4 Co1 O1 C7 67(6) 17_766 . . . ? O4 Co1 O1 C7 -71(5) 3_465 . . . ? O6 Co1 O1 C7 -10(2) . . . . ? N1 Co1 O1 C7 82(2) . . . . ? N1 Co1 O1 C7 -103(2) 27_656 . . . ? N2 Co1 O1 C7 172(2) . . . . ? N2 Co1 O1 C7 168(2) 27_656 . . . ? O1 Co1 O1 C7 -10(2) 27_656 . . . ? O3 O2 C7 C15 -16(21) 17_766 . . 17_766 ? C15 O2 C7 O3 16(21) 17_766 . . 17_766 ? O3 O2 C7 O1 -117(4) 17_766 . . . ? C15 O2 C7 O1 -101(21) 17_766 . . . ? O3 O2 C7 O4 -97(4) 17_766 . . 17_766 ? C15 O2 C7 O4 -81(21) 17_766 . . 17_766 ? O3 O2 C7 C8 81(4) 17_766 . . . ? C15 O2 C7 C8 96(21) 17_766 . . . ? O3 O2 C7 C14 86(5) 17_766 . . 17_766 ? C15 O2 C7 C14 102(22) 17_766 . . 17_766 ? O4 O1 C7 C15 -42(16) 17_766 . . 17_766 ? Co1 O1 C7 C15 -96(16) . . . 17_766 ? O4 O1 C7 O3 61(9) 17_766 . . 17_766 ? C15 O1 C7 O3 104(19) 17_766 . . 17_766 ? Co1 O1 C7 O3 8(4) . . . 17_766 ? O4 O1 C7 O2 100(9) 17_766 . . . ? C15 O1 C7 O2 142(18) 17_766 . . . ? Co1 O1 C7 O2 47(3) . . . . ? C15 O1 C7 O4 42(16) 17_766 . . 17_766 ? Co1 O1 C7 O4 -53(7) . . . 17_766 ? O4 O1 C7 C8 -101(8) 17_766 . . . ? C15 O1 C7 C8 -58(15) 17_766 . . . ? Co1 O1 C7 C8 -153.7(18) . . . . ? O4 O1 C7 C14 -97(8) 17_766 . . 17_766 ? C15 O1 C7 C14 -55(15) 17_766 . . 17_766 ? Co1 O1 C7 C14 -150.7(15) . . . 17_766 ? C15 C7 C8 C14 -48(19) 17_766 . . 17_766 ? O3 C7 C8 C14 -158(4) 17_766 . . 17_766 ? O2 C7 C8 C14 169(3) . . . 17_766 ? O1 C7 C8 C14 8(4) . . . 17_766 ? O4 C7 C8 C14 -13(4) 17_766 . . 17_766 ? C15 C7 C8 O5 148(18) 17_766 . . 17_766 ? O3 C7 C8 O5 38(4) 17_766 . . 17_766 ? O2 C7 C8 O5 5(4) . . . 17_766 ? O1 C7 C8 O5 -156(3) . . . 17_766 ? O4 C7 C8 O5 -177(3) 17_766 . . 17_766 ? C14 C7 C8 O5 -164(5) 17_766 . . 17_766 ? C15 C7 C8 C9 152(18) 17_766 . . . ? O3 C7 C8 C9 43(3) 17_766 . . . ? O2 C7 C8 C9 10(3) . . . . ? O1 C7 C8 C9 -152(2) . . . . ? O4 C7 C8 C9 -173(2) 17_766 . . . ? C14 C7 C8 C9 -160(3) 17_766 . . . ? C15 C7 C8 C13 -31(19) 17_766 . . . ? O3 C7 C8 C13 -140.8(18) 17_766 . . . ? O2 C7 C8 C13 -173.8(15) . . . . ? O1 C7 C8 C13 25(3) . . . . ? O4 C7 C8 C13 3(3) 17_766 . . . ? C14 C7 C8 C13 17(3) 17_766 . . . ? O3 C7 C8 C15 -110(20) 17_766 . . 17_766 ? O2 C7 C8 C15 -143(20) . . . 17_766 ? O1 C7 C8 C15 56(17) . . . 17_766 ? O4 C7 C8 C15 35(17) 17_766 . . 17_766 ? C14 C7 C8 C15 48(19) 17_766 . . 17_766 ? C14 C8 C9 O5 48(5) 17_766 . . 17_766 ? C13 C8 C9 O5 12(4) . . . 17_766 ? C15 C8 C9 O5 -169(5) 17_766 . . 17_766 ? C7 C8 C9 O5 -172(5) . . . 17_766 ? C14 C8 C9 C10 36(5) 17_766 . . . ? O5 C8 C9 C10 -12(4) 17_766 . . . ? C13 C8 C9 C10 0.0 . . . . ? C15 C8 C9 C10 178.7(15) 17_766 . . . ? C7 C8 C9 C10 176.2(16) . . . . ? C14 C8 C9 C11 36(5) 17_766 . . 17_766 ? O5 C8 C9 C11 -12(4) 17_766 . . 17_766 ? C13 C8 C9 C11 0.4(10) . . . 17_766 ? C15 C8 C9 C11 179.1(16) 17_766 . . 17_766 ? C7 C8 C9 C11 176.6(18) . . . 17_766 ? O5 C8 C9 C14 -48(5) 17_766 . . 17_766 ? C13 C8 C9 C14 -36(5) . . . 17_766 ? C15 C8 C9 C14 143(6) 17_766 . . 17_766 ? C7 C8 C9 C14 140(6) . . . 17_766 ? O5 C9 C10 C11 -6(2) 17_766 . . 17_766 ? C8 C9 C10 C11 1(2) . . . 17_766 ? C14 C9 C10 C11 7(3) 17_766 . . 17_766 ? O5 C9 C10 C12 172(7) 17_766 . . 17_766 ? C8 C9 C10 C12 179(5) . . . 17_766 ? C11 C9 C10 C12 178(8) 17_766 . . 17_766 ? C14 C9 C10 C12 -175(5) 17_766 . . 17_766 ? O5 C9 C10 C11 -7(2) 17_766 . . . ? C8 C9 C10 C11 0.0 . . . . ? C11 C9 C10 C11 -1(2) 17_766 . . . ? C14 C9 C10 C11 6.0(10) 17_766 . . . ? C8 C9 C10 O5 7(2) . . . 17_766 ? C11 C9 C10 O5 6(2) 17_766 . . 17_766 ? C14 C9 C10 O5 13(2) 17_766 . . 17_766 ? O5 C9 C10 C10 -7(2) 17_766 . . 17_766 ? C8 C9 C10 C10 0.3(9) . . . 17_766 ? C11 C9 C10 C10 -0.6(19) 17_766 . . 17_766 ? C14 C9 C10 C10 6.4(15) 17_766 . . 17_766 ? C11 C10 C11 C10 0(4) 17_766 . . 17_766 ? C12 C10 C11 C10 -177(8) 17_766 . . 17_766 ? C9 C10 C11 C10 2(6) . . . 17_766 ? O5 C10 C11 C10 -1(6) 17_766 . . 17_766 ? C12 C10 C11 C11 -177(9) 17_766 . . 17_766 ? C9 C10 C11 C11 2(6) . . . 17_766 ? O5 C10 C11 C11 -1(5) 17_766 . . 17_766 ? C10 C10 C11 C11 0(4) 17_766 . . 17_766 ? C11 C10 C11 C12 -2(6) 17_766 . . . ? C12 C10 C11 C12 -179(3) 17_766 . . . ? C9 C10 C11 C12 0.0 . . . . ? O5 C10 C11 C12 -2.7(9) 17_766 . . . ? C10 C10 C11 C12 -2(6) 17_766 . . . ? C11 C10 C11 O5 -179(100) 17_766 . . . ? C12 C10 C11 O5 4(3) 17_766 . . . ? C9 C10 C11 O5 -177.2(14) . . . . ? O5 C10 C11 O5 -179.9(14) 17_766 . . . ? C10 C10 C11 O5 -179(100) 17_766 . . . ? C11 C10 C11 C9 177(8) 17_766 . . 17_766 ? C12 C10 C11 C9 0(3) 17_766 . . 17_766 ? C9 C10 C11 C9 179(3) . . . 17_766 ? O5 C10 C11 C9 177(3) 17_766 . . 17_766 ? C10 C10 C11 C9 177(9) 17_766 . . 17_766 ? C11 C10 C11 C12 177(9) 17_766 . . 17_766 ? C9 C10 C11 C12 179(3) . . . 17_766 ? O5 C10 C11 C12 177(4) 17_766 . . 17_766 ? C10 C10 C11 C12 177(8) 17_766 . . 17_766 ? C11 C11 C12 C10 178(6) 17_766 . . 17_766 ? C10 C11 C12 C10 178(5) . . . 17_766 ? O5 C11 C12 C10 -4(4) . . . 17_766 ? C9 C11 C12 C10 -1(3) 17_766 . . 17_766 ? C12 C11 C12 C10 178(7) 17_766 . . 17_766 ? C10 C11 C12 C13 -178(5) 17_766 . . . ? C11 C11 C12 C13 -1(2) 17_766 . . . ? C10 C11 C12 C13 0.0 . . . . ? O5 C11 C12 C13 177.4(13) . . . . ? C9 C11 C12 C13 -179.6(19) 17_766 . . . ? C12 C11 C12 C13 -1(3) 17_766 . . . ? C10 C11 C12 C11 -178(6) 17_766 . . 17_766 ? C10 C11 C12 C11 1(2) . . . 17_766 ? O5 C11 C12 C11 178(3) . . . 17_766 ? C9 C11 C12 C11 -179(4) 17_766 . . 17_766 ? C12 C11 C12 C11 0.0(17) 17_766 . . 17_766 ? C10 C12 C13 C14 -17(4) 17_766 . . 17_766 ? C11 C12 C13 C14 -16(2) . . . 17_766 ? C11 C12 C13 C14 -16(3) 17_766 . . 17_766 ? C10 C12 C13 C8 -1(3) 17_766 . . . ? C11 C12 C13 C8 0.0 . . . . ? C11 C12 C13 C8 -0.4(9) 17_766 . . . ? C10 C12 C13 O5 1(3) 17_766 . . 17_766 ? C11 C12 C13 O5 2.1(7) . . . 17_766 ? C11 C12 C13 O5 1.7(8) 17_766 . . 17_766 ? O5 C8 C13 C14 152(5) 17_766 . . 17_766 ? C9 C8 C13 C14 148(5) . . . 17_766 ? C15 C8 C13 C14 -31(4) 17_766 . . 17_766 ? C7 C8 C13 C14 -29(4) . . . 17_766 ? C14 C8 C13 C12 -148(5) 17_766 . . . ? O5 C8 C13 C12 4.0(14) 17_766 . . . ? C9 C8 C13 C12 0.0 . . . . ? C15 C8 C13 C12 -178.8(13) 17_766 . . . ? C7 C8 C13 C12 -176.5(15) . . . . ? C14 C8 C13 O5 -152(5) 17_766 . . 17_766 ? C9 C8 C13 O5 -4.0(14) . . . 17_766 ? C15 C8 C13 O5 177(2) 17_766 . . 17_766 ? C7 C8 C13 O5 179(2) . . . 17_766 ? C10 C11 O5 C9 6.0(12) 17_766 . . 17_766 ? C11 C11 O5 C9 -175(7) 17_766 . . 17_766 ? C12 C11 O5 C9 8(2) . . . 17_766 ? C10 C11 O5 C9 -174(3) . . . 17_766 ? C12 C11 O5 C9 -173(4) 17_766 . . 17_766 ? C10 C11 O5 C8 171(3) 17_766 . . 17_766 ? C11 C11 O5 C8 -10(5) 17_766 . . 17_766 ? C12 C11 O5 C8 173(2) . . . 17_766 ? C10 C11 O5 C8 -9(3) . . . 17_766 ? C9 C11 O5 C8 165(4) 17_766 . . 17_766 ? C12 C11 O5 C8 -8(3) 17_766 . . 17_766 ? C10 C11 O5 C14 166(3) 17_766 . . . ? C11 C11 O5 C14 -15(5) 17_766 . . . ? C12 C11 O5 C14 168.4(13) . . . . ? C10 C11 O5 C14 -14.3(16) . . . . ? C9 C11 O5 C14 160(3) 17_766 . . . ? C12 C11 O5 C14 -12.5(17) 17_766 . . . ? C11 C11 O5 C10 179(100) 17_766 . . 17_766 ? C12 C11 O5 C10 2(2) . . . 17_766 ? C10 C11 O5 C10 180(3) . . . 17_766 ? C9 C11 O5 C10 -6.0(12) 17_766 . . 17_766 ? C12 C11 O5 C10 -178(4) 17_766 . . 17_766 ? C10 C11 O5 C13 177(4) 17_766 . . 17_766 ? C11 C11 O5 C13 -4(3) 17_766 . . 17_766 ? C12 C11 O5 C13 179.1(19) . . . 17_766 ? C10 C11 O5 C13 -3.6(15) . . . 17_766 ? C9 C11 O5 C13 171(4) 17_766 . . 17_766 ? C12 C11 O5 C13 -1.7(4) 17_766 . . 17_766 ? C9 O5 C14 C8 -43(7) 17_766 . . 17_766 ? C11 O5 C14 C8 169(5) . . . 17_766 ? C10 O5 C14 C8 179(100) 17_766 . . 17_766 ? C13 O5 C14 C8 148(6) 17_766 . . 17_766 ? C9 O5 C14 C13 169(6) 17_766 . . 17_766 ? C8 O5 C14 C13 -148(6) 17_766 . . 17_766 ? C11 O5 C14 C13 21(3) . . . 17_766 ? C10 O5 C14 C13 31(2) 17_766 . . 17_766 ? C9 O5 C14 C15 -33(5) 17_766 . . . ? C8 O5 C14 C15 10(4) 17_766 . . . ? C11 O5 C14 C15 178.6(15) . . . . ? C10 O5 C14 C15 -170.9(19) 17_766 . . . ? C13 O5 C14 C15 158(3) 17_766 . . . ? C9 O5 C14 C7 -30(5) 17_766 . . 17_766 ? C8 O5 C14 C7 13(4) 17_766 . . 17_766 ? C11 O5 C14 C7 -178.5(16) . . . 17_766 ? C10 O5 C14 C7 -168(2) 17_766 . . 17_766 ? C13 O5 C14 C7 161(3) 17_766 . . 17_766 ? C8 O5 C14 C9 43(7) 17_766 . . 17_766 ? C11 O5 C14 C9 -149(5) . . . 17_766 ? C10 O5 C14 C9 -138(6) 17_766 . . 17_766 ? C13 O5 C14 C9 -169(6) 17_766 . . 17_766 ? O2 O3 C15 C7 10(13) 17_766 . . 17_766 ? O2 O3 C15 O1 -76(4) 17_766 . . 17_766 ? C7 O3 C15 O1 -86(13) 17_766 . . 17_766 ? O2 O3 C15 O4 -96(4) 17_766 . . . ? C7 O3 C15 O4 -106(13) 17_766 . . . ? C7 O3 C15 O2 -10(12) 17_766 . . 17_766 ? O2 O3 C15 C8 104(3) 17_766 . . 17_766 ? C7 O3 C15 C8 94(13) 17_766 . . 17_766 ? O2 O3 C15 C14 111(4) 17_766 . . . ? C7 O3 C15 C14 102(13) 17_766 . . . ? O1 O4 C15 C7 47(19) 17_766 . . 17_766 ? Co1 O4 C15 C7 -58(20) 17_766 . . 17_766 ? C7 O4 C15 O1 -47(19) 17_766 . . 17_766 ? Co1 O4 C15 O1 -105(9) 17_766 . . 17_766 ? O1 O4 C15 O3 120(8) 17_766 . . . ? C7 O4 C15 O3 73(18) 17_766 . . . ? Co1 O4 C15 O3 15(4) 17_766 . . . ? O1 O4 C15 O2 85(8) 17_766 . . 17_766 ? C7 O4 C15 O2 38(18) 17_766 . . 17_766 ? Co1 O4 C15 O2 -20(3) 17_766 . . 17_766 ? O1 O4 C15 C8 -87(9) 17_766 . . 17_766 ? C7 O4 C15 C8 -134(21) 17_766 . . 17_766 ? Co1 O4 C15 C8 167.6(17) 17_766 . . 17_766 ? O1 O4 C15 C14 -84(8) 17_766 . . . ? C7 O4 C15 C14 -131(20) 17_766 . . . ? Co1 O4 C15 C14 170.7(17) 17_766 . . . ? C8 C14 C15 C7 53(19) 17_766 . . 17_766 ? C13 C14 C15 C7 -176(19) 17_766 . . 17_766 ? O5 C14 C15 C7 48(20) . . . 17_766 ? C9 C14 C15 C7 42(19) 17_766 . . 17_766 ? C8 C14 C15 O1 167(3) 17_766 . . 17_766 ? C13 C14 C15 O1 -62(5) 17_766 . . 17_766 ? O5 C14 C15 O1 161.9(18) . . . 17_766 ? C7 C14 C15 O1 114(20) 17_766 . . 17_766 ? C9 C14 C15 O1 155.8(18) 17_766 . . 17_766 ? C8 C14 C15 O3 -19(4) 17_766 . . . ? C13 C14 C15 O3 112(4) 17_766 . . . ? O5 C14 C15 O3 -24(3) . . . . ? C7 C14 C15 O3 -73(19) 17_766 . . . ? C9 C14 C15 O3 -30(2) 17_766 . . . ? C8 C14 C15 O4 -174(3) 17_766 . . . ? C13 C14 C15 O4 -43(5) 17_766 . . . ? O5 C14 C15 O4 -179.2(16) . . . . ? C7 C14 C15 O4 133(20) 17_766 . . . ? C9 C14 C15 O4 174.7(17) 17_766 . . . ? C8 C14 C15 O2 18(4) 17_766 . . 17_766 ? C13 C14 C15 O2 149(4) 17_766 . . 17_766 ? O5 C14 C15 O2 13(3) . . . 17_766 ? C7 C14 C15 O2 -35(18) 17_766 . . 17_766 ? C9 C14 C15 O2 7(2) 17_766 . . 17_766 ? C13 C14 C15 C8 131(6) 17_766 . . 17_766 ? O5 C14 C15 C8 -5(2) . . . 17_766 ? C7 C14 C15 C8 -53(19) 17_766 . . 17_766 ? C9 C14 C15 C8 -11(3) 17_766 . . 17_766 ? O4 Co1 N2 N2 -142(10) 17_766 . . 27_656 ? O4 Co1 N2 N2 39(10) 3_465 . . 27_656 ? O6 Co1 N2 N2 -179.99(2) . . . 27_656 ? N1 Co1 N2 N2 -59(10) . . . 27_656 ? N1 Co1 N2 N2 121(10) 27_656 . . 27_656 ? O1 Co1 N2 N2 -151(10) . . . 27_656 ? O1 Co1 N2 N2 30(10) 27_656 . . 27_656 ? O4 Co1 N2 C20 41(4) 17_766 . . 27_656 ? O4 Co1 N2 C20 -139(4) 3_465 . . 27_656 ? O6 Co1 N2 C20 2(14) . . . 27_656 ? N1 Co1 N2 C20 123(4) . . . 27_656 ? N1 Co1 N2 C20 -57(4) 27_656 . . 27_656 ? N2 Co1 N2 C20 -178(14) 27_656 . . 27_656 ? O1 Co1 N2 C20 32(4) . . . 27_656 ? O1 Co1 N2 C20 -148(4) 27_656 . . 27_656 ? O4 Co1 N2 C16 51.0(10) 17_766 . . . ? O4 Co1 N2 C16 -128.6(10) 3_465 . . . ? O6 Co1 N2 C16 13(10) . . . . ? N1 Co1 N2 C16 133.4(8) . . . . ? N1 Co1 N2 C16 -46.9(7) 27_656 . . . ? N2 Co1 N2 C16 -167(10) 27_656 . . . ? O1 Co1 N2 C16 42.0(9) . . . . ? O1 Co1 N2 C16 -137.8(9) 27_656 . . . ? O4 Co1 N2 C20 -139.9(10) 17_766 . . . ? O4 Co1 N2 C20 40.4(11) 3_465 . . . ? O6 Co1 N2 C20 -178(100) . . . . ? N1 Co1 N2 C20 -57.5(8) . . . . ? N1 Co1 N2 C20 122.1(9) 27_656 . . . ? N2 Co1 N2 C20 2(9) 27_656 . . . ? O1 Co1 N2 C20 -148.9(10) . . . . ? O1 Co1 N2 C20 31.2(11) 27_656 . . . ? O4 Co1 N2 C16 -132.4(19) 17_766 . . 27_656 ? O4 Co1 N2 C16 48(2) 3_465 . . 27_656 ? O6 Co1 N2 C16 -171(8) . . . 27_656 ? N1 Co1 N2 C16 -50.0(19) . . . 27_656 ? N1 Co1 N2 C16 129.7(19) 27_656 . . 27_656 ? N2 Co1 N2 C16 9(8) 27_656 . . 27_656 ? O1 Co1 N2 C16 -141(2) . . . 27_656 ? O1 Co1 N2 C16 39(2) 27_656 . . 27_656 ? N2 N2 C16 C20 79(12) 27_656 . . 27_656 ? C20 N2 C16 C20 68(9) . . . 27_656 ? C16 N2 C16 C20 60(8) 27_656 . . 27_656 ? Co1 N2 C16 C20 -124(10) . . . 27_656 ? N2 N2 C16 C19 39(16) 27_656 . . 27_656 ? C20 N2 C16 C19 -41(8) 27_656 . . 27_656 ? C20 N2 C16 C19 26.9(10) . . . 27_656 ? C16 N2 C16 C19 19.2(13) 27_656 . . 27_656 ? Co1 N2 C16 C19 -165(2) . . . 27_656 ? N2 N2 C16 C17 12(17) 27_656 . . . ? C20 N2 C16 C17 -68(9) 27_656 . . . ? C20 N2 C16 C17 0.0 . . . . ? C16 N2 C16 C17 -7.8(14) 27_656 . . . ? Co1 N2 C16 C17 168.4(16) . . . . ? C20 N2 C16 N2 -79(12) 27_656 . . 27_656 ? C20 N2 C16 N2 -12(17) . . . 27_656 ? C16 N2 C16 N2 -20(15) 27_656 . . 27_656 ? Co1 N2 C16 N2 157(18) . . . 27_656 ? C20 C16 C17 C19 40(7) 27_656 . . 27_656 ? N2 C16 C17 C19 70.5(19) . . . 27_656 ? N2 C16 C17 C19 72(3) 27_656 . . 27_656 ? C20 C16 C17 C18 -31(7) 27_656 . . . ? C19 C16 C17 C18 -70.5(19) 27_656 . . . ? N2 C16 C17 C18 0.0 . . . . ? N2 C16 C17 C18 1(2) 27_656 . . . ? C19 C16 C17 C20 -40(7) 27_656 . . 27_656 ? N2 C16 C17 C20 31(7) . . . 27_656 ? N2 C16 C17 C20 32(6) 27_656 . . 27_656 ? C20 C16 C17 C18 0(8) 27_656 . . 27_656 ? C19 C16 C17 C18 -39.6(15) 27_656 . . 27_656 ? N2 C16 C17 C18 30.8(7) . . . 27_656 ? N2 C16 C17 C18 32(2) 27_656 . . 27_656 ? C19 C17 C18 C18 8.4(7) 27_656 . . 27_656 ? C16 C17 C18 C18 76.6(8) . . . 27_656 ? C20 C17 C18 C18 70(2) 27_656 . . 27_656 ? C19 C17 C18 C19 -68.2(9) 27_656 . . . ? C16 C17 C18 C19 0.0 . . . . ? C20 C17 C18 C19 -6.8(18) 27_656 . . . ? C18 C17 C18 C19 -76.6(8) 27_656 . . . ? C16 C17 C18 C19 68.2(9) . . . 27_656 ? C20 C17 C18 C19 61.4(18) 27_656 . . 27_656 ? C18 C17 C18 C19 -8.4(7) 27_656 . . 27_656 ? C19 C17 C18 C21 111.2(15) 27_656 . . . ? C16 C17 C18 C21 179.4(11) . . . . ? C20 C17 C18 C21 172.6(14) 27_656 . . . ? C18 C17 C18 C21 102.8(15) 27_656 . . . ? C19 C17 C18 C17 -43.3(9) 27_656 . . 27_656 ? C16 C17 C18 C17 24.9(7) . . . 27_656 ? C20 C17 C18 C17 18(2) 27_656 . . 27_656 ? C18 C17 C18 C17 -51.7(7) 27_656 . . 27_656 ? C19 C17 C18 C21 62.3(12) 27_656 . . 27_656 ? C16 C17 C18 C21 130.5(9) . . . 27_656 ? C20 C17 C18 C21 123.7(15) 27_656 . . 27_656 ? C18 C17 C18 C21 53.9(11) 27_656 . . 27_656 ? C18 C18 C19 C17 9.0(6) 27_656 . . 27_656 ? C17 C18 C19 C17 97.4(12) . . . 27_656 ? C19 C18 C19 C17 71.5(13) 27_656 . . 27_656 ? C21 C18 C19 C17 -82.0(14) . . . 27_656 ? C21 C18 C19 C17 -35.7(11) 27_656 . . 27_656 ? C18 C18 C19 C16 -78(2) 27_656 . . 27_656 ? C17 C18 C19 C16 10.4(18) . . . 27_656 ? C19 C18 C19 C16 -15.5(16) 27_656 . . 27_656 ? C21 C18 C19 C16 -169.0(15) . . . 27_656 ? C17 C18 C19 C16 -87(2) 27_656 . . 27_656 ? C21 C18 C19 C16 -122.7(15) 27_656 . . 27_656 ? C18 C18 C19 C20 -88.5(9) 27_656 . . . ? C17 C18 C19 C20 0.0 . . . . ? C19 C18 C19 C20 -25.9(9) 27_656 . . . ? C21 C18 C19 C20 -179.4(11) . . . . ? C17 C18 C19 C20 -97.4(12) 27_656 . . . ? C21 C18 C19 C20 -133.2(9) 27_656 . . . ? C17 C18 C19 C18 88.5(9) . . . 27_656 ? C19 C18 C19 C18 62.6(10) 27_656 . . 27_656 ? C21 C18 C19 C18 -90.9(12) . . . 27_656 ? C17 C18 C19 C18 -9.0(6) 27_656 . . 27_656 ? C21 C18 C19 C18 -44.7(8) 27_656 . . 27_656 ? C17 C19 C20 C16 38(5) 27_656 . . 27_656 ? C18 C19 C20 C16 146(5) . . . 27_656 ? C18 C19 C20 C16 108(5) 27_656 . . 27_656 ? C17 C19 C20 N2 -111(4) 27_656 . . 27_656 ? C16 C19 C20 N2 -149(8) 27_656 . . 27_656 ? C18 C19 C20 N2 -2(3) . . . 27_656 ? C18 C19 C20 N2 -41(3) 27_656 . . 27_656 ? C17 C19 C20 N2 -109(2) 27_656 . . . ? C16 C19 C20 N2 -146(5) 27_656 . . . ? C18 C19 C20 N2 0.0 . . . . ? C18 C19 C20 N2 -38.6(8) 27_656 . . . ? C16 C19 C20 C17 -38(5) 27_656 . . 27_656 ? C18 C19 C20 C17 109(2) . . . 27_656 ? C18 C19 C20 C17 70.0(18) 27_656 . . 27_656 ? N2 N2 C20 C16 75(18) 27_656 . . 27_656 ? C20 N2 C20 C16 -109(6) 27_656 . . 27_656 ? C16 N2 C20 C16 -119(5) . . . 27_656 ? Co1 N2 C20 C16 72(4) . . . 27_656 ? C20 N2 C20 N2 176(23) 27_656 . . 27_656 ? C16 N2 C20 N2 166(20) . . . 27_656 ? C16 N2 C20 N2 -75(18) 27_656 . . 27_656 ? Co1 N2 C20 N2 -3(19) . . . 27_656 ? N2 N2 C20 C19 -166(20) 27_656 . . . ? C20 N2 C20 C19 10(3) 27_656 . . . ? C16 N2 C20 C19 0.0 . . . . ? C16 N2 C20 C19 119(5) 27_656 . . . ? Co1 N2 C20 C19 -169.7(14) . . . . ? N2 N2 C20 C17 164(20) 27_656 . . 27_656 ? C20 N2 C20 C17 -20(3) 27_656 . . 27_656 ? C16 N2 C20 C17 -29.9(8) . . . 27_656 ? C16 N2 C20 C17 89(5) 27_656 . . 27_656 ? Co1 N2 C20 C17 160.5(17) . . . 27_656 ? C18 C18 C21 C21 46(11) 27_656 . . 8_644 ? C19 C18 C21 C21 123(12) . . . 8_644 ? C17 C18 C21 C21 -56(12) . . . 8_644 ? C19 C18 C21 C21 -25(12) 27_656 . . 8_644 ? C17 C18 C21 C21 100(12) 27_656 . . 8_644 ? C21 C18 C21 C21 39(10) 27_656 . . 8_644 ? C18 C18 C21 C21 6.4(17) 27_656 . . 27_656 ? C19 C18 C21 C21 84.3(16) . . . 27_656 ? C17 C18 C21 C21 -95.1(16) . . . 27_656 ? C19 C18 C21 C21 -64.2(18) 27_656 . . 27_656 ? C17 C18 C21 C21 60.7(17) 27_656 . . 27_656 ? C18 C18 C21 C21 4.4(17) 27_656 . . 22_556 ? C19 C18 C21 C21 82.3(7) . . . 22_556 ? C17 C18 C21 C21 -97.1(8) . . . 22_556 ? C19 C18 C21 C21 -66.2(12) 27_656 . . 22_556 ? C17 C18 C21 C21 58.7(10) 27_656 . . 22_556 ? C21 C18 C21 C21 -2.0(13) 27_656 . . 22_556 ? C19 C18 C21 C18 77.9(16) . . . 27_656 ? C17 C18 C21 C18 -101.5(19) . . . 27_656 ? C19 C18 C21 C18 -70.6(15) 27_656 . . 27_656 ? C17 C18 C21 C18 54.2(12) 27_656 . . 27_656 ? C21 C18 C21 C18 -6.4(17) 27_656 . . 