# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Jian-Fang Ma' _publ_contact_author_address ; Department of Chemistry Northeast Normal University Changchun 130024 P.R.China ; _publ_contact_author_email jianfangma@yahoo.com.cn _publ_contact_author_fax +86-431-85098620 _publ_contact_author_phone +86-431-85098620 _publ_section_title ; A series of coordination polymers based on 5,5'-(ethane-1,2-diyl)-bis(oxy)diisophthalic acid and structurally related N-donor ligands: syntheses, structures and properties ; _publ_author_name 'Jian-Fang Ma' # Attachment '- CIFs.cif' #=============================================== data_compound-1 _database_code_depnum_ccdc_archive 'CCDC 834798' #TrackingRef '- CIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H16 O13 Ni2, 5(H2 O)' _chemical_formula_sum 'C18 H26 N0 Ni2 O18' _chemical_formula_weight 647.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'p 21/n' _symmetry_space_group_name_hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.3464(6) _cell_length_b 13.8945(4) _cell_length_c 14.5650(6) _cell_angle_alpha 90.00 _cell_angle_beta 114.553(5) _cell_angle_gamma 90.00 _cell_volume 2456.73(17) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6377 _cell_measurement_theta_min 3.3045 _cell_measurement_theta_max 29.0223 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.751 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1336 _exptl_absorpt_coefficient_mu 1.620 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.88742 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _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 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9267 _diffrn_reflns_av_R_equivalents 0.0172 _diffrn_reflns_av_sigmaI/netI 0.0305 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.31 _diffrn_reflns_theta_max 25.35 _reflns_number_total 4480 _reflns_number_gt 3701 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0545P)^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 4480 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0381 _refine_ls_R_factor_gt 0.0306 _refine_ls_wR_factor_ref 0.0909 _refine_ls_wR_factor_gt 0.0893 _refine_ls_goodness_of_fit_ref 1.115 _refine_ls_restrained_S_all 1.115 _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 0.52330(3) 0.40123(2) 0.76308(2) 0.01541(11) Uani 1 1 d . . . Ni2 Ni 0.34173(3) 0.26583(2) 0.57491(2) 0.01970(12) Uani 1 1 d . . . C1 C 0.3056(2) 0.47432(19) 0.6274(2) 0.0209(6) Uani 1 1 d . . . O6 O -0.10117(17) 0.69038(15) 0.15280(13) 0.0303(5) Uani 1 1 d . . . O5 O 0.06609(19) 0.67792(16) 0.35431(14) 0.0389(6) Uani 1 1 d . . . O8 O -0.37774(18) 0.51594(15) -0.24595(14) 0.0325(5) Uani 1 1 d . . . C3 C 0.2291(2) 0.5596(2) 0.5917(2) 0.0239(6) Uani 1 1 d . . . C15 C -0.2592(2) 0.60498(19) -0.10154(19) 0.0206(6) Uani 1 1 d . . . O1 O 0.38641(16) 0.48206(14) 0.71216(14) 0.0294(5) Uani 1 1 d . . . O7 O -0.38592(17) 0.48078(15) -0.10450(14) 0.0294(5) Uani 1 1 d . . . O2 O 0.28269(16) 0.40234(13) 0.57060(14) 0.0280(5) Uani 1 1 d . . . C7 C 0.1094(2) 0.6607(2) 0.45679(19) 0.0277(7) Uani 1 1 d . . . C10 C -0.0310(3) 0.7683(2) 0.2062(2) 0.0276(7) Uani 1 1 d . . . H10A H -0.0670 0.8294 0.1806 0.033 Uiso 1 1 calc R . . H10B H 0.0372 0.7663 0.1974 0.033 Uiso 1 1 calc R . . C5 C 0.1335(2) 0.6907(2) 0.62693(19) 0.0232(6) Uani 1 1 d . . . C6 C 0.0843(2) 0.7146(2) 0.5241(2) 0.0258(6) Uani 1 1 d . . . H6 H 0.0355 0.7661 0.5016 0.031 Uiso 1 1 calc R . . C4 C 0.2065(2) 0.6147(2) 0.6608(2) 0.0237(6) Uani 1 1 d . . . H4 H 0.2404 0.6004 0.7293 0.028 Uiso 1 1 calc R . . C8 C 0.1810(3) 0.5838(2) 0.4899(2) 0.0291(7) Uani 1 1 d . . . H8 H 0.1971 0.5480 0.4439 0.035 Uiso 1 1 calc R . . C12 C -0.0968(2) 0.7423(2) -0.0061(2) 0.0231(6) Uani 1 1 d . . . H12 H -0.0423 0.7879 0.0258 0.028 Uiso 1 1 calc R . . C16 C -0.2173(2) 0.6168(2) 0.0028(2) 0.0224(6) Uani 1 1 d . . . H16 H -0.2432 0.5785 0.0407 0.027 Uiso 1 1 calc R . . C11 C -0.1370(2) 0.6854(2) 0.04980(19) 0.0224(6) Uani 1 1 d . . . C14 C -0.2205(2) 0.6618(2) -0.15797(19) 0.0228(6) Uani 1 1 d . . . H14 H -0.2490 0.6543 -0.2277 0.027 Uiso 1 1 calc R . . C17 C -0.3453(2) 0.5303(2) -0.15285(19) 0.0220(6) Uani 1 1 d . . . C9 C -0.0076(3) 0.7577(2) 0.3155(2) 0.0281(7) Uani 1 1 d . . . H9A H 0.0259 0.8160 0.3520 