27_656 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.329 _refine_diff_density_min -0.294 _refine_diff_density_rms 0.057 #===END data_complex3 _database_code_depnum_ccdc_archive 'CCDC 637134' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H30 Co N4 O10' _chemical_formula_weight 761.59 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 4.7808(16) _cell_length_b 9.229(3) _cell_length_c 18.829(7) _cell_angle_alpha 91.954(6) _cell_angle_beta 95.509(6) _cell_angle_gamma 99.022(5) _cell_volume 815.7(5) _cell_formula_units_Z 1 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 1511 _cell_measurement_theta_min 0.00 _cell_measurement_theta_max 0.00 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 1.550 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 393 _exptl_absorpt_coefficient_mu 0.597 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.767035 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 4171 _diffrn_reflns_av_R_equivalents 0.0284 _diffrn_reflns_av_sigmaI/netI 0.0588 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.09 _diffrn_reflns_theta_max 25.01 _reflns_number_total 2852 _reflns_number_gt 2265 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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^)+(0.0655P)^2^+0.8472P] 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_number_reflns 2852 _refine_ls_number_parameters 355 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0757 _refine_ls_R_factor_gt 0.0544 _refine_ls_wR_factor_ref 0.1450 _refine_ls_wR_factor_gt 0.1299 _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_restrained_S_all 1.112 _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 1.0000 0.0000 0.5000 0.0230(2) Uani 1 2 d S . . O1 O 1.2719(5) 0.1822(3) 0.46811(13) 0.0294(6) Uani 1 1 d . . . O2 O 1.7036(5) 0.1400(3) 0.51002(14) 0.0316(6) Uani 1 1 d . . . O3 O 1.4942(6) 0.4464(3) 0.41662(14) 0.0355(7) Uani 1 1 d . A . N1 N 0.8682(6) -0.0592(3) 0.38622(16) 0.0258(7) Uani 1 1 d . . . C1 C 1.5372(7) 0.2141(4) 0.47852(18) 0.0229(8) Uani 1 1 d . . . C2 C 1.6802(8) 0.3584(4) 0.4531(2) 0.0308(9) Uani 1 1 d . . . H2A H 1.7837 0.4160 0.4941 0.037 Uiso 1 1 calc R . . H2B H 1.8187 0.3378 0.4213 0.037 Uiso 1 1 calc R . . C3 C 1.3879(8) 0.4065(4) 0.3479(2) 0.0307(9) Uani 1 1 d . . . C4 C 1.155(2) 0.4637(10) 0.3208(5) 0.034(2) Uani 0.50 1 d P A 1 H4A H 1.0761 0.5273 0.3495 0.041 Uiso 0.50 1 calc PR A 1 C5 C 1.036(2) 0.4280(10) 0.2510(5) 0.038(2) Uani 0.50 1 d P A 1 H5 H 0.8702 0.4629 0.2345 0.045 Uiso 0.50 1 calc PR A 1 C4' C 1.306(2) 0.5225(12) 0.3086(5) 0.046(2) Uani 0.50 1 d P A 2 H4'A H 1.3263 0.6167 0.3295 0.055 Uiso 0.50 1 calc PR A 2 C5' C 1.192(2) 0.4929(15) 0.2371(6) 0.062(3) Uani 0.50 1 d P A 2 H5'A H 1.1402 0.5680 0.2095 0.074 Uiso 0.50 1 calc PR A 2 C6 C 1.1559(10) 0.3429(6) 0.2066(2) 0.0464(12) Uani 1 1 d D . . C7 C 1.403(2) 0.2816(11) 0.2336(5) 0.040(2) Uani 0.50 1 d P A 1 H7A H 1.4834 0.2201 0.2043 0.048 Uiso 0.50 1 calc PR A 1 C8 C 1.518(2) 0.3157(10) 0.3037(5) 0.0347(19) Uani 0.50 1 d P A 1 H8A H 1.6793 0.2789 0.3215 0.042 Uiso 0.50 1 calc PR A 1 C7' C 1.234(3) 0.2439(13) 0.2457(5) 0.047(2) Uani 0.50 1 d P A 2 H7'A H 1.2131 0.1491 0.2254 0.056 Uiso 0.50 1 calc PR A 2 C8' C 1.346(2) 0.2676(10) 0.3160(4) 0.0355(19) Uani 0.50 1 d P A 2 H8'A H 1.3937 0.1894 0.3420 0.043 Uiso 0.50 1 calc PR A 2 C9 C 1.0251(12) 0.2989(8) 0.1312(3) 0.0696(18) Uani 1 1 d D A . O4 O 1.000(3) 0.1791(15) 0.1016(10) 0.111(7) Uani 0.50 1 d PD A 1 O5 O 0.952(3) 0.4125(15) 0.1010(8) 0.135(8) Uani 0.50 1 d PD A 1 H5A H 0.8684 0.3891 0.0578 0.162 Uiso 0.50 1 d PRD A 1 O4' O 1.127(3) 0.2068(14) 0.0979(9) 0.083(5) Uani 0.50 1 d PD A 2 O5' O 0.814(2) 0.3594(15) 0.1089(6) 0.085(4) Uani 0.50 1 d PD A 2 H5A' H 0.7280 0.3241 0.0690 0.102 Uiso 0.50 1 d PRD A 2 C10 C 0.5986(16) -0.0463(9) 0.3559(4) 0.0303(17) Uani 0.50 1 d P B 1 H10A H 0.4724 -0.0134 0.3850 0.036 Uiso 0.50 1 calc PR B 1 C11 C 0.5084(17) -0.0801(9) 0.2847(4) 0.0356(19) Uani 0.50 1 d P B 1 H11A H 0.3293 -0.0641 0.2661 0.043 Uiso 0.50 1 calc PR B 1 C10' C 0.8715(16) 0.0426(9) 0.3367(4) 0.0305(17) Uani 0.50 1 d P B 2 H10B H 0.9394 0.1404 0.3506 0.037 Uiso 0.50 1 calc PR B 2 C11' C 0.7764(18) 0.0054(10) 0.2656(4) 0.039(2) Uani 0.50 1 d P B 2 H11B H 0.7742 0.0797 0.2335 0.047 Uiso 0.50 1 calc PR B 2 C12 C 0.6848(8) -0.1380(5) 0.2410(2) 0.0311(9) Uani 1 1 d . . . C13 C 0.9544(17) -0.1526(10) 0.2720(4) 0.038(2) Uani 0.50 1 d P B 1 H13A H 1.0837 -0.1876 0.2445 0.046 Uiso 0.50 1 calc PR B 1 C14 C 1.0288(16) -0.1150(10) 0.3432(4) 0.036(2) Uani 0.50 1 d P B 1 H14A H 1.2075 -0.1303 0.3627 0.044 Uiso 0.50 1 calc PR B 1 C13' C 0.7042(17) -0.2433(9) 0.2939(5) 0.038(2) Uani 0.50 1 d P B 2 H13B H 0.6551 -0.3429 0.2811 0.045 Uiso 0.50 1 calc PR B 2 C14' C 0.7953(17) -0.1986(9) 0.3640(4) 0.0354(19) Uani 0.50 1 d P B 2 H14B H 0.8059 -0.2701 0.3973 0.042 Uiso 0.50 1 calc PR B 2 C15 C 0.5876(9) -0.1767(5) 0.16323(17) 0.036(8) Uani 0.50 1 d PG B 1 C16 C 0.3711(11) -0.1128(6) 0.1286(2) 0.047(3) Uani 0.50 1 d PG B 1 H16A H 0.2891 -0.0438 0.1530 0.057 Uiso 0.50 1 calc PR B 1 C17 C 0.2771(11) -0.1522(7) 0.0573(2) 0.065(5) Uani 0.50 1 d PG B 1 H17A H 0.1323 -0.1095 0.0342 0.078 Uiso 0.50 1 calc PR B 1 N2 N 0.3997(11) -0.2554(7) 0.02078(15) 0.087(6) Uani 0.50 1 d PG B 1 C18 C 0.6162(11) -0.3192(6) 0.0554(2) 0.045(2) Uani 0.50 1 d PG B 1 H18A H 0.6982 -0.3882 0.0310 0.054 Uiso 0.50 1 calc PR B 1 C19 C 0.7102(10) -0.2798(6) 0.1267(2) 0.041(2) Uani 0.50 1 d PG B 1 H19A H 0.8551 -0.3225 0.1498 0.049 Uiso 0.50 1 calc PR B 1 C15' C 0.5732(10) -0.1857(5) 0.16632(16) 0.048(9) Uani 0.50 1 d PG B 2 C16' C 0.4702(12) -0.0891(4) 0.1192(2) 0.079(5) Uani 0.50 1 d PG B 2 H16B H 0.4782 0.0089 0.1337 0.095 Uiso 0.50 1 calc PR B 2 C17' C 0.3552(12) -0.1391(6) 0.0505(2) 0.099(8) Uani 0.50 1 d PG B 2 H17B H 0.2862 -0.0745 0.0190 0.118 Uiso 0.50 1 calc PR B 2 N2' N 0.3432(11) -0.2857(6) 0.02889(19) 0.071(4) Uani 0.50 1 d PG B 2 C18' C 0.4463(14) -0.3823(4) 0.0760(3) 0.116(6) Uani 0.50 1 d PG B 2 H18B H 0.4383 -0.4803 0.0615 0.139 Uiso 0.50 1 calc PR B 2 C19' C 0.5613(13) -0.3323(5) 0.1447(2) 0.081(4) Uani 0.50 1 d PG B 2 H19B H 0.6302 -0.3969 0.1762 0.097 Uiso 0.50 1 calc PR B 2 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 0.0172(4) 0.0296(4) 0.0213(4) 0.0032(3) -0.0019(3) 0.0030(3) O1 0.0192(13) 0.0340(15) 0.0339(15) 0.0056(12) -0.0034(11) 0.0042(11) O2 0.0238(13) 0.0388(16) 0.0321(15) 0.0056(12) -0.0013(11) 0.0063(12) O3 0.0481(17) 0.0282(15) 0.0289(15) 0.0031(12) -0.0023(12) 0.0058(13) N1 0.0225(15) 0.0303(18) 0.0239(16) 0.0021(14) -0.0017(13) 0.0042(13) C1 0.0214(18) 0.030(2) 0.0182(17) -0.0017(15) 0.0003(14) 0.0068(15) C2 0.028(2) 0.035(2) 0.027(2) 0.0043(17) -0.0038(16) 0.0011(17) C3 0.030(2) 0.033(2) 0.027(2) 0.0060(17) 0.0008(16) -0.0005(17) C4 0.035(5) 0.037(5) 0.031(5) 0.005(4) 0.006(4) 0.004(4) C5 0.041(5) 0.042(5) 0.032(5) 0.013(4) -0.002(4) 0.012(4) C4' 0.048(6) 0.041(6) 0.050(6) 0.014(5) 0.002(5) 0.010(5) C5' 0.036(6) 0.098(10) 0.055(7) 0.048(7) -0.001(5) 0.019(6) C6 0.038(2) 0.066(3) 0.032(2) 0.001(2) 0.000(2) 0.003(2) C7 0.036(5) 0.047(6) 0.039(5) 0.004(4) 0.006(5) 0.010(5) C8 0.033(5) 0.038(5) 0.035(5) 0.004(4) 0.002(4) 0.010(4) C7' 0.058(7) 0.058(7) 0.025(5) -0.003(5) -0.004(5) 0.018(6) C8' 0.041(5) 0.040(5) 0.027(4) 0.000(4) 0.004(4) 0.012(4) C9 0.056(4) 0.120(6) 0.037(3) 0.020(4) 0.001(3) 0.025(4) O4 0.138(14) 0.116(10) 0.046(6) -0.004(6) -0.049(9) -0.045(10) O5 0.099(12) 0.25(2) 0.064(7) -0.026(9) -0.038(9) 0.083(12) O4' 0.096(10) 0.093(9) 0.057(6) -0.035(8) -0.032(8) 0.041(8) O5' 0.067(8) 0.146(9) 0.046(5) -0.040(6) -0.040(5) 0.068(7) C10 0.027(4) 0.037(5) 0.028(4) -0.001(3) 0.007(3) 0.006(3) C11 0.029(4) 0.049(5) 0.030(4) 0.001(4) -0.004(3) 0.013(4) C10' 0.027(4) 0.028(4) 0.033(4) 0.002(3) -0.005(3) -0.001(3) C11' 0.041(5) 0.050(6) 0.023(4) 0.008(4) -0.001(4) 0.004(4) C12 0.0251(19) 0.044(2) 0.023(2) -0.0021(18) -0.0010(16) 0.0047(17) C13 0.032(4) 0.056(6) 0.029(4) -0.005(4) 0.000(3) 0.019(4) C14 0.024(4) 0.060(6) 0.027(4) -0.005(4) -0.003(3) 0.017(4) C13' 0.034(4) 0.031(5) 0.046(5) -0.013(4) 0.001(4) -0.001(4) C14' 0.034(4) 0.033(5) 0.038(5) 0.004(4) 0.003(4) 0.003(4) C15 0.035(12) 0.048(13) 0.015(11) -0.008(9) -0.007(8) -0.020(9) C16 0.052(6) 0.076(8) 0.018(5) -0.005(5) 0.000(4) 0.028(6) C17 0.033(5) 0.122(14) 0.038(7) 0.020(8) -0.002(5) 0.013(6) N2 0.056(7) 0.157(15) 0.032(7) -0.001(8) -0.013(5) -0.024(9) C18 0.047(6) 0.058(6) 0.032(5) -0.007(4) 0.005(4) 0.012(5) C19 0.047(6) 0.054(6) 0.024(4) -0.002(4) 0.004(4) 0.017(5) C15' 0.030(12) 0.080(18) 0.036(15) 0.004(12) 0.001(10) 0.021(10) C16' 0.054(8) 0.152(15) 0.032(7) 0.019(8) 0.007(6) 0.011(8) C17' 0.055(8) 0.21(3) 0.040(9) 0.018(12) 0.010(7) 0.053(11) N2' 0.071(8) 0.085(8) 0.056(8) -0.035(7) 0.008(6) 0.014(6) C18' 0.100(12) 0.196(19) 0.044(7) -0.063(10) -0.011(8) 0.028(12) C19' 0.054(8) 0.116(12) 0.063(8) -0.049(8) -0.001(6) 0.005(7) _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 2.079(3) 2_856 ? Co1 O2 2.079(3) 1_455 ? Co1 O1 2.100(3) . ? Co1 O1 2.100(3) 2_756 ? Co1 N1 2.200(3) 2_756 ? Co1 N1 2.200(3) . ? O1 C1 1.251(4) . ? O2 C1 1.249(4) . ? O2 Co1 2.079(3) 1_655 ? O3 C3 1.360(5) . ? O3 C2 1.439(4) . ? N1 C14 1.313(8) . ? N1 C14' 1.322(9) . ? N1 C10' 1.345(8) . ? N1 C10 1.382(8) . ? C1 C2 1.514(5) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.368(10) . ? C3 C8' 1.374(10) . ? C3 C4' 1.407(10) . ? C3 C8 1.412(10) . ? C4 C5 1.390(12) . ? C4 H4A 0.9300 . ? C5 C6 1.355(10) . ? C5 H5 0.9300 . ? C4' C5' 1.403(14) . ? C4' H4'A 0.9300 . ? C5' C6 1.459(14) . ? C5' H5'A 0.9300 . ? C6 C7' 1.270(11) . ? C6 C7 1.443(11) . ? C6 C9 1.511(6) . ? C7 C8 1.387(12) . ? C7 H7A 0.9300 . ? C8 H8A 0.9300 . ? C7' C8' 1.377(12) . ? C7' H7'A 0.9300 . ? C8' H8'A 0.9300 . ? C9 O4 1.205(9) . ? C9 O4' 1.226(9) . ? C9 O5' 1.271(7) . ? C9 O5 1.290(8) . ? O5 H5A 0.8742 . ? O5' H5A' 0.8500 . ? C10 C11 1.378(11) . ? C10 H10A 0.9300 . ? C11 C12 1.386(9) . ? C11 H11A 0.9300 . ? C10' C11' 1.385(11) . ? C10' H10B 0.9300 . ? C11' C12 1.377(10) . ? C11' H11B 0.9300 . ? C12 C13 1.391(9) . ? C12 C13' 1.421(10) . ? C12 C15' 1.482(4) . ? C12 C15 1.506(4) . ? C13 C14 1.373(11) . ? C13 H13A 0.9300 . ? C14 H14A 0.9300 . ? C13' C14' 1.378(11) . ? C13' H13B 0.9300 . ? C14' H14B 0.9300 . ? C15 C16 1.3900 . ? C15 C19 1.3900 . ? C16 C17 1.3900 . ? C16 H16A 0.9300 . ? C17 N2 1.3900 . ? C17 H17A 0.9300 . ? N2 C18 1.3900 . ? C18 C19 1.3900 . ? C18 H18A 0.9300 . ? C19 H19A 0.9300 . ? C15' C16' 1.3900 . ? C15' C19' 1.3900 . ? C16' C17' 1.3900 . ? C16' H16B 0.9300 . ? C17' N2' 1.3900 . ? C17' H17B 0.9300 . ? N2' C18' 1.3900 . ? C18' C19' 1.3900 . ? C18' H18B 0.9300 . ? C19' H19B 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Co1 O2 179.997(2) 2_856 1_455 ? O2 Co1 O1 93.13(10) 2_856 . ? O2 Co1 O1 86.87(10) 1_455 . ? O2 Co1 O1 86.87(10) 2_856 2_756 ? O2 Co1 O1 93.13(10) 1_455 2_756 ? O1 Co1 O1 180.0 . 2_756 ? O2 Co1 N1 94.93(11) 2_856 2_756 ? O2 Co1 N1 85.08(11) 1_455 2_756 ? O1 Co1 N1 92.09(11) . 2_756 ? O1 Co1 N1 87.91(10) 2_756 2_756 ? O2 Co1 N1 85.07(11) 2_856 . ? O2 Co1 N1 94.92(11) 1_455 . ? O1 Co1 N1 87.91(10) . . ? O1 Co1 N1 92.09(11) 2_756 . ? N1 Co1 N1 180.0 2_756 . ? C1 O1 Co1 129.6(2) . . ? C1 O2 Co1 146.6(2) . 1_655 ? C3 O3 C2 118.6(3) . . ? C14 N1 C14' 61.8(5) . . ? C14 N1 C10' 81.9(5) . . ? C14' N1 C10' 117.7(5) . . ? C14 N1 C10 115.2(5) . . ? C14' N1 C10 84.1(5) . . ? C10' N1 C10 67.2(5) . . ? C14 N1 Co1 123.7(4) . . ? C14' N1 Co1 120.2(4) . . ? C10' N1 Co1 122.0(4) . . ? C10 N1 Co1 121.1(4) . . ? O2 C1 O1 126.8(4) . . ? O2 C1 C2 114.5(3) . . ? O1 C1 C2 118.7(3) . . ? O3 C2 C1 115.9(3) . . ? O3 C2 H2A 108.3 . . ? C1 C2 H2A 108.3 . . ? O3 C2 H2B 108.3 . . ? C1 C2 H2B 108.3 . . ? H2A C2 H2B 107.4 . . ? O3 C3 C4 117.6(5) . . ? O3 C3 C8' 126.8(5) . . ? C4 C3 C8' 103.6(6) . . ? O3 C3 C4' 114.0(5) . . ? C8' C3 C4' 119.2(6) . . ? O3 C3 C8 122.4(5) . . ? C4 C3 C8 120.0(6) . . ? C4' C3 C8 109.4(6) . . ? C3 C4 C5 120.7(8) . . ? C3 C4 H4A 119.6 . . ? C5 C4 H4A 119.6 . . ? C6 C5 C4 121.0(8) . . ? C6 C5 H5 119.5 . . ? C4 C5 H5 119.5 . . ? C5' C4' C3 118.6(9) . . ? C5' C4' H4'A 120.7 . . ? C3 C4' H4'A 120.7 . . ? C4' C5' C6 119.2(9) . . ? C4' C5' H5'A 120.4 . . ? C6 C5' H5'A 120.4 . . ? C7' C6 C5 104.3(7) . . ? C5 C6 C7 119.4(6) . . ? C7' C6 C5' 118.5(7) . . ? C7 C6 C5' 107.0(6) . . ? C7' C6 C9 118.4(6) . . ? C5 C6 C9 122.0(5) . . ? C7 C6 C9 118.4(6) . . ? C5' C6 C9 123.2(6) . . ? C8 C7 C6 119.2(8) . . ? C8 C7 H7A 120.4 . . ? C6 C7 H7A 120.4 . . ? C7 C8 C3 119.6(8) . . ? C7 C8 H8A 120.2 . . ? C3 C8 H8A 120.2 . . ? C6 C7' C8' 124.5(9) . . ? C6 C7' H7'A 117.8 . . ? C8' C7' H7'A 117.8 . . ? C3 C8' C7' 120.1(8) . . ? C3 C8' H8'A 120.0 . . ? C7' C8' H8'A 120.0 . . ? O4 C9 O5' 108.6(11) . . ? O4' C9 O5' 126.2(10) . . ? O4 C9 O5 124.0(13) . . ? O4' C9 O5 121.3(13) . . ? O4 C9 C6 126.7(11) . . ? O4' C9 C6 117.6(9) . . ? O5' C9 C6 116.3(7) . . ? O5 C9 C6 109.3(9) . . ? C9 O5 H5A 111.0 . . ? C9 O5 H5A' 87.3 . . ? C9 O5' H5A 101.1 . . ? C9 O5' H5A' 114.9 . . ? H5A O5' H5A' 53.4 . . ? C11 C10 N1 123.0(6) . . ? C11 C10 H10A 118.5 . . ? N1 C10 H10A 118.5 . . ? C10 C11 C12 120.0(6) . . ? C10 C11 H11A 120.0 . . ? C12 C11 H11A 120.0 . . ? N1 C10' C11' 121.7(7) . . ? N1 C10' H10B 119.1 . . ? C11' C10' H10B 119.1 . . ? C12 C11' C10' 122.1(7) . . ? C12 C11' H11B 119.0 . . ? C10' C11' H11B 119.0 . . ? C11' C12 C11 64.7(5) . . ? C11' C12 C13 81.2(5) . . ? C11 C12 C13 116.7(5) . . ? C11' C12 C13' 114.5(5) . . ? C11 C12 C13' 85.1(5) . . ? C13 C12 C13' 62.1(5) . . ? C11' C12 C15' 125.1(5) . . ? C11 C12 C15' 118.9(4) . . ? C13 C12 C15' 124.4(5) . . ? C13' C12 C15' 120.4(5) . . ? C11' C12 C15 121.4(5) . . ? C11 C12 C15 120.5(4) . . ? C13 C12 C15 122.8(5) . . ? C13' C12 C15 124.1(5) . . ? C14 C13 C12 119.6(7) . . ? C14 C13 H13A 120.2 . . ? C12 C13 H13A 120.2 . . ? N1 C14 C13 125.3(7) . . ? N1 C14 H14A 117.3 . . ? C13 C14 H14A 117.3 . . ? C14' C13' C12 120.4(7) . . ? C14' C13' H13B 119.8 . . ? C12 C13' H13B 119.8 . . ? N1 C14' C13' 123.3(7) . . ? N1 C14' H14B 118.4 . . ? C13' C14' H14B 118.4 . . ? C16 C15 C19 120.0 . . ? C16 C15 C12 120.4(3) . . ? C19 C15 C12 119.6(3) . . ? C15 C16 C17 120.0 . . ? C15 C16 H16A 120.0 . . ? C17 C16 H16A 120.0 . . ? N2 C17 C16 120.0 . . ? N2 C17 H17A 120.0 . . ? C16 C17 H17A 120.0 . . ? C18 N2 C17 120.0 . . ? N2 C18 C19 120.0 . . ? N2 C18 H18A 120.0 . . ? C19 C18 H18A 120.0 . . ? C18 C19 C15 120.0 . . ? C18 C19 H19A 120.0 . . ? C15 C19 H19A 120.0 . . ? C16' C15' C19' 120.0 . . ? C16' C15' C12 121.5(3) . . ? C19' C15' C12 118.4(3) . . ? C15' C16' C17' 120.0 . . ? C15' C16' H16B 120.0 . . ? C17' C16' H16B 120.0 . . ? N2' C17' C16' 120.0 . . ? N2' C17' H17B 120.0 . . ? C16' C17' H17B 120.0 . . ? C17' N2' C18' 120.0 . . ? N2' C18' C19' 120.0 . . ? N2' C18' H18B 120.0 . . ? C19' C18' H18B 120.0 . . ? C18' C19' C15' 120.0 . . ? C18' C19' H19B 120.0 . . ? C15' C19' H19B 120.0 . . ? 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 C1 -33.5(3) 2_856 . . . ? O2 Co1 O1 C1 146.6(3) 1_455 . . . ? N1 Co1 O1 C1 61.6(3) 2_756 . . . ? N1 Co1 O1 C1 -118.4(3) . . . . ? O2 Co1 N1 C14 -19.7(5) 2_856 . . . ? O2 Co1 N1 C14 160.3(5) 1_455 . . . ? O1 Co1 N1 C14 73.7(5) . . . . ? O1 Co1 N1 C14 -106.3(5) 2_756 . . . ? O2 Co1 N1 C14' 54.7(5) 2_856 . . . ? O2 Co1 N1 C14' -125.3(5) 1_455 . . . ? O1 Co1 N1 C14' 148.0(5) . . . . ? O1 Co1 N1 C14' -32.0(5) 2_756 . . . ? O2 Co1 N1 C10' -122.1(4) 2_856 . . . ? O2 Co1 N1 C10' 57.9(4) 1_455 . . . ? O1 Co1 N1 C10' -28.8(4) . . . . ? O1 Co1 N1 C10' 151.2(4) 2_756 . . . ? O2 Co1 N1 C10 156.9(4) 2_856 . . . ? O2 Co1 N1 C10 -23.1(4) 1_455 . . . ? O1 Co1 N1 C10 -109.8(4) . . . . ? O1 Co1 N1 C10 70.2(4) 2_756 . . . ? Co1 O2 C1 O1 104.1(5) 1_655 . . . ? Co1 O2 C1 C2 -77.7(5) 1_655 . . . ? Co1 O1 C1 O2 1.6(5) . . . . ? Co1 O1 C1 C2 -176.5(2) . . . . ? C3 O3 C2 C1 -76.2(4) . . . . ? O2 C1 C2 O3 -180.0(3) . . . . ? O1 C1 C2 O3 -1.6(5) . . . . ? C2 O3 C3 C4 162.2(6) . . . . ? C2 O3 C3 C8' 26.0(8) . . . . ? C2 O3 C3 C4' -156.6(6) . . . . ? C2 O3 C3 C8 -21.1(7) . . . . ? O3 C3 C4 C5 179.9(7) . . . . ? C8' C3 C4 C5 -34.9(11) . . . . ? C4' C3 C4 C5 85.8(12) . . . . ? C8 C3 C4 C5 3.1(12) . . . . ? C3 C4 C5 C6 -4.1(14) . . . . ? O3 C3 C4' C5' -179.7(8) . . . . ? C4 C3 C4' C5' -75.2(12) . . . . ? C8' C3 C4' C5' -2.1(13) . . . . ? C8 C3 C4' C5' 39.2(12) . . . . ? C3 C4' C5' C6 1.6(15) . . . . ? C4 C5 C6 C7' 40.7(12) . . . . ? C4 C5 C6 C7 3.7(13) . . . . ? C4 C5 C6 C5' -77.1(11) . . . . ? C4 C5 C6 C9 178.2(8) . . . . ? C4' C5' C6 C7' -1.1(14) . . . . ? C4' C5' C6 C5 76.1(12) . . . . ? C4' C5' C6 C7 -39.8(12) . . . . ? C4' C5' C6 C9 177.6(8) . . . . ? C7' C6 C7 C8 -76.7(12) . . . . ? C5 C6 C7 C8 -2.4(13) . . . . ? C5' C6 C7 C8 38.2(12) . . . . ? C9 C6 C7 C8 -177.1(8) . . . . ? C6 C7 C8 C3 1.5(14) . . . . ? O3 C3 C8 C7 -178.5(7) . . . . ? C4 C3 C8 C7 -1.9(12) . . . . ? C8' C3 C8 C7 71.5(10) . . . . ? C4' C3 C8 C7 -41.3(11) . . . . ? C5 C6 C7' C8' -38.2(14) . . . . ? C7 C6 C7' C8' 81.8(15) . . . . ? C5' C6 C7' C8' 1.2(16) . . . . ? C9 C6 C7' C8' -177.6(9) . . . . ? O3 C3 C8' C7' 179.4(8) . . . . ? C4 C3 C8' C7' 38.6(11) . . . . ? C4' C3 C8' C7' 2.1(13) . . . . ? C8 C3 C8' C7' -82.7(12) . . . . ? C6 C7' C8' C3 -1.8(17) . . . . ? C7' C6 C9 O4 -4.6(15) . . . . ? C5 C6 C9 O4 -136.5(13) . . . . ? C7 C6 C9 O4 38.0(15) . . . . ? C5' C6 C9 O4 176.7(13) . . . . ? C7' C6 C9 O4' -38.8(14) . . . . ? C5 C6 C9 O4' -170.7(12) . . . . ? C7 C6 C9 O4' 3.8(13) . . . . ? C5' C6 C9 O4' 142.5(12) . . . . ? C7' C6 C9 O5' 139.7(11) . . . . ? C5 C6 C9 O5' 7.7(12) . . . . ? C7 C6 C9 O5' -177.7(10) . . . . ? C5' C6 C9 O5' -39.0(12) . . . . ? C7' C6 C9 O5 177.8(10) . . . . ? C5 C6 C9 O5 45.8(11) . . . . ? C7 C6 C9 O5 -139.6(10) . . . . ? C5' C6 C9 O5 -0.9(11) . . . . ? C14 N1 C10 C11 -4.1(10) . . . . ? C14' N1 C10 C11 -59.1(8) . . . . ? C10' N1 C10 C11 64.4(8) . . . . ? Co1 N1 C10 C11 179.0(6) . . . . ? N1 C10 C11 C12 4.0(12) . . . . ? C14 N1 C10' C11' 58.1(8) . . . . ? C14' N1 C10' C11' 6.1(10) . . . . ? C10 N1 C10' C11' -63.7(8) . . . . ? Co1 N1 C10' C11' -177.1(6) . . . . ? N1 C10' C11' C12 -2.9(12) . . . . ? C10' C11' C12 C11 69.6(8) . . . . ? C10' C11' C12 C13 -55.5(8) . . . . ? C10' C11' C12 C13' -1.7(10) . . . . ? C10' C11' C12 C15' 178.3(6) . . . . ? C10' C11' C12 C15 -178.8(6) . . . . ? C10 C11 C12 C11' -67.6(8) . . . . ? C10 C11 C12 C13 -2.9(10) . . . . ? C10 C11 C12 C13' 52.5(8) . . . . ? C10 C11 C12 C15' 174.6(6) . . . . ? C10 C11 C12 C15 179.5(6) . . . . ? C11' C12 C13 C14 58.1(9) . . . . ? C11 C12 C13 C14 2.3(11) . . . . ? C13' C12 C13 C14 -65.7(8) . . . . ? C15' C12 C13 C14 -175.1(7) . . . . ? C15 C12 C13 C14 179.9(7) . . . . ? C14' N1 C14 C13 71.2(9) . . . . ? C10' N1 C14 C13 -56.5(9) . . . . ? C10 N1 C14 C13 3.6(11) . . . . ? Co1 N1 C14 C13 -179.7(7) . . . . ? C12 C13 C14 N1 -2.9(14) . . . . ? C11' C12 C13' C14' 3.1(10) . . . . ? C11 C12 C13' C14' -56.2(8) . . . . ? C13 C12 C13' C14' 67.6(8) . . . . ? C15' C12 C13' C14' -176.9(6) . . . . ? C15 C12 C13' C14' -180.0(6) . . . . ? C14 N1 C14' C13' -67.0(8) . . . . ? C10' N1 C14' C13' -4.7(10) . . . . ? C10 N1 C14' C13' 55.7(8) . . . . ? Co1 N1 C14' C13' 178.4(6) . . . . ? C12 C13' C14' N1 0.1(12) . . . . ? C11' C12 C15 C16 -55.7(7) . . . . ? C11 C12 C15 C16 21.5(7) . . . . ? C13 C12 C15 C16 -156.0(6) . . . . ? C13' C12 C15 C16 127.6(5) . . . . ? C15' C12 C15 C16 91.8(2) . . . . ? C11' C12 C15 C19 126.2(6) . . . . ? C11 C12 C15 C19 -156.7(5) . . . . ? C13 C12 C15 C19 25.8(7) . . . . ? C13' C12 C15 C19 -50.6(7) . . . . ? C15' C12 C15 C19 -86.4(2) . . . . ? C19 C15 C16 C17 0.0 . . . . ? C12 C15 C16 C17 -178.2(5) . . . . ? C15 C16 C17 N2 0.0 . . . . ? C16 C17 N2 C18 0.0 . . . . ? C17 N2 C18 C19 0.0 . . . . ? N2 C18 C19 C15 0.0 . . . . ? C16 C15 C19 C18 0.0 . . . . ? C12 C15 C19 C18 178.2(5) . . . . ? C11' C12 C15' C16' -20.0(7) . . . . ? C11 C12 C15' C16' 57.9(6) . . . . ? C13 C12 C15' C16' -124.8(6) . . . . ? C13' C12 C15' C16' 160.0(5) . . . . ? C15 C12 C15' C16' -54.2(2) . . . . ? C11' C12 C15' C19' 162.9(6) . . . . ? C11 C12 C15' C19' -119.2(5) . . . . ? C13 C12 C15' C19' 58.1(7) . . . . ? C13' C12 C15' C19' -17.1(6) . . . . ? C15 C12 C15' C19' 128.7(2) . . . . ? C19' C15' C16' C17' 0.0 . . . . ? C12 C15' C16' C17' -177.1(4) . . . . ? C15' C16' C17' N2' 0.0 . . . . ? C16' C17' N2' C18' 0.0 . . . . ? C17' N2' C18' C19' 0.0 . . . . ? N2' C18' C19' C15' 0.0 . . . . ? C16' C15' C19' C18' 0.0 . . . . ? C12 C15' C19' C18' 177.2(4) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.577 _refine_diff_density_min -0.486 _refine_diff_density_rms 0.080 #===END data_complex4 _database_code_depnum_ccdc_archive 'CCDC 637135' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H36 Co2 N2 O18' _chemical_formula_weight 806.45 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 7.6417(19) _cell_length_b 10.106(3) _cell_length_c 10.638(3) _cell_angle_alpha 93.557(4) _cell_angle_beta 101.146(4) _cell_angle_gamma 101.551(4) _cell_volume 785.3(3) _cell_formula_units_Z 1 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 1325 _cell_measurement_theta_min 2.78 _cell_measurement_theta_max 26.67 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.705 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 416 _exptl_absorpt_coefficient_mu 1.145 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.669929 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 4024 _diffrn_reflns_av_R_equivalents 0.0272 _diffrn_reflns_av_sigmaI/netI 0.0640 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 25.02 _reflns_number_total 2751 _reflns_number_gt 1925 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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^)+(0.0426P)^2^+0.0730P] 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_number_reflns 2751 _refine_ls_number_parameters 229 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0686 _refine_ls_R_factor_gt 0.0384 _refine_ls_wR_factor_ref 0.0958 _refine_ls_wR_factor_gt 0.0830 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.022 _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 0.0000 0.5000 0.0000 0.01717(19) Uani 1 2 d S . . Co2 Co 0.5000 0.5000 0.5000 0.0184(2) Uani 1 2 d S . . O1 O 0.4281(3) 0.6022(2) 0.3324(2) 0.0242(6) Uani 1 1 d . . . O2 O 0.5326(3) 0.5972(3) 0.1525(2) 0.0288(6) Uani 1 1 d . . . O3 O 0.9488(3) 1.1899(2) 0.3928(2) 0.0299(7) Uani 1 1 d . . . O4 O 1.1408(3) 1.4648(3) 0.6342(2) 0.0270(6) Uani 1 1 d . . . O5 O 1.2299(3) 1.3927(2) 0.4602(2) 0.0229(6) Uani 1 1 d . . . O6 O 0.4394(3) 0.6510(2) 0.6165(2) 0.0263(6) Uani 1 1 d D . . H6A H 0.5222 0.6890 0.6802 0.032 Uiso 1 1 d RD . . H6B H 0.3465 0.5981 0.6318 0.032 Uiso 1 1 d RD . . O7 O 0.2426(3) 0.4184(2) 0.0153(2) 0.0245(6) Uani 1 1 d D . . H7A H 0.2755 0.4011 -0.0544 0.029 Uiso 1 1 d RD . . H7B H 0.3180 0.4724 0.0739 0.029 Uiso 1 1 d RD . . O8 O 0.0724(3) 0.5361(3) 0.1978(2) 0.0282(6) Uani 1 1 d D . . H8A H -0.0058 0.5301 0.2446 0.034 Uiso 1 1 d RD . . H8B H 0.1840 0.5517 0.2346 0.034 Uiso 1 1 d RD . . N1 N 0.1694(4) 0.6956(3) -0.0095(3) 0.0214(7) Uani 1 1 d . . . C1 C 0.5296(4) 0.6556(4) 0.2585(3) 0.0184(8) Uani 1 1 d . . . C2 C 0.6416(4) 0.7957(4) 0.2989(3) 0.0204(8) Uani 1 1 d . . . C3 C 0.6318(5) 0.8697(4) 0.4091(3) 0.0252(9) Uani 1 1 d . . . H3 H 0.5558 0.8299 0.4612 0.030 Uiso 1 1 calc R . . C4 C 0.7309(5) 1.0016(4) 0.4454(3) 0.0269(9) Uani 1 1 d . . . H4 H 0.7209 1.0496 0.5202 0.032 Uiso 1 1 calc R . . C5 C 0.8453(5) 1.0606(4) 0.3684(3) 0.0232(9) Uani 1 1 d . . . C6 C 0.8594(5) 0.9889(4) 0.2570(3) 0.0265(9) Uani 1 1 d . . . H6 H 0.9374 1.0283 0.2059 0.032 Uiso 1 1 calc R . . C7 C 0.7570(5) 0.8586(4) 0.2223(3) 0.0248(9) Uani 1 1 d . . . H7 H 0.7646 0.8113 0.1464 0.030 Uiso 1 1 calc R . . C8 C 0.9607(5) 1.2652(4) 0.5122(3) 0.0222(8) Uani 1 1 d U . . H8C H 0.9748 1.2074 0.5812 0.027 Uiso 1 1 calc R . . H8D H 0.8493 1.2977 0.5110 0.027 Uiso 1 1 calc R . . C9 C 1.1221(5) 1.3842(4) 0.5357(3) 0.0188(8) Uani 1 1 d . . . C10 C 0.1813(5) 0.8039(4) 0.0717(4) 0.0329(10) Uani 1 1 d . . . H10 H 0.1010 0.7978 0.1276 0.040 Uiso 1 1 calc R . . C11 C 0.3056(5) 0.9247(4) 0.0778(4) 0.0330(10) Uani 1 1 d . . . H11 H 0.3063 0.9980 0.1353 0.040 Uiso 1 1 calc R . . C12 C 0.4300(4) 0.9361(3) -0.0027(3) 0.0178(8) Uani 1 1 d . . . C13 C 0.4146(5) 0.8260(4) -0.0872(4) 0.0312(10) Uani 1 1 d . . . H13 H 0.4924 0.8295 -0.1448 0.037 Uiso 1 1 calc R . . C14 C 0.2852(5) 0.7088(4) -0.0886(3) 0.0286(9) Uani 1 1 d . . . H14 H 0.2788 0.6355 -0.1479 0.034 Uiso 1 1 calc R . . O9 O 0.2309(3) 0.2347(3) 0.2202(2) 0.0352(7) Uani 1 1 d D . . H9A H 0.1988 0.2696 0.2839 0.042 Uiso 1 1 d RD . . H9B H 0.2163 0.2716 0.1509 0.042 Uiso 1 1 d RD . . 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 0.0164(4) 0.0159(4) 0.0170(4) -0.0001(3) 0.0058(3) -0.0032(3) Co2 0.0166(4) 0.0191(4) 0.0181(4) -0.0008(3) 0.0061(3) -0.0013(3) O1 0.0213(14) 0.0280(15) 0.0211(14) 0.0053(11) 0.0070(11) -0.0032(11) O2 0.0246(14) 0.0320(16) 0.0239(15) -0.0069(12) 0.0070(11) -0.0067(12) O3 0.0348(16) 0.0221(15) 0.0262(15) -0.0018(11) 0.0094(12) -0.0108(12) O4 0.0249(14) 0.0290(16) 0.0247(15) -0.0064(12) 0.0114(11) -0.0029(12) O5 0.0179(13) 0.0269(15) 0.0217(14) -0.0027(11) 0.0078(11) -0.0020(11) O6 0.0242(14) 0.0242(15) 0.0268(14) -0.0066(11) 0.0069(11) -0.0020(11) O7 0.0198(14) 0.0277(15) 0.0227(14) -0.0040(11) 0.0051(11) -0.0009(11) O8 0.0149(13) 0.0453(17) 0.0198(14) -0.0002(12) 0.0055(10) -0.0051(12) N1 0.0217(17) 0.0183(17) 0.0220(17) 0.0009(13) 0.0076(13) -0.0030(13) C1 0.0144(18) 0.020(2) 0.0176(19) 0.0025(16) -0.0017(15) 0.0008(15) C2 0.0163(19) 0.022(2) 0.021(2) 0.0050(16) 0.0032(15) 0.0006(16) C3 0.022(2) 0.026(2) 0.026(2) 0.0023(17) 0.0090(16) -0.0012(17) C4 0.027(2) 0.026(2) 0.025(2) -0.0022(17) 0.0074(17) -0.0001(17) C5 0.023(2) 0.020(2) 0.023(2) 0.0062(16) 0.0034(16) -0.0031(16) C6 0.027(2) 0.026(2) 0.022(2) 0.0040(17) 0.0066(16) -0.0059(17) C7 0.031(2) 0.022(2) 0.017(2) -0.0018(16) 0.0050(16) -0.0009(17) C8 0.0207(19) 0.021(2) 0.021(2) 0.0008(16) 0.0035(15) -0.0019(16) C9 0.0162(19) 0.021(2) 0.021(2) 0.0065(16) 0.0038(15) 0.0061(15) C10 0.029(2) 0.027(2) 0.044(3) -0.0009(19) 0.0209(19) -0.0026(18) C11 0.037(2) 0.020(2) 0.042(2) -0.0086(18) 0.023(2) -0.0046(18) C12 0.0152(18) 0.017(2) 0.0193(19) 0.0036(15) 0.0039(15) -0.0002(15) C13 0.041(2) 0.021(2) 0.030(2) -0.0031(17) 0.0209(19) -0.0087(18) C14 0.038(2) 0.016(2) 0.029(2) -0.0087(16) 0.0157(18) -0.0060(17) O9 0.0379(17) 0.0344(17) 0.0328(16) 0.0005(13) 0.0105(13) 0.0047(13) _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 O8 2.060(2) . ? Co1 O8 2.060(2) 2_565 ? Co1 N1 2.155(3) 2_565 ? Co1 N1 2.155(3) . ? Co1 O7 2.158(2) 2_565 ? Co1 O7 2.158(2) . ? Co2 O5 2.080(2) 2_776 ? Co2 O5 2.080(2) 1_445 ? Co2 O6 2.086(2) . ? Co2 O6 2.086(2) 2_666 ? Co2 O1 2.151(2) 2_666 ? Co2 O1 2.151(2) . ? O1 C1 1.277(4) . ? O2 C1 1.246(4) . ? O3 C5 1.365(4) . ? O3 C8 1.418(4) . ? O4 C9 1.254(4) . ? O5 C9 1.252(4) . ? O5 Co2 2.080(2) 1_665 ? O6 H6A 0.8435 . ? O6 H6B 0.8483 . ? O7 H7A 0.8463 . ? O7 H7B 0.8430 . ? O8 H8A 0.8446 . ? O8 H8B 0.8456 . ? N1 C14 1.328(4) . ? N1 C10 1.328(5) . ? C1 C2 1.490(5) . ? C2 C3 1.374(5) . ? C2 C7 1.401(5) . ? C3 C4 1.385(5) . ? C3 H3 0.9300 . ? C4 C5 1.386(5) . ? C4 H4 0.9300 . ? C5 C6 1.385(5) . ? C6 C7 1.378(5) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.510(5) . ? C8 H8C 0.9700 . ? C8 H8D 0.9700 . ? C10 C11 1.378(5) . ? C10 H10 0.9300 . ? C11 C12 1.391(5) . ? C11 H11 0.9300 . ? C12 C13 1.357(5) . ? C12 C12 1.493(6) 2_675 ? C13 C14 1.379(5) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? O9 H9A 0.8437 . ? O9 H9B 0.8451 . ? 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 O8 Co1 O8 180.0 . 2_565 ? O8 Co1 N1 91.80(10) . 2_565 ? O8 Co1 N1 88.20(10) 2_565 2_565 ? O8 Co1 N1 88.20(10) . . ? O8 Co1 N1 91.80(10) 2_565 . ? N1 Co1 N1 180.0 2_565 . ? O8 Co1 O7 94.59(10) . 2_565 ? O8 Co1 O7 85.41(10) 2_565 2_565 ? N1 Co1 O7 87.49(10) 2_565 2_565 ? N1 Co1 O7 92.51(10) . 2_565 ? O8 Co1 O7 85.41(10) . . ? O8 Co1 O7 94.59(10) 2_565 . ? N1 Co1 O7 92.51(10) 2_565 . ? N1 Co1 O7 87.49(10) . . ? O7 Co1 O7 180.0 2_565 . ? O5 Co2 O5 180.0 2_776 1_445 ? O5 Co2 O6 88.50(9) 2_776 . ? O5 Co2 O6 91.50(9) 1_445 . ? O5 Co2 O6 91.50(9) 2_776 2_666 ? O5 Co2 O6 88.50(9) 1_445 2_666 ? O6 Co2 O6 180.00(11) . 2_666 ? O5 Co2 O1 87.09(9) 2_776 2_666 ? O5 Co2 O1 92.91(9) 1_445 2_666 ? O6 Co2 O1 89.31(10) . 2_666 ? O6 Co2 O1 90.69(10) 2_666 2_666 ? O5 Co2 O1 92.91(9) 2_776 . ? O5 Co2 O1 87.09(9) 1_445 . ? O6 Co2 O1 90.70(10) . . ? O6 Co2 O1 89.30(10) 2_666 . ? O1 Co2 O1 180.0 2_666 . ? C1 O1 Co2 128.9(2) . . ? C5 O3 C8 119.0(3) . . ? C9 O5 Co2 126.3(2) . 1_665 ? Co2 O6 H6A 116.7 . . ? Co2 O6 H6B 92.9 . . ? H6A O6 H6B 117.6 . . ? Co1 O7 H7A 116.6 . . ? Co1 O7 H7B 102.6 . . ? H7A O7 H7B 118.1 . . ? Co1 O8 H8A 122.4 . . ? Co1 O8 H8B 119.4 . . ? H8A O8 H8B 118.1 . . ? C14 N1 C10 116.2(3) . . ? C14 N1 Co1 120.3(2) . . ? C10 N1 Co1 123.0(2) . . ? O2 C1 O1 122.6(3) . . ? O2 C1 C2 119.2(3) . . ? O1 C1 C2 118.1(3) . . ? C3 C2 C7 117.5(3) . . ? C3 C2 C1 121.9(3) . . ? C7 C2 C1 120.5(3) . . ? C2 C3 C4 122.4(3) . . ? C2 C3 H3 118.8 . . ? C4 C3 H3 118.8 . . ? C3 C4 C5 118.8(3) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? O3 C5 C6 115.0(3) . . ? O3 C5 C4 124.6(3) . . ? C6 C5 C4 120.4(3) . . ? C7 C6 C5 119.4(3) . . ? C7 C6 H6 120.3 . . ? C5 C6 H6 120.3 . . ? C6 C7 C2 121.4(3) . . ? C6 C7 H7 119.3 . . ? C2 C7 H7 119.3 . . ? O3 C8 C9 109.7(3) . . ? O3 C8 H8C 109.7 . . ? C9 C8 H8C 109.7 . . ? O3 C8 H8D 109.7 . . ? C9 C8 H8D 109.7 . . ? H8C C8 H8D 108.2 . . ? O5 C9 O4 125.0(3) . . ? O5 C9 C8 118.7(3) . . ? O4 C9 C8 116.2(3) . . ? N1 C10 C11 123.8(4) . . ? N1 C10 H10 118.1 . . ? C11 C10 H10 118.1 . . ? C10 C11 C12 119.5(4) . . ? C10 C11 H11 120.2 . . ? C12 C11 H11 120.2 . . ? C13 C12 C11 116.3(3) . . ? C13 C12 C12 122.3(4) . 2_675 ? C11 C12 C12 121.4(4) . 2_675 ? C12 C13 C14 120.9(3) . . ? C12 C13 H13 119.6 . . ? C14 C13 H13 119.6 . . ? N1 C14 C13 123.3(3) . . ? N1 C14 H14 118.4 . . ? C13 C14 H14 118.4 . . ? H9A O9 H9B 117.9 . . ? 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 O5 Co2 O1 C1 27.2(3) 2_776 . . . ? O5 Co2 O1 C1 -152.8(3) 1_445 . . . ? O6 Co2 O1 C1 115.8(3) . . . . ? O6 Co2 O1 C1 -64.2(3) 2_666 . . . ? O8 Co1 N1 C14 133.4(3) . . . . ? O8 Co1 N1 C14 -46.6(3) 2_565 . . . ? O7 Co1 N1 C14 -132.1(3) 2_565 . . . ? O7 Co1 N1 C14 47.9(3) . . . . ? O8 Co1 N1 C10 -38.2(3) . . . . ? O8 Co1 N1 C10 141.8(3) 2_565 . . . ? O7 Co1 N1 C10 56.3(3) 2_565 . . . ? O7 Co1 N1 C10 -123.7(3) . . . . ? Co2 O1 C1 O2 100.1(4) . . . . ? Co2 O1 C1 C2 -82.8(4) . . . . ? O2 C1 C2 C3 174.2(3) . . . . ? O1 C1 C2 C3 -3.0(5) . . . . ? O2 C1 C2 C7 -3.5(5) . . . . ? O1 C1 C2 C7 179.2(3) . . . . ? C7 C2 C3 C4 -0.1(6) . . . . ? C1 C2 C3 C4 -177.9(3) . . . . ? C2 C3 C4 C5 -0.5(6) . . . . ? C8 O3 C5 C6 -172.4(3) . . . . ? C8 O3 C5 C4 8.4(5) . . . . ? C3 C4 C5 O3 179.4(3) . . . . ? C3 C4 C5 C6 0.2(5) . . . . ? O3 C5 C6 C7 -178.5(3) . . . . ? C4 C5 C6 C7 0.8(6) . . . . ? C5 C6 C7 C2 -1.4(6) . . . . ? C3 C2 C7 C6 1.1(5) . . . . ? C1 C2 C7 C6 178.9(3) . . . . ? C5 O3 C8 C9 162.8(3) . . . . ? Co2 O5 C9 O4 19.6(5) 1_665 . . . ? Co2 O5 C9 C8 -157.4(2) 1_665 . . . ? O3 C8 C9 O5 -7.5(5) . . . . ? O3 C8 C9 O4 175.2(3) . . . . ? C14 N1 C10 C11 -0.6(6) . . . . ? Co1 N1 C10 C11 171.4(3) . . . . ? N1 C10 C11 C12 -1.3(6) . . . . ? C10 C11 C12 C13 2.5(6) . . . . ? C10 C11 C12 C12 -178.5(4) . . . 2_675 ? C11 C12 C13 C14 -1.9(6) . . . . ? C12 C12 C13 C14 179.2(4) 2_675 . . . ? C10 N1 C14 C13 1.3(6) . . . . ? Co1 N1 C14 C13 -170.9(3) . . . . ? C12 C13 C14 N1 -0.1(6) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.393 _refine_diff_density_min -0.453 _refine_diff_density_rms 0.085 #===END data_complex5 _database_code_depnum_ccdc_archive 'CCDC 637136' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H18 N2 Ni O7' _chemical_formula_weight 445.06 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 Trigonal _symmetry_space_group_name_H-M P3(1)21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+1/3' '-x+y, -x, z+2/3' 'y, x, -z' 'x-y, -y, -z+2/3' '-x, -x+y, -z+1/3' _cell_length_a 11.2742(8) _cell_length_b 11.2742(8) _cell_length_c 13.5885(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1495.8(3) _cell_formula_units_Z 3 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 3506 _cell_measurement_theta_min 2.57 _cell_measurement_theta_max 25.82 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.482 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 690 _exptl_absorpt_coefficient_mu 1.016 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.735566 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 8446 _diffrn_reflns_av_R_equivalents 0.0415 _diffrn_reflns_av_sigmaI/netI 0.0348 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 26.34 _reflns_number_total 2035 _reflns_number_gt 1828 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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^)+(0.0321P)^2^+0.4180P] 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 0.004(19) _refine_ls_number_reflns 2035 _refine_ls_number_parameters 185 _refine_ls_number_restraints 28 _refine_ls_R_factor_all 0.0367 _refine_ls_R_factor_gt 0.0303 _refine_ls_wR_factor_ref 0.0718 _refine_ls_wR_factor_gt 0.0697 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.047 _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 Ni1 Ni 0.45642(4) 0.45642(4) 0.0000 0.02924(14) Uani 1 2 d S . . N1 N 0.6417(3) 0.6417(3) 0.0000 0.0392(9) Uani 1 2 d S . . N2 N 1.2687(3) 1.2687(3) 0.0000 0.0357(7) Uani 1 2 d S . . C1 C 0.6778(3) 0.7306(3) 0.0746(2) 0.0505(9) Uani 1 1 d . . . H1 H 0.6180 0.7076 0.1275 0.061 Uiso 1 1 calc R . . C2 C 0.7981(4) 0.8539(3) 0.0776(3) 0.0510(9) Uani 1 1 d . . . H2 H 0.8182 0.9128 0.1308 0.061 Uiso 1 1 calc R . . C3 C 0.8887(4) 0.8887(4) 0.0000 0.0418(11) Uani 1 2 d S . . C4 C 1.0211(4) 1.0211(4) 0.0000 0.0411(11) Uani 1 2 d S . . C5 C 1.0296(3) 1.1416(3) 0.0332(3) 0.0459(8) Uani 1 1 d . . . H5 H 0.9518 1.1413 0.0564 0.055 Uiso 1 1 calc R . . C6 C 1.1543(3) 1.2621(3) 0.0317(2) 0.0432(7) Uani 1 1 d . . . H6 H 1.1581 1.3420 0.0539 0.052 Uiso 1 1 calc R . . O1 O 0.4482(17) 0.450(2) 0.1512(13) 0.045(4) Uani 0.50 1 d PD . . O2 O 0.549(2) 0.3373(16) 0.2049(15) 0.047(3) Uani 0.50 1 d PD . . O3 O 0.3768(17) 0.572(2) 0.8031(16) 0.052(3) Uani 0.50 1 d PD . . O4 O 0.463(2) 0.4437(12) 0.8525(12) 0.029(3) Uani 0.50 1 d PD . . O5 O 0.3788(8) 0.4774(7) 0.6119(4) 0.069(2) Uani 0.50 1 d PD . . C7 C 0.490(2) 0.405(2) 0.2176(11) 0.039(5) Uani 0.50 1 d PDU . . C8 C 0.4763(6) 0.4423(8) 0.3222(3) 0.036(2) Uani 0.50 1 d PGU . . C9 C 0.5592(6) 0.4394(8) 0.3967(4) 0.053(2) Uani 0.50 1 d PG . . H9A H 0.6375 0.4307 0.3806 0.063 Uiso 0.50 1 d PR . . C10 C 0.5289(6) 0.4489(7) 0.4945(4) 0.064(3) Uani 0.50 1 d PG . . H10A H 0.5862 0.4469 0.5460 0.077 Uiso 0.50 1 d PR . . C11 C 0.4156(6) 0.4614(6) 0.5179(3) 0.059(3) Uani 0.50 1 d PGD . . C12 C 0.3326(5) 0.4643(7) 0.4434(3) 0.073(3) Uani 0.50 1 d PG . . H12A H 0.2544 0.4730 0.4595 0.088 Uiso 0.50 1 d PR . . C13 C 0.3629(6) 0.4548(7) 0.3455(3) 0.065(2) Uani 0.50 1 d PG . . H13A H 0.3056 0.4568 0.2941 0.078 Uiso 0.50 1 d PR . . C14 C 0.4490(16) 0.4543(15) 0.6886(7) 0.076(4) Uani 0.50 1 d PD . . H14A H 0.5462 0.5052 0.6779 0.092 Uiso 0.50 1 d PR . . H14B H 0.4202 0.3585 0.6856 0.092 Uiso 0.50 1 d PR . . C15 C 0.425(2) 0.496(2) 0.7894(9) 0.032(4) Uani 0.50 1 d PDU . . O6 O 0.3485(2) 0.5634(2) -0.00167(12) 0.0402(5) Uani 1 1 d . . . H6A H 0.3497 0.5815 -0.0632 0.060 Uiso 1 1 d R . . H6B H 0.3493 0.6266 0.0327 0.060 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.02746(18) 0.02746(18) 0.0235(2) 0.00022(10) -0.00022(10) 0.0067(2) N1 0.0315(13) 0.0315(13) 0.036(2) -0.0020(9) 0.0020(9) 0.0021(16) N2 0.0316(11) 0.0316(11) 0.0351(16) -0.0004(7) 0.0004(7) 0.0093(14) C1 0.0406(18) 0.0422(19) 0.0423(18) -0.0019(15) 0.0063(14) 0.0010(15) C2 0.044(2) 0.0414(19) 0.046(2) -0.0107(15) 0.0046(16) 0.0045(16) C3 0.0326(18) 0.0326(18) 0.044(3) 0.0024(12) -0.0024(12) 0.004(2) C4 0.0351(17) 0.0351(17) 0.040(2) 0.0011(10) -0.0011(10) 0.0076(19) C5 0.0309(16) 0.0355(17) 0.0588(19) 0.0018(15) 0.0057(14) 0.0074(14) C6 0.0330(16) 0.0326(15) 0.0540(18) -0.0022(13) 0.0059(14) 0.0089(13) O1 0.076(8) 0.053(6) 0.022(6) 0.004(4) 0.005(5) 0.044(5) O2 0.096(8) 0.051(8) 0.024(4) 0.011(5) 0.010(4) 0.057(8) O3 0.051(9) 0.090(7) 0.032(5) 0.001(4) -0.011(5) 0.047(7) O4 0.035(5) 0.024(4) 0.024(5) 0.005(4) -0.002(4) 0.012(3) O5 0.128(6) 0.105(5) 0.027(3) 0.014(3) 0.014(3) 0.098(5) C7 0.042(6) 0.037(9) 0.025(6) 0.018(4) 0.002(4) 0.011(5) C8 0.057(5) 0.051(5) 0.015(4) -0.006(3) -0.003(3) 0.039(4) C9 0.082(6) 0.095(7) 0.023(4) -0.011(4) -0.015(4) 0.075(6) C10 0.105(8) 0.121(8) 0.025(4) -0.013(4) -0.010(4) 0.100(7) C11 0.116(7) 0.078(6) 0.026(4) 0.007(4) -0.005(4) 0.081(5) C12 0.100(6) 0.143(8) 0.035(4) -0.005(4) -0.005(4) 0.104(7) C13 0.091(6) 0.111(7) 0.031(4) 0.008(4) 0.002(4) 0.079(6) C14 0.119(10) 0.110(9) 0.029(5) 0.021(6) -0.001(5) 0.080(8) C15 0.022(5) 0.049(7) 0.023(7) -0.008(5) 0.003(5) 0.016(5) O6 0.0511(14) 0.0372(11) 0.0302(10) -0.0026(9) 0.0006(9) 0.0205(9) _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 O4 2.013(17) 1_554 ? Ni1 O4 2.013(17) 4_556 ? Ni1 O1 2.056(18) 4 ? Ni1 O1 2.056(18) . ? Ni1 N1 2.089(4) . ? Ni1 O6 2.0983(19) . ? Ni1 O6 2.0983(19) 4 ? Ni1 N2 2.116(4) 1_445 ? N1 C1 1.338(4) 4 ? N1 C1 1.338(4) . ? N2 C6 1.326(3) 4 ? N2 C6 1.326(3) . ? N2 Ni1 2.116(4) 1_665 ? C1 C2 1.374(4) . ? C1 H1 0.9300 . ? C2 C3 1.381(4) . ? C2 H2 0.9300 . ? C3 C2 1.381(4) 4 ? C3 C4 1.492(5) . ? C4 C5 1.389(4) . ? C4 C5 1.389(4) 4 ? C5 C6 1.383(4) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? O1 O4 0.19(4) 4_556 ? O1 C15 1.08(3) 4_556 ? O1 C7 1.241(11) . ? O2 O3 0.40(3) 4_556 ? O2 C7 1.248(11) . ? O2 C15 1.40(3) 4_556 ? O3 O2 0.40(3) 4_556 ? O3 C7 1.15(3) 4_556 ? O3 C15 1.241(11) . ? O4 O1 0.19(4) 4_556 ? O4 C15 1.234(11) . ? O4 C7 1.40(3) 4_556 ? O4 Ni1 2.013(17) 1_556 ? O5 C9 0.838(13) 4_556 ? O5 C8 1.150(11) 4_556 ? O5 C11 1.383(5) . ? O5 C14 1.409(8) . ? O5 C10 1.611(7) 4_556 ? C7 C15 0.23(4) 4_556 ? C7 O3 1.15(3) 4_556 ? C7 O4 1.40(3) 4_556 ? C7 C14 1.50(2) 4_556 ? C7 C8 1.514(14) . ? C8 C14 0.328(14) 4_556 ? C8 O5 1.150(11) 4_556 ? C8 C9 1.3900 . ? C8 C13 1.3900 . ? C8 C15 1.559(12) 4_556 ? C9 O5 0.838(8) 4_556 ? C9 C10 1.3900 . ? C9 C11 1.530(9) 4_556 ? C9 C14 1.698(14) 4_556 ? C9 H9A 0.9600 . ? C10 C11 0.680(4) 4_556 ? C10 C11 1.3900 . ? C10 C12 1.417(6) 4_556 ? C10 C10 1.570(10) 4_556 ? C10 O5 1.611(8) 4_556 ? C10 H10A 0.9600 . ? C11 C10 0.680(6) 4_556 ? C11 C11 1.017(9) 4_556 ? C11 C12 1.3900 . ? C11 C9 1.530(8) 4_556 ? C12 C13 1.3900 . ? C12 C10 1.417(7) 4_556 ? C12 H12A 0.9600 . ? C13 C14 1.160(13) 4_556 ? C13 H13A 0.9600 . ? C14 C8 0.328(14) 4_556 ? C14 C13 1.160(14) 4_556 ? C14 C7 1.50(2) 4_556 ? C14 C15 1.516(9) . ? C14 C9 1.698(14) 4_556 ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C15 C7 0.23(4) 4_556 ? C15 O1 1.08(3) 4_556 ? C15 O2 1.40(3) 4_556 ? C15 C8 1.559(12) 4_556 ? O6 H6A 0.8585 . ? O6 H6B 0.8477 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Ni1 O4 178.2(10) 1_554 4_556 ? O4 Ni1 O1 5.3(11) 1_554 4 ? O4 Ni1 O1 174.0(9) 4_556 4 ? O4 Ni1 O1 174.0(9) 1_554 . ? O4 Ni1 O1 5.3(11) 4_556 . ? O1 Ni1 O1 175.3(12) 4 . ? O4 Ni1 N1 90.9(5) 1_554 . ? O4 Ni1 N1 90.9(5) 4_556 . ? O1 Ni1 N1 92.3(6) 4 . ? O1 Ni1 N1 92.3(6) . . ? O4 Ni1 O6 94.9(5) 1_554 . ? O4 Ni1 O6 85.1(5) 4_556 . ? O1 Ni1 O6 89.8(5) 4 . ? O1 Ni1 O6 90.2(5) . . ? N1 Ni1 O6 90.13(6) . . ? O4 Ni1 O6 85.1(5) 1_554 4 ? O4 Ni1 O6 94.9(5) 4_556 4 ? O1 Ni1 O6 90.2(5) 4 4 ? O1 Ni1 O6 89.8(5) . 4 ? N1 Ni1 O6 90.14(6) . 4 ? O6 Ni1 O6 179.73(12) . 4 ? O4 Ni1 N2 89.1(5) 1_554 1_445 ? O4 Ni1 N2 89.1(5) 4_556 1_445 ? O1 Ni1 N2 87.7(6) 4 1_445 ? O1 Ni1 N2 87.7(6) . 1_445 ? N1 Ni1 N2 180.0 . 1_445 ? O6 Ni1 N2 89.87(6) . 1_445 ? O6 Ni1 N2 89.86(6) 4 1_445 ? C1 N1 C1 116.4(4) 4 . ? C1 N1 Ni1 121.79(19) 4 . ? C1 N1 Ni1 121.79(19) . . ? C6 N2 C6 118.1(4) 4 . ? C6 N2 Ni1 120.9(2) 4 1_665 ? C6 N2 Ni1 120.9(2) . 1_665 ? N1 C1 C2 123.9(3) . . ? N1 C1 H1 118.1 . . ? C2 C1 H1 118.1 . . ? C1 C2 C3 118.7(3) . . ? C1 C2 H2 120.6 . . ? C3 C2 H2 120.6 . . ? C2 C3 C2 118.4(4) . 4 ? C2 C3 C4 120.8(2) . . ? C2 C3 C4 120.8(2) 4 . ? C5 C4 C5 116.8(4) . 4 ? C5 C4 C3 121.6(2) . . ? C5 C4 C3 121.6(2) 4 . ? C6 C5 C4 119.7(3) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? N2 C6 C5 122.8(3) . . ? N2 C6 H6 118.6 . . ? C5 C6 H6 118.6 . . ? O4 O1 C15 140(10) 4_556 4_556 ? O4 O1 C7 146(10) 4_556 . ? O4 O1 Ni1 74(10) 4_556 . ? C15 O1 Ni1 137.4(16) 4_556 . ? C7 O1 Ni1 136.2(14) . . ? O3 O2 C7 67(5) 4_556 . ? O3 O2 C15 60(4) 4_556 4_556 ? O2 O3 C7 95(5) 4_556 4_556 ? O2 O3 C15 104(6) 4_556 . ? O1 O4 Ni1 100(10) 4_556 1_556 ? C15 O4 Ni1 128.5(12) . 