0.034 Uiso 1 1 calc R . . H9B H -0.0754 0.7461 0.3231 0.034 Uiso 1 1 calc R . . C13 C -0.1391(2) 0.73002(19) -0.11051(19) 0.0205(6) Uani 1 1 d . . . C2 C 0.1048(2) 0.74647(19) 0.7005(2) 0.0221(6) Uani 1 1 d . . . O4 O 0.02617(17) 0.80635(15) 0.66446(13) 0.0308(5) Uani 1 1 d . . . O3 O 0.15734(18) 0.72904(15) 0.79210(14) 0.0338(5) Uani 1 1 d . . . C18 C -0.0974(2) 0.78927(19) -0.1720(2) 0.0204(6) Uani 1 1 d . . . O10 O -0.00069(15) 0.82678(13) -0.13210(13) 0.0193(4) Uani 1 1 d . . . O9 O -0.15567(16) 0.80583(15) -0.26324(13) 0.0284(5) Uani 1 1 d . . . O1W O 0.32556(18) 0.29103(15) 0.42966(14) 0.0328(5) Uani 1 1 d . . . O2W O 0.18273(18) 0.21183(17) 0.52066(15) 0.0402(6) Uani 1 1 d . . . O3W O 0.3987(2) 0.13102(16) 0.56370(17) 0.0458(6) Uani 1 1 d . . . O4W O 0.3669(2) 0.0961(2) 0.3637(2) 0.0627(8) Uani 1 1 d . . . O5W O 0.1128(3) 0.0498(2) 0.5901(2) 0.0751(9) Uani 1 1 d . . . O6W O 0.4994(3) 0.0044(2) 0.7162(2) 0.0787(10) Uani 1 1 d . . . O7W O 0.1100(3) 0.3784(3) 0.3744(3) 0.1030(13) Uani 1 1 d . . . O8W O -0.3911(5) 0.5177(3) -0.4363(3) 0.142(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.01671(19) 0.01536(18) 0.01379(18) -0.00060(12) 0.00598(14) -0.00113(13) Ni2 0.0245(2) 0.01907(19) 0.01399(19) -0.00110(13) 0.00644(16) -0.00189(14) C1 0.0191(15) 0.0239(14) 0.0198(14) -0.0008(12) 0.0083(12) 0.0044(11) O6 0.0383(13) 0.0346(11) 0.0135(9) -0.0027(8) 0.0063(9) -0.0171(10) O5 0.0539(15) 0.0428(13) 0.0150(9) 0.0013(9) 0.0092(10) 0.0254(11) O8 0.0424(13) 0.0351(12) 0.0184(10) -0.0048(9) 0.0111(10) -0.0198(10) C3 0.0219(15) 0.0259(15) 0.0213(14) -0.0021(12) 0.0065(12) 0.0058(12) C15 0.0206(15) 0.0209(14) 0.0184(13) 0.0008(11) 0.0061(12) -0.0029(11) O1 0.0269(12) 0.0291(11) 0.0230(10) -0.0061(9) 0.0013(9) 0.0115(9) O7 0.0354(12) 0.0344(11) 0.0202(9) -0.0048(9) 0.0135(9) -0.0188(10) O2 0.0253(11) 0.0264(11) 0.0259(10) -0.0053(9) 0.0043(9) 0.0065(9) C7 0.0317(17) 0.0342(16) 0.0138(13) -0.0008(12) 0.0062(13) 0.0078(13) C10 0.0308(18) 0.0243(15) 0.0212(15) -0.0025(12) 0.0043(13) -0.0024(13) C5 0.0226(15) 0.0279(15) 0.0178(13) -0.0012(11) 0.0070(12) 0.0056(12) C6 0.0258(16) 0.0307(16) 0.0180(14) 0.0008(12) 0.0062(12) 0.0136(13) C4 0.0252(16) 0.0299(15) 0.0132(13) 0.0004(12) 0.0051(12) 0.0070(12) C8 0.0335(18) 0.0330(16) 0.0203(14) -0.0058(12) 0.0107(13) 0.0121(13) C12 0.0198(15) 0.0257(14) 0.0195(14) -0.0021(11) 0.0039(12) -0.0076(12) C16 0.0242(15) 0.0247(14) 0.0185(13) 0.0018(11) 0.0090(12) -0.0039(12) C11 0.0236(16) 0.0265(14) 0.0130(13) -0.0004(11) 0.0036(12) -0.0026(12) C14 0.0230(15) 0.0278(15) 0.0137(13) -0.0017(11) 0.0038(12) -0.0050(12) C17 0.0226(15) 0.0221(14) 0.0185(14) -0.0003(11) 0.0058(12) -0.0005(12) C9 0.0308(17) 0.0260(15) 0.0220(15) -0.0017(12) 0.0057(13) 0.0070(13) C13 0.0208(15) 0.0219(14) 0.0181(13) 0.0022(11) 0.0073(12) -0.0015(11) C2 0.0241(16) 0.0233(14) 0.0170(14) -0.0007(11) 0.0067(12) 0.0018(12) O4 0.0347(12) 0.0355(12) 0.0185(10) -0.0025(9) 0.0075(9) 0.0184(10) O3 0.0420(14) 0.0418(13) 0.0160(10) 0.0010(9) 0.0104(10) 0.0194(10) C18 0.0225(15) 0.0182(13) 0.0210(14) -0.0022(11) 0.0095(12) -0.0014(11) O10 0.0177(10) 0.0207(9) 0.0179(9) 0.0023(8) 0.0059(8) -0.0024(8) O9 0.0252(11) 0.0380(12) 0.0162(10) 0.0072(9) 0.0029(9) -0.0071(9) O1W 0.0373(13) 0.0425(12) 0.0178(10) -0.0007(9) 0.0106(9) -0.0051(10) O2W 0.0293(13) 0.0516(14) 0.0308(12) -0.0008(10) 0.0035(10) -0.0155(11) O3W 0.0661(18) 0.0244(11) 0.0465(14) -0.0013(10) 0.0232(13) 0.0080(11) O4W 0.0568(18) 0.074(2) 0.0554(16) -0.0119(14) 0.0211(15) -0.0055(15) O5W 0.110(3) 0.076(2) 0.0567(17) -0.0156(15) 0.0517(18) -0.0390(19) O6W 0.112(3) 0.0479(17) 0.0565(17) 0.0128(14) 0.0155(18) 0.0119(17) O7W 0.096(3) 0.077(2) 0.087(2) 0.016(2) -0.010(2) -0.032(2) O8W 0.306(6) 0.075(2) 0.122(3) 0.006(2) 0.166(4) -0.013(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O4 1.9665(18) 2_546 ? Ni1 O1 2.0057(19) . ? Ni1 O10 2.0790(17) 2_545 ? Ni1 O8 2.1086(19) 1_656 ? Ni1 O7 2.1136(19) 1_656 ? Ni1 O9 2.2079(19) 2_545 ? Ni1 C17 2.450(3) 1_656 ? Ni1 C18 2.500(3) 2_545 ? Ni2 O3 1.9983(18) 2_546 ? Ni2 O2 2.0448(18) . ? Ni2 O3W 2.053(2) . ? Ni2 O1W 2.0653(18) . ? Ni2 O2W 2.073(2) . ? Ni2 O10 2.1079(18) 2_545 ? C1 O2 1.252(3) . ? C1 O1 1.262(3) . ? C1 C3 1.509(4) . ? O6 C11 1.374(3) . ? O6 C10 