1_556 ? C7 O4 Ni1 127.3(14) 4_556 1_556 ? C9 O5 C8 87.3(8) 4_556 4_556 ? C9 O5 C11 83.2(6) 4_556 . ? C8 O5 C11 119.3(6) 4_556 . ? C9 O5 C14 94.8(13) 4_556 . ? C11 O5 C14 115.3(6) . . ? C9 O5 C10 59.6(4) 4_556 4_556 ? C8 O5 C10 120.5(7) 4_556 4_556 ? C14 O5 C10 120.7(7) . 4_556 ? C15 C7 O3 109(10) 4_556 4_556 ? O3 C7 O1 117(2) 4_556 . ? C15 C7 O2 127(9) 4_556 . ? O1 C7 O2 125.4(14) . . ? O3 C7 O4 120.2(19) 4_556 4_556 ? O2 C7 O4 129.3(16) . 4_556 ? C15 C7 C14 90(6) 4_556 4_556 ? O3 C7 C14 134(2) 4_556 4_556 ? O1 C7 C14 105.0(14) . 4_556 ? O2 C7 C14 129.6(14) . 4_556 ? O4 C7 C14 101.1(14) 4_556 4_556 ? C15 C7 C8 97(6) 4_556 . ? O3 C7 C8 121(2) 4_556 . ? O1 C7 C8 116.9(14) . . ? O2 C7 C8 117.6(14) . . ? O4 C7 C8 112.9(14) 4_556 . ? C14 C8 O5 137(3) 4_556 4_556 ? C14 C8 C9 158(2) 4_556 . ? O5 C8 C13 100.5(4) 4_556 . ? C9 C8 C13 120.0 . . ? C14 C8 C7 81(2) 4_556 . ? O5 C8 C7 121.4(9) 4_556 . ? C9 C8 C7 120.7(8) . . ? C13 C8 C7 118.2(8) . . ? C14 C8 C15 76(2) 4_556 4_556 ? O5 C8 C15 129.3(9) 4_556 4_556 ? C9 C8 C15 124.5(8) . 4_556 ? C13 C8 C15 115.4(8) . 4_556 ? O5 C9 C10 89.0(6) 4_556 . ? O5 C9 C8 55.7(7) 4_556 . ? C10 C9 C8 120.0 . . ? O5 C9 C11 63.8(5) 4_556 4_556 ? C8 C9 C11 97.0(2) . 4_556 ? O5 C9 C14 55.8(8) 4_556 4_556 ? C10 C9 C14 116.2(4) . 4_556 ? C11 C9 C14 93.7(5) 4_556 4_556 ? O5 C9 H9A 125.4 4_556 . ? C10 C9 H9A 120.0 . . ? C8 C9 H9A 120.0 . . ? C11 C9 H9A 140.7 4_556 . ? C14 C9 H9A 123.8 4_556 . ? C11 C10 C9 88.4(8) 4_556 . ? C11 C10 C9 120.0 . . ? C11 C10 C12 73.8(4) 4_556 4_556 ? C11 C10 C12 83.4(5) . 4_556 ? C9 C10 C12 122.1(7) . 4_556 ? C11 C10 C10 62.2(7) 4_556 4_556 ? C9 C10 C10 111.7(3) . 4_556 ? C12 C10 C10 107.3(6) 4_556 4_556 ? C11 C10 O5 58.5(7) 4_556 4_556 ? C11 C10 O5 97.5(2) . 4_556 ? C12 C10 O5 100.9(4) 4_556 4_556 ? C10 C10 O5 101.4(4) 4_556 4_556 ? C11 C10 H10A 138.4 4_556 . ? C11 C10 H10A 120.0 . . ? C9 C10 H10A 120.0 . . ? C12 C10 H10A 65.5 4_556 . ? C10 C10 H10A 122.1 4_556 . ? O5 C10 H10A 136.4 4_556 . ? C10 C11 C11 108.3(8) 4_556 4_556 ? C10 C11 O5 96.7(7) 4_556 . ? C11 C11 O5 140.2(6) 4_556 . ? C10 C11 C10 92.1(7) 4_556 . ? O5 C11 C10 125.1(4) . . ? C10 C11 C12 78.1(7) 4_556 . ? C11 C11 C12 100.5(4) 4_556 . ? O5 C11 C12 114.9(4) . . ? C10 C11 C12 120.0 . . ? C10 C11 C9 65.2(6) 4_556 4_556 ? C11 C11 C9 141.0(6) 4_556 4_556 ? C10 C11 C9 114.1(5) . 4_556 ? C12 C11 C9 114.4(6) . 4_556 ? C10 C11 C12 136.7(8) 4_556 4_556 ? C11 C11 C12 47.1(4) 4_556 4_556 ? O5 C11 C12 93.7(4) . 4_556 ? C10 C11 C12 48.9(3) . 4_556 ? C12 C11 C12 133.4(3) . 4_556 ? C9 C11 C12 109.5(5) 4_556 4_556 ? C13 C12 C11 120.0 . . ? C13 C12 C10 114.2(3) . 4_556 ? C13 C12 C11 89.4(3) . 4_556 ? C10 C12 C11 47.7(3) 4_556 4_556 ? C13 C12 H12A 120.0 . . ? C11 C12 H12A 120.0 . . ? C10 C12 H12A 118.2 4_556 . ? C11 C12 H12A 148.7 4_556 . ? C14 C13 C12 130.2(6) 4_556 . ? C12 C13 C8 120.0 . . ? C14 C13 H13A 109.7 4_556 . ? C12 C13 H13A 120.0 . . ? C8 C13 H13A 120.0 . . ? C8 C14 C13 129(2) 4_556 4_556 ? C13 C14 O5 98.9(7) 4_556 . ? C8 C14 C7 87(2) 4_556 4_556 ? C13 C14 C7 139.1(14) 4_556 4_556 ? O5 C14 C7 106.5(10) . 4_556 ? C8 C14 C15 92(2) 4_556 . ? C13 C14 C15 137.2(13) 4_556 . ? O5 C14 C15 114.1(10) . . ? C13 C14 C9 113.4(8) 4_556 4_556 ? C7 C14 C9 104.2(10) 4_556 4_556 ? C15 C14 C9 108.5(10) . 4_556 ? C8 C14 H14A 96.1 4_556 . ? C13 C14 H14A 85.3 4_556 . ? O5 C14 H14A 110.9 . . ? C7 C14 H14A 113.7 4_556 . ? C15 C14 H14A 106.1 . . ? C9 C14 H14A 86.1 4_556 . ? C8 C14 H14B 139.0 4_556 . ? O5 C14 H14B 105.7 . . ? C7 C14 H14B 111.7 4_556 . ? C15 C14 H14B 111.9 . . ? C9 C14 H14B 130.6 4_556 . ? H14A C14 H14B 108.1 . . ? C7 C15 O1 131(10) 4_556 4_556 ? C7 C15 O4 135(10) 4_556 . ? C7 C15 O3 61(8) 4_556 . ? O1 C15 O3 123.0(17) 4_556 . ? O4 C15 O3 127.3(13) . . ? C7 C15 O2 46(7) 4_556 4_556 ? O1 C15 O2 126.1(17) 4_556 4_556 ? O4 C15 O2 131.4(18) . 4_556 ? C7 C15 C14 81(6) 4_556 . ? O1 C15 C14 113.0(16) 4_556 . ? O4 C15 C14 108.8(13) . . ? O3 C15 C14 123.9(15) . . ? O2 C15 C14 117.3(15) 4_556 . ? C7 C15 C8 74(6) 4_556 4_556 ? O1 C15 C8 125.1(16) 4_556 4_556 ? O4 C15 C8 120.7(12) . 4_556 ? O3 C15 C8 111.9(15) . 4_556 ? O2 C15 C8 106.3(14) 4_556 4_556 ? Ni1 O6 H6A 101.7 . . ? Ni1 O6 H6B 135.4 . . ? H6A O6 H6B 110.1 . . ? 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 O4 Ni1 N1 C1 -21.4(6) 1_554 . . 4 ? O4 Ni1 N1 C1 158.6(6) 4_556 . . 4 ? O1 Ni1 N1 C1 -26.5(5) 4 . . 4 ? O1 Ni1 N1 C1 153.5(5) . . . 4 ? O6 Ni1 N1 C1 -116.3(2) . . . 4 ? O6 Ni1 N1 C1 63.7(2) 4 . . 4 ? O4 Ni1 N1 C1 158.6(6) 1_554 . . . ? O4 Ni1 N1 C1 -21.4(6) 4_556 . . . ? O1 Ni1 N1 C1 153.5(5) 4 . . . ? O1 Ni1 N1 C1 -26.5(5) . . . . ? O6 Ni1 N1 C1 63.7(2) . . . . ? O6 Ni1 N1 C1 -116.3(2) 4 . . . ? C1 N1 C1 C2 0.4(3) 4 . . . ? Ni1 N1 C1 C2 -179.6(3) . . . . ? N1 C1 C2 C3 -0.7(6) . . . . ? C1 C2 C3 C2 0.3(3) . . . 4 ? C1 C2 C3 C4 -179.7(3) . . . . ? C2 C3 C4 C5 -40.3(2) . . . . ? C2 C3 C4 C5 139.7(2) 4 . . . ? C2 C3 C4 C5 139.7(2) . . . 4 ? C2 C3 C4 C5 -40.3(2) 4 . . 4 ? C5 C4 C5 C6 0.2(2) 4 . . . ? C3 C4 C5 C6 -179.8(2) . . . . ? C6 N2 C6 C5 0.2(2) 4 . . . ? Ni1 N2 C6 C5 -179.8(2) 1_665 . . . ? C4 C5 C6 N2 -0.3(5) . . . . ? N1 Ni1 O1 O4 74(10) . . . 4_556 ? O6 Ni1 O1 O4 -16(10) . . . 4_556 ? O6 Ni1 O1 O4 164(10) 4 . . 4_556 ? N2 Ni1 O1 O4 -106(10) 1_445 . . 4_556 ? O4 Ni1 O1 C15 -151(12) 4_556 . . 4_556 ? N1 Ni1 O1 C15 -77(3) . . . 4_556 ? O6 Ni1 O1 C15 -167(3) . . . 4_556 ? O6 Ni1 O1 C15 13(3) 4 . . 4_556 ? N2 Ni1 O1 C15 103(3) 1_445 . . 4_556 ? O4 Ni1 O1 C7 -163(12) 4_556 . . . ? N1 Ni1 O1 C7 -89(3) . . . . ? O6 Ni1 O1 C7 -179(3) . . . . ? O6 Ni1 O1 C7 1(3) 4 . . . ? N2 Ni1 O1 C7 91(3) 1_445 . . . ? O4 O1 C7 C15 -50(22) 4_556 . . 4_556 ? Ni1 O1 C7 C15 103(9) . . . 4_556 ? O4 O1 C7 O3 -134(18) 4_556 . . 4_556 ? C15 O1 C7 O3 -88(11) 4_556 . . 4_556 ? Ni1 O1 C7 O3 15(4) . . . 4_556 ? O4 O1 C7 O2 -154(17) 4_556 . . . ? C15 O1 C7 O2 -107(11) 4_556 . . . ? Ni1 O1 C7 O2 -5(4) . . . . ? C15 O1 C7 O4 50(22) 4_556 . . 4_556 ? Ni1 O1 C7 O4 149(20) . . . 4_556 ? O4 O1 C7 C14 26(19) 4_556 . . 4_556 ? C15 O1 C7 C14 73(9) 4_556 . . 4_556 ? Ni1 O1 C7 C14 175.4(17) . . . 4_556 ? O4 O1 C7 C8 22(19) 4_556 . . . ? C15 O1 C7 C8 69(9) 4_556 . . . ? Ni1 O1 C7 C8 171.4(15) . . . . ? O3 O2 C7 C15 18(13) 4_556 . . 4_556 ? C15 O2 C7 O3 -18(13) 4_556 . . 4_556 ? O3 O2 C7 O1 70(7) 4_556 . . . ? C15 O2 C7 O1 51(11) 4_556 . . . ? O3 O2 C7 O4 67(8) 4_556 . . 4_556 ? C15 O2 C7 O4 49(11) 4_556 . . 4_556 ? O3 O2 C7 C14 -110(7) 4_556 . . 4_556 ? C15 O2 C7 C14 -128(15) 4_556 . . 4_556 ? O3 O2 C7 C8 -106(7) 4_556 . . . ? C15 O2 C7 C8 -124(14) 4_556 . . . ? C15 C7 C8 C14 56(12) 4_556 . . 4_556 ? O3 C7 C8 C14 173(5) 4_556 . . 4_556 ? O1 C7 C8 C14 18(4) . . . 4_556 ? O2 C7 C8 C14 -166(4) . . . 4_556 ? O4 C7 C8 C14 20(4) 4_556 . . 4_556 ? C15 C7 C8 O5 -163(11) 4_556 . . 4_556 ? O3 C7 C8 O5 -46(3) 4_556 . . 4_556 ? O1 C7 C8 O5 159.0(17) . . . 4_556 ? O2 C7 C8 O5 -25(3) . . . 4_556 ? O4 C7 C8 O5 160.8(13) 4_556 . . 4_556 ? C14 C7 C8 O5 141(4) 4_556 . . 4_556 ? C15 C7 C8 C9 -119(11) 4_556 . . . ? O3 C7 C8 C9 -2(3) 4_556 . . . ? O1 C7 C8 C9 -157.5(17) . . . . ? O2 C7 C8 C9 19(3) . . . . ? O4 C7 C8 C9 -155.7(12) 4_556 . . . ? C14 C7 C8 C9 -176(4) 4_556 . . . ? C15 C7 C8 C13 72(12) 4_556 . . . ? O3 C7 C8 C13 -170.5(19) 4_556 . . . ? O1 C7 C8 C13 34(3) . . . . ? O2 C7 C8 C13 -149.4(16) . . . . ? O4 C7 C8 C13 36(2) 4_556 . . . ? C14 C7 C8 C13 16(4) 4_556 . . . ? O3 C7 C8 C15 117(13) 4_556 . . 4_556 ? O1 C7 C8 C15 -38(10) . . . 4_556 ? O2 C7 C8 C15 138(13) . . . 4_556 ? O4 C7 C8 C15 -36(10) 4_556 . . 4_556 ? C14 C7 C8 C15 -56(12) 4_556 . . 4_556 ? C14 C8 C9 O5 89(10) 4_556 . . 4_556 ? C13 C8 C9 O5 65.4(6) . . . 4_556 ? C7 C8 C9 O5 -102.6(14) . . . 4_556 ? C15 C8 C9 O5 -111.4(15) 4_556 . . 4_556 ? C14 C8 C9 C10 24(10) 4_556 . . . ? O5 C8 C9 C10 -65.4(6) 4_556 . . . ? C13 C8 C9 C10 0.0 . . . . ? C7 C8 C9 C10 -168.0(12) . . . . ? C15 C8 C9 C10 -176.8(13) 4_556 . . . ? C14 C8 C9 C11 38(10) 4_556 . . 4_556 ? O5 C8 C9 C11 -51.6(5) 4_556 . . 4_556 ? C13 C8 C9 C11 13.76(19) . . . 4_556 ? C7 C8 C9 C11 -154.2(12) . . . 4_556 ? C15 C8 C9 C11 -163.0(13) 4_556 . . 4_556 ? O5 C8 C9 C14 -89(10) 4_556 . . 4_556 ? C13 C8 C9 C14 -24(10) . . . 4_556 ? C7 C8 C9 C14 168(11) . . . 4_556 ? C15 C8 C9 C14 159(11) 4_556 . . 4_556 ? O5 C9 C10 C11 -16.6(7) 4_556 . . 4_556 ? C8 C9 C10 C11 32.1(5) . . . 4_556 ? C14 C9 C10 C11 33.9(10) 4_556 . . 4_556 ? O5 C9 C10 C11 -48.7(6) 4_556 . . . ? C8 C9 C10 C11 0.0 . . . . ? C11 C9 C10 C11 -32.1(5) 4_556 . . . ? C14 C9 C10 C11 1.9(8) 4_556 . . . ? O5 C9 C10 C12 53.1(8) 4_556 . . 4_556 ? C8 C9 C10 C12 101.8(4) . . . 4_556 ? C11 C9 C10 C12 69.7(3) 4_556 . . 4_556 ? C14 C9 C10 C12 103.7(10) 4_556 . . 4_556 ? O5 C9 C10 C10 -75.8(6) 4_556 . . 4_556 ? C8 C9 C10 C10 -27.1 . . . 4_556 ? C11 C9 C10 C10 -59.2(5) 4_556 . . 4_556 ? C14 C9 C10 C10 -25.2(8) 4_556 . . 4_556 ? C8 C9 C10 O5 48.7(7) . . . 4_556 ? C11 C9 C10 O5 16.6(7) 4_556 . . 4_556 ? C14 C9 C10 O5 50.6(8) 4_556 . . 4_556 ? C9 O5 C11 C10 -16.9(5) 4_556 . . 4_556 ? C8 O5 C11 C10 -99.9(8) 4_556 . . 4_556 ? C14 O5 C11 C10 -109.1(12) . . . 4_556 ? C9 O5 C11 C11 112.4(9) 4_556 . . 4_556 ? C8 O5 C11 C11 29.4(11) 4_556 . . 4_556 ? C14 O5 C11 C11 20.3(15) . . . 4_556 ? C10 O5 C11 C11 129.3(10) 4_556 . . 4_556 ? C9 O5 C11 C10 80.4(8) 4_556 . . . ? C8 O5 C11 C10 -2.7(9) 4_556 . . . ? C14 O5 C11 C10 -11.8(13) . . . . ? C10 O5 C11 C10 97.3(7) 4_556 . . . ? C9 O5 C11 C12 -96.9(10) 4_556 . . . ? C8 O5 C11 C12 -179.9(6) 4_556 . . . ? C14 O5 C11 C12 170.9(8) . . . . ? C10 O5 C11 C12 -80.0(8) 4_556 . . . ? C8 O5 C11 C9 -83.0(10) 4_556 . . 4_556 ? C14 O5 C11 C9 -92.1(14) . . . 4_556 ? C10 O5 C11 C9 16.9(5) 4_556 . . 4_556 ? C9 O5 C11 C12 121.0(9) 4_556 . . 4_556 ? C8 O5 C11 C12 37.9(6) 4_556 . . 4_556 ? C14 O5 C11 C12 28.8(10) . . . 4_556 ? C10 O5 C11 C12 137.9(8) 4_556 . . 4_556 ? C11 C10 C11 C10 -127.3(13) 4_556 . . 4_556 ? C9 C10 C11 C10 -77.5(7) . . . 4_556 ? C12 C10 C11 C10 159.1(9) 4_556 . . 4_556 ? O5 C10 C11 C10 -100.7(9) 4_556 . . 4_556 ? C9 C10 C11 C11 49.8(8) . . . 4_556 ? C12 C10 C11 C11 -73.5(6) 4_556 . . 4_556 ? C10 C10 C11 C11 127.3(13) 4_556 . . 4_556 ? O5 C10 C11 C11 26.6(7) 4_556 . . 4_556 ? C11 C10 C11 O5 133.0(10) 4_556 . . . ? C9 C10 C11 O5 -177.1(7) . . . . ? C12 C10 C11 O5 59.5(6) 4_556 . . . ? C10 C10 C11 O5 -99.6(7) 4_556 . . . ? O5 C10 C11 O5 159.7(8) 4_556 . . . ? C11 C10 C11 C12 -49.8(8) 4_556 . . . ? C9 C10 C11 C12 0.0 . . . . ? C12 C10 C11 C12 -123.4(5) 4_556 . . . ? C10 C10 C11 C12 77.5(7) 4_556 . . . ? O5 C10 C11 C12 -23.2(4) 4_556 . . . ? C11 C10 C11 C9 169.0(10) 4_556 . . 4_556 ? C9 C10 C11 C9 -141.2(5) . . . 4_556 ? C12 C10 C11 C9 95.4(5) 4_556 . . 4_556 ? C10 C10 C11 C9 -63.7(5) 4_556 . . 4_556 ? O5 C10 C11 C9 -164.4(6) 4_556 . . 4_556 ? C11 C10 C11 C12 73.5(6) 4_556 . . 4_556 ? C9 C10 C11 C12 123.4(5) . . . 4_556 ? C10 C10 C11 C12 -159.1(9) 4_556 . . 4_556 ? O5 C10 C11 C12 100.2(4) 4_556 . . 4_556 ? C10 C11 C12 C13 85.5(8) 4_556 . . . ? C11 C11 C12 C13 -21.18(14) 4_556 . . . ? O5 C11 C12 C13 177.4(6) . . . . ? C10 C11 C12 C13 0.0 . . . . ? C9 C11 C12 C13 141.10(19) 4_556 . . . ? C12 C11 C12 C13 -60.1(5) 4_556 . . . ? C11 C11 C12 C10 -106.7(8) 4_556 . . 4_556 ? O5 C11 C12 C10 91.9(8) . . . 4_556 ? C10 C11 C12 C10 -85.5(8) . . . 4_556 ? C9 C11 C12 C10 55.6(6) 4_556 . . 4_556 ? C12 C11 C12 C10 -145.6(11) 4_556 . . 4_556 ? C10 C11 C12 C11 106.7(8) 4_556 . . 4_556 ? O5 C11 C12 C11 -161.4(6) . . . 4_556 ? C10 C11 C12 C11 21.18(14) . . . 4_556 ? C9 C11 C12 C11 162.3(3) 4_556 . . 4_556 ? C12 C11 C12 C11 -38.9(4) 4_556 . . 4_556 ? C11 C12 C13 C14 -3.2(14) . . . 4_556 ? C10 C12 C13 C14 27.7(15) 4_556 . . 4_556 ? C11 C12 C13 C14 -14.4(14) 4_556 . . 4_556 ? C11 C12 C13 C8 0.0 . . . . ? C10 C12 C13 C8 30.9(4) 4_556 . . . ? C11 C12 C13 C8 -11.16(6) 4_556 . . . ? O5 C8 C13 C14 -160(6) 4_556 . . 4_556 ? C9 C8 C13 C14 167(6) . . . 4_556 ? C7 C8 C13 C14 -25(6) . . . 4_556 ? C15 C8 C13 C14 -16(6) 4_556 . . 4_556 ? C14 C8 C13 C12 -167(6) 4_556 . . . ? O5 C8 C13 C12 33.8(4) 4_556 . . . ? C9 C8 C13 C12 0.0 . . . . ? C7 C8 C13 C12 168.3(12) . . . . ? C15 C8 C13 C12 177.0(11) 4_556 . . . ? C9 O5 C14 C8 34(5) 4_556 . . 4_556 ? C11 O5 C14 C8 119(5) . . . 4_556 ? C10 O5 C14 C8 91(5) 4_556 . . 4_556 ? C9 O5 C14 C13 -122.8(12) 4_556 . . 4_556 ? C8 O5 C14 C13 -157(6) 4_556 . . 4_556 ? C11 O5 C14 C13 -38.0(13) . . . 4_556 ? C10 O5 C14 C13 -65.5(13) 4_556 . . 4_556 ? C9 O5 C14 C7 89.7(14) 4_556 . . 4_556 ? C8 O5 C14 C7 56(5) 4_556 . . 4_556 ? C11 O5 C14 C7 174.5(12) . . . 4_556 ? C10 O5 C14 C7 147.0(12) 4_556 . . 4_556 ? C9 O5 C14 C15 85.3(16) 4_556 . . . ? C8 O5 C14 C15 52(4) 4_556 . . . ? C11 O5 C14 C15 170.0(13) . . . . ? C10 O5 C14 C15 142.5(13) 4_556 . . . ? C8 O5 C14 C9 -34(5) 4_556 . . 4_556 ? C11 O5 C14 C9 84.8(9) . . . 4_556 ? C10 O5 C14 C9 57.3(7) 4_556 . . 4_556 ? O1 O4 C15 C7 -43(19) 4_556 . . 4_556 ? Ni1 O4 C15 C7 -82(10) 1_556 . . 4_556 ? C7 O4 C15 O1 43(19) 4_556 . . 4_556 ? Ni1 O4 C15 O1 -40(15) 1_556 . . 4_556 ? O1 O4 C15 O3 42(16) 4_556 . . . ? C7 O4 C15 O3 85(9) 4_556 . . . ? Ni1 O4 C15 O3 3(4) 1_556 . . . ? O1 O4 C15 O2 22(17) 4_556 . . 4_556 ? C7 O4 C15 O2 65(9) 4_556 . . 4_556 ? Ni1 O4 C15 O2 -18(4) 1_556 . . 4_556 ? O1 O4 C15 C14 -139(16) 4_556 . . . ? C7 O4 C15 C14 -96(10) 4_556 . . . ? Ni1 O4 C15 C14 -178.8(13) 1_556 . . . ? O1 O4 C15 C8 -142(16) 4_556 . . 4_556 ? C7 O4 C15 C8 -99(11) 4_556 . . 4_556 ? Ni1 O4 C15 C8 178.7(12) 1_556 . . 4_556 ? O2 O3 C15 C7 16(11) 4_556 . . 4_556 ? O2 O3 C15 O1 -107(7) 4_556 . . 4_556 ? C7 O3 C15 O1 -122(12) 4_556 . . 4_556 ? O2 O3 C15 O4 -111(7) 4_556 . . . ? C7 O3 C15 O4 -127(12) 4_556 . . . ? C7 O3 C15 O2 -16(11) 4_556 . . 4_556 ? O2 O3 C15 C14 71(8) 4_556 . . . ? C7 O3 C15 C14 55(9) 4_556 . . . ? O2 O3 C15 C8 73(7) 4_556 . . 4_556 ? C7 O3 C15 C8 57(9) 4_556 . . 4_556 ? C8 C14 C15 C7 55(12) 4_556 . . 4_556 ? C13 C14 C15 C7 -107(11) 4_556 . . 4_556 ? O5 C14 C15 C7 30(12) . . . 4_556 ? C9 C14 C15 C7 61(12) 4_556 . . 4_556 ? C8 C14 C15 O1 -174(4) 4_556 . . 4_556 ? C13 C14 C15 O1 24(4) 4_556 . . 4_556 ? O5 C14 C15 O1 161(2) . . . 4_556 ? C7 C14 C15 O1 131(13) 4_556 . . 4_556 ? C9 C14 C15 O1 -168(2) 4_556 . . 4_556 ? C8 C14 C15 O4 -170(4) 4_556 . . . ? C13 C14 C15 O4 28(3) 4_556 . . . ? O5 C14 C15 O4 164.7(17) . . . . ? C7 C14 C15 O4 135(13) 4_556 . . . ? C9 C14 C15 O4 -164.2(17) 4_556 . . . ? C8 C14 C15 O3 9(5) 4_556 . . . ? C13 C14 C15 O3 -154(2) 4_556 . . . ? O5 C14 C15 O3 -17(3) . . . . ? C7 C14 C15 O3 -46(10) 4_556 . . . ? C9 C14 C15 O3 15(3) 4_556 . . . ? C8 C14 C15 O2 26(5) 4_556 . . 4_556 ? C13 C14 C15 O2 -136(2) 4_556 . . 4_556 ? O5 C14 C15 O2 1(3) . . . 4_556 ? C7 C14 C15 O2 -29(10) 4_556 . . 4_556 ? C9 C14 C15 O2 32(3) 4_556 . . 4_556 ? C13 C14 C15 C8 -163(5) 4_556 . . 4_556 ? O5 C14 C15 C8 -26(3) . . . 4_556 ? C7 C14 C15 C8 -55(12) 4_556 . . 4_556 ? C9 C14 C15 C8 6(3) 4_556 . . 4_556 ? 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 O6 H6A O3 0.86 1.85 2.67(2) 157.5 1_554 O6 H6A O2 0.86 1.95 2.77(2) 157.7 4 O6 H6B O2 0.85 2.06 2.818(17) 149.2 6_665 O6 H6B O3 0.85 2.24 3.047(16) 158.8 2_664 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.34 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.224 _refine_diff_density_min -0.187 _refine_diff_density_rms 0.045 #===END data_complex6 _database_code_depnum_ccdc_archive 'CCDC 637137' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H28 N3 Ni O7' _chemical_formula_weight 565.23 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 Orthorhombic _symmetry_space_group_name_H-M Fddd loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+3/4, -y+3/4, z' '-x+3/4, y, -z+3/4' 'x, -y+3/4, -z+3/4' 'x, y+1/2, z+1/2' '-x+3/4, -y+5/4, z+1/2' '-x+3/4, y+1/2, -z+5/4' 'x, -y+5/4, -z+5/4' 'x+1/2, y, z+1/2' '-x+5/4, -y+3/4, z+1/2' '-x+5/4, y, -z+5/4' 'x+1/2, -y+3/4, -z+5/4' 'x+1/2, y+1/2, z' '-x+5/4, -y+5/4, z' '-x+5/4, y+1/2, -z+3/4' 'x+1/2, -y+5/4, -z+3/4' '-x, -y, -z' 'x-3/4, y-3/4, -z' 'x-3/4, -y, z-3/4' '-x, y-3/4, z-3/4' '-x, -y+1/2, -z+1/2' 'x-3/4, y-1/4, -z+1/2' 'x-3/4, -y+1/2, z-1/4' '-x, y-1/4, z-1/4' '-x+1/2, -y, -z+1/2' 'x-1/4, y-3/4, -z+1/2' 'x-1/4, -y, z-1/4' '-x+1/2, y-3/4, z-1/4' '-x+1/2, -y+1/2, -z' 'x-1/4, y-1/4, -z' 'x-1/4, -y+1/2, z-3/4' '-x+1/2, y-1/4, z-3/4' _cell_length_a 13.8794(18) _cell_length_b 21.611(4) _cell_length_c 35.005(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 10500(3) _cell_formula_units_Z 16 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4382 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 25.22 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 1.430 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4720 _exptl_absorpt_coefficient_mu 0.790 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.648210 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 14238 _diffrn_reflns_av_R_equivalents 0.0457 _diffrn_reflns_av_sigmaI/netI 0.0317 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 26.41 _reflns_number_total 2691 _reflns_number_gt 2106 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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^)+(0.0212P)^2^+135.8844P] 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_number_reflns 2691 _refine_ls_number_parameters 244 _refine_ls_number_restraints 41 _refine_ls_R_factor_all 0.0809 _refine_ls_R_factor_gt 0.0622 _refine_ls_wR_factor_ref 0.1447 _refine_ls_wR_factor_gt 0.1363 _refine_ls_goodness_of_fit_ref 1.169 _refine_ls_restrained_S_all 1.242 _refine_ls_shift/su_max 0.005 _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 0.6250 0.81088(2) 0.6250 0.03562(11) Uani 1 2 d S . . O1 O 0.4467(3) 0.7124(2) 0.60237(12) 0.0615(13) Uani 0.50 1 d PU . . O2 O 0.4941(2) 0.8076(2) 0.59339(11) 0.0437(11) Uani 0.50 1 d P . . O3 O 0.3218(3) 0.7331(2) 0.53903(12) 0.0667(13) Uani 0.50 1 d P . . O4 O 0.0257(4) 0.7928(3) 0.41625(16) 0.0789(16) Uani 0.50 1 d PU . . O5 O 0.0066(4) 0.6906(3) 0.40759(14) 0.0627(16) Uani 0.50 1 d P . . C1 C 0.4461(3) 0.7625(3) 0.57901(13) 0.0353(14) Uani 0.50 1 d PD . . C2 C 0.3794(4) 0.7858(3) 0.54781(14) 0.0472(16) Uani 0.50 1 d PD . . H2A H 0.3420 0.8209 0.5553 0.057 Uiso 0.50 1 d PR . . H2B H 0.4140 0.7929 0.5243 0.057 Uiso 0.50 1 d PR . . C3 C 0.2575(2) 0.73963(15) 0.50910(8) 0.0427(16) Uani 0.50 1 d PGU . . C4 C 0.1889(3) 0.69304(16) 0.50604(11) 0.124(3) Uani 0.50 1 d PG . . H4A H 0.1879 0.6598 0.5243 0.149 Uiso 0.50 1 d PR . . C5 C 0.1217(3) 0.6945(2) 0.47661(12) 0.075(2) Uani 0.50 1 d PG . . H5A H 0.0743 0.6624 0.4745 0.090 Uiso 0.50 1 d PR . . C6 C 0.1231(3) 0.7426(2) 0.45024(11) 0.0425(16) Uani 0.50 1 d PG . . C7 C 0.1917(3) 0.7892(2) 0.45330(11) 0.070(2) Uani 0.50 1 d PG . . H7A H 0.1927 0.8224 0.4351 0.084 Uiso 0.50 1 d PR . . C8 C 0.2589(3) 0.78771(16) 0.48273(10) 0.0579(19) Uani 0.50 1 d PG . . H8A H 0.3063 0.8199 0.4848 0.070 Uiso 0.50 1 d PR . . C9 C 0.0454(5) 0.7384(5) 0.4154(2) 0.065(3) Uani 0.50 1 d P . . N1 N 0.55242(16) 0.81440(11) 0.67759(6) 0.0418(6) Uani 1 1 d . . . C10 C 0.4675(2) 0.78805(14) 0.68355(8) 0.0453(8) Uani 1 1 d . . . H10A H 0.4410 0.7642 0.6641 0.054 Uiso 1 1 calc R . . C11 C 0.4170(2) 0.79422(15) 0.71678(8) 0.0535(9) Uani 1 1 d . . . H11A H 0.3581 0.7743 0.7196 0.064 Uiso 1 1 calc R . . C12 C 0.4536(3) 0.83032(15) 0.74663(8) 0.0580(9) Uani 1 1 d . . . C13 C 0.5426(3) 0.85664(16) 0.74045(9) 0.0666(11) Uani 1 1 d . . . H13A H 0.5713 0.8801 0.7596 0.080 Uiso 1 1 calc R . . C14 C 0.5891(2) 0.84863(15) 0.70638(9) 0.0553(9) Uani 1 1 d . . . H14A H 0.6486 0.8676 0.7029 0.066 Uiso 1 1 calc R . . C15 C 0.3965(3) 0.84193(17) 0.78238(9) 0.0871(13) Uani 1 1 d . . . H15A H 0.4365 0.8357 0.8044 0.105 Uiso 1 1 d R . . H15B H 0.3443 0.8128 0.7834 0.105 Uiso 1 1 d R . . N2 N 0.6250 0.90865(8) 0.6250 0.0471(9) Uani 1 2 d SG . . C16 C 0.70970(10) 0.94276(13) 0.62265(9) 0.0514(17) Uani 0.50 1 d PG . . H16A H 0.7695 0.9224 0.6169 0.062 Uiso 0.50 1 d PR . . C17 C 0.7079(3) 1.00635(13) 0.62857(12) 0.0567(19) Uani 0.50 1 d PG . . H17A H 0.7664 1.0299 0.6270 0.068 Uiso 0.50 1 d PR . . C18 C 0.6213(4) 1.03583(8) 0.63683(11) 0.0490(16) Uani 0.50 1 d PGDU . . C19 C 0.5366(3) 1.00172(13) 0.63918(12) 0.067(2) Uani 0.50 1 d PG . . H19A H 0.4769 1.0221 0.6449 0.080 Uiso 0.50 1 d PR . . C20 C 0.53846(10) 0.93813(13) 0.63327(9) 0.077(2) Uani 0.50 1 d PG . . H20A H 0.4800 0.9146 0.6348 0.093 Uiso 0.50 1 d PR . . C21 C 0.6260(6) 1.10595(18) 0.64328(17) 0.063(2) Uani 0.50 1 d PD . . H21A H 0.6817 1.1168 0.6581 0.076 Uiso 0.50 1 d PR . . H21B H 0.5698 1.1163 0.6579 0.076 Uiso 0.50 1 d PR . . O6 O 0.6250 0.71558(13) 0.6250 0.0608(9) Uani 1 2 d SU . . H6A H 0.5752 0.6990 0.6159 0.073 Uiso 1 1 d R . . O7 O 0.3674(5) 0.6076(3) 0.5952(2) 0.138(3) Uani 0.50 1 d PDU . . H7B H 0.3544 0.6213 0.6201 0.165 Uiso 0.50 1 d PRD . . H7C H 0.3265 0.6064 0.5768 0.165 Uiso 0.50 1 d PRD . . 