1.431(3) . ? O5 C7 1.379(3) . ? O5 C9 1.433(3) . ? O8 C17 1.256(3) . ? O8 Ni1 2.1086(19) 1_454 ? C3 C8 1.390(4) . ? C3 C4 1.393(4) . ? C15 C14 1.385(4) . ? C15 C16 1.393(4) . ? C15 C17 1.497(4) . ? O7 C17 1.257(3) . ? O7 Ni1 2.1136(19) 1_454 ? C7 C8 1.380(4) . ? C7 C6 1.381(4) . ? C10 C9 1.497(4) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C5 C4 1.381(4) . ? C5 C6 1.403(4) . ? C5 C2 1.495(4) . ? C6 H6 0.9300 . ? C4 H4 0.9300 . ? C8 H8 0.9300 . ? C12 C11 1.393(4) . ? C12 C13 1.396(4) . ? C12 H12 0.9300 . ? C16 C11 1.385(4) . ? C16 H16 0.9300 . ? C14 C13 1.390(4) . ? C14 H14 0.9300 . ? C17 Ni1 2.450(3) 1_454 ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C13 C18 1.485(4) . ? C2 O3 1.246(3) . ? C2 O4 1.269(3) . ? O4 Ni1 1.9665(18) 2_556 ? O3 Ni2 1.9983(18) 2_556 ? C18 O9 1.251(3) . ? C18 O10 1.286(3) . ? C18 Ni1 2.500(3) 2 ? O10 Ni1 2.0790(17) 2 ? O10 Ni2 2.1079(18) 2 ? O9 Ni1 2.2079(19) 2 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Ni1 O1 96.69(9) 2_546 . ? O4 Ni1 O10 101.87(8) 2_546 2_545 ? O1 Ni1 O10 100.18(7) . 2_545 ? O4 Ni1 O8 154.02(8) 2_546 1_656 ? O1 Ni1 O8 92.96(9) . 1_656 ? O10 Ni1 O8 100.06(7) 2_545 1_656 ? O4 Ni1 O7 93.09(7) 2_546 1_656 ? O1 Ni1 O7 97.66(8) . 1_656 ? O10 Ni1 O7 155.11(8) 2_545 1_656 ? O8 Ni1 O7 61.66(7) 1_656 1_656 ? O4 Ni1 O9 92.51(9) 2_546 2_545 ? O1 Ni1 O9 160.40(7) . 2_545 ? O10 Ni1 O9 60.87(7) 2_545 2_545 ? O8 Ni1 O9 86.11(8) 1_656 2_545 ? O7 Ni1 O9 99.09(8) 1_656 2_545 ? O4 Ni1 C17 123.54(8) 2_546 1_656 ? O1 Ni1 C17 97.35(9) . 1_656 ? O10 Ni1 C17 128.57(8) 2_545 1_656 ? O8 Ni1 C17 30.84(8) 1_656 1_656 ? O7 Ni1 C17 30.86(8) 1_656 1_656 ? O9 Ni1 C17 91.86(8) 2_545 1_656 ? O4 Ni1 C18 99.37(9) 2_546 2_545 ? O1 Ni1 C18 130.75(8) . 2_545 ? O10 Ni1 C18 30.91(8) 2_545 2_545 ? O8 Ni1 C18 92.35(8) 1_656 2_545 ? O7 Ni1 C18 127.33(9) 1_656 2_545 ? O9 Ni1 C18 30.00(8) 2_545 2_545 ? C17 Ni1 C18 111.20(9) 1_656 2_545 ? O3 Ni2 O2 96.55(9) 2_546 . ? O3 Ni2 O3W 89.44(9) 2_546 . ? O2 Ni2 O3W 173.93(8) . . ? O3 Ni2 O1W 172.83(8) 2_546 . ? O2 Ni2 O1W 86.35(8) . . ? O3W Ni2 O1W 87.58(9) . . ? O3 Ni2 O2W 82.53(8) 2_546 . ? O2 Ni2 O2W 90.21(9) . . ? O3W Ni2 O2W 89.64(10) . . ? O1W Ni2 O2W 90.93(8) . . ? O3 Ni2 O10 96.89(7) 2_546 2_545 ? O2 Ni2 O10 87.20(8) . 2_545 ? O3W Ni2 O10 93.03(9) . 2_545 ? O1W Ni2 O10 89.78(7) . 2_545 ? O2W Ni2 O10 177.26(8) . 2_545 ? O2 C1 O1 126.1(2) . . ? O2 C1 C3 117.1(2) . . ? O1 C1 C3 116.8(2) . . ? C11 O6 C10 118.9(2) . . ? C7 O5 C9 118.1(2) . . ? C17 O8 Ni1 89.79(16) . 1_454 ? C8 C3 C4 119.7(3) . . ? C8 C3 C1 120.3(2) . . ? C4 C3 C1 120.1(2) . . ? C14 C15 C16 120.0(2) . . ? C14 C15 C17 119.8(2) . . ? C16 C15 C17 120.2(2) . . ? C1 O1 Ni1 126.21(17) . . ? C17 O7 Ni1 89.54(15) . 1_454 ? C1 O2 Ni2 137.34(18) . . ? O5 C7 C8 115.5(2) . . ? O5 C7 C6 123.9(3) . . ? C8 C7 C6 120.6(2) . . ? O6 C10 C9 107.7(2) . . ? O6 C10 H10A 110.2 . . ? C9 C10 H10A 110.2 . . ? O6 C10 H10B 110.2 . . ? C9 C10 H10B 110.2 . . ? H10A C10 H10B 108.5 . . ? C4 C5 C6 120.7(2) . . ? C4 C5 C2 119.6(2) . . ? C6 C5 C2 119.8(2) . . ? C7 C6 C5 119.0(3) . . ? C7 C6 H6 120.5 . . ? C5 C6 H6 120.5 . . ? C5 C4 C3 119.6(2) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? C7 C8 C3 120.4(3) . . ? C7 C8 H8 119.8 . . ? C3 C8 H8 119.8 . . ? C11 C12 C13 119.2(2) . . ? C11 C12 H12 120.4 . . ? C13 C12 H12 120.4 . . ? C11 C16 C15 119.9(2) . . ? C11 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? O6 C11 C16 114.9(2) . . ? O6 C11 C12 124.5(2) . . ? C16 C11 C12 120.6(2) . . ? C15 C14 C13 120.0(2) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? O8 C17 O7 118.9(2) . . ? O8 C17 C15 119.8(2) . . ? O7 C17 C15 121.3(2) . . ? O8 C17 Ni1 59.37(14) . 1_454 ? O7 C17 Ni1 59.60(14) . 1_454 ? C15 C17 Ni1 176.3(2) . 1_454 ? O5 C9 C10 107.5(2) . . ? O5 C9 H9A 110.2 . . ? C10 C9 H9A 110.2 . . ? O5 C9 H9B 110.2 . . ? C10 C9 H9B 110.2 . . ? H9A C9 H9B 108.5 . . ? C14 C13 C12 120.3(2) . . ? C14 C13 C18 119.3(2) . . ? C12 C13 C18 120.4(2) . . ? O3 C2 O4 124.8(2) . . ? O3 C2 C5 118.0(2) . . ? O4 C2 C5 117.2(2) . . ? C2 O4 Ni1 128.46(17) . 2_556 ? C2 O3 Ni2 139.66(19) . 2_556 ? O9 C18 O10 118.0(2) . . ? O9 C18 C13 121.3(2) . . ? O10 C18 C13 120.6(2) . . ? O9 C18 Ni1 61.97(14) . 2 ? O10 C18 Ni1 56.16(12) . 2 ? C13 C18 Ni1 174.55(19) . 2 ? C18 O10 Ni1 92.94(15) . 2 ? C18 O10 Ni2 132.27(17) . 2 ? Ni1 O10 Ni2 107.52(8) 2 2 ? C18 O9 Ni1 88.02(16) . 2 ? 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 C1 C3 C8 -36.5(4) . . . . ? O1 C1 C3 C8 144.0(3) . . . . ? O2 C1 C3 C4 143.7(3) . . . . ? O1 C1 C3 C4 -35.8(4) . . . . ? O2 C1 O1 Ni1 19.1(4) . . . . ? C3 C1 O1 Ni1 -161.51(18) . . . . ? O4 Ni1 O1 C1 -94.2(2) 2_546 . . . ? O10 Ni1 O1 C1 9.2(2) 2_545 . . . ? O8 Ni1 O1 C1 110.0(2) 1_656 . . . ? O7 Ni1 O1 C1 171.8(2) 1_656 . . . ? O9 Ni1 O1 C1 23.3(4) 2_545 . . . ? C17 Ni1 O1 C1 140.7(2) 1_656 . . . ? C18 Ni1 O1 C1 14.3(3) 2_545 . . . ? O1 C1 O2 Ni2 4.0(5) . . . . ? C3 C1 O2 Ni2 -175.39(19) . . . . ? O3 Ni2 O2 C1 51.3(3) 2_546 . . . ? O3W Ni2 O2 C1 -137.7(8) . . . . ? O1W Ni2 O2 C1 -135.3(3) . . . . ? O2W Ni2 O2 C1 133.8(3) . . . . ? O10 Ni2 O2 C1 -45.3(3) 2_545 . . . ? C9 O5 C7 C8 -179.1(3) . . . . ? C9 O5 C7 C6 1.3(5) . . . . ? C11 O6 C10 C9 178.3(2) . . . . ? O5 C7 C6 C5 -179.8(3) . . . . ? C8 C7 C6 C5 0.6(5) . . . . ? C4 C5 C6 C7 0.4(4) . . . . ? C2 C5 C6 C7 -178.2(3) . . . . ? C6 C5 C4 C3 -1.8(4) . . . . ? C2 C5 C4 C3 176.8(3) . . . . ? C8 C3 C4 C5 2.3(4) . . . . ? C1 C3 C4 C5 -177.9(3) . . . . ? O5 C7 C8 C3 -179.7(3) . . . . ? C6 C7 C8 C3 -0.1(5) . . . . ? C4 C3 C8 C7 -1.4(5) . . . . ? C1 C3 C8 C7 178.8(3) . . . . ? C14 C15 C16 C11 0.1(4) . . . . ? C17 C15 C16 C11 179.5(3) . . . . ? C10 O6 C11 C16 -170.7(3) . . . . ? C10 O6 C11 C12 10.5(4) . . . . ? C15 C16 C11 O6 -179.6(2) . . . . ? C15 C16 C11 C12 -0.8(4) . . . . ? C13 C12 C11 O6 179.4(3) . . . . ? C13 C12 C11 C16 0.7(4) . . . . ? C16 C15 C14 C13 0.5(4) . . . . ? C17 C15 C14 C13 -178.8(2) . . . . ? Ni1 O8 C17 O7 -3.9(3) 1_454 . . . ? Ni1 O8 C17 C15 175.8(2) 1_454 . . . ? Ni1 O7 C17 O8 3.9(3) 1_454 . . . ? Ni1 O7 C17 C15 -175.8(2) 1_454 . . . ? C14 C15 C17 O8 3.8(4) . . . . ? C16 C15 C17 O8 -175.6(3) . . . . ? C14 C15 C17 O7 -176.5(3) . . . . ? C16 C15 C17 O7 4.1(4) . . . . ? C14 C15 C17 Ni1 80(3) . . . 1_454 ? C16 C15 C17 Ni1 -99(3) . . . 1_454 ? C7 O5 C9 C10 172.9(3) . . . . ? O6 C10 C9 O5 72.4(3) . . . . ? C15 C14 C13 C12 -0.6(4) . . . . ? C15 C14 C13 C18 179.1(2) . . . . ? C11 C12 C13 C14 0.0(4) . . . . ? C11 C12 C13 C18 -179.7(2) . . . . ? C4 C5 C2 O3 7.8(4) . . . . ? C6 C5 C2 O3 -173.6(3) . . . . ? C4 C5 C2 O4 -170.2(3) . . . . ? C6 C5 C2 O4 8.4(4) . . . . ? O3 C2 O4 Ni1 9.5(4) . . . 2_556 ? C5 C2 O4 Ni1 -172.60(19) . . . 2_556 ? O4 C2 O3 Ni2 3.0(5) . . . 2_556 ? C5 C2 O3 Ni2 -174.8(2) . . . 2_556 ? C14 C13 C18 O9 26.0(4) . . . . ? C12 C13 C18 O9 -154.3(3) . . . . ? C14 C13 C18 O10 -155.4(3) . . . . ? C12 C13 C18 O10 24.3(4) . . . . ? C14 C13 C18 Ni1 152(2) . . . 2 ? C12 C13 C18 Ni1 -28(2) . . . 2 ? O9 C18 O10 Ni1 3.8(2) . . . 2 ? C13 C18 O10 Ni1 -174.8(2) . . . 2 ? O9 C18 O10 Ni2 -113.1(2) . . . 2 ? C13 C18 O10 Ni2 68.2(3) . . . 2 ? Ni1 C18 O10 Ni2 -116.99(19) 2 . . 2 ? O10 C18 O9 Ni1 -3.6(2) . . . 2 ? C13 C18 O9 Ni1 175.0(2) . . . 2 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.545 _refine_diff_density_min -0.483 _refine_diff_density_rms 0.070 #============================================================================= data_compoud-2 _database_code_depnum_ccdc_archive 'CCDC 834799' #TrackingRef '- CIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H40 N8 Ni2 O11, (H2 O)' _chemical_formula_sum 'C46 H42 N8 Ni2 O12' _chemical_formula_weight 1016.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'p 21/c' _symmetry_space_group_name_hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.429 _cell_length_b 24.143 _cell_length_c 24.275 _cell_angle_alpha 90.00 _cell_angle_beta 96.58 _cell_angle_gamma 90.00 _cell_volume 4325.2 _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7552 _cell_measurement_theta_min 2.7865 _cell_measurement_theta_max 29.1241 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.561 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2104 _exptl_absorpt_coefficient_mu 0.947 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.97841 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _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 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17898 _diffrn_reflns_av_R_equivalents 0.0280 _diffrn_reflns_av_sigmaI/netI 0.0637 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 