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 0.0320(2) 0.0382(2) 0.0366(2) 0.000 -0.0113(2) 0.000 O1 0.055(2) 0.080(3) 0.050(2) 0.000(2) -0.011(2) -0.027(2) O2 0.0200(15) 0.059(2) 0.052(2) 0.019(2) -0.0192(16) 0.0038(17) O3 0.069(2) 0.070(3) 0.061(2) 0.019(2) -0.046(2) -0.035(2) O4 0.064(3) 0.083(3) 0.090(3) -0.020(3) -0.033(2) -0.011(2) O5 0.061(3) 0.080(3) 0.047(3) -0.017(3) -0.017(2) -0.022(3) C1 0.026(2) 0.055(3) 0.025(2) 0.000(2) -0.0144(19) -0.011(2) C2 0.040(3) 0.060(3) 0.041(3) -0.007(3) -0.013(3) -0.016(3) C3 0.040(3) 0.042(3) 0.046(3) -0.003(2) -0.018(3) -0.006(2) C4 0.121(5) 0.130(5) 0.120(5) 0.084(4) -0.093(4) -0.092(4) C5 0.088(4) 0.074(4) 0.064(4) 0.019(3) -0.041(4) -0.032(4) C6 0.038(3) 0.053(3) 0.036(3) -0.001(3) -0.005(3) -0.001(3) C7 0.055(3) 0.088(5) 0.068(4) 0.027(4) -0.027(3) -0.042(3) C8 0.053(3) 0.072(4) 0.050(3) 0.016(3) -0.020(3) -0.033(3) C9 0.037(3) 0.121(7) 0.036(3) -0.012(4) -0.021(3) 0.001(4) N1 0.0418(11) 0.0463(12) 0.0374(11) -0.0036(11) -0.0091(10) 0.0036(11) C10 0.0472(15) 0.0493(16) 0.0396(14) -0.0014(13) -0.0026(13) 0.0064(13) C11 0.0589(17) 0.0556(17) 0.0459(16) 0.0118(14) 0.0066(14) 0.0168(15) C12 0.088(2) 0.0560(16) 0.0297(13) 0.0094(13) -0.0025(15) 0.0345(16) C13 0.090(2) 0.067(2) 0.0429(16) -0.0145(15) -0.0206(17) 0.0241(19) C14 0.0593(18) 0.0591(18) 0.0474(16) -0.0087(15) -0.0149(14) 0.0012(16) C15 0.126(3) 0.103(2) 0.0323(15) 0.0179(16) 0.0116(18) 0.066(2) N2 0.0449(17) 0.0375(17) 0.059(2) 0.000 -0.0099(17) 0.000 C16 0.044(3) 0.039(3) 0.071(4) -0.001(3) 0.021(3) 0.019(3) C17 0.048(3) 0.044(3) 0.078(4) -0.010(3) -0.002(3) -0.012(3) C18 0.061(3) 0.038(2) 0.048(3) 0.007(2) 0.009(3) -0.004(3) C19 0.056(4) 0.045(4) 0.100(6) 0.027(4) -0.013(4) -0.003(3) C20 0.064(3) 0.049(4) 0.118(6) 0.006(4) -0.056(4) 0.033(3) C21 0.083(4) 0.030(3) 0.076(4) -0.008(2) -0.022(4) -0.005(4) O6 0.0639(17) 0.0479(16) 0.0706(18) 0.000 -0.0309(16) 0.000 O7 0.116(4) 0.109(4) 0.188(5) 0.017(4) 0.013(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 Ni1 O6 2.059(3) . ? Ni1 N1 2.100(2) 11 ? Ni1 N1 2.100(2) . ? Ni1 N2 2.1130(19) . ? Ni1 O2 2.128(4) 11 ? Ni1 O2 2.128(3) . ? Ni1 O5 2.153(5) 29_566 ? Ni1 O5 2.153(5) 31_666 ? O1 O4 0.764(7) 29_566 ? O1 C9 1.237(11) 29_566 ? O1 C1 1.357(7) . ? O2 O5 0.053(8) 29_566 ? O2 C9 1.177(10) 29_566 ? O2 C1 1.283(7) . ? O3 C7 0.583(6) 29_566 ? O3 C6 1.000(6) 29_566 ? O3 C3 1.384(5) . ? O3 C2 1.424(7) . ? O3 C8 1.428(5) 29_566 ? O3 C5 1.833(6) 29_566 ? O4 O1 0.764(7) 29_566 ? O4 C9 1.205(11) . ? O4 C1 1.267(8) 29_566 ? O5 O2 0.053(8) 29_566 ? O5 C9 1.198(11) . ? O5 C1 1.295(8) 29_566 ? O5 Ni1 2.153(5) 29_566 ? C1 C9 0.229(9) 29_566 ? C1 O4 1.267(8) 29_566 ? C1 O5 1.295(8) 29_566 ? C1 C6 1.409(5) 29_566 ? C1 C2 1.518(6) . ? C2 C6 0.618(9) 29_566 ? C2 C5 0.955(8) 29_566 ? C2 H2A 0.9575 . ? C2 H2B 0.9647 . ? C3 C8 0.695(6) 29_566 ? C3 C3 0.806(6) 29_566 ? C3 C4 1.3900 . ? C3 C8 1.3900 . ? C3 C7 1.618(6) 29_566 ? C4 C8 0.923(7) 29_566 ? C4 C5 1.3900 . ? C4 H4A 0.9601 . ? C5 C2 0.955(7) 29_566 ? C5 C6 1.3900 . ? C5 O3 1.833(6) 29_566 ? C5 H5A 0.9599 . ? C6 C2 0.618(7) 29_566 ? C6 O3 1.000(6) 29_566 ? C6 C7 1.3900 . ? C6 C1 1.409(5) 29_566 ? C6 C9 1.630(8) . ? C7 O3 0.583(6) 29_566 ? C7 C8 1.3900 . ? C7 C3 1.618(6) 29_566 ? C7 H7A 0.9602 . ? C8 C3 0.695(6) 29_566 ? C8 C4 0.923(7) 29_566 ? C8 O3 1.428(6) 29_566 ? C8 H8A 0.9601 . ? C9 C1 0.229(9) 29_566 ? C9 O2 1.177(10) 29_566 ? C9 O1 1.237(11) 29_566 ? N1 C10 1.325(4) . ? N1 C14 1.350(4) . ? C10 C11 1.365(4) . ? C10 H10A 0.9300 . ? C11 C12 1.399(4) . ? C11 H11A 0.9300 . ? C12 C13 1.376(5) . ? C12 C15 1.502(4) . ? C13 C14 1.367(5) . ? C13 H13A 0.9300 . ? C14 H14A 0.9300 . ? C15 C15 1.549(7) 2_565 ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? N2 C16 1.3900 . ? N2 C20 1.390(2) 11 ? N2 C20 1.3900 . ? N2 C16 1.390(2) 11 ? C16 C20 0.231(6) 11 ? C16 C19 1.341(3) 11 ? C16 C17 1.3900 . ? C16 H16A 0.9603 . ? C17 C19 0.634(8) 11 ? C17 C18 1.380(9) 11 ? C17 C18 1.3900 . ? C17 C20 1.5321(17) 11 ? C17 H17A 0.9602 . ? C18 C18 0.835(7) 11 ? C18 C17 1.380(7) 11 ? C18 C19 1.3900 . ? C18 C21 1.534(4) . ? C19 C17 0.634(8) 11 ? C19 C16 1.341(2) 11 ? C19 C20 1.3900 . ? C19 H19A 0.9597 . ? C20 C16 0.231(6) 11 ? C20 C17 1.532(2) 11 ? C20 H20A 0.9598 . ? C21 C21 0.824(8) 14_565 ? C21 C21 1.280(12) 11 ? C21 C21 1.522(11) 8_565 ? C21 H21A 0.9600 . ? C21 H21B 0.9601 . ? O6 H6A 0.8412 . ? O7 H7B 0.9354 . ? O7 H7C 0.8604 . ? 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 O6 Ni1 N1 92.08(6) . 11 ? O6 Ni1 N1 92.08(7) . . ? N1 Ni1 N1 175.85(13) 11 . ? O6 Ni1 N2 180.000(1) . . ? N1 Ni1 N2 87.92(7) 11 . ? N1 Ni1 N2 87.93(7) . . ? O6 Ni1 O2 88.07(11) . 11 ? N1 Ni1 O2 92.72(12) 11 11 ? N1 Ni1 O2 87.42(12) . 11 ? N2 Ni1 O2 91.93(12) . 11 ? O6 Ni1 O2 88.07(12) . . ? N1 Ni1 O2 87.42(12) 11 . ? N1 Ni1 O2 92.72(12) . . ? N2 Ni1 O2 91.93(11) . . ? O2 Ni1 O2 176.1(2) 11 . ? O6 Ni1 O5 89.14(15) . 29_566 ? N1 Ni1 O5 86.73(15) 11 29_566 ? N1 Ni1 O5 93.33(15) . 29_566 ? N2 Ni1 O5 90.86(15) . 29_566 ? O2 Ni1 O5 177.14(16) 11 29_566 ? O2 Ni1 O5 1.2(2) . 29_566 ? O6 Ni1 O5 89.14(15) . 31_666 ? N1 Ni1 O5 93.34(15) 11 31_666 ? N1 Ni1 O5 86.72(15) . 31_666 ? N2 Ni1 O5 90.86(15) . 31_666 ? O2 Ni1 O5 1.2(2) 11 31_666 ? O2 Ni1 O5 177.13(16) . 31_666 ? O5 Ni1 O5 178.3(3) 29_566 31_666 ? O4 O1 C9 69.5(7) 29_566 29_566 ? O4 O1 C1 66.7(6) 29_566 . ? O5 O2 C9 112(9) 29_566 29_566 ? O5 O2 C1 102(9) 29_566 . ? O5 O2 Ni1 118(8) 29_566 . ? C9 O2 Ni1 124.2(5) 29_566 . ? C1 O2 Ni1 132.3(3) . . ? C7 O3 C6 120.5(7) 29_566 29_566 ? C7 O3 C3 102.9(6) 29_566 . ? C6 O3 C3 136.4(5) 29_566 . ? C7 O3 C2 138.0(7) 29_566 . ? C3 O3 C2 116.4(4) . . ? C7 O3 C8 74.4(5) 29_566 29_566 ? C6 O3 C8 164.9(6) 29_566 29_566 ? C2 O3 C8 143.9(4) . 29_566 ? C7 O3 C5 168.9(7) 29_566 29_566 ? C6 O3 C5 48.5(3) 29_566 29_566 ? C3 O3 C5 87.9(3) . 29_566 ? C8 O3 C5 116.4(3) 29_566 29_566 ? O1 O4 C9 74.0(7) 29_566 . ? O1 O4 C1 79.7(6) 29_566 29_566 ? O2 O5 C9 66(9) 29_566 . ? O2 O5 C1 75(9) 29_566 29_566 ? O2 O5 Ni1 61(8) 29_566 29_566 ? C9 O5 Ni1 121.1(5) . 29_566 ? C1 O5 Ni1 129.3(4) 29_566 29_566 ? C9 C1 O4 69(3) 29_566 29_566 ? C9 C1 O2 58(3) 29_566 . ? O4 C1 O2 120.3(4) 29_566 . ? C9 C1 O5 60(3) 29_566 29_566 ? O4 C1 O5 122.3(5) 29_566 29_566 ? C9 C1 O1 54(3) 29_566 . ? O2 C1 O1 111.5(4) . . ? O5 C1 O1 113.8(4) 29_566 . ? C9 C1 C6 165(3) 29_566 29_566 ? O4 C1 C6 103.4(5) 29_566 29_566 ? O2 C1 C6 134.3(5) . 29_566 ? O5 C1 C6 132.1(5) 29_566 29_566 ? O1 C1 C6 112.3(5) . 29_566 ? C9 C1 C2 163(3) 29_566 . ? O4 C1 C2 126.5(5) 29_566 . ? O2 C1 C2 110.3(5) . . ? O5 C1 C2 108.1(5) 29_566 . ? O1 C1 C2 134.5(5) . . ? C6 C2 C5 122.7(9) 29_566 29_566 ? C5 C2 O3 98.9(5) 29_566 . ? C6 C2 C1 68.1(6) 29_566 . ? C5 C2 C1 143.3(6) 29_566 . ? O3 C2 C1 103.5(4) . . ? C6 C2 C9 69.7(6) 29_566 29_566 ? C5 C2 C9 143.8(6) 29_566 29_566 ? O3 C2 C9 104.9(5) . 29_566 ? C5 C2 C7 110.7(5) 29_566 29_566 ? C1 C2 C7 92.8(4) . 29_566 ? C9 C2 C7 94.1(4) 29_566 29_566 ? C6 C2 H2A 136.6 29_566 . ? C5 C2 H2A 83.2 29_566 . ? O3 C2 H2A 112.9 . . ? C1 C2 H2A 113.4 . . ? C9 C2 H2A 111.2 29_566 . ? C7 C2 H2A 113.6 29_566 . ? C6 C2 H2B 106.4 29_566 . ? O3 C2 H2B 102.9 . . ? C1 C2 H2B 111.3 . . ? C9 C2 H2B 112.4 29_566 . ? C7 C2 H2B 112.2 29_566 . ? H2A C2 H2B 112.1 . . ? C8 C3 C3 135.5(8) 29_566 29_566 ? C8 C3 O3 79.2(5) 29_566 . ? C3 C3 O3 145.2(6) 29_566 . ? C3 C3 C4 99.5(4) 29_566 . ? O3 C3 C4 115.3(3) . . ? C8 C3 C8 156.0(5) 29_566 . ? O3 C3 C8 124.7(3) . . ? C4 C3 C8 120.0 . . ? C8 C3 C7 58.7(4) 29_566 29_566 ? C3 C3 C7 165.8(7) 29_566 29_566 ? C4 C3 C7 94.7(3) . 29_566 ? C8 C3 C7 145.3(3) . 29_566 ? C8 C3 C4 171.5(7) 29_566 29_566 ? C3 C3 C4 52.9(4) 29_566 29_566 ? O3 C3 C4 92.3(3) . 29_566 ? C4 C3 C4 152.4(3) . 29_566 ? C7 C3 C4 112.9(3) 29_566 29_566 ? C8 C4 C5 146.3(4) 29_566 . ? C5 C4 C3 120.0 . . ? C8 C4 C3 53.8(3) 29_566 29_566 ? C5 C4 C3 92.43(19) . 29_566 ? C8 C4 H4A 93.7 29_566 . ? C5 C4 H4A 120.0 . . ? C3 C4 H4A 120.0 . . ? C3 C4 H4A 147.6 29_566 . ? C2 C5 C4 133.2(4) 29_566 . ? C6 C5 C4 120.0 . . ? C2 C5 O3 50.1(4) 29_566 29_566 ? C4 C5 O3 87.38(17) . 29_566 ? C2 C5 H5A 104.0 29_566 . ? C6 C5 H5A 120.0 . . ? C4 C5 H5A 120.0 . . ? O3 C5 H5A 152.6 29_566 . ? C2 C6 O3 121.5(7) 29_566 29_566 ? O3 C6 C5 98.8(3) 29_566 . ? C2 C6 C7 138.5(6) 29_566 . ? C5 C6 C7 120.0 . . ? C2 C6 C1 87.9(6) 29_566 29_566 ? O3 C6 C1 146.7(5) 29_566 29_566 ? C5 C6 C1 114.5(4) . 29_566 ? C7 C6 C1 125.5(4) . 29_566 ? C2 C6 C9 89.4(7) 29_566 . ? O3 C6 C9 144.6(6) 29_566 . ? C5 C6 C9 116.5(4) . . ? C7 C6 C9 123.4(4) . . ? O3 C7 C8 81.7(5) 29_566 . ? C8 C7 C6 120.0 . . ? O3 C7 C3 56.5(5) 29_566 29_566 ? C6 C7 C3 94.7(2) . 29_566 ? C8 C7 C2 110.15(18) . 29_566 ? C3 C7 C2 85.1(3) 29_566 29_566 ? O3 C7 H7A 158.2 29_566 . ? C8 C7 H7A 120.0 . . ? C6 C7 H7A 120.0 . . ? C3 C7 H7A 145.3 29_566 . ? C2 C7 H7A 129.2 29_566 . ? C3 C8 C4 117.7(8) 29_566 29_566 ? C3 C8 C7 96.0(5) 29_566 . ? C4 C8 C7 146.3(5) 29_566 . ? C4 C8 C3 93.7(5) 29_566 . ? C7 C8 C3 120.0 . . ? C3 C8 O3 72.2(5) 29_566 29_566 ? C4 C8 O3 170.1(6) 29_566 29_566 ? C3 C8 O3 96.2(2) . 29_566 ? C3 C8 H8A 144.0 29_566 . ? C7 C8 H8A 120.0 . . ? C3 C8 H8A 120.0 . . ? O3 C8 H8A 143.8 29_566 . ? C1 C9 O2 113(4) 29_566 29_566 ? C1 C9 O5 111(4) 29_566 . ? C1 C9 O4 100(3) 29_566 . ? O2 C9 O4 136.3(7) 29_566 . ? O5 C9 O4 138.1(7) . . ? C1 C9 O1 117(3) 29_566 29_566 ? O2 C9 O1 129.5(7) 29_566 29_566 ? O5 C9 O1 131.8(7) . 29_566 ? O2 C9 C6 123.4(8) 29_566 . ? O5 C9 C6 121.1(8) . . ? O4 C9 C6 94.5(6) . . ? O1 C9 C6 105.7(7) 29_566 . ? O2 C9 C2 102.7(7) 29_566 29_566 ? O5 C9 C2 100.4(7) . 29_566 ? O4 C9 C2 114.3(6) . 29_566 ? O1 C9 C2 125.3(7) 29_566 29_566 ? C10 N1 C14 116.9(3) . . ? C10 N1 Ni1 123.31(19) . . ? C14 N1 Ni1 119.6(2) . . ? N1 C10 C11 123.3(3) . . ? N1 C10 H10A 118.3 . . ? C11 C10 H10A 118.3 . . ? C10 C11 C12 120.3(3) . . ? C10 C11 H11A 119.9 . . ? C12 C11 H11A 119.9 . . ? C13 C12 C11 116.0(3) . . ? C13 C12 C15 122.4(3) . . ? C11 C12 C15 121.6(3) . . ? C14 C13 C12 120.6(3) . . ? C14 C13 H13A 119.7 . . ? C12 C13 H13A 119.7 . . ? N1 C14 C13 122.9(3) . . ? N1 C14 H14A 118.6 . . ? C13 C14 H14A 118.6 . . ? C12 C15 C15 111.0(3) . 2_565 ? C12 C15 H15A 110.0 . . ? C15 C15 H15A 110.6 2_565 . ? C12 C15 H15B 108.7 . . ? C15 C15 H15B 108.3 2_565 . ? H15A C15 H15B 108.2 . . ? C16 N2 C20 120.0 . . ? C20 N2 C20 125.4 11 . ? C16 N2 C16 115.94(6) . 11 ? C20 N2 C16 120.0 11 11 ? C16 N2 Ni1 122.03(11) . . ? C20 N2 Ni1 117.28(6) 11 . ? C20 N2 Ni1 117.28(10) . . ? C16 N2 Ni1 122.0 11 . ? C20 C16 C19 97.5(10) 11 11 ? C20 C16 N2 85.2(5) 11 . ? C19 C16 N2 123.7(4) 11 . ? C20 C16 C17 124.3(7) 11 . ? N2 C16 C17 120.0 . . ? C20 C16 H16A 61.2 11 . ? C19 C16 H16A 109.7 11 . ? N2 C16 H16A 120.0 . . ? C17 C16 H16A 120.0 . . ? C19 C17 C18 77.6(7) 11 11 ? C19 C17 C16 72.29(11) 11 . ? C18 C17 C16 114.38(19) 11 . ? C19 C17 C18 112.4(7) 11 . ? C16 C17 C18 120.0 . . ? C19 C17 C20 65.13(13) 11 11 ? C18 C17 C20 111.4(3) 11 11 ? C18 C17 C20 121.74(10) . 11 ? C19 C17 H17A 85.6 11 . ? C18 C17 H17A 113.9 11 . ? C16 C17 H17A 120.0 . . ? C18 C17 H17A 120.0 . . ? C20 C17 H17A 117.8 11 . ? C18 C18 C17 73.1(6) 11 11 ? C18 C18 C19 99.3(6) 11 . ? C18 C18 C17 71.8(6) 11 . ? C17 C18 C17 113.3(2) 11 . ? C19 C18 C17 120.0 . . ? C18 C18 C21 98.1(3) 11 . ? C17 C18 C21 123.2(5) 11 . ? C19 C18 C21 123.5(4) . . ? C17 C18 C21 116.5(4) . . ? C18 C18 C19 52.3(5) 11 11 ? C17 C18 C19 100.7(2) 11 11 ? C19 C18 C19 115.40(18) . 11 ? C21 C18 C19 117.8(5) . 11 ? C18 C18 C21 55.3(2) 11 11 ? C17 C18 C21 99.9(4) 11 11 ? C19 C18 C21 119.1(4) . 11 ? C17 C18 C21 103.9(4) . 11 ? C19 C18 C21 92.0(4) 11 11 ? C17 C19 C16 80.9(4) 11 11 ? C17 C19 C20 90.44(12) 11 . ? C17 C19 C18 75.9(6) 11 . ? C16 C19 C18 116.97(12) 11 . ? C20 C19 C18 120.0 . . ? C17 C19 C18 47.9(5) 11 11 ? C16 C19 C18 102.3(3) 11 11 ? C20 C19 C18 109.19(12) . 11 ? C17 C19 H19A 103.7 11 . ? C16 C19 H19A 122.2 11 . ? C20 C19 H19A 120.0 . . ? C18 C19 H19A 120.0 . . ? C18 C19 H19A 123.5 11 . ? C16 C20 C19 73.0(7) 11 . ? C16 C20 N2 85.2(6) 11 . ? C19 C20 N2 120.0 . . ? C16 C20 C17 48.5(4) 11 11 ? N2 C20 C17 110.9(3) . 11 ? C16 C20 H20A 111.9 11 . ? C19 C20 H20A 120.0 . . ? N2 C20 H20A 120.0 . . ? C17 C20 H20A 123.6 11 . ? C21 C21 C21 89.96(6) 14_565 11 ? C21 C21 C21 57.3(3) 14_565 8_565 ? C21 C21 C18 170.4(8) 14_565 . ? C21 C21 C18 81.5(3) 11 . ? C21 C21 C18 114.3(5) 8_565 . ? C21 C21 C18 145.2(2) 14_565 11 ? C21 C21 C18 55.2(2) 11 11 ? C21 C21 C18 87.9(4) 8_565 11 ? C21 C21 H21A 77.5 14_565 . ? C21 C21 H21A 124.0 11 . ? C21 C21 H21A 108.9 8_565 . ? C18 C21 H21A 110.8 . . ? C18 C21 H21A 119.6 11 . ? C21 C21 H21B 74.9 14_565 . ? C21 C21 H21B 121.0 11 . ? C21 C21 H21B 108.9 8_565 . ? C18 C21 H21B 105.9 . . ? C18 C21 H21B 120.8 11 . ? H21A C21 H21B 107.9 . . ? Ni1 O6 H6A 115.2 . . ? H7B O7 H7C 125.6 . . ? 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 O6 Ni1 O2 O5 -149(10) . . . 29_566 ? N1 Ni1 O2 O5 -57(10) 11 . . 29_566 ? N1 Ni1 O2 O5 119(10) . . . 29_566 ? N2 Ni1 O2 O5 31(10) . . . 29_566 ? O6 Ni1 O2 C9 1.3(5) . . . 29_566 ? N1 Ni1 O2 C9 93.5(5) 11 . . 29_566 ? N1 Ni1 O2 C9 -90.7(5) . . . 29_566 ? N2 Ni1 O2 C9 -178.7(5) . . . 29_566 ? O5 Ni1 O2 C9 150(10) 29_566 . . 29_566 ? O6 Ni1 O2 C1 -5.1(4) . . . . ? N1 Ni1 O2 C1 87.1(4) 11 . . . ? N1 Ni1 O2 C1 -97.0(4) . . . . ? N2 Ni1 O2 C1 174.9(4) . . . . ? O5 Ni1 O2 C1 144(10) 29_566 . . . ? O5 O2 C1 C9 -179(100) 29_566 . . 29_566 ? Ni1 O2 C1 C9 34(3) . . . 29_566 ? O5 O2 C1 O4 150(8) 29_566 . . 29_566 ? C9 O2 C1 O4 -31(3) 29_566 . . 29_566 ? Ni1 O2 C1 O4 2.4(7) . . . 29_566 ? C9 O2 C1 O5 179(100) 29_566 . . 29_566 ? Ni1 O2 C1 O5 -147(9) . . . 29_566 ? O5 O2 C1 O1 -174(9) 29_566 . . . ? C9 O2 C1 O1 5(3) 29_566 . . . ? Ni1 O2 C1 O1 38.6(6) . . . . ? O5 O2 C1 C6 -11(9) 29_566 . . 29_566 ? C9 O2 C1 C6 168(3) 29_566 . . 29_566 ? Ni1 O2 C1 C6 -158.6(5) . . . 29_566 ? O5 O2 C1 C2 -12(9) 29_566 . . . ? C9 O2 C1 C2 167(3) 29_566 . . . ? Ni1 O2 C1 C2 -159.5(3) . . . . ? O4 O1 C1 C9 -108(3) 29_566 . . 29_566 ? C9 O1 C1 O4 108(3) 29_566 . . 29_566 ? O4 O1 C1 O2 -112.7(6) 29_566 . . . ? C9 O1 C1 O2 -5(3) 29_566 . . . ? O4 O1 C1 O5 -113.0(7) 29_566 . . 29_566 ? C9 O1 C1 O5 -5(3) 29_566 . . 29_566 ? O4 O1 C1 C6 80.6(7) 29_566 . . 29_566 ? C9 O1 C1 C6 -172(3) 29_566 . . 29_566 ? O4 O1 C1 C2 91.5(8) 29_566 . . . ? C9 O1 C1 C2 -161(3) 29_566 . . . ? C7 O3 C2 C6 42.6(12) 29_566 . . 29_566 ? C3 O3 C2 C6 -159.9(10) . . . 29_566 ? C8 O3 C2 C6 -170.4(13) 29_566 . . 29_566 ? C5 O3 C2 C6 -134.9(14) 29_566 . . 29_566 ? C7 O3 C2 C5 177.5(13) 29_566 . . 29_566 ? C6 O3 C2 C5 134.9(14) 29_566 . . 29_566 ? C3 O3 C2 C5 -25.1(8) . . . 29_566 ? C8 O3 C2 C5 -35.6(10) 29_566 . . 29_566 ? C7 O3 C2 C1 26.8(13) 29_566 . . . ? C6 O3 C2 C1 -15.8(9) 29_566 . . . ? C3 O3 C2 C1 -175.7(4) . . . . ? C8 O3 C2 C1 173.7(6) 29_566 . . . ? C5 O3 C2 C1 -150.7(8) 29_566 . . . ? C7 O3 C2 C9 25.1(13) 29_566 . . 29_566 ? C6 O3 C2 C9 -17.6(10) 29_566 . . 29_566 ? C3 O3 C2 C9 -177.5(4) . . . 29_566 ? C8 O3 C2 C9 172.0(6) 29_566 . . 29_566 ? C5 O3 C2 C9 -152.4(8) 29_566 . . 29_566 ? C6 O3 C2 C7 -42.6(12) 29_566 . . 29_566 ? C3 O3 C2 C7 157.5(14) . . . 29_566 ? C8 O3 C2 C7 146.9(17) 29_566 . . 29_566 ? C5 O3 C2 C7 -177.5(13) 29_566 . . 29_566 ? C9 C1 C2 C6 -139(10) 29_566 . . 29_566 ? O4 C1 C2 C6 17.9(9) 29_566 . . 29_566 ? O2 C1 C2 C6 178.4(8) . . . 29_566 ? O5 C1 C2 C6 177.9(8) 29_566 . . 29_566 ? O1 C1 C2 C6 -25.6(10) . . . 29_566 ? C9 C1 C2 C5 105(10) 29_566 . . 29_566 ? O4 C1 C2 C5 -97.9(12) 29_566 . . 29_566 ? O2 C1 C2 C5 62.6(12) . . . 29_566 ? O5 C1 C2 C5 62.1(12) 29_566 . . 29_566 ? O1 C1 C2 C5 -141.4(10) . . . 29_566 ? C6 C1 C2 C5 -115.8(15) 29_566 . . 29_566 ? C9 C1 C2 O3 -129(10) 29_566 . . . ? O4 C1 C2 O3 28.0(7) 29_566 . . . ? O2 C1 C2 O3 -171.4(4) . . . . ? O5 C1 C2 O3 -171.9(4) 29_566 . . . ? O1 C1 C2 O3 -15.5(8) . . . . ? C6 C1 C2 O3 10.1(6) 29_566 . . . ? O4 C1 C2 C9 157(11) 29_566 . . 29_566 ? O2 C1 C2 C9 -42(10) . . . 29_566 ? O5 C1 C2 C9 -43(10) 29_566 . . 29_566 ? O1 C1 C2 C9 114(10) . . . 29_566 ? C6 C1 C2 C9 139(10) 29_566 . . 29_566 ? C9 C1 C2 C7 -124(10) 29_566 . . 29_566 ? O4 C1 C2 C7 33.4(6) 29_566 . . 29_566 ? O2 C1 C2 C7 -166.1(4) . . . 29_566 ? O5 C1 C2 C7 -166.6(4) 29_566 . . 29_566 ? O1 C1 C2 C7 -10.1(7) . . . 29_566 ? C6 C1 C2 C7 15.5(5) 29_566 . . 29_566 ? C7 O3 C3 C8 -2.2(5) 29_566 . . 29_566 ? C6 O3 C3 C8 -177.6(10) 29_566 . . 29_566 ? C2 O3 C3 C8 -167.0(6) . . . 29_566 ? C5 O3 C3 C8 -179.6(7) 29_566 . . 29_566 ? C7 O3 C3 C3 179.7(14) 29_566 . . 29_566 ? C6 O3 C3 C3 4.4(12) 29_566 . . 29_566 ? C2 O3 C3 C3 15.0(12) . . . 29_566 ? C8 O3 C3 C3 -178.1(15) 29_566 . . 29_566 ? C5 O3 C3 C3 2.4(10) 29_566 . . 29_566 ? C7 O3 C3 C4 -2.6(7) 29_566 . . . ? C6 O3 C3 C4 -177.9(7) 29_566 . . . ? C2 O3 C3 C4 -167.3(4) . . . . ? C8 O3 C3 C4 -0.3(5) 29_566 . . . ? C5 O3 C3 C4 -179.9(4) 29_566 . . . ? C7 O3 C3 C8 178.5(7) 29_566 . . . ? C6 O3 C3 C8 3.2(8) 29_566 . . . ? C2 O3 C3 C8 13.8(6) . . . . ? C8 O3 C3 C8 -179.2(7) 29_566 . . . ? C5 O3 C3 C8 1.2(4) 29_566 . . . ? C6 O3 C3 C7 -175.3(14) 29_566 . . 29_566 ? C2 O3 C3 C7 -164.7(9) . . . 29_566 ? C8 O3 C3 C7 2.2(5) 29_566 . . 29_566 ? C5 O3 C3 C7 -177.3(9) 29_566 . . 29_566 ? C7 O3 C3 C4 178.0(8) 29_566 . . 29_566 ? C6 O3 C3 C4 2.7(7) 29_566 . . 29_566 ? C2 O3 C3 C4 13.3(5) . . . 29_566 ? C8 O3 C3 C4 -179.7(7) 29_566 . . 29_566 ? C5 O3 C3 C4 0.71(18) 29_566 . . 29_566 ? C3 C3 C4 C8 179.2(14) 29_566 . . 29_566 ? O3 C3 C4 C8 0.5(9) . . . 29_566 ? C8 C3 C4 C8 179.5(10) . . . 29_566 ? C7 C3 C4 C8 -0.4(7) 29_566 . . 29_566 ? C4 C3 C4 C8 179(100) 29_566 . . 29_566 ? C8 C3 C4 C5 -179.5(10) 29_566 . . . ? C3 C3 C4 C5 -0.3(5) 29_566 . . . ? O3 C3 C4 C5 -179.0(3) . . . . ? C8 C3 C4 C5 0.0 . . . . ? C7 C3 C4 C5 -179.9(3) 29_566 . . . ? C4 C3 C4 C5 -0.3(8) 29_566 . . . ? C8 C3 C4 C3 -179.2(14) 29_566 . . 29_566 ? O3 C3 C4 C3 -178.7(7) . . . 29_566 ? C8 C3 C4 C3 0.3(5) . . . 29_566 ? C7 C3 C4 C3 -179.6(7) 29_566 . . 29_566 ? C4 C3 C4 C3 0.0(5) 29_566 . . 29_566 ? C8 C4 C5 C2 21.6(9) 29_566 . . 29_566 ? C3 C4 C5 C2 22.0(7) . . . 