25.35 _reflns_number_total 7887 _reflns_number_gt 5230 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXS-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0267P)^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 7887 _refine_ls_number_parameters 613 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0523 _refine_ls_R_factor_gt 0.0308 _refine_ls_wR_factor_ref 0.0660 _refine_ls_wR_factor_gt 0.0640 _refine_ls_goodness_of_fit_ref 0.953 _refine_ls_restrained_S_all 0.953 _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 Ni1 Ni 0.47151(4) 0.211698(14) 0.482814(12) 0.02865(9) Uani 1 1 d . . . Ni2 Ni 0.07671(4) 0.003383(15) 0.206466(12) 0.02850(9) Uani 1 1 d . . . O5 O -0.3338(2) -0.00799(8) 0.45320(6) 0.0378(5) Uani 1 1 d . . . O8 O -0.0426(2) -0.05181(8) 0.14912(6) 0.0364(5) Uani 1 1 d . . . O6 O -0.7704(2) -0.00199(8) 0.03144(7) 0.0427(5) Uani 1 1 d . . . O4 O -0.0241(2) -0.02942(8) 0.28097(6) 0.0349(4) Uani 1 1 d . . . O3 O 0.1191(2) 0.04992(8) 0.27906(6) 0.0406(5) Uani 1 1 d . . . O7 O -0.2046(2) 0.02186(8) 0.16350(7) 0.0377(5) Uani 1 1 d . . . C4 C -0.1380(3) 0.00121(11) 0.38570(9) 0.0291(6) Uani 1 1 d . . . H4 H -0.2039 -0.0266 0.3660 0.035 Uiso 1 1 calc R . . O2 O 0.1278(2) 0.13987(9) 0.52450(7) 0.0443(5) Uani 1 1 d . . . O1 O 0.3024(2) 0.14800(7) 0.45605(6) 0.0313(4) Uani 1 1 d . . . N1 N 0.6200(2) 0.17155(9) 0.54665(7) 0.0286(5) Uani 1 1 d . . . C14 C -0.4803(3) -0.12605(11) 0.05223(9) 0.0303(6) Uani 1 1 d . . . N5 N 0.1783(3) 0.06184(9) 0.15929(8) 0.0341(5) Uani 1 1 d . . . N6 N 0.3761(3) 0.12368(10) 0.13711(9) 0.0437(6) Uani 1 1 d . . . N2 N 0.8418(2) 0.15502(10) 0.61279(7) 0.0334(5) Uani 1 1 d . . . C12 C -0.3397(3) -0.04729(11) 0.10051(9) 0.0265(6) Uani 1 1 d . . . C13 C -0.3360(3) -0.10275(11) 0.08555(9) 0.0297(6) Uani 1 1 d . . . H13 H -0.2360 -0.1244 0.0980 0.036 Uiso 1 1 calc R . . C2 C 0.0368(3) 0.01402(12) 0.30485(10) 0.0302(6) Uani 1 1 d . . . C16 C -0.6315(3) -0.03783(12) 0.04719(9) 0.0313(6) Uani 1 1 d . . . C9 C -0.4144(3) 0.01618(12) 0.49775(10) 0.0345(7) Uani 1 1 d . . . H9A H -0.4421 0.0549 0.4902 0.041 Uiso 1 1 calc R . . H9B H -0.3334 0.0136 0.5320 0.041 Uiso 1 1 calc R . . C6 C -0.0831(3) 0.05775(11) 0.46714(9) 0.0265(6) Uani 1 1 d . . . H6 H -0.1144 0.0688 0.5015 0.032 Uiso 1 1 calc R . . C19 C 0.7837(3) 0.18640(12) 0.56867(9) 0.0329(6) Uani 1 1 d . . . H19 H 0.8504 0.2150 0.5553 0.040 Uiso 1 1 calc R . . C21 C 0.7089(3) 0.11779(12) 0.61909(10) 0.0372(7) Uani 1 1 d . . . H21 H 0.7112 0.0904 0.6461 0.045 Uiso 1 1 calc R . . C5 C -0.1846(3) 0.01760(11) 0.43678(9) 0.0275(6) Uani 1 1 d . . . C3 C 0.0060(3) 0.02581(11) 0.36364(9) 0.0259(6) Uani 1 1 d . . . C1 C 0.1725(3) 0.12649(11) 0.47842(9) 0.0263(6) Uani 1 1 d . . . C7 C 0.0666(3) 0.08154(11) 0.44599(9) 0.0244(6) Uani 1 1 d . . . C10 C -0.1878(3) -0.02355(12) 0.13985(9) 0.0296(6) Uani 1 1 d . . . C40 C 0.4772(3) 0.28866(14) 0.26131(10) 0.0376(7) Uani 1 1 d . . . C23 C 0.9999(3) 0.19650(13) 0.69903(10) 0.0324(7) Uani 1 1 d . . . C26 C 1.0022(3) 0.26190(14) 0.79434(11) 0.0401(7) Uani 1 1 d . . . C20 C 0.5721(3) 0.12819(12) 0.57854(9) 0.0337(6) Uani 1 1 d . . . H20 H 0.4630 0.1090 0.5732 0.040 Uiso 1 1 calc R . . C35 C 0.2108(4) 0.13864(14) 0.11060(11) 0.0528(8) Uani 1 1 d . . . H35 H 0.1856 0.1691 0.0876 0.063 Uiso 1 1 calc R . . C38 C 0.5167(4) 0.25808(14) 0.16934(12) 0.0488(8) Uani 1 1 d . . . H38 H 0.5287 0.2669 0.1326 0.059 Uiso 1 1 calc R . . C15 C -0.6275(3) -0.09315(11) 0.03273(9) 0.0336(6) Uani 1 1 d . . . H15 H -0.7238 -0.1084 0.0099 0.040 Uiso 1 1 calc R . . C37 C 0.5185(3) 0.20417(13) 0.18520(11) 0.0398(7) Uani 1 1 d . . . C18 C -0.9352(3) -0.02398(12) 0.00384(11) 0.0420(7) Uani 1 1 d . . . H18A H -0.9827 -0.0527 0.0261 0.050 Uiso 1 1 calc R . . H18B H -0.9151 -0.0396 -0.0317 0.050 Uiso 1 1 calc R . . C34 C 0.0920(4) 0.10045(13) 0.12441(11) 0.0457(8) Uani 1 1 d . . . H34 H -0.0312 0.1003 0.1120 0.055 Uiso 1 1 calc R . . C17 C -0.4859(3) -0.01493(11) 0.08124(9) 0.0304(6) Uani 1 1 d . . . H17 H -0.4878 0.0223 0.0909 0.037 Uiso 1 1 calc R . . C33 C 0.3492(4) 0.07776(12) 0.16601(10) 0.0397(7) Uani 1 1 d . . . H33 H 0.4403 0.0593 0.1882 0.048 Uiso 1 1 calc R . . C27 C 0.9850(3) 0.20559(14) 0.79691(10) 0.0419(7) Uani 1 1 d . . . H27 H 0.9736 0.1889 