29_566 ? C3 C4 C5 C2 21.9(6) 29_566 . . 29_566 ? C8 C4 C5 C6 -0.4(8) 29_566 . . . ? C3 C4 C5 C6 0.0 . . . . ? C3 C4 C5 C6 -0.1(2) 29_566 . . . ? C8 C4 C5 O3 -1.0(8) 29_566 . . 29_566 ? C3 C4 C5 O3 -0.6(2) . . . 29_566 ? C3 C4 C5 O3 -0.7(2) 29_566 . . 29_566 ? C4 C5 C6 C2 133.0(12) . . . 29_566 ? O3 C5 C6 C2 134.1(13) 29_566 . . 29_566 ? C2 C5 C6 O3 -134.1(13) 29_566 . . 29_566 ? C4 C5 C6 O3 -1.1(4) . . . 29_566 ? C2 C5 C6 C7 -133.0(12) 29_566 . . . ? C4 C5 C6 C7 0.0 . . . . ? O3 C5 C6 C7 1.1(4) 29_566 . . . ? C2 C5 C6 C1 44.6(10) 29_566 . . 29_566 ? C4 C5 C6 C1 177.6(4) . . . 29_566 ? O3 C5 C6 C1 178.7(7) 29_566 . . 29_566 ? C2 C5 C6 C9 43.8(11) 29_566 . . . ? C4 C5 C6 C9 176.7(4) . . . . ? O3 C5 C6 C9 177.8(7) 29_566 . . . ? C2 C6 C7 O3 -42.7(12) 29_566 . . 29_566 ? C5 C6 C7 O3 -3.0(11) . . . 29_566 ? C1 C6 C7 O3 179.7(13) 29_566 . . 29_566 ? C9 C6 C7 O3 -179.5(13) . . . 29_566 ? C2 C6 C7 C8 -39.7(10) 29_566 . . . ? O3 C6 C7 C8 3.0(11) 29_566 . . . ? C5 C6 C7 C8 0.0 . . . . ? C1 C6 C7 C8 -177.3(5) 29_566 . . . ? C9 C6 C7 C8 -176.5(5) . . . . ? C2 C6 C7 C3 -39.5(10) 29_566 . . 29_566 ? O3 C6 C7 C3 3.1(10) 29_566 . . 29_566 ? C5 C6 C7 C3 0.1(2) . . . 29_566 ? C1 C6 C7 C3 -177.2(6) 29_566 . . 29_566 ? C9 C6 C7 C3 -176.4(6) . . . 29_566 ? O3 C6 C7 C2 42.7(12) 29_566 . . 29_566 ? C5 C6 C7 C2 39.7(10) . . . 29_566 ? C1 C6 C7 C2 -137.7(13) 29_566 . . 29_566 ? C9 C6 C7 C2 -136.8(13) . . . 29_566 ? O3 C7 C8 C3 2.2(6) 29_566 . . 29_566 ? C6 C7 C8 C3 0.3(5) . . . 29_566 ? C2 C7 C8 C3 -8.1(5) 29_566 . . 29_566 ? O3 C7 C8 C4 -178.5(16) 29_566 . . 29_566 ? C6 C7 C8 C4 179.6(12) . . . 29_566 ? C3 C7 C8 C4 179(100) 29_566 . . 29_566 ? C2 C7 C8 C4 171.2(12) 29_566 . . 29_566 ? O3 C7 C8 C3 1.9(7) 29_566 . . . ? C6 C7 C8 C3 0.0 . . . . ? C3 C7 C8 C3 -0.3(5) 29_566 . . . ? C2 C7 C8 C3 -8.4(3) 29_566 . . . ? C6 C7 C8 O3 -1.9(7) . . . 29_566 ? C3 C7 C8 O3 -2.2(6) 29_566 . . 29_566 ? C2 C7 C8 O3 -10.3(6) 29_566 . . 29_566 ? C8 C3 C8 C3 0.0(9) 29_566 . . 29_566 ? O3 C3 C8 C3 178.1(15) . . . 29_566 ? C4 C3 C8 C3 -0.8(13) . . . 29_566 ? C7 C3 C8 C3 179(100) 29_566 . . 29_566 ? C4 C3 C8 C3 179(100) 29_566 . . 29_566 ? C8 C3 C8 C4 -179(100) 29_566 . . 29_566 ? C3 C3 C8 C4 -179(100) 29_566 . . 29_566 ? O3 C3 C8 C4 -0.9(6) . . . 29_566 ? C4 C3 C8 C4 -179.8(6) . . . 29_566 ? C7 C3 C8 C4 0.0(8) 29_566 . . 29_566 ? C8 C3 C8 C7 0.7(15) 29_566 . . . ? C3 C3 C8 C7 0.8(13) 29_566 . . . ? O3 C3 C8 C7 178.9(3) . . . . ? C4 C3 C8 C7 0.0 . . . . ? C7 C3 C8 C7 179.8(6) 29_566 . . . ? C4 C3 C8 C7 179.8(6) 29_566 . . . ? C8 C3 C8 O3 1.5(15) 29_566 . . 29_566 ? C3 C3 C8 O3 1.5(12) 29_566 . . 29_566 ? O3 C3 C8 O3 179.6(3) . . . 29_566 ? C4 C3 C8 O3 0.8(3) . . . 29_566 ? C7 C3 C8 O3 -179.5(6) 29_566 . . 29_566 ? C4 C3 C8 O3 -179.5(8) 29_566 . . 29_566 ? O2 O5 C9 C1 179(100) 29_566 . . 29_566 ? Ni1 O5 C9 C1 152(3) 29_566 . . 29_566 ? C1 O5 C9 O2 -179(100) 29_566 . . 29_566 ? Ni1 O5 C9 O2 -27(9) 29_566 . . 29_566 ? O2 O5 C9 O4 44(9) 29_566 . . . ? C1 O5 C9 O4 -135(3) 29_566 . . . ? Ni1 O5 C9 O4 16.6(13) 29_566 . . . ? O2 O5 C9 O1 -8(9) 29_566 . . 29_566 ? C1 O5 C9 O1 173(4) 29_566 . . 29_566 ? Ni1 O5 C9 O1 -35.1(12) 29_566 . . 29_566 ? O2 O5 C9 C6 -172(9) 29_566 . . . ? C1 O5 C9 C6 9(2) 29_566 . . . ? Ni1 O5 C9 C6 160.5(4) 29_566 . . . ? O2 O5 C9 C2 -170(9) 29_566 . . 29_566 ? C1 O5 C9 C2 11(3) 29_566 . . 29_566 ? Ni1 O5 C9 C2 162.6(3) 29_566 . . 29_566 ? O1 O4 C9 C1 123(3) 29_566 . . 29_566 ? O1 O4 C9 O2 -97.5(11) 29_566 . . 29_566 ? C1 O4 C9 O2 140(3) 29_566 . . 29_566 ? O1 O4 C9 O5 -99.9(11) 29_566 . . . ? C1 O4 C9 O5 138(3) 29_566 . . . ? C1 O4 C9 O1 -123(3) 29_566 . . 29_566 ? O1 O4 C9 C6 110.5(6) 29_566 . . . ? C1 O4 C9 C6 -12(2) 29_566 . . . ? O1 O4 C9 C2 117.2(7) 29_566 . . 29_566 ? C1 O4 C9 C2 -5(2) 29_566 . . 29_566 ? C2 C6 C9 C1 45(13) 29_566 . . 29_566 ? O3 C6 C9 C1 -162(12) 29_566 . . 29_566 ? C5 C6 C9 C1 22(13) . . . 29_566 ? C7 C6 C9 C1 -162(12) . . . 29_566 ? C2 C6 C9 O2 5.4(10) 29_566 . . 29_566 ? O3 C6 C9 O2 158.2(9) 29_566 . . 29_566 ? C5 C6 C9 O2 -18.1(8) . . . 29_566 ? C7 C6 C9 O2 158.5(5) . . . 29_566 ? C1 C6 C9 O2 -40(12) 29_566 . . 29_566 ? C2 C6 C9 O5 5.8(10) 29_566 . . . ? O3 C6 C9 O5 158.6(9) 29_566 . . . ? C5 C6 C9 O5 -17.7(8) . . . . ? C7 C6 C9 O5 158.9(5) . . . . ? C1 C6 C9 O5 -39(12) 29_566 . . . ? C2 C6 C9 O4 162.6(9) 29_566 . . . ? O3 C6 C9 O4 -44.6(12) 29_566 . . . ? C5 C6 C9 O4 139.0(5) . . . . ? C7 C6 C9 O4 -44.3(6) . . . . ? C1 C6 C9 O4 117(13) 29_566 . . . ? C2 C6 C9 O1 -162.1(9) 29_566 . . 29_566 ? O3 C6 C9 O1 -9.4(13) 29_566 . . 29_566 ? C5 C6 C9 O1 174.3(4) . . . 29_566 ? C7 C6 C9 O1 -9.1(7) . . . 29_566 ? C1 C6 C9 O1 153(13) 29_566 . . 29_566 ? O3 C6 C9 C2 152.8(15) 29_566 . . 29_566 ? C5 C6 C9 C2 -23.6(7) . . . 29_566 ? C7 C6 C9 C2 153.1(9) . . . 29_566 ? C1 C6 C9 C2 -45(13) 29_566 . . 29_566 ? O6 Ni1 N1 C10 -57.4(2) . . . . ? N2 Ni1 N1 C10 122.6(2) . . . . ? O2 Ni1 N1 C10 -145.4(2) 11 . . . ? O2 Ni1 N1 C10 30.7(3) . . . . ? O5 Ni1 N1 C10 31.8(3) 29_566 . . . ? O5 Ni1 N1 C10 -146.5(3) 31_666 . . . ? O6 Ni1 N1 C14 127.6(2) . . . . ? N2 Ni1 N1 C14 -52.4(2) . . . . ? O2 Ni1 N1 C14 39.6(2) 11 . . . ? O2 Ni1 N1 C14 -144.2(2) . . . . ? O5 Ni1 N1 C14 -143.1(3) 29_566 . . . ? O5 Ni1 N1 C14 38.6(3) 31_666 . . . ? C14 N1 C10 C11 0.2(4) . . . . ? Ni1 N1 C10 C11 -174.9(2) . . . . ? N1 C10 C11 C12 0.8(5) . . . . ? C10 C11 C12 C13 -1.8(5) . . . . ? C10 C11 C12 C15 175.3(3) . . . . ? C11 C12 C13 C14 2.0(5) . . . . ? C15 C12 C13 C14 -175.1(3) . . . . ? C10 N1 C14 C13 0.0(4) . . . . ? Ni1 N1 C14 C13 175.3(2) . . . . ? C12 C13 C14 N1 -1.1(5) . . . . ? C13 C12 C15 C15 73.3(5) . . . 2_565 ? C11 C12 C15 C15 -103.6(5) . . . 2_565 ? N1 Ni1 N2 C16 -57.31(17) 11 . . . ? N1 Ni1 N2 C16 122.69(17) . . . . ? O2 Ni1 N2 C16 35.35(19) 11 . . . ? O2 Ni1 N2 C16 -144.66(19) . . . . ? O5 Ni1 N2 C16 -144.0(2) 29_566 . . . ? O5 Ni1 N2 C16 36.0(2) 31_666 . . . ? N1 Ni1 N2 C20 -47.78(16) 11 . . 11 ? N1 Ni1 N2 C20 132.22(16) . . . 11 ? O2 Ni1 N2 C20 44.88(18) 11 . . 11 ? O2 Ni1 N2 C20 -135.12(18) . . . 11 ? O5 Ni1 N2 C20 -134.5(2) 29_566 . . 11 ? O5 Ni1 N2 C20 45.5(2) 31_666 . . 11 ? N1 Ni1 N2 C20 132.23(16) 11 . . . ? N1 Ni1 N2 C20 -47.77(16) . . . . ? O2 Ni1 N2 C20 -135.11(18) 11 . . . ? O2 Ni1 N2 C20 44.89(18) . . . . ? O5 Ni1 N2 C20 45.5(2) 29_566 . . . ? O5 Ni1 N2 C20 -134.5(2) 31_666 . . . ? N1 Ni1 N2 C16 122.70(16) 11 . . 11 ? N1 Ni1 N2 C16 -57.30(16) . . . 11 ? O2 Ni1 N2 C16 -144.65(18) 11 . . 11 ? O2 Ni1 N2 C16 35.35(18) . . . 11 ? O5 Ni1 N2 C16 36.0(2) 29_566 . . 11 ? O5 Ni1 N2 C16 -144.0(2) 31_666 . . 11 ? C20 N2 C16 C20 -127.2(9) . . . 11 ? C16 N2 C16 C20 -117.4(7) 11 . . 11 ? Ni1 N2 C16 C20 62.6(10) . . . 11 ? C20 N2 C16 C19 95.8(13) 11 . . 11 ? C20 N2 C16 C19 -31.3(4) . . . 11 ? C16 N2 C16 C19 -21.5(6) 11 . . 11 ? Ni1 N2 C16 C19 158.5(3) . . . 11 ? C20 N2 C16 C17 127.2(9) 11 . . . ? C20 N2 C16 C17 0.0 . . . . ? C16 N2 C16 C17 9.8(3) 11 . . . ? Ni1 N2 C16 C17 -170.20(9) . . . . ? C20 C16 C17 C19 0.0(4) 11 . . 11 ? N2 C16 C17 C19 -106.1(8) . . . 11 ? C20 C16 C17 C18 67.0(9) 11 . . 11 ? C19 C16 C17 C18 67.0(7) 11 . . 11 ? N2 C16 C17 C18 -39.1(4) . . . 11 ? C20 C16 C17 C18 106.1(10) 11 . . . ? C19 C16 C17 C18 106.1(8) 11 . . . ? N2 C16 C17 C18 0.0 . . . . ? C19 C16 C17 C20 0.0(4) 11 . . 11 ? N2 C16 C17 C20 -106.1(10) . . . 11 ? C19 C17 C18 C18 -8.59(9) 11 . . 11 ? C16 C17 C18 C18 -90.4(4) . . . 11 ? C20 C17 C18 C18 -82.3(5) 11 . . 11 ? C19 C17 C18 C17 53.1(4) 11 . . 11 ? C18 C17 C18 C17 61.7(4) 11 . . 11 ? C16 C17 C18 C17 -28.7(3) . . . 11 ? C20 C17 C18 C17 -20.6(5) 11 . . 11 ? C19 C17 C18 C19 81.8(3) 11 . . . ? C18 C17 C18 C19 90.4(4) 11 . . . ? C16 C17 C18 C19 0.0 . . . . ? C20 C17 C18 C19 8.1(3) 11 . . . ? C19 C17 C18 C21 -98.7(5) 11 . . . ? C18 C17 C18 C21 -90.1(4) 11 . . . ? C16 C17 C18 C21 179.5(3) . . . . ? C20 C17 C18 C21 -172.4(5) 11 . . . ? C18 C17 C18 C19 8.59(9) 11 . . 11 ? C16 C17 C18 C19 -81.8(3) . . . 11 ? C20 C17 C18 C19 -73.7(5) 11 . . 11 ? C19 C17 C18 C21 -54.3(3) 11 . . 11 ? C18 C17 C18 C21 -45.7(3) 11 . . 11 ? C16 C17 C18 C21 -136.1(3) . . . 11 ? C20 C17 C18 C21 -128.0(4) 11 . . 11 ? C18 C18 C19 C17 -7.89(7) 11 . . 11 ? C17 C18 C19 C17 -82.2(4) . . . 11 ? C21 C18 C19 C17 98.3(6) . . . 11 ? C19 C18 C19 C17 -60.4(4) 11 . . 11 ? C21 C18 C19 C17 47.5(4) 11 . . 11 ? C18 C18 C19 C16 64.1(5) 11 . . 11 ? C17 C18 C19 C16 71.9(5) 11 . . 11 ? C17 C18 C19 C16 -10.2(3) . . . 11 ? C21 C18 C19 C16 170.3(5) . . . 11 ? C19 C18 C19 C16 11.5(5) 11 . . 11 ? C21 C18 C19 C16 119.4(4) 11 . . 11 ? C18 C18 C19 C20 74.3(4) 11 . . . ? C17 C18 C19 C20 82.2(4) 11 . . . ? C17 C18 C19 C20 0.0 . . . . ? C21 C18 C19 C20 -179.5(4) . . . . ? C19 C18 C19 C20 21.8(3) 11 . . . ? C21 C18 C19 C20 129.7(3) 11 . . . ? C17 C18 C19 C18 7.89(7) 11 . . 11 ? C17 C18 C19 C18 -74.3(4) . . . 11 ? C21 C18 C19 C18 106.2(6) . . . 11 ? C19 C18 C19 C18 -52.6(3) 11 . . 11 ? C21 C18 C19 C18 55.4(4) 11 . . 11 ? C17 C19 C20 C16 0.0(3) 11 . . 11 ? C18 C19 C20 C16 -73.9(8) . . . 11 ? C18 C19 C20 C16 -44.9(6) 11 . . 11 ? C17 C19 C20 N2 73.9(7) 11 . . . ? C16 C19 C20 N2 73.9(8) 11 . . . ? C18 C19 C20 N2 0.0 . . . . ? C18 C19 C20 N2 29.0(3) 11 . . . ? C16 C19 C20 C17 0.0(3) 11 . . 11 ? C18 C19 C20 C17 -73.9(7) . . . 11 ? C18 C19 C20 C17 -45.0(5) 11 . . 11 ? C16 N2 C20 C16 67.2(8) . . . 11 ? C20 N2 C20 C16 57.9(11) 11 . . 11 ? Ni1 N2 C20 C16 -122.1(8) . . . 11 ? C16 N2 C20 C19 0.0 . . . . ? C20 N2 C20 C19 -9.3(3) 11 . . . ? C16 N2 C20 C19 -67.2(8) 11 . . . ? Ni1 N2 C20 C19 170.66(9) . . . . ? C16 N2 C20 C17 25.2(3) . . . 11 ? C20 N2 C20 C17 15.8(5) 11 . . 11 ? C16 N2 C20 C17 -42.0(5) 11 . . 11 ? Ni1 N2 C20 C17 -164.2(3) . . . 11 ? C18 C18 C21 C21 8.4(11) 11 . . 11 ? C17 C18 C21 C21 -66.7(10) 11 . . 11 ? C19 C18 C21 C21 -98.5(8) . . . 11 ? C17 C18 C21 C21 82.0(8) . . . 11 ? C19 C18 C21 C21 59.8(9) 11 . . 11 ? C18 C18 C21 C21 8.6(8) 11 . . 8_565 ? C17 C18 C21 C21 -66.5(6) 11 . . 8_565 ? C19 C18 C21 C21 -98.3(3) . . . 8_565 ? C17 C18 C21 C21 82.2(3) . . . 8_565 ? C19 C18 C21 C21 60.0(5) 11 . . 8_565 ? C21 C18 C21 C21 0.2(6) 11 . . 8_565 ? C17 C18 C21 C18 -75.1(7) 11 . . 11 ? C19 C18 C21 C18 -106.9(8) . . . 11 ? C17 C18 C21 C18 73.7(7) . . . 11 ? C19 C18 C21 C18 51.5(6) 11 . . 11 ? C21 C18 C21 C18 -8.4(11) 11 . . 11 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.41 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.611 _refine_diff_density_min -0.702 _refine_diff_density_rms 0.072 #===END data_complex7 _database_code_depnum_ccdc_archive 'CCDC 637138' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H26 N2 O11 Zn2' _chemical_formula_weight 721.27 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' Zn Zn 0.2839 1.4301 '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 8.116(2) _cell_length_b 12.279(3) _cell_length_c 16.009(4) _cell_angle_alpha 69.271(4) _cell_angle_beta 86.078(4) _cell_angle_gamma 79.166(4) _cell_volume 1465.5(6) _cell_formula_units_Z 2 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 1729 _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 26.37 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 1.635 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 736 _exptl_absorpt_coefficient_mu 1.703 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.631780 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 7224 _diffrn_reflns_av_R_equivalents 0.0472 _diffrn_reflns_av_sigmaI/netI 0.1197 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.36 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5072 _reflns_number_gt 2954 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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^)+(0.0303P)^2^+2.5909P] 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 contra _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5072 _refine_ls_number_parameters 414 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.1307 _refine_ls_R_factor_gt 0.0533 _refine_ls_wR_factor_ref 0.1223 _refine_ls_wR_factor_gt 0.0911 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.005 _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 Zn1 Zn 0.54301(5) 0.84454(3) 0.81136(3) 0.03158(12) Uani 1 1 d . . . Zn2 Zn 0.71007(5) 0.34996(3) 1.32567(3) 0.02922(12) Uani 1 1 d . . . O1 O 0.4278(3) 0.93693(19) 0.70065(15) 0.0389(8) Uani 1 1 d . . . O2 O 0.3671(4) 1.0714(2) 0.76532(16) 0.0576(10) Uani 1 1 d . . . O3 O 0.1360(3) 1.38519(19) 0.36664(15) 0.0376(8) Uani 1 1 d . . . O4 O 0.4254(3) 1.31042(19) 0.20696(15) 0.0417(8) Uani 1 1 d . . . O5 O 0.4638(3) 1.37530(19) 0.31695(15) 0.0367(7) Uani 1 1 d . . . O6 O 0.7412(3) 0.8965(2) 0.83586(15) 0.0424(8) Uani 1 1 d . . . O7 O 0.9019(3) 0.8813(2) 0.72080(15) 0.0411(8) Uani 1 1 d . . . O8 O 0.9981(3) 0.90606(19) 0.92843(15) 0.0379(7) Uani 1 1 d . . . O9 O 0.7406(4) 0.5423(2) 1.28196(17) 0.0599(10) Uani 1 1 d . . . O10 O 0.8126(3) 0.4263(2) 1.20450(18) 0.0540(9) Uani 1 1 d . . . O11 O 0.7916(3) 0.18109(18) 1.33532(15) 0.0366(7) Uani 1 1 d D . . H11C H 0.7283 0.1360 1.3311 0.044 Uiso 1 1 d RD . . H11D H 0.9031 0.1558 1.3184 0.044 Uiso 1 1 d RD . . N1 N 0.4450(3) 0.7988(2) 0.93574(18) 0.0340(9) Uani 1 1 d . A . N2 N 0.2668(4) 0.6829(2) 1.54181(18) 0.0336(9) Uani 1 1 d . . . C1 C 0.3661(4) 1.0450(3) 0.6975(2) 0.0378(11) Uani 1 1 d . . . C2 C 0.3004(4) 1.1303(3) 0.6110(2) 0.0309(10) Uani 1 1 d . . . C3 C 0.2269(5) 1.2457(3) 0.6025(2) 0.0457(13) Uani 1 1 d . . . H3 H 0.2170 1.2685 0.6525 0.055 Uiso 1 1 calc R . . C4 C 0.1686(5) 1.3267(3) 0.5211(2) 0.0424(12) Uani 1 1 d . . . H4 H 0.1147 1.4022 0.5171 0.051 Uiso 1 1 calc R . . C5 C 0.1900(4) 1.2958(3) 0.4449(2) 0.0336(11) Uani 1 1 d . . . C6 C 0.2592(5) 1.1808(3) 0.4525(2) 0.0379(12) Uani 1 1 d . . . H6 H 0.2695 1.1585 0.4024 0.045 Uiso 1 1 calc R . . C7 C 0.3129(4) 1.0994(3) 0.5346(2) 0.0341(11) Uani 1 1 d . . . H7 H 0.3585 1.0222 0.5391 0.041 Uiso 1 1 calc R . . C8 C 0.1866(4) 1.3657(3) 0.2858(2) 0.0351(11) Uani 1 1 d . . . H8A H 0.1332 1.4328 0.2366 0.042 Uiso 1 1 calc R . . H8B H 0.1453 1.2965 0.2858 0.042 Uiso 1 1 calc R . . C9 C 0.3728(5) 1.3479(3) 0.2687(2) 0.0348(11) Uani 1 1 d . . . C10 C 0.8810(4) 0.8913(3) 0.7952(2) 0.0319(11) Uani 1 1 d . . . C11 C 1.0324(4) 0.8999(3) 0.8420(2) 0.0340(11) Uani 1 1 d . . . H11A H 1.1186 0.8315 0.8469 0.041 Uiso 1 1 calc R . . H11B H 1.0770 0.9696 0.8052 0.041 Uiso 1 1 calc R . . C12 C 0.9547(4) 0.8075(3) 0.9947(2) 0.0322(11) Uani 1 1 d . . . C13 C 0.9686(5) 0.6978(3) 0.9874(2) 0.0447(12) Uani 1 1 d . . . H13 H 1.0095 0.6847 0.9355 0.054 Uiso 1 1 calc R . . C14 C 0.9203(5) 0.6083(3) 1.0591(3) 0.0508(13) Uani 1 1 d . . . H14 H 0.9318 0.5332 1.0556 0.061 Uiso 1 1 calc R . . C15 C 0.8554(4) 0.6258(3) 1.1361(2) 0.0362(12) Uani 1 1 d . . . C16 C 0.8447(5) 0.7358(3) 1.1417(2) 0.0445(12) Uani 1 1 d . . . H16 H 0.8039 0.7486 1.1938 0.053 Uiso 1 1 calc R . . C17 C 0.8936(5) 0.8277(3) 1.0714(2) 0.0414(12) Uani 1 1 d . . . H17 H 0.8855 0.9021 1.0757 0.050 Uiso 1 1 calc R . . C18 C 0.7998(5) 0.5269(3) 1.2127(3) 0.0454(13) Uani 1 1 d . . . C19 C 0.4485(5) 0.6872(3) 0.9888(2) 0.0518(14) Uani 1 1 d . . . H19 H 0.4775 0.6287 0.9635 0.062 Uiso 1 1 calc R . . C20 C 0.4124(6) 0.6527(4) 1.0775(3) 0.0652(16) Uani 1 1 d . A . H20 H 0.4181 0.5728 1.1108 0.078 Uiso 1 1 calc R . . C21 C 0.3678(6) 0.7351(4) 1.11790(19) 0.0602(16) Uani 1 1 d D . . C22 C 0.3602(6) 0.8524(4) 1.0633(2) 0.0589(15) Uani 1 1 d . A . H22 H 0.3284 0.9122 1.0872 0.071 Uiso 1 1 calc R . . C23 C 0.4001(5) 0.8809(3) 0.9734(2) 0.0458(13) Uani 1 1 d . . . H23 H 0.3952 0.9600 0.9381 0.055 Uiso 1 1 calc R A . C24 C 0.3858(8) 0.7065(7) 1.2179(3) 0.071(3) Uiso 0.50 1 d PD A 1 H24A H 0.4041 0.6213 1.2476 0.085 Uiso 0.50 1 calc PR A 1 H24B H 0.4835 0.7348 1.2283 0.085 Uiso 0.50 1 calc PR A 1 C25 C 0.2361(8) 0.7604(7) 1.2576(3) 0.062(3) Uani 0.50 1 d PD A 1 H25A H 0.1388 0.7278 1.2526 0.074 Uiso 0.50 1 calc PR A 1 H25B H 0.2125 0.8453 1.2268 0.074 Uiso 0.50 1 calc PR A 1 C24' C 0.2991(8) 0.6926(5) 1.2124(3) 0.040(2) Uani 0.50 1 d PD A 2 H24C H 0.1777 0.7031 1.2110 0.048 Uiso 0.50 1 calc PR A 2 H24D H 0.3428 0.6092 1.2418 0.048 Uiso 0.50 1 calc PR A 2 C25' C 0.3503(10) 0.7624(6) 1.2623(3) 0.079(3) Uiso 0.50 1 d PD A 2 H25C H 0.3147 0.8460 1.2294 0.095 Uiso 0.50 1 calc PR A 2 H25D H 0.4717 0.7472 1.2665 0.095 Uiso 0.50 1 calc PR A 2 C26 C 0.2756(7) 0.7322(4) 1.3558(2) 0.081(2) Uani 1 1 d D . . C27 C 0.3041(7) 0.6172(4) 1.4166(3) 0.0709(17) Uani 1 1 d . A . H27 H 0.3274 0.5539 1.3961 0.085 Uiso 1 1 calc R . . C28 C 0.2981(5) 0.5963(3) 1.5070(3) 0.0508(14) Uani 1 1 d . . . H28 H 0.3165 0.5182 1.5459 0.061 Uiso 1 1 calc R A . C29 C 0.2356(6) 0.7920(3) 1.4823(3) 0.0540(15) Uani 1 1 d . . . H29 H 0.2095 0.8542 1.5040 0.065 Uiso 1 1 calc R A . C30 C 0.2388(7) 0.8192(4) 1.3925(3) 0.0771(19) Uani 1 1 d . A . H30 H 0.2157 0.8980 1.3554 0.093 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 Zn1 0.0313(2) 0.0390(2) 0.0250(2) -0.01156(16) 0.00221(18) -0.00768(17) Zn2 0.0324(2) 0.03006(19) 0.0249(2) -0.00960(16) 0.00254(18) -0.00550(17) O1 0.0461(15) 0.0306(12) 0.0374(14) -0.0081(10) -0.0079(13) -0.0050(11) O2 0.093(2) 0.0481(14) 0.0289(14) -0.0138(11) -0.0039(15) -0.0035(15) O3 0.0326(14) 0.0355(13) 0.0302(14) 0.0008(11) -0.0029(12) 0.0061(11) O4 0.0581(16) 0.0369(12) 0.0307(13) -0.0127(10) 0.0037(12) -0.0091(12) O5 0.0321(13) 0.0454(12) 0.0392(13) -0.0212(10) -0.0030(11) -0.0086(11) O6 0.0315(13) 0.0607(14) 0.0410(14) -0.0235(11) 0.0105(11) -0.0153(11) O7 0.0382(14) 0.0532(13) 0.0375(14) -0.0215(11) 0.0017(12) -0.0110(12) O8 0.0561(15) 0.0368(12) 0.0235(12) -0.0062(10) 0.0023(12) -0.0237(11) O9 0.0708(19) 0.0690(17) 0.0317(15) -0.0029(13) 0.0097(14) -0.0250(15) O10 0.0522(16) 0.0407(14) 0.0549(17) 0.0011(13) 0.0126(14) -0.0136(13) O11 0.0358(14) 0.0328(11) 0.0465(14) -0.0206(10) 0.0046(12) -0.0066(10) N1 0.0267(16) 0.0421(15) 0.0334(16) -0.0136(13) 0.0044(13) -0.0074(13) N2 0.0387(17) 0.0309(14) 0.0289(16) -0.0081(12) 0.0009(14) -0.0050(13) C1 0.033(2) 0.0367(18) 0.044(2) -0.0133(16) 0.0070(18) -0.0107(16) C2 0.037(2) 0.0280(16) 0.0257(18) -0.0062(14) 0.0016(16) -0.0078(15) C3 0.065(3) 0.0395(19) 0.030(2) -0.0124(16) 0.001(2) -0.0018(19) C4 0.051(2) 0.0249(17) 0.046(2) -0.0134(15) 0.0057(19) 0.0052(17) C5 0.0199(18) 0.0384(19) 0.036(2) -0.0080(16) 0.0021(16) 0.0011(15) C6 0.052(2) 0.0343(18) 0.0267(19) -0.0107(15) 0.0017(18) -0.0053(17) C7 0.045(2) 0.0274(16) 0.0317(19) -0.0130(14) -0.0007(17) -0.0045(16) C8 0.033(2) 0.0386(19) 0.028(2) -0.0053(16) -0.0043(17) -0.0024(16) C9 0.041(2) 0.0182(16) 0.035(2) 0.0010(15) 0.0023(18) -0.0008(16) C10 0.037(2) 0.0323(17) 0.0249(19) -0.0062(14) -0.0028(17) -0.0080(16) C11 0.0276(19) 0.0480(19) 0.0269(19) -0.0089(16) -0.0029(16) -0.0151(16) C12 0.031(2) 0.0379(18) 0.0249(18) -0.0075(15) -0.0010(16) -0.0057(16) C13 0.067(3) 0.0302(17) 0.038(2) -0.0166(15) 0.0215(19) -0.0094(18) C14 0.068(3) 0.0252(17) 0.053(2) -0.0116(16) 0.019(2) -0.0046(19) C15 0.035(2) 0.0325(18) 0.027(2) 0.0045(15) 0.0042(17) -0.0036(16) C16 0.050(2) 0.053(2) 0.031(2) -0.0188(16) 0.0070(19) -0.0063(19) C17 0.061(2) 0.0302(17) 0.038(2) -0.0153(15) 0.0044(19) -0.0164(17) C18 0.029(2) 0.043(2) 0.047(3) 0.0043(19) 0.001(2) -0.0062(18) C19 0.075(3) 0.038(2) 0.038(2) -0.0107(17) 0.015(2) -0.009(2) C20 0.100(3) 0.048(2) 0.035(2) -0.0039(19) 0.024(2) -0.011(2) C21 0.085(3) 0.064(3) 0.019(2) -0.0074(19) 0.007(2) 0.001(3) C22 0.088(3) 0.052(2) 0.030(2) -0.0149(17) 0.012(2) 0.001(2) C23 0.058(3) 0.042(2) 0.031(2) -0.0076(17) -0.002(2) -0.003(2) C25 0.044(5) 0.116(7) 0.013(4) -0.022(4) -0.014(4) 0.020(5) C24' 0.055(4) 0.061(4) 0.018(3) -0.015(3) 0.015(3) -0.045(3) C26 0.162(5) 0.053(3) 0.018(2) -0.0053(19) 0.008(3) -0.016(3) C27 0.136(4) 0.054(2) 0.032(2) -0.0278(17) 0.008(3) -0.017(3) C28 0.077(3) 0.0340(19) 0.039(2) -0.0115(17) 0.001(2) -0.006(2) C29 0.090(3) 0.0310(19) 0.035(2) -0.0094(17) -0.004(2) -0.001(2) C30 0.155(5) 0.041(2) 0.020(2) 0.0039(19) -0.010(3) -0.008(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 Zn1 O1 1.925(2) . ? Zn1 O6 1.949(3) . ? Zn1 O4 1.993(3) 2_676 ? Zn1 N1 2.018(3) . ? Zn2 O5 1.971(2) 1_546 ? Zn2 O11 2.008(2) . ? Zn2 O10 2.030(3) . ? Zn2 N2 2.030(3) 2_668 ? Zn2 O9 2.270(3) . ? Zn2 C18 2.481(4) . ? O1 C1 1.312(4) . ? O2 C1 1.239(5) . ? O3 C5 1.374(4) . ? O3 C8 1.417(4) . ? O4 C9 1.251(4) . ? O4 Zn1 1.993(3) 2_676 ? O5 C9 1.269(5) . ? O5 Zn2 1.971(2) 1_564 ? O6 C10 1.271(4) . ? O7 C10 1.237(4) . ? O8 C12 1.384(4) . ? O8 C11 1.418(4) . ? O9 C18 1.240(5) . ? O10 C18 1.272(5) . ? O11 H11C 0.8449 . ? O11 H11D 0.9533 . ? N1 C19 1.329(4) . ? N1 C23 1.331(5) . ? N2 C29 1.329(4) . ? N2 C28 1.344(5) . ? N2 Zn2 2.030(3) 2_668 ? C1 C2 1.471(5) . ? C2 C3 1.392(5) . ? C2 C7 1.397(5) . ? C3 C4 1.379(5) . ? C3 H3 0.9300 . ? C4 C5 1.391(5) . ? C4 H4 0.9300 . ? C5 C6 1.383(5) . ? C6 C7 1.378(4) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.505(5) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C10 C11 1.521(5) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.376(5) . ? C12 C17 1.379(5) . ? C13 C14 1.374(5) . ? C13 H13 0.9300 . ? C14 C15 1.378(5) . ? C14 H14 0.9300 . ? C15 C16 1.371(5) . ? C15 C18 1.503(5) . ? C16 C17 1.381(5) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C19 C20 1.359(5) . ? C19 H19 0.9300 . ? C20 C21 1.366(6) . ? C20 H20 0.9300 . ? C21 C22 1.388(5) . ? C21 C24' 1.519(5) . ? C21 C24 1.524(6) . ? C22 C23 1.387(5) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 C25 1.486(7) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.528(6) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C24' C25' 1.485(7) . ? C24' H24C 0.9700 . ? C24' H24D 0.9700 . ? C25' C26 1.521(6) . ? C25' H25C 0.9700 . ? C25' H25D 0.9700 . ? C26 C30 1.371(6) . ? C26 C27 1.389(5) . ? C27 C28 1.376(5) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? C29 C30 1.355(6) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn1 O6 117.05(10) . . ? O1 Zn1 O4 96.37(10) . 2_676 ? O6 Zn1 O4 117.90(11) . 2_676 ? O1 Zn1 N1 127.64(11) . . ? O6 Zn1 N1 98.07(11) . . ? O4 Zn1 N1 99.94(11) 2_676 . ? O5 Zn2 O11 105.82(10) 1_546 . ? O5 Zn2 O10 110.60(10) 1_546 . ? O11 Zn2 O10 97.11(10) . . ? O5 Zn2 N2 99.67(11) 1_546 2_668 ? O11 Zn2 N2 94.45(10) . 2_668 ? O10 Zn2 N2 143.02(12) . 2_668 ? O5 Zn2 O9 98.16(10) 1_546 . ? O11 Zn2 O9 152.14(10) . . ? O10 Zn2 O9 60.59(11) . . ? N2 Zn2 O9 95.30(11) 2_668 . ? O5 Zn2 C18 106.23(10) 1_546 . ? O11 Zn2 C18 126.23(12) . . ? O10 Zn2 C18 30.74(13) . . ? N2 Zn2 C18 120.87(14) 2_668 . ? O9 Zn2 C18 29.85(12) . . ? C1 O1 Zn1 111.7(2) . . ? C5 O3 C8 117.2(3) . . ? C9 O4 Zn1 135.9(2) . 2_676 ? C9 O5 Zn2 130.0(2) . 1_564 ? C10 O6 Zn1 125.8(3) . . ? C12 O8 C11 117.8(3) . . ? C18 O9 Zn2 84.5(2) . . ? C18 O10 Zn2 94.6(2) . . ? Zn2 O11 H11C 123.7 . . ? Zn2 O11 H11D 121.1 . . ? H11C O11 H11D 109.8 . . ? C19 N1 C23 116.5(3) . . ? C19 N1 Zn1 123.0(3) . . ? C23 N1 Zn1 119.4(2) . . ? C29 N2 C28 115.0(3) . . ? C29 N2 Zn2 122.5(3) . 2_668 ? C28 N2 Zn2 122.2(2) . 2_668 ? O2 C1 O1 119.9(3) . . ? O2 C1 C2 123.1(3) . . ? O1 C1 C2 117.0(3) . . ? C3 C2 C7 117.9(3) . . ? C3 C2 C1 120.8(3) . . ? C7 C2 C1 121.3(3) . . ? C4 C3 C2 120.9(4) . . ? C4 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? C3 C4 C5 120.3(3) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? O3 C5 C6 125.2(3) . . ? O3 C5 C4 115.4(3) . . ? C6 C5 C4 119.5(3) . . ? C7 C6 C5 119.9(4) . . ? C7 C6 H6 120.1 . . ? C5 C6 H6 120.1 . . ? C6 C7 C2 121.5(3) . . ? C6 C7 H7 119.3 . . ? C2 C7 H7 119.3 . . ? O3 C8 C9 115.7(3) . . ? O3 C8 H8A 108.4 . . ? C9 C8 H8A 108.4 . . ? O3 C8 H8B 108.4 . . ? C9 C8 H8B 108.4 . . ? H8A C8 H8B 107.4 . . ? O4 C9 O5 125.0(3) . . ? O4 C9 C8 117.8(4) . . ? O5 C9 C8 117.1(3) . . ? O7 C10 O6 125.0(4) . . ? O7 C10 C11 118.2(3) . . ? O6 C10 C11 116.7(3) . . ? O8 C11 C10 114.3(3) . . ? O8 C11 H11A 108.7 . . ? C10 C11 H11A 108.7 . . ? O8 C11 H11B 108.7 . . ? C10 C11 H11B 108.7 . . ? H11A C11 H11B 107.6 . . ? C13 C12 C17 121.3(3) . . ? C13 C12 O8 124.8(3) . . ? C17 C12 O8 114.0(3) . . ? C14 C13 C12 118.1(4) . . ? C14 C13 H13 121.0 . . ? C12 C13 H13 121.0 . . ? C13 C14 C15 122.3(4) . . ? C13 C14 H14 118.9 . . ? C15 C14 H14 118.9 . . ? C16 C15 C14 118.3(3) . . ? C16 C15 C18 120.6(4) . . ? C14 C15 C18 121.1(4) . . ? C15 C16 C17 121.1(4) . . ? C15 C16 H16 119.5 . . ? C17 C16 H16 119.5 . . ? C12 C17 C16 119.0(3) . . ? C12 C17 H17 120.5 . . ? C16 C17 H17 120.5 . . ? O9 C18 O10 120.3(3) . . ? O9 C18 C15 121.4(4) . . ? O10 C18 C15 118.3(4) . . ? O9 C18 Zn2 65.6(2) . . ? O10 C18 Zn2 54.64(18) . . ? C15 C18 Zn2 172.7(3) . . ? N1 C19 C20 124.4(4) . . ? N1 C19 H19 117.8 . . ? C20 C19 H19 117.8 . . ? C19 C20 C21 120.2(4) . . ? C19 C20 H20 119.9 . . ? C21 C20 H20 119.9 . . ? C20 C21 C22 116.3(3) . . ? C20 C21 C24' 117.0(4) . . ? C22 C21 C24' 125.5(4) . . ? C20 C21 C24 123.2(4) . . ? C22 C21 C24 117.0(5) . . ? C23 C22 C21 120.3(4) . . ? C23 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? N1 C23 C22 122.3(3) . . ? N1 C23 H23 118.9 . . ? C22 C23 H23 118.9 . . ? C25 C24 C21 112.8(4) . . ? C25 C24 H24A 109.0 . . ? C21 C24 H24A 109.0 . . ? C25 C24 H24B 109.0 . . ? C21 C24 H24B 109.0 . . ? H24A C24 H24B 107.8 . . ? C24 C25 C26 107.3(4) . . ? C24 C25 H25A 110.3 . . ? C26 C25 H25A 110.3 . . ? C24 C25 H25B 110.3 . . ? C26 C25 H25B 110.3 . . ? H25A C25 H25B 108.5 . . ? C25' C24' C21 108.7(4) . . ? C25' C24' H24C 109.9 . . ? C21 C24' H24C 109.9 . . ? C25' C24' H24D 109.9 . . ? C21 C24' H24D 109.9 . . ? H24C C24' H24D 108.3 . . ? C24' C25' C26 112.3(5) . . ? C24' C25' H25C 109.1 . . ? C26 C25' H25C 109.1 . . ? C24' C25' H25D 109.1 . . ? C26 C25' H25D 109.1 . . ? H25C C25' H25D 107.9 . . ? C30 C26 C27 115.4(3) . . ? C30 C26 C25' 118.6(4) . . ? C27 C26 C25' 121.1(4) . . ? C30 C26 C25 120.0(4) . . ? C27 C26 C25 122.3(5) . . ? C28 C27 C26 120.5(4) . . ? C28 C27 H27 119.7 . . ? C26 C27 H27 119.7 . . ? N2 C28 C27 123.3(3) . . ? N2 C28 H28 118.4 . . ? C27 C28 H28 118.4 . . ? N2 C29 C30 124.9(4) . . ? N2 C29 H29 117.6 . . ? C30 C29 H29 117.6 . . ? C29 C30 C26 120.9(4) . . ? C29 C30 H30 119.6 . . ? C26 C30 H30 119.6 . . ? 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 O6 Zn1 O1 C1 -63.4(2) . . . . ? O4 Zn1 O1 C1 170.7(2) 2_676 . . . ? N1 Zn1 O1 C1 62.9(3) . . . . ? O1 Zn1 O6 C10 -69.9(3) . . . . ? O4 Zn1 O6 C10 44.4(3) 2_676 . . . ? N1 Zn1 O6 C10 150.2(2) . . . . ? O5 Zn2 O9 C18 -108.5(2) 1_546 . . . ? O11 Zn2 O9 C18 40.9(3) . . . . ? O10 Zn2 O9 C18 0.6(2) . . . . ? N2 Zn2 O9 C18 150.9(2) 2_668 . . . ? O5 Zn2 O10 C18 87.3(2) 1_546 . . . ? O11 Zn2 O10 C18 -162.8(2) . . . . ? N2 Zn2 O10 C18 -55.6(3) 2_668 . . . ? O9 Zn2 O10 C18 -0.6(2) . . . . ? O1 Zn1 N1 C19 119.8(3) . . . . ? O6 Zn1 N1 C19 -106.6(3) . . . . ? O4 Zn1 N1 C19 13.7(3) 2_676 . . . ? O1 Zn1 N1 C23 -72.0(3) . . . . ? O6 Zn1 N1 C23 61.6(3) . . . . ? O4 Zn1 N1 C23 -178.1(3) 2_676 . . . ? Zn1 O1 C1 O2 -9.1(4) . . . . ? Zn1 O1 C1 C2 169.9(2) . . . . ? O2 C1 C2 C3 -3.4(6) . . . . ? O1 C1 C2 C3 177.6(3) . . . . ? O2 C1 C2 C7 175.1(4) . . . . ? O1 C1 C2 C7 -3.9(5) . . . . ? C7 C2 C3 C4 0.0(6) . . . . ? C1 C2 C3 C4 178.5(4) . . . . ? C2 C3 C4 C5 -3.3(6) . . . . ? C8 O3 C5 C6 -14.2(5) . . . . ? C8 O3 C5 C4 167.0(3) . . . . ? C3 C4 C5 O3 -176.4(3) . . . . ? C3 C4 C5 C6 4.7(6) . . . . ? O3 C5 C6 C7 178.3(3) . . . . ? C4 C5 C6 C7 -2.9(6) . . . . ? C5 C6 C7 C2 -0.5(6) . . . . ? C3 C2 C7 C6 1.9(6) . . . . ? C1 C2 C7 C6 -176.7(4) . . . . ? C5 O3 C8 C9 -62.3(4) . . . . ? Zn1 O4 C9 O5 107.7(4) 2_676 . . . ? Zn1 O4 C9 C8 -74.2(4) 2_676 . . . ? Zn2 O5 C9 O4 -9.4(4) 1_564 . . . ? Zn2 O5 C9 C8 172.47(19) 1_564 . . . ? O3 C8 C9 O4 167.8(3) . . . . ? O3 C8 C9 O5 -13.9(4) . . . . ? Zn1 O6 C10 O7 19.4(4) . . . . ? Zn1 O6 C10 C11 -161.5(2) . . . . ? C12 O8 C11 C10 66.9(4) . . . . ? O7 C10 C11 O8 -177.5(3) . . . . ? O6 C10 C11 O8 3.4(4) . . . . ? C11 O8 C12 C13 11.1(5) . . . . ? C11 O8 C12 C17 -168.6(3) . . . . ? C17 C12 C13 C14 -0.2(6) . . . . ? O8 C12 C13 C14 -180.0(3) . . . . ? C12 C13 C14 C15 1.6(6) . . . . ? C13 C14 C15 C16 -2.3(6) . . . . ? C13 C14 C15 C18 178.6(4) . . . . ? C14 C15 C16 C17 1.6(6) . . . . ? C18 C15 C16 C17 -179.2(4) . . . . ? C13 C12 C17 C16 -0.4(6) . . . . ? O8 C12 C17 C16 179.3(3) . . . . ? C15 C16 C17 C12 -0.3(6) . . . . ? Zn2 O9 C18 O10 -1.0(4) . . . . ? Zn2 O9 C18 C15 178.1(3) . . . . ? Zn2 O10 C18 O9 1.1(4) . . . . ? Zn2 O10 C18 C15 -178.0(3) . . . . ? C16 C15 C18 O9 1.2(6) . . . . ? C14 C15 C18 O9 -179.7(4) . . . . ? C16 C15 C18 O10 -179.7(4) . . . . ? C14 C15 C18 O10 -0.6(6) . . . . ? O5 Zn2 C18 O9 77.9(2) 1_546 . . . ? O11 Zn2 C18 O9 -157.7(2) . . . . ? O10 Zn2 C18 O9 -179.0(4) . . . . ? N2 Zn2 C18 O9 -34.3(3) 2_668 . . . ? O5 Zn2 C18 O10 -103.2(2) 1_546 . . . ? O11 Zn2 C18 O10 21.3(3) . . . . ? N2 Zn2 C18 O10 144.7(2) 2_668 . . . ? O9 Zn2 C18 O10 179.0(4) . . . . ? C23 N1 C19 C20 -1.2(6) . . . . ? Zn1 N1 C19 C20 167.3(4) . . . . ? N1 C19 C20 C21 0.5(7) . . . . ? C19 C20 C21 C22 0.8(7) . . . . ? C19 C20 C21 C24' 169.2(5) . . . . ? C19 C20 C21 C24 -157.4(5) . . . . ? C20 C21 C22 C23 -1.3(7) . . . . ? C24' C21 C22 C23 -168.6(5) . . . . ? C24 C21 C22 C23 158.3(5) . . . . ? C19 N1 C23 C22 0.6(6) . . . . ? Zn1 N1 C23 C22 -168.3(3) . . . . ? C21 C22 C23 N1 0.6(7) . . . . ? C20 C21 C24 C25 -135.9(6) . . . . ? C22 C21 C24 C25 66.1(8) . . . . ? C24' C21 C24 C25 -49.0(7) . . . . ? C21 C24 C25 C26 -176.1(6) . . . . ? C20 C21 C24' C25' 147.1(5) . . . . ? C22 C21 C24' C25' -45.6(7) . . . . ? C24 C21 C24' C25' 36.9(7) . . . . ? C21 C24' C25' C26 175.6(5) . . . . ? C24' C25' C26 C30 -148.3(6) . . . . ? C24' C25' C26 C27 57.5(8) . . . . ? C24' C25' C26 C25 -45.8(7) . . . . ? C24 C25 C26 C30 134.4(7) . . . . ? C24 C25 C26 C27 -63.9(8) . . . . ? C24 C25 C26 C25' 35.9(6) . . . . ? C30 C26 C27 C28 -1.3(8) . . . . ? C25' C26 C27 C28 153.6(6) . . . . ? C25 C26 C27 C28 -163.8(5) . . . . ? C29 N2 C28 C27 2.4(6) . . . . ? Zn2 N2 C28 C27 -171.5(4) 2_668 . . . ? C26 C27 C28 N2 -0.7(8) . . . . ? C28 N2 C29 C30 -2.2(7) . . . . ? Zn2 N2 C29 C30 171.7(4) 2_668 . . . ? N2 C29 C30 C26 0.2(9) . . . . ? C27 C26 C30 C29 1.6(8) . . . . ? C25' C26 C30 C29 -154.1(6) . . . . ? C25 C26 C30 C29 164.5(5) . . . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.955 _refine_diff_density_min -1.233 _refine_diff_density_rms 0.119 #===END data_complex8 _database_code_depnum_ccdc_archive 'CCDC 637139' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16.5 H16 N O5.5 Zn' _chemical_formula_sum 'C16.5 H16 N O5.5 Zn' _chemical_formula_weight 381.67 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 30.931(8) _cell_length_b 9.8752(13) _cell_length_c 20.370(3) _cell_angle_alpha 90.00 _cell_angle_beta 149.310(6) _cell_angle_gamma 90.00 _cell_volume 3175.8(10) _cell_formula_units_Z 8 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 3884 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 27.9 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.597 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1568 _exptl_absorpt_coefficient_mu 1.576 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8334 _exptl_absorpt_correction_T_max 0.8843 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11950 _diffrn_reflns_av_R_equivalents 0.0291 _diffrn_reflns_av_sigmaI/netI 0.0298 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 40 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 27.87 _reflns_number_total 3770 _reflns_number_gt 3184 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.7.0' _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^)+(0.0730P)^2^+3.0279P] 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_number_reflns 3770 _refine_ls_number_parameters 236 _refine_ls_number_restraints 54 _refine_ls_R_factor_all 0.0549 _refine_ls_R_factor_gt 0.0464 _refine_ls_wR_factor_ref 0.1296 _refine_ls_wR_factor_gt 0.1222 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.117 _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 Zn1 Zn 0.53101(2) 0.47976(3) 0.47152(3) 0.03187(14) Uani 1 1 d . . . O4 O 0.58129(16) -0.3330(2) 0.5452(2) 0.0474(6) Uani 1 1 d . . . O2 O 0.58207(15) 0.4325(3) 0.7044(2) 0.0471(5) Uani 1 1 d . . . O3 O 0.74306(14) 0.2262(2) 0.8477(2) 0.0434(5) Uani 1 1 d . . . O1 O 0.62654(16) 0.4122(3) 0.6589(2) 0.0495(6) Uani 1 1 d . . . O5 O 0.53346(18) -0.3120(2) 0.5850(3) 0.0570(7) Uani 1 1 d . . . N1 N 0.58529(16) 0.3991(3) 0.4607(2) 0.0342(5) Uani 1 1 d . . . C4 C 0.7198(2) 0.0297(3) 0.7555(3) 0.0362(6) Uani 1 1 d . . . H4 H 0.7641 0.0564 0.7861 0.043 Uiso 1 1 calc R . . C9 C 0.57281(19) -0.2691(3) 0.5871(3) 0.0368(6) Uani 1 1 d . . . C1 C 0.63300(19) 0.3939(3) 0.7271(3) 0.0351(6) Uani 1 1 d . . . C5 C 0.67892(19) -0.0913(3) 0.6910(3) 0.0368(6) Uani 1 1 d . . . H5 H 0.6949 -0.1454 0.6766 0.044 Uiso 1 1 calc R . . C3 C 0.69469(18) 0.1125(3) 0.7748(3) 0.0354(6) Uani 1 1 d . . . C10 C 0.6195(3) 0.2763(3) 0.5090(4) 0.0500(8) Uani 1 1 d . . . H10 H 0.6137 0.2277 0.5402 0.060 Uiso 1 1 calc R . . C8 C 0.6271(2) 0.0753(3) 0.7256(3) 0.0426(7) Uani 1 1 d . . . H8 H 0.6080 0.1327 0.7336 0.051 Uiso 1 1 calc R . . C6 C 0.61352(19) -0.1332(3) 0.6471(3) 0.0345(6) Uani 1 1 d . . . C7 C 0.5881(2) -0.0484(3) 0.6640(4) 0.0434(7) Uani 1 1 d . . . H7 H 0.5438 -0.0750 0.6335 0.052 Uiso 1 1 calc R . . C2 C 0.7119(2) 0.3213(3) 0.8536(3) 0.0416(7) Uani 1 1 d . . . H2A H 0.7557 0.3876 0.9198 0.050 Uiso 1 1 calc R . . H2B H 0.6993 0.2744 0.8778 0.050 Uiso 1 1 calc R . . C14 C 0.5944(3) 0.4682(4) 0.4166(4) 0.0520(9) Uani 1 1 d . . . H14 H 0.5728 0.5556 0.3858 0.062 Uiso 1 1 calc R . . C15 C 0.7120(4) 0.2224(6) 0.4592(7) 0.107(2) Uani 1 1 d . . . H15A H 0.7206 0.1267 0.4790 0.128 Uiso 1 1 calc R . . H15B H 0.6736 0.2296 0.3721 0.128 Uiso 1 1 calc R . . C11 C 0.6632(3) 0.2179(4) 0.5150(5) 0.0654(11) Uani 1 1 d . . . H11 H 0.6889 0.1340 0.5541 0.078 Uiso 1 1 calc R . . C12 C 0.6687(3) 0.2845(5) 0.4625(5) 0.0646(11) Uani 1 1 d . . . C13 C 0.6349(3) 0.4132(5) 0.4155(5) 0.0696(12) Uani 1 1 d . . . H13 H 0.6394 0.4633 0.3828 0.084 Uiso 1 1 calc R . . O6 O 0.4511(6) 0.8876(11) 0.1310(10) 0.134(3) Uani 0.50 1 d PDU . . H6A H 0.4733 0.9290 0.1278 0.201 Uiso 0.50 1 d PR . . C16 C 0.4749(11) 0.807(2) 0.2704(18) 0.198(6) Uani 0.50 1 d PDU . . H16A H 0.4375 0.8705 0.2426 0.297 Uiso 0.50 1 d PR . . H16B H 0.4423 0.7358 0.2083 0.297 Uiso 0.50 1 d PR . . H16C H 0.5130 0.7699 0.3521 0.297 Uiso 0.50 1 d PR . . C18 C 0.5729(7) 0.7477(11) 0.3090(12) 0.098(3) Uani 0.50 1 d PDU . . H18A H 0.6069 0.7870 0.3193 0.147 Uiso 0.50 1 d PR . . H18B H 0.6090 0.7109 0.3897 0.147 Uiso 0.50 1 d PR . . H18C H 0.5384 0.6769 0.2459 0.147 Uiso 0.50 1 d PR . . C17 C 0.5210(8) 0.8640(13) 0.2680(13) 0.159(5) Uani 0.50 1 d PDU . . H17A H 0.5512 0.9421 0.3228 0.191 Uiso 0.50 1 d PRU . . 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 Zn1 0.0412(2) 0.0281(2) 0.0495(2) -0.00250(13) 0.0425(2) -0.00042(12) O4 0.0611(15) 0.0311(11) 0.0684(15) -0.0095(11) 0.0584(15) -0.0074(10) O2 0.0471(13) 0.0559(14) 0.0494(13) 0.0035(11) 0.0432(12) 0.0077(11) O3 0.0378(12) 0.0298(11) 0.0541(13) -0.0067(9) 0.0382(12) -0.0035(9) O1 0.0606(15) 0.0528(15) 0.0561(14) 0.0127(11) 0.0534(14) 0.0155(12) O5 0.0716(17) 0.0333(12) 0.102(2) -0.0142(13) 0.0800(18) -0.0149(11) N1 0.0376(13) 0.0361(13) 0.0441(13) -0.0010(10) 0.0374(12) 0.0017(10) C4 0.0330(15) 0.0318(15) 0.0467(17) 0.0008(12) 0.0347(15) 0.0001(11) C9 0.0352(15) 0.0276(14) 0.0461(16) 0.0006(12) 0.0347(15) 0.0008(11) C1 0.0401(15) 0.0281(14) 0.0403(15) -0.0061(11) 0.0351(14) -0.0036(11) C5 0.0394(16) 0.0315(15) 0.0492(17) 0.0012(12) 0.0395(16) 0.0023(12) C3 0.0332(14) 0.0252(13) 0.0405(15) 0.0010(11) 0.0306(14) 0.0002(11) C10 0.071(2) 0.0332(16) 0.085(3) 0.0049(16) 0.073(2) 0.0076(15) C8 0.0500(18) 0.0316(15) 0.064(2) -0.0069(14) 0.0515(18) -0.0033(13) C6 0.0355(15) 0.0280(14) 0.0446(15) 0.0011(11) 0.0351(14) 0.0008(11) C7 0.0466(18) 0.0376(17) 0.064(2) -0.0077(15) 0.0505(19) -0.0067(13) C2 0.0432(17) 0.0325(15) 0.0423(16) -0.0040(12) 0.0357(16) -0.0011(13) C14 0.060(2) 0.068(2) 0.066(2) 0.0208(18) 0.060(2) 0.0204(18) C15 0.122(5) 0.096(4) 0.185(6) -0.042(4) 0.144(5) -0.021(3) C11 0.083(3) 0.042(2) 0.111(4) 0.005(2) 0.089(3) 0.0110(19) C12 0.072(3) 0.066(3) 0.100(3) -0.015(2) 0.081(3) -0.004(2) C13 0.087(3) 0.089(3) 0.094(3) 0.018(3) 0.087(3) 0.018(3) O6 0.133(5) 0.154(6) 0.147(5) 0.018(5) 0.126(5) 0.014(5) C16 0.175(8) 0.201(9) 0.203(8) -0.007(7) 0.160(6) 0.015(6) C18 0.126(5) 0.109(6) 0.130(5) 0.027(5) 0.121(5) 0.019(5) C17 0.160(5) 0.164(5) 0.169(5) -0.007(5) 0.144(4) 0.028(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 Zn1 O4 2.019(2) 1_565 ? Zn1 O5 2.024(2) 5_656 ? Zn1 N1 2.036(6) . ? Zn1 O2 2.066(2) 5_666 ? Zn1 O1 2.084(2) . ? Zn1 Zn1 3.0020(8) 5_666 ? O4 C9 1.258(4) . ? O4 Zn1 2.019(2) 1_545 ? O2 C1 1.260(9) . ? O2 Zn1 2.066(2) 5_666 ? O3 C3 1.373(4) . ? O3 C2 1.422(4) . ? O1 C1 1.236(4) . ? O5 C9 1.254(10) . ? O5 Zn1 2.024(2) 5_656 ? N1 C10 1.329(4) . ? N1 C14 1.337(11) . ? C4 C5 1.377(4) . ? C4 C3 1.397(9) . ? C4 H4 0.9300 . ? C9 C6 1.495(4) . ? C1 C2 1.514(4) . ? C5 C6 1.397(10) . ? C5 H5 0.9300 . ? C3 C8 1.381(10) . ? C10 C11 1.375(16) . ? C10 H10 0.9300 . ? C8 C7 1.386(4) . ? C8 H8 0.9300 . ? C6 C7 1.380(10) . ? C7 H7 0.9300 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C14 C13 1.383(16) . ? C14 H14 0.9300 . ? C15 C15 1.368(10) 7_656 ? C15 C12 1.53(2) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C11 C12 1.385(15) . ? C11 H11 0.9300 . ? C12 C13 1.379(6) . ? C13 H13 0.9300 . ? O6 C17 1.406(19) 2_655 ? O6 C16 1.41(2) 2_655 ? O6 C17 1.463(10) . ? O6 H6A 0.8501 . ? C16 C18 1.02(2) 2_655 ? C16 C17 1.054(19) 2_655 ? C16 O6 1.41(2) 2_655 ? C16 C17 1.571(10) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C18 C16 1.02(2) 2_655 ? C18 C17 1.511(9) . ? C18 H18A 0.9597 . ? C18 H18B 0.9601 . ? C18 H18C 0.9600 . ? C17 C17 0.77(3) 2_655 ? C17 C16 1.054(19) 2_655 ? C17 O6 1.406(19) 2_655 ? C17 H17A 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Zn1 O5 157.63(10) 1_565 5_656 ? O4 Zn1 N1 105.00(10) 1_565 . ? O5 Zn1 N1 96.86(10) 5_656 . ? O4 Zn1 O2 88.74(10) 1_565 5_666 ? O5 Zn1 O2 89.23(12) 5_656 5_666 ? N1 Zn1 O2 107.46(10) . 5_666 ? O4 Zn1 O1 87.67(10) 1_565 . ? O5 Zn1 O1 86.07(12) 5_656 . ? N1 Zn1 O1 94.04(10) . . ? O2 Zn1 O1 158.41(9) 5_666 . ? O4 Zn1 Zn1 86.05(7) 1_565 5_666 ? O5 Zn1 Zn1 71.58(7) 5_656 5_666 ? N1 Zn1 Zn1 162.78(7) . 5_666 ? O2 Zn1 Zn1 85.61(7) 5_666 5_666 ? O1 Zn1 Zn1 72.91(7) . 5_666 ? C9 O4 Zn1 119.1(2) . 1_545 ? C1 O2 Zn1 118.7(2) . 5_666 ? C3 O3 C2 116.4(5) . . ? C1 O1 Zn1 135.2(2) . . ? C9 O5 Zn1 138.5(2) . 