0.8309 0.050 Uiso 1 1 calc R . . C22 C 1.0145(3) 0.16044(14) 0.64855(10) 0.0447(8) Uani 1 1 d . . . H22A H 1.1043 0.1762 0.6271 0.054 Uiso 1 1 calc R . . H22B H 1.0562 0.1239 0.6607 0.054 Uiso 1 1 calc R . . C36 C 0.5392(4) 0.15787(14) 0.14387(12) 0.0529(8) Uani 1 1 d . . . H36A H 0.5600 0.1736 0.1084 0.063 Uiso 1 1 calc R . . H36B H 0.6431 0.1351 0.1570 0.063 Uiso 1 1 calc R . . C8 C 0.1086(3) 0.06554(11) 0.39443(9) 0.0270(6) Uani 1 1 d . . . H8 H 0.2071 0.0816 0.3801 0.032 Uiso 1 1 calc R . . C25 C 1.0131(3) 0.28579(14) 0.74331(13) 0.0514(8) Uani 1 1 d . . . H25 H 1.0217 0.3241 0.7404 0.062 Uiso 1 1 calc R . . C24 C 1.0112(3) 0.25310(14) 0.69616(11) 0.0466(8) Uani 1 1 d . . . H24 H 1.0177 0.2699 0.6620 0.056 Uiso 1 1 calc R . . C28 C 0.9843(3) 0.17252(13) 0.74972(10) 0.0387(7) Uani 1 1 d . . . H28 H 0.9733 0.1343 0.7525 0.046 Uiso 1 1 calc R . . C41 C 0.4754(4) 0.23403(15) 0.27684(12) 0.0501(8) Uani 1 1 d . . . H41 H 0.4597 0.2250 0.3132 0.060 Uiso 1 1 calc R . . C42 C 0.4966(4) 0.19252(14) 0.23963(12) 0.0524(8) Uani 1 1 d . . . H42 H 0.4961 0.1558 0.2513 0.063 Uiso 1 1 calc R . . C11 C -0.4782(3) -0.18662(12) 0.03991(10) 0.0344(6) Uani 1 1 d . . . N3 N 0.8558(3) 0.31111(11) 0.86909(9) 0.0446(6) Uani 1 1 d . . . C29 C 1.0253(3) 0.29650(15) 0.84672(12) 0.0603(10) Uani 1 1 d . . . H29A H 1.1020 0.2764 0.8750 0.072 Uiso 1 1 calc R . . H29B H 1.0880 0.3304 0.8392 0.072 Uiso 1 1 calc R . . C32 C 0.6124(3) 0.35433(13) 0.88748(10) 0.0392(7) Uani 1 1 d . . . H32 H 0.5186 0.3800 0.8863 0.047 Uiso 1 1 calc R . . C30 C 0.7847(3) 0.28546(14) 0.91007(11) 0.0446(8) Uani 1 1 d . . . H30 H 0.8350 0.2540 0.9278 0.054 Uiso 1 1 calc R . . C31 C 0.7478(4) 0.35538(14) 0.85472(11) 0.0456(8) Uani 1 1 d . . . H31 H 0.7639 0.3815 0.8275 0.055 Uiso 1 1 calc R . . N4 N 0.6341(3) 0.30957(10) 0.92284(8) 0.0350(5) Uani 1 1 d . . . N7 N 0.5105(3) 0.38789(10) 0.28829(8) 0.0396(6) Uani 1 1 d . . . C39 C 0.4973(4) 0.30024(14) 0.20693(12) 0.0520(8) Uani 1 1 d . . . H39 H 0.4979 0.3369 0.1952 0.062 Uiso 1 1 calc R . . C43 C 0.4536(4) 0.33290(14) 0.30365(11) 0.0518(8) Uani 1 1 d . . . H43A H 0.3269 0.3344 0.3097 0.062 Uiso 1 1 calc R . . H43B H 0.5225 0.3225 0.3385 0.062 Uiso 1 1 calc R . . C44 C 0.6727(3) 0.41078(12) 0.30429(10) 0.0326(6) Uani 1 1 d . . . H44 H 0.7604 0.3949 0.3299 0.039 Uiso 1 1 calc R . . C46 C 0.5320(3) 0.46655(14) 0.24585(11) 0.0450(8) Uani 1 1 d . . . H46 H 0.5052 0.4970 0.2229 0.054 Uiso 1 1 calc R . . C45 C 0.4204(3) 0.42375(14) 0.25154(11) 0.0497(8) Uani 1 1 d . . . H45 H 0.3036 0.4194 0.2337 0.060 Uiso 1 1 calc R . . N8 N 0.6927(2) 0.45835(10) 0.27946(8) 0.0326(5) Uani 1 1 d . . . O10 O -0.6021(2) -0.20812(8) 0.00586(7) 0.0423(5) Uani 1 1 d . . . O9 O -0.3538(2) -0.21703(8) 0.06346(7) 0.0415(5) Uani 1 1 d . . . O1W O 0.2796(2) 0.23541(8) 0.53843(7) 0.0448(5) Uani 1 1 d . . . O2W O -0.9848(4) -0.19115(14) 0.00110(15) 0.1376(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.03288(17) 0.0234(2) 0.02799(17) 0.00215(15) -0.00397(13) -0.00475(15) Ni2 0.03120(16) 0.0276(2) 0.02624(16) -0.00410(15) 0.00127(12) -0.00294(16) O5 0.0362(9) 0.0375(13) 0.0438(10) -0.0131(9) 0.0217(8) -0.0148(9) O8 0.0308(9) 0.0359(13) 0.0394(10) -0.0088(9) -0.0083(8) 0.0028(9) O6 0.0338(9) 0.0307(12) 0.0586(11) -0.0084(10) -0.0163(8) 0.0074(9) O4 0.0377(9) 0.0345(12) 0.0335(9) -0.0107(9) 0.0079(7) -0.0117(9) O3 0.0581(11) 0.0370(13) 0.0291(9) -0.0062(9) 0.0152(8) -0.0150(10) O7 0.0349(9) 0.0345(13) 0.0423(10) -0.0136(10) -0.0016(8) 0.0013(9) C4 0.0301(12) 0.0270(16) 0.0300(13) -0.0065(12) 0.0028(10) -0.0068(12) O2 0.0463(10) 0.0553(15) 0.0343(10) -0.0180(10) 0.0176(8) -0.0170(10) O1 0.0331(9) 0.0314(12) 0.0301(9) -0.0085(8) 0.0063(7) -0.0132(8) N1 0.0350(11) 0.0267(14) 0.0230(10) -0.0037(10) -0.0016(9) 0.0001(10) C14 0.0356(14) 0.0227(16) 0.0305(13) -0.0019(12) -0.0053(11) 0.0026(12) N5 0.0425(12) 0.0296(15) 0.0313(11) -0.0004(11) 0.0090(9) -0.0013(11) N6 0.0587(15) 0.0291(16) 0.0458(13) 0.0007(12) 0.0170(12) -0.0025(13) N2 0.0349(11) 0.0417(16) 0.0227(11) -0.0009(10) -0.0004(9) 0.0062(11) C12 0.0272(12) 0.0254(16) 0.0267(13) -0.0020(12) 0.0025(10) 0.0000(12) C13 0.0269(12) 0.0286(17) 0.0323(13) 0.0014(12) -0.0022(10) 0.0061(12) C2 0.0247(12) 0.0343(19) 0.0313(14) -0.0033(14) 0.0023(11) -0.0018(13) C16 0.0298(13) 0.0290(17) 0.0330(13) -0.0007(13) -0.0052(11) 0.0072(13) C9 0.0338(12) 0.0342(18) 0.0378(14) -0.0062(13) 0.0136(11) -0.0056(13) C6 0.0288(12) 0.0289(16) 0.0229(12) -0.0022(12) 0.0079(10) -0.0022(12) C19 0.0375(14) 0.0344(18) 0.0277(13) 0.0010(13) 0.0072(11) 0.0001(13) C21 0.0540(16) 0.0293(18) 0.0281(14) 0.0043(12) 0.0044(12) 0.0016(15) C5 0.0222(12) 0.0262(16) 0.0356(14) -0.0005(12) 0.0092(10) -0.0048(11) C3 0.0257(12) 0.0261(16) 0.0262(13) -0.0024(11) 0.0045(10) -0.0030(11) C1 0.0230(12) 0.0278(16) 0.0277(14) 0.0005(12) 0.0008(11) 0.0006(12) C7 0.0243(12) 0.0256(16) 0.0232(12) 0.0001(11) 0.0015(10) -0.0015(11) C10 0.0327(14) 0.0305(17) 0.0254(13) 0.0001(13) 0.0027(11) -0.0018(13) C40 0.0312(13) 0.045(2) 0.0354(15) -0.0015(15) 0.0002(11) -0.0119(14) C23 0.0229(12) 0.045(2) 0.0284(14) -0.0016(13) -0.0012(10) 0.0025(13) C26 0.0249(13) 0.052(2) 0.0439(17) -0.0159(16) 0.0067(12) -0.0017(14) C20 0.0422(14) 0.0259(17) 0.0329(14) -0.0003(13) 0.0034(12) -0.0036(13) C35 0.076(2) 0.035(2) 0.0451(17) 0.0091(15) -0.0047(15) -0.0011(18) C38 0.0660(19) 0.043(2) 0.0406(16) 0.0023(16) 0.0212(14) -0.0146(17) C15 0.0313(13) 0.0278(17) 0.0383(14) -0.0067(13) -0.0108(11) 0.0008(13) C37 0.0337(14) 0.040(2) 0.0468(17) 0.0019(15) 0.0112(12) -0.0070(14) C18 0.0367(14) 0.0370(19) 0.0483(16) -0.0112(14) -0.0126(13) 0.0092(13) C34 0.0535(17) 0.040(2) 0.0419(16) 0.0019(15) -0.0029(14) 0.0007(16) C17 0.0337(13) 0.0226(16) 0.0337(13) -0.0055(12) -0.0021(11) 0.0021(12) C33 0.0514(17) 0.0305(19) 0.0389(15) 0.0046(14) 0.0123(13) 0.0028(15) C27 0.0419(15) 0.057(2) 0.0285(14) -0.0011(15) 0.0108(11) -0.0065(15) C22 0.0348(14) 0.068(2) 0.0297(14) -0.0053(15) -0.0022(11) 0.0123(15) C36 0.0570(18) 0.040(2) 0.067(2) 0.0033(17) 0.0298(15) -0.0080(16) C8 0.0246(12) 0.0277(16) 0.0296(13) 0.0012(12) 0.0062(10) -0.0030(11) C25 0.0492(17) 0.0357(19) 0.069(2) -0.0033(18) 0.0069(15) 0.0024(16) C24 0.0476(16) 0.053(2) 0.0386(16) 0.0087(16) 0.0044(13) 0.0034(16) C28 0.0404(14) 0.0379(19) 0.0388(16) -0.0018(14) 0.0081(12) -0.0058(14) C41 0.0588(18) 0.054(2) 0.0361(16) 0.0109(17) -0.0017(13) -0.0034(17) C42 0.070(2) 0.036(2) 0.0509(19) 0.0131(17) 0.0062(15) 0.0017(17) C11 0.0380(14) 0.0272(17) 0.0361(14) -0.0018(13) -0.0036(12) 0.0034(14) N3 0.0336(12) 0.0559(19) 0.0446(14) -0.0209(13) 0.0064(11) -0.0002(13) C29 0.0315(14) 0.077(3) 0.074(2) -0.045(2) 0.0138(14) -0.0063(16) C32 0.0349(14) 0.039(2) 0.0440(16) -0.0062(15) 0.0044(12) 0.0040(13) C30 0.0445(16) 0.045(2) 0.0434(16) -0.0108(16) 0.0022(14) 0.0123(16) C31 0.0439(16) 0.046(2) 0.0469(17) -0.0064(15) 0.0046(14) -0.0018(16) N4 0.0364(12) 0.0346(15) 0.0335(12) -0.0076(11) 0.0024(9) 0.0079(11) N7 0.0321(12) 0.0436(17) 0.0428(13) -0.0086(12) 0.0033(10) -0.0078(12) C39 0.0720(19) 0.036(2) 0.0516(19) 0.0026(16) 0.0220(15) -0.0140(17) C43 0.0500(17) 0.058(2) 0.0484(18) -0.0072(17) 0.0113(14) -0.0217(17) C44 0.0242(13) 0.0390(19) 0.0344(14) -0.0039(14) 0.0021(11) 0.0015(13) C46 0.0425(16) 0.044(2) 0.0446(16) -0.0039(15) -0.0109(13) 0.0105(16) C45 0.0306(14) 0.059(2) 0.0560(18) -0.0145(17) -0.0121(13) 0.0037(16) N8 0.0299(11) 0.0346(15) 0.0324(11) -0.0012(11) 0.0004(9) 0.0039(11) O10 0.0462(10) 0.0253(11) 0.0502(10) -0.0072(9) -0.0169(9) 0.0032(9) O9 0.0474(10) 0.0266(12) 0.0462(10) -0.0061(9) -0.0141(9) 0.0094(9) O1W 0.0492(10) 0.0422(13) 0.0440(10) -0.0153(10) 0.0093(8) 0.0017(10) O2W 0.0993(19) 0.089(3) 0.210(3) 0.019(2) -0.042(2) -0.0070(19) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N1 2.0411(18) . ? Ni1 O1 2.0441(16) . ? Ni1 N4 2.061(2) 4_565 ? Ni1 O1W 2.1504(17) . ? Ni1 O10 2.1686(18) 2 ? Ni1 O9 2.1821(17) 2 ? Ni1 C11 2.518(3) 2 ? Ni2 N5 2.018(2) . ? Ni2 N8 2.024(2) 2_645 ? Ni2 O8 2.0533(16) . ? Ni2 O3 2.0832(16) . ? Ni2 O4 2.1839(16) . ? Ni2 O7 2.2701(15) . ? Ni2 C2 2.454(2) . ? Ni2 C10 2.484(2) . ? O5 C5 1.368(3) . ? O5 C9 1.420(3) . ? O8 C10 1.274(3) . ? O6 C16 1.367(3) . ? O6 C18 1.429(3) . ? O4 C2 1.257(3) . ? O3 C2 1.267(3) . ? O7 C10 1.250(3) . ? C4 C5 1.383(3) . ? C4 C3 1.383(3) . ? C4 H4 0.9300 . ? O2 C1 1.246(3) . ? O1 C1 1.271(3) . ? N1 C19 1.321(3) . ? N1 C20 1.373(3) . ? C14 C13 1.386(3) . ? C14 C15 1.391(3) . ? C14 C11 1.493(4) . ? N5 C33 1.319(3) . ? N5 C34 1.368(3) . ? N6 C33 1.339(3) . ? N6 C35 