5_656 ? C10 N1 C14 118.0(7) . . ? C10 N1 Zn1 118.9(6) . . ? C14 N1 Zn1 122.9(2) . . ? C5 C4 C3 120.0(7) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? O5 C9 O4 124.8(3) . . ? O5 C9 C6 116.2(3) . . ? O4 C9 C6 119.0(3) . . ? O1 C1 O2 126.9(3) . . ? O1 C1 C2 116.6(3) . . ? O2 C1 C2 116.4(3) . . ? C4 C5 C6 120.3(3) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? O3 C3 C8 124.3(3) . . ? O3 C3 C4 115.5(3) . . ? C8 C3 C4 120.1(3) . . ? N1 C10 C11 123.0(8) . . ? N1 C10 H10 118.5 . . ? C11 C10 H10 118.5 . . ? C3 C8 C7 119.3(3) . . ? C3 C8 H8 120.4 . . ? C7 C8 H8 120.4 . . ? C7 C6 C5 118.9(3) . . ? C7 C6 C9 119.2(3) . . ? C5 C6 C9 121.8(3) . . ? C6 C7 C8 121.5(7) . . ? C6 C7 H7 119.3 . . ? C8 C7 H7 119.3 . . ? O3 C2 C1 112.8(3) . . ? O3 C2 H2A 109.0 . . ? C1 C2 H2A 109.0 . . ? O3 C2 H2B 109.0 . . ? C1 C2 H2B 109.0 . . ? H2A C2 H2B 107.8 . . ? N1 C14 C13 121.9(4) . . ? N1 C14 H14 119.1 . . ? C13 C14 H14 119.1 . . ? C15 C15 C12 116.3(6) 7_656 . ? C15 C15 H15A 108.2 7_656 . ? C12 C15 H15A 108.2 . . ? C15 C15 H15B 108.2 7_656 . ? C12 C15 H15B 108.2 . . ? H15A C15 H15B 107.4 . . ? C10 C11 C12 119.8(4) . . ? C10 C11 H11 120.1 . . ? C12 C11 H11 120.1 . . ? C13 C12 C11 116.8(10) . . ? C13 C12 C15 120.6(9) . . ? C11 C12 C15 122.5(5) . . ? C12 C13 C14 120.5(9) . . ? C12 C13 H13 119.8 . . ? C14 C13 H13 119.8 . . ? C17 O6 C16 67.8(8) 2_655 2_655 ? C17 O6 H6A 132.3 2_655 . ? C16 O6 H6A 87.1 2_655 . ? C17 O6 H6A 104.9 . . ? C18 C16 C17 93.6(16) 2_655 2_655 ? C18 C16 O6 161.2(15) 2_655 2_655 ? C17 C16 O6 71.1(12) 2_655 2_655 ? C18 C16 C17 105.8(13) 2_655 . ? O6 C16 C17 55.9(9) 2_655 . ? C18 C16 H16A 94.2 2_655 . ? C17 C16 H16A 94.0 2_655 . ? O6 C16 H16A 97.6 2_655 . ? C17 C16 H16A 114.6 . . ? C17 C16 H16B 94.1 2_655 . ? O6 C16 H16B 150.2 2_655 . ? C17 C16 H16B 100.0 . . ? H16A C16 H16B 109.5 . . ? C18 C16 H16C 118.2 2_655 . ? C17 C16 H16C 137.7 2_655 . ? O6 C16 H16C 71.3 2_655 . ? C17 C16 H16C 113.4 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C16 C18 H18A 86.2 2_655 . ? C17 C18 H18A 104.9 . . ? C16 C18 H18B 154.4 2_655 . ? C17 C18 H18B 110.8 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 82.5 2_655 . ? C17 C18 H18C 112.6 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C17 C16 118(2) 2_655 2_655 ? C17 C17 O6 78.7(18) 2_655 2_655 ? C16 C17 O6 149.3(17) 2_655 2_655 ? C17 C17 O6 70.4(18) 2_655 . ? C16 C17 O6 66.0(13) 2_655 . ? O6 C17 O6 143.6(11) 2_655 . ? C17 C17 C18 130.5(7) 2_655 . ? O6 C17 C18 107.1(11) 2_655 . ? O6 C17 C18 107.5(8) . . ? C16 C17 C16 121.7(19) 2_655 . ? O6 C17 C16 56.3(10) 2_655 . ? O6 C17 C16 102.9(8) . . ? C18 C17 C16 105.8(8) . . ? C17 C17 H17A 105.4 2_655 . ? C16 C17 H17A 132.4 2_655 . ? O6 C17 H17A 53.5 2_655 . ? O6 C17 H17A 117.0 . . ? C18 C17 H17A 117.4 . . ? C16 C17 H17A 104.5 . . ? 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 O4 Zn1 O1 C1 94.2(3) 1_565 . . . ? O5 Zn1 O1 C1 -64.3(3) 5_656 . . . ? N1 Zn1 O1 C1 -160.9(3) . . . . ? O2 Zn1 O1 C1 13.6(5) 5_666 . . . ? Zn1 Zn1 O1 C1 7.6(3) 5_666 . . . ? O4 Zn1 N1 C10 130.2(3) 1_565 . . . ? O5 Zn1 N1 C10 -45.0(3) 5_656 . . . ? O2 Zn1 N1 C10 -136.3(3) 5_666 . . . ? O1 Zn1 N1 C10 41.5(3) . . . . ? Zn1 Zn1 N1 C10 1.6(5) 5_666 . . . ? O4 Zn1 N1 C14 -44.2(3) 1_565 . . . ? O5 Zn1 N1 C14 140.7(3) 5_656 . . . ? O2 Zn1 N1 C14 49.3(3) 5_666 . . . ? O1 Zn1 N1 C14 -132.8(3) . . . . ? Zn1 Zn1 N1 C14 -172.7(2) 5_666 . . . ? Zn1 O5 C9 O4 1.1(6) 5_656 . . . ? Zn1 O5 C9 C6 -177.5(3) 5_656 . . . ? Zn1 O4 C9 O5 -1.4(4) 1_545 . . . ? Zn1 O4 C9 C6 177.2(2) 1_545 . . . ? Zn1 O1 C1 O2 -11.6(5) . . . . ? Zn1 O1 C1 C2 170.6(2) . . . . ? Zn1 O2 C1 O1 6.4(5) 5_666 . . . ? Zn1 O2 C1 C2 -175.7(2) 5_666 . . . ? C3 C4 C5 C6 -1.4(5) . . . . ? C2 O3 C3 C8 -10.8(4) . . . . ? C2 O3 C3 C4 171.4(3) . . . . ? C5 C4 C3 O3 175.6(3) . . . . ? C5 C4 C3 C8 -2.2(5) . . . . ? C14 N1 C10 C11 -0.3(6) . . . . ? Zn1 N1 C10 C11 -174.9(3) . . . . ? O3 C3 C8 C7 -173.6(3) . . . . ? C4 C3 C8 C7 4.0(5) . . . . ? C4 C5 C6 C7 3.1(5) . . . . ? C4 C5 C6 C9 -174.5(3) . . . . ? O5 C9 C6 C7 -17.3(4) . . . . ? O4 C9 C6 C7 164.0(3) . . . . ? O5 C9 C6 C5 160.3(3) . . . . ? O4 C9 C6 C5 -18.4(5) . . . . ? C5 C6 C7 C8 -1.3(5) . . . . ? C9 C6 C7 C8 176.4(3) . . . . ? C3 C8 C7 C6 -2.2(5) . . . . ? C3 O3 C2 C1 -69.6(3) . . . . ? O1 C1 C2 O3 -31.2(4) . . . . ? O2 C1 C2 O3 150.7(3) . . . . ? C10 N1 C14 C13 2.7(6) . . . . ? Zn1 N1 C14 C13 177.1(3) . . . . ? N1 C10 C11 C12 -3.7(7) . . . . ? C10 C11 C12 C13 5.1(7) . . . . ? C10 C11 C12 C15 -176.6(4) . . . . ? C15 C15 C12 C13 69.9(11) 7_656 . . . ? C15 C15 C12 C11 -108.4(9) 7_656 . . . ? C11 C12 C13 C14 -2.8(7) . . . . ? C15 C12 C13 C14 178.8(5) . . . . ? N1 C14 C13 C12 -1.1(7) . . . . ? C16 O6 C17 C17 -135.4(13) 2_655 . . 2_655 ? C17 O6 C17 C16 135.4(13) 2_655 . . 2_655 ? C17 O6 C17 O6 -33(2) 2_655 . . 2_655 ? C16 O6 C17 O6 -169(3) 2_655 . . 2_655 ? C17 O6 C17 C18 127.6(8) 2_655 . . . ? C16 O6 C17 C18 -7.8(13) 2_655 . . . ? C17 O6 C17 C16 16.1(10) 2_655 . . . ? C16 O6 C17 C16 -119.2(19) 2_655 . . . ? C16 C18 C17 C17 89(4) 2_655 . . 2_655 ? C16 C18 C17 O6 179(2) 2_655 . . 2_655 ? C16 C18 C17 O6 10.6(17) 2_655 . . . ? C16 C18 C17 C16 120(2) 2_655 . . . ? C18 C16 C17 C17 64(2) 2_655 . . 2_655 ? O6 C16 C17 C17 -120.7(18) 2_655 . . 2_655 ? C18 C16 C17 C16 -32(2) 2_655 . . 2_655 ? C17 C16 C17 C16 -96(3) 2_655 . . 2_655 ? O6 C16 C17 C16 143.4(19) 2_655 . . 2_655 ? C18 C16 C17 O6 -176(2) 2_655 . . 2_655 ? C17 C16 C17 O6 120.7(18) 2_655 . . 2_655 ? C18 C16 C17 O6 37.4(19) 2_655 . . . ? C17 C16 C17 O6 -26(2) 2_655 . . . ? O6 C16 C17 O6 -147.1(13) 2_655 . . . ? C18 C16 C17 C18 -75.3(19) 2_655 . . . ? C17 C16 C17 C18 -139(2) 2_655 . . . ? O6 C16 C17 C18 100.2(13) 2_655 . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.87 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.537 _refine_diff_density_min -0.687 _refine_diff_density_rms 0.082 #===END data_complex9 _database_code_depnum_ccdc_archive 'CCDC 637140' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16.50 H16 N O5.50 Zn' _chemical_formula_weight 381.67 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.595(4) _cell_length_b 15.012(3) _cell_length_c 10.363(2) _cell_angle_alpha 90.00 _cell_angle_beta 93.967(4) _cell_angle_gamma 90.00 _cell_volume 3196.1(12) _cell_formula_units_Z 8 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 1456 _cell_measurement_theta_min 2.54 _cell_measurement_theta_max 21.95 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.586 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1568 _exptl_absorpt_coefficient_mu 1.566 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.683349 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 8858 _diffrn_reflns_av_R_equivalents 0.0741 _diffrn_reflns_av_sigmaI/netI 0.0973 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 26.41 _reflns_number_total 3253 _reflns_number_gt 1909 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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^)+(0.0330P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3253 _refine_ls_number_parameters 235 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.1035 _refine_ls_R_factor_gt 0.0432 _refine_ls_wR_factor_ref 0.0948 _refine_ls_wR_factor_gt 0.0763 _refine_ls_goodness_of_fit_ref 0.970 _refine_ls_restrained_S_all 0.972 _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 Zn1 Zn 0.30090(2) 0.27905(3) 0.10029(4) 0.02887(16) Uani 1 1 d . . . O1 O 0.32800(14) 0.15064(17) 0.0961(3) 0.0435(8) Uani 1 1 d . . . O2 O 0.24802(14) 0.10835(18) -0.0482(3) 0.0414(8) Uani 1 1 d . . . O3 O 0.35698(15) -0.27019(18) 0.1127(3) 0.0450(8) Uani 1 1 d . . . O4 O 0.36256(14) -0.30460(19) 0.4551(3) 0.0453(8) Uani 1 1 d . . . O5 O 0.28106(14) -0.26464(18) 0.3122(3) 0.0437(8) Uani 1 1 d . . . N1 N 0.35339(15) 0.3317(2) 0.2543(3) 0.0287(8) Uani 1 1 d . . . C1 C 0.2956(2) 0.0924(3) 0.0324(4) 0.0316(10) Uani 1 1 d . . . C2 C 0.31360(19) -0.0023(2) 0.0537(4) 0.0287(9) Uani 1 1 d . . . C3 C 0.3516(2) -0.0283(3) 0.1632(4) 0.0351(10) Uani 1 1 d . . . H3 H 0.3672 0.0149 0.2218 0.042 Uiso 1 1 calc R . . C4 C 0.3667(2) -0.1164(3) 0.1871(4) 0.0375(11) Uani 1 1 d . . . H4 H 0.3917 -0.1324 0.2617 0.045 Uiso 1 1 calc R . . C5 C 0.3442(2) -0.1814(3) 0.0989(4) 0.0319(10) Uani 1 1 d . . . C6 C 0.3072(2) -0.1570(3) -0.0122(4) 0.0352(10) Uani 1 1 d . . . H6 H 0.2929 -0.1999 -0.0723 0.042 Uiso 1 1 calc R . . C7 C 0.2915(2) -0.0684(3) -0.0332(4) 0.0330(10) Uani 1 1 d . . . H7 H 0.2657 -0.0526 -0.1068 0.040 Uiso 1 1 calc R . . C8 C 0.3832(2) -0.3010(3) 0.2346(4) 0.0446(12) Uani 1 1 d . . . H8A H 0.4237 -0.2699 0.2569 0.053 Uiso 1 1 calc R . . H8B H 0.3932 -0.3639 0.2278 0.053 Uiso 1 1 calc R . . C9 C 0.3379(2) -0.2880(3) 0.3430(4) 0.0345(10) Uani 1 1 d . . . C10 C 0.4107(2) 0.2983(3) 0.2983(4) 0.0363(11) Uani 1 1 d . . . H10 H 0.4241 0.2443 0.2651 0.044 Uiso 1 1 calc R . . C11 C 0.4509(2) 0.3404(3) 0.3909(4) 0.0433(12) Uani 1 1 d . . . H11 H 0.4907 0.3151 0.4184 0.052 Uiso 1 1 calc R . . C12 C 0.4322(2) 0.4194(3) 0.4424(4) 0.0343(10) Uani 1 1 d . . . C13 C 0.3721(2) 0.4524(3) 0.4016(4) 0.0410(11) Uani 1 1 d . . . H13 H 0.3570 0.5049 0.4366 0.049 Uiso 1 1 calc R . . C14 C 0.3343(2) 0.4070(3) 0.3082(4) 0.0383(11) Uani 1 1 d . . . H14 H 0.2936 0.4299 0.2816 0.046 Uiso 1 1 calc R . . C15 C 0.4773(2) 0.4707(3) 0.5366(4) 0.0458(13) Uani 1 1 d . . . H15A H 0.5027 0.4294 0.5915 0.055 Uiso 1 1 calc R . . H15B H 0.4519 0.5075 0.5913 0.055 Uiso 1 1 calc R . . O6 O 0.4674(5) 0.1508(6) 0.0319(17) 0.172(7) Uani 0.50 1 d PD . . H6A H 0.4796 0.1891 0.0889 0.258 Uiso 0.50 1 d PR . . C16 C 0.5041(10) 0.0715(9) 0.0526(17) 0.091(8) Uani 0.50 1 d PD . . H16A H 0.4978 0.0482 0.1371 0.109 Uiso 0.50 1 d PR . . H16B H 0.5496 0.0839 0.0477 0.109 Uiso 0.50 1 d PR . . C17 C 0.4821(6) 0.0033(8) -0.0492(9) 0.064(3) Uani 0.50 1 d PD . . H17A H 0.4933 0.0235 -0.1327 0.077 Uiso 0.50 1 d PR . . H17C H 0.4356 -0.0034 -0.0516 0.077 Uiso 0.50 1 d PR . . C18 C 0.5150(11) -0.0870(10) -0.018(3) 0.148(15) Uani 0.50 1 d PD . . H18D H 0.5008 -0.1296 -0.0835 0.222 Uiso 0.50 1 d PR . . H18A H 0.5614 -0.0803 -0.0172 0.222 Uiso 0.50 1 d PR . . H18B H 0.5032 -0.1074 0.0646 0.222 Uiso 0.50 1 d PR . . 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 Zn1 0.0314(3) 0.0247(2) 0.0295(3) -0.0035(2) -0.00483(19) -0.0056(2) O1 0.0409(18) 0.0234(16) 0.065(2) -0.0060(14) -0.0078(16) -0.0024(14) O2 0.050(2) 0.0298(16) 0.0421(19) 0.0020(13) -0.0089(15) 0.0058(14) O3 0.069(2) 0.0304(17) 0.0372(18) 0.0057(14) 0.0167(16) 0.0168(17) O4 0.051(2) 0.051(2) 0.0341(19) 0.0024(14) 0.0034(15) 0.0126(16) O5 0.0416(19) 0.0457(19) 0.0454(19) 0.0035(14) 0.0130(15) 0.0109(16) N1 0.029(2) 0.0284(19) 0.029(2) -0.0039(15) -0.0019(16) -0.0054(16) C1 0.035(3) 0.025(2) 0.035(3) 0.0043(19) 0.009(2) 0.000(2) C2 0.031(2) 0.024(2) 0.031(2) 0.0049(18) 0.0062(19) -0.0039(18) C3 0.040(3) 0.031(2) 0.034(3) -0.0034(19) 0.000(2) 0.001(2) C4 0.043(3) 0.037(3) 0.032(3) 0.006(2) -0.003(2) 0.005(2) C5 0.041(3) 0.024(2) 0.032(3) 0.0035(18) 0.013(2) 0.005(2) C6 0.050(3) 0.025(2) 0.030(3) -0.0038(18) 0.003(2) -0.001(2) C7 0.038(3) 0.033(2) 0.028(2) 0.0019(18) -0.0016(19) -0.001(2) C8 0.058(3) 0.033(3) 0.044(3) 0.011(2) 0.018(2) 0.018(2) C9 0.042(3) 0.019(2) 0.043(3) -0.002(2) 0.007(2) 0.004(2) C10 0.038(3) 0.031(3) 0.039(3) -0.0087(19) -0.002(2) 0.002(2) C11 0.030(3) 0.056(3) 0.042(3) -0.005(2) -0.007(2) -0.006(2) C12 0.038(3) 0.041(3) 0.023(2) -0.0023(19) -0.001(2) -0.017(2) C13 0.049(3) 0.031(2) 0.042(3) -0.012(2) -0.006(2) -0.001(2) C14 0.030(3) 0.040(3) 0.044(3) -0.011(2) -0.004(2) 0.002(2) C15 0.048(3) 0.060(3) 0.029(3) -0.004(2) -0.003(2) -0.027(2) O6 0.099(10) 0.090(9) 0.329(19) -0.094(12) 0.026(10) -0.002(7) C16 0.052(13) 0.11(2) 0.107(13) -0.054(13) 0.013(9) -0.001(10) C17 0.051(8) 0.096(10) 0.046(7) -0.004(8) 0.006(5) -0.018(8) C18 0.032(11) 0.13(2) 0.29(4) 0.09(3) 0.005(14) -0.004(14) _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 Zn1 O1 2.008(3) . ? Zn1 O2 2.022(3) 7 ? Zn1 N1 2.025(3) . ? Zn1 O4 2.071(3) 6 ? Zn1 O5 2.077(3) 4 ? Zn1 Zn1 2.9789(10) 7 ? O1 C1 1.259(4) . ? O2 C1 1.266(5) . ? O2 Zn1 2.022(3) 7 ? O3 C5 1.363(4) . ? O3 C8 1.417(5) . ? O4 C9 1.260(5) . ? O4 Zn1 2.071(3) 6_556 ? O5 C9 1.242(5) . ? O5 Zn1 2.077(3) 4_545 ? N1 C14 1.332(5) . ? N1 C10 1.334(5) . ? C1 C2 1.482(5) . ? C2 C3 1.389(5) . ? C2 C7 1.395(5) . ? C3 C4 1.377(5) . ? C3 H3 0.9300 . ? C4 C5 1.394(5) . ? C4 H4 0.9300 . ? C5 C6 1.387(5) . ? C6 C7 1.381(5) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.523(5) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C10 C11 1.377(5) . ? C10 H10 0.9300 . ? C11 C12 1.367(6) . ? C11 H11 0.9300 . ? C12 C13 1.374(5) . ? C12 C15 1.510(5) . ? C13 C14 1.380(5) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 C15 1.524(8) 5_666 ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? O6 C18 1.038(17) 5_655 ? O6 C16 1.419(9) . ? O6 H6A 0.8500 . ? C16 C18 0.56(2) 5_655 ? C16 C17 1.158(19) 5_655 ? C16 C17 1.517(9) . ? C16 H16A 0.9600 . ? C16 H16B 0.9599 . ? C17 C16 1.158(19) 5_655 ? C17 C17 1.221(19) 5_655 ? C17 C18 1.44(2) 5_655 ? C17 C18 1.538(9) . ? C17 H17A 0.9600 . ? C17 H17C 0.9598 . ? C18 C16 0.56(2) 5_655 ? C18 O6 1.038(17) 5_655 ? C18 C17 1.44(2) 5_655 ? C18 H18D 0.9600 . ? C18 H18A 0.9598 . ? C18 H18B 0.9600 . ? 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 Zn1 O2 158.56(11) . 7 ? O1 Zn1 N1 104.93(12) . . ? O2 Zn1 N1 96.49(12) 7 . ? O1 Zn1 O4 88.66(12) . 6 ? O2 Zn1 O4 88.32(12) 7 6 ? N1 Zn1 O4 100.35(12) . 6 ? O1 Zn1 O5 86.67(12) . 4 ? O2 Zn1 O5 88.59(12) 7 4 ? N1 Zn1 O5 100.64(12) . 4 ? O4 Zn1 O5 158.99(11) 6 4 ? O1 Zn1 Zn1 83.51(8) . 7 ? O2 Zn1 Zn1 75.23(8) 7 7 ? N1 Zn1 Zn1 167.34(10) . 7 ? O4 Zn1 Zn1 89.11(8) 6 7 ? O5 Zn1 Zn1 70.02(8) 4 7 ? C1 O1 Zn1 122.7(3) . . ? C1 O2 Zn1 133.1(3) . 7 ? C5 O3 C8 118.1(3) . . ? C9 O4 Zn1 113.8(3) . 6_556 ? C9 O5 Zn1 139.1(3) . 4_545 ? C14 N1 C10 117.1(3) . . ? C14 N1 Zn1 120.3(3) . . ? C10 N1 Zn1 122.3(3) . . ? O1 C1 O2 124.9(4) . . ? O1 C1 C2 118.0(4) . . ? O2 C1 C2 117.0(4) . . ? C3 C2 C7 117.9(4) . . ? C3 C2 C1 120.8(4) . . ? C7 C2 C1 121.3(4) . . ? C4 C3 C2 121.6(4) . . ? C4 C3 H3 119.2 . . ? C2 C3 H3 119.2 . . ? C3 C4 C5 119.6(4) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? O3 C5 C6 115.9(4) . . ? O3 C5 C4 124.3(4) . . ? C6 C5 C4 119.8(4) . . ? C7 C6 C5 119.7(4) . . ? C7 C6 H6 120.2 . . ? C5 C6 H6 120.2 . . ? C6 C7 C2 121.3(4) . . ? C6 C7 H7 119.3 . . ? C2 C7 H7 119.3 . . ? O3 C8 C9 113.6(4) . . ? O3 C8 H8A 108.8 . . ? C9 C8 H8A 108.8 . . ? O3 C8 H8B 108.8 . . ? C9 C8 H8B 108.8 . . ? H8A C8 H8B 107.7 . . ? O5 C9 O4 127.3(4) . . ? O5 C9 C8 117.5(4) . . ? O4 C9 C8 115.2(4) . . ? N1 C10 C11 122.8(4) . . ? N1 C10 H10 118.6 . . ? C11 C10 H10 118.6 . . ? C12 C11 C10 119.9(4) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C11 C12 C13 117.7(4) . . ? C11 C12 C15 121.2(4) . . ? C13 C12 C15 121.0(4) . . ? C12 C13 C14 119.4(4) . . ? C12 C13 H13 120.3 . . ? C14 C13 H13 120.3 . . ? N1 C14 C13 123.0(4) . . ? N1 C14 H14 118.5 . . ? C13 C14 H14 118.5 . . ? C12 C15 C15 110.1(4) . 5_666 ? C12 C15 H15A 109.6 . . ? C15 C15 H15A 109.6 5_666 . ? C12 C15 H15B 109.6 . . ? C15 C15 H15B 109.6 5_666 . ? H15A C15 H15B 108.2 . . ? C18 O6 H6A 128.9 5_655 . ? C16 O6 H6A 109.4 . . ? C18 C16 C17 123(3) 5_655 5_655 ? C17 C16 O6 159.7(16) 5_655 . ? C18 C16 C17 71(2) 5_655 . ? C17 C16 C17 52.3(9) 5_655 . ? O6 C16 C17 109.3(9) . . ? C18 C16 H16A 126.4 5_655 . ? C17 C16 H16A 74.1 5_655 . ? O6 C16 H16A 109.8 . . ? C17 C16 H16A 109.7 . . ? C18 C16 H16B 122.0 5_655 . ? C17 C16 H16B 86.8 5_655 . ? O6 C16 H16B 109.9 . . ? C17 C16 H16B 109.9 . . ? H16A C16 H16B 108.3 . . ? C16 C17 C17 79.2(13) 5_655 5_655 ? C16 C17 C18 149.2(17) 5_655 5_655 ? C17 C17 C18 70.1(10) 5_655 5_655 ? C16 C17 C16 127.7(9) 5_655 . ? C17 C17 C16 48.6(9) 5_655 . ? C17 C17 C18 61.6(11) 5_655 . ? C18 C17 C18 131.7(8) 5_655 . ? C16 C17 C18 110.1(9) . . ? C16 C17 H17A 101.8 5_655 . ? C17 C17 H17A 127.5 5_655 . ? C18 C17 H17A 99.1 5_655 . ? C16 C17 H17A 109.5 . . ? C18 C17 H17A 109.6 . . ? C16 C17 H17C 98.3 5_655 . ? C17 C17 H17C 123.8 5_655 . ? C18 C17 H17C 96.4 5_655 . ? C16 C17 H17C 109.7 . . ? C18 C17 H17C 109.7 . . ? H17A C17 H17C 108.2 . . ? C16 C18 O6 122(4) 5_655 5_655 ? C16 C18 C17 87(2) 5_655 5_655 ? O6 C18 C17 150(2) 5_655 5_655 ? O6 C18 C17 160(2) 5_655 . ? C17 C18 C17 48.3(8) 5_655 . ? C16 C18 H18D 70.6 5_655 . ? O6 C18 H18D 51.9 5_655 . ? C17 C18 H18D 157.7 5_655 . ? C17 C18 H18D 109.4 . . ? C16 C18 H18A 128.2 5_655 . ? O6 C18 H18A 75.0 5_655 . ? C17 C18 H18A 83.9 5_655 . ? C17 C18 H18A 109.6 . . ? H18D C18 H18A 109.5 . . ? C16 C18 H18B 119.3 5_655 . ? O6 C18 H18B 86.4 5_655 . ? C17 C18 H18B 81.2 5_655 . ? C17 C18 H18B 109.4 . . ? H18D C18 H18B 109.5 . . ? H18A C18 H18B 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 Zn1 O1 C1 -14.2(5) 7 . . . ? N1 Zn1 O1 C1 163.5(3) . . . . ? O4 Zn1 O1 C1 -96.1(3) 6 . . . ? O5 Zn1 O1 C1 63.4(3) 4 . . . ? Zn1 Zn1 O1 C1 -6.9(3) 7 . . . ? O1 Zn1 N1 C14 -160.0(3) . . . . ? O2 Zn1 N1 C14 19.1(3) 7 . . . ? O4 Zn1 N1 C14 108.6(3) 6 . . . ? O5 Zn1 N1 C14 -70.7(3) 4 . . . ? Zn1 Zn1 N1 C14 -29.2(6) 7 . . . ? O1 Zn1 N1 C10 26.3(3) . . . . ? O2 Zn1 N1 C10 -154.6(3) 7 . . . ? O4 Zn1 N1 C10 -65.1(3) 6 . . . ? O5 Zn1 N1 C10 115.7(3) 4 . . . ? Zn1 Zn1 N1 C10 157.1(3) 7 . . . ? Zn1 O1 C1 O2 9.6(6) . . . . ? Zn1 O1 C1 C2 -169.7(3) . . . . ? Zn1 O2 C1 O1 -5.9(6) 7 . . . ? Zn1 O2 C1 C2 173.5(3) 7 . . . ? O1 C1 C2 C3 17.7(6) . . . . ? O2 C1 C2 C3 -161.7(4) . . . . ? O1 C1 C2 C7 -164.2(4) . . . . ? O2 C1 C2 C7 16.4(6) . . . . ? C7 C2 C3 C4 -0.7(6) . . . . ? C1 C2 C3 C4 177.4(4) . . . . ? C2 C3 C4 C5 0.9(6) . . . . ? C8 O3 C5 C6 -167.7(4) . . . . ? C8 O3 C5 C4 13.1(6) . . . . ? C3 C4 C5 O3 179.3(4) . . . . ? C3 C4 C5 C6 0.2(6) . . . . ? O3 C5 C6 C7 179.4(4) . . . . ? C4 C5 C6 C7 -1.4(6) . . . . ? C5 C6 C7 C2 1.6(6) . . . . ? C3 C2 C7 C6 -0.5(6) . . . . ? C1 C2 C7 C6 -178.7(4) . . . . ? C5 O3 C8 C9 63.5(5) . . . . ? Zn1 O5 C9 O4 11.4(7) 4_545 . . . ? Zn1 O5 C9 C8 -170.5(3) 4_545 . . . ? Zn1 O4 C9 O5 -5.2(6) 6_556 . . . ? Zn1 O4 C9 C8 176.7(3) 6_556 . . . ? O3 C8 C9 O5 9.9(5) . . . . ? O3 C8 C9 O4 -171.8(3) . . . . ? C14 N1 C10 C11 -3.1(6) . . . . ? Zn1 N1 C10 C11 170.8(3) . . . . ? N1 C10 C11 C12 0.6(7) . . . . ? C10 C11 C12 C13 2.1(7) . . . . ? C10 C11 C12 C15 -175.3(4) . . . . ? C11 C12 C13 C14 -2.3(6) . . . . ? C15 C12 C13 C14 175.1(4) . . . . ? C10 N1 C14 C13 2.9(6) . . . . ? Zn1 N1 C14 C13 -171.1(3) . . . . ? C12 C13 C14 N1 -0.2(7) . . . . ? C11 C12 C15 C15 85.0(6) . . . 5_666 ? C13 C12 C15 C15 -92.3(6) . . . 5_666 ? C18 O6 C16 C17 -27(5) 5_655 . . 5_655 ? C18 O6 C16 C17 -4(6) 5_655 . . . ? C18 C16 C17 C16 -173(6) 5_655 . . 5_655 ? C17 C16 C17 C16 0.004(4) 5_655 . . 5_655 ? O6 C16 C17 C16 -170(3) . . . 5_655 ? C18 C16 C17 C17 -173(6) 5_655 . . 5_655 ? O6 C16 C17 C17 -170(3) . . . 5_655 ? C17 C16 C17 C18 173(6) 5_655 . . 5_655 ? O6 C16 C17 C18 3(4) . . . 5_655 ? C18 C16 C17 C18 -175(4) 5_655 . . . ? C17 C16 C17 C18 -3(2) 5_655 . . . ? O6 C16 C17 C18 -172.8(14) . . . . ? C17 C17 C18 C16 171(8) 5_655 . . 5_655 ? C18 C17 C18 C16 171(8) 5_655 . . 5_655 ? C16 C17 C18 C16 173(6) . . . 5_655 ? C16 C17 C18 O6 27(5) 5_655 . . 5_655 ? C17 C17 C18 O6 -162(8) 5_655 . . 5_655 ? C18 C17 C18 O6 -162(8) 5_655 . . 5_655 ? C16 C17 C18 O6 -160(7) . . . 5_655 ? C16 C17 C18 C17 -171(8) 5_655 . . 5_655 ? C18 C17 C18 C17 -0.001(3) 5_655 . . 5_655 ? C16 C17 C18 C17 2.3(19) . . . 5_655 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.41 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.478 _refine_diff_density_min -0.409 _refine_diff_density_rms 0.086