1.368(3) . ? N6 C36 1.460(3) . ? N2 C19 1.342(3) . ? N2 C21 1.357(3) . ? N2 C22 1.470(3) . ? C12 C17 1.375(3) . ? C12 C13 1.388(3) . ? C12 C10 1.506(3) . ? C13 H13 0.9300 . ? C2 C3 1.498(3) . ? C16 C15 1.382(4) . ? C16 C17 1.398(3) . ? C9 C9 1.507(5) 3_456 ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C6 C5 1.387(3) . ? C6 C7 1.400(3) . ? C6 H6 0.9300 . ? C19 H19 0.9300 . ? C21 C20 1.355(3) . ? C21 H21 0.9300 . ? C3 C8 1.389(3) . ? C1 C7 1.508(3) . ? C7 C8 1.379(3) . ? C40 C41 1.372(4) . ? C40 C39 1.374(4) . ? C40 C43 1.506(4) . ? C23 C24 1.371(4) . ? C23 C28 1.377(3) . ? C23 C22 1.517(4) . ? C26 C27 1.368(4) . ? C26 C25 1.377(4) . ? C26 C29 1.515(4) . ? C20 H20 0.9300 . ? C35 C34 1.345(4) . ? C35 H35 0.9300 . ? C38 C37 1.357(4) . ? C38 C39 1.386(4) . ? C38 H38 0.9300 . ? C15 H15 0.9300 . ? C37 C42 1.379(4) . ? C37 C36 1.522(4) . ? C18 C18 1.504(5) 3_355 ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C34 H34 0.9300 . ? C17 H17 0.9300 . ? C33 H33 0.9300 . ? C27 C28 1.396(4) . ? C27 H27 0.9300 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C8 H8 0.9300 . ? C25 C24 1.389(4) . ? C25 H25 0.9300 . ? C24 H24 0.9300 . ? C28 H28 0.9300 . ? C41 C42 1.370(4) . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? C11 O9 1.265(3) . ? C11 O10 1.275(3) . ? C11 Ni1 2.518(3) 2_545 ? N3 C30 1.332(3) . ? N3 C31 1.358(4) . ? N3 C29 1.470(3) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C32 C31 1.353(3) . ? C32 N4 1.378(3) . ? C32 H32 0.9300 . ? C30 N4 1.329(3) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? N4 Ni1 2.061(2) 4_566 ? N7 C44 1.342(3) . ? N7 C45 1.363(3) . ? N7 C43 1.455(4) . ? C39 H39 0.9300 . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 N8 1.313(3) . ? C44 H44 0.9300 . ? C46 C45 1.342(4) . ? C46 N8 1.381(3) . ? C46 H46 0.9300 . ? C45 H45 0.9300 . ? N8 Ni2 2.024(2) 2_655 ? O10 Ni1 2.1686(18) 2_545 ? O9 Ni1 2.1821(17) 2_545 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 O1 98.22(7) . . ? N1 Ni1 N4 96.23(8) . 4_565 ? O1 Ni1 N4 88.67(7) . 4_565 ? N1 Ni1 O1W 89.38(7) . . ? O1 Ni1 O1W 88.41(7) . . ? N4 Ni1 O1W 174.00(7) 4_565 . ? N1 Ni1 O10 97.63(7) . 2 ? O1 Ni1 O10 164.06(6) . 2 ? N4 Ni1 O10 91.26(8) 4_565 2 ? O1W Ni1 O10 90.10(7) . 2 ? N1 Ni1 O9 156.22(7) . 2 ? O1 Ni1 O9 103.55(6) . 2 ? N4 Ni1 O9 93.76(8) 4_565 2 ? O1W Ni1 O9 81.83(7) . 2 ? O10 Ni1 O9 60.55(6) 2 2 ? N1 Ni1 C11 127.36(8) . 2 ? O1 Ni1 C11 133.70(7) . 2 ? N4 Ni1 C11 93.45(9) 4_565 2 ? O1W Ni1 C11 84.79(8) . 2 ? O10 Ni1 C11 30.41(6) 2 2 ? O9 Ni1 C11 30.15(6) 2 2 ? N5 Ni2 N8 96.16(8) . 2_645 ? N5 Ni2 O8 103.27(7) . . ? N8 Ni2 O8 93.28(8) 2_645 . ? N5 Ni2 O3 94.18(8) . . ? N8 Ni2 O3 95.97(8) 2_645 . ? O8 Ni2 O3 159.24(7) . . ? N5 Ni2 O4 155.47(8) . . ? N8 Ni2 O4 91.67(7) 2_645 . ? O8 Ni2 O4 99.42(6) . . ? O3 Ni2 O4 61.82(7) . . ? N5 Ni2 O7 89.21(7) . . ? N8 Ni2 O7 154.09(8) 2_645 . ? O8 Ni2 O7 60.85(6) . . ? O3 Ni2 O7 108.94(7) . . ? O4 Ni2 O7 93.83(6) . . ? N5 Ni2 C2 125.04(9) . . ? N8 Ni2 C2 94.96(8) 2_645 . ? O8 Ni2 C2 129.55(8) . . ? O3 Ni2 C2 31.08(7) . . ? O4 Ni2 C2 30.76(7) . . ? O7 Ni2 C2 102.65(7) . . ? N5 Ni2 C10 97.64(8) . . ? N8 Ni2 C10 124.06(9) 2_645 . ? O8 Ni2 C10 30.79(8) . . ? O3 Ni2 C10 136.34(8) . . ? O4 Ni2 C10 97.10(7) . . ? O7 Ni2 C10 30.07(7) . . ? C2 Ni2 C10 119.09(8) . . ? C5 O5 C9 117.59(18) . . ? C10 O8 Ni2 93.63(15) . . ? C16 O6 C18 118.3(2) . . ? C2 O4 Ni2 86.56(15) . . ? C2 O3 Ni2 90.82(15) . . ? C10 O7 Ni2 84.47(14) . . ? C5 C4 C3 120.6(2) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C1 O1 Ni1 129.84(15) . . ? C19 N1 C20 105.37(19) . . ? C19 N1 Ni1 124.80(18) . . ? C20 N1 Ni1 129.63(15) . . ? C13 C14 C15 119.5(2) . . ? C13 C14 C11 119.3(2) . . ? C15 C14 C11 121.1(2) . . ? C33 N5 C34 104.7(2) . . ? C33 N5 Ni2 123.44(18) . . ? C34 N5 Ni2 130.43(18) . . ? C33 N6 C35 106.6(2) . . ? C33 N6 C36 125.5(2) . . ? C35 N6 C36 126.3(3) . . ? C19 N2 C21 107.01(19) . . ? C19 N2 C22 126.9(2) . . ? C21 N2 C22 126.1(2) . . ? C17 C12 C13 119.8(2) . . ? C17 C12 C10 120.3(2) . . ? C13 C12 C10 119.8(2) . . ? C14 C13 C12 120.5(2) . . ? C14 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? O4 C2 O3 120.8(2) . . ? O4 C2 C3 120.8(2) . . ? O3 C2 C3 118.4(2) . . ? O4 C2 Ni2 62.68(12) . . ? O3 C2 Ni2 58.10(12) . . ? C3 C2 Ni2 174.7(2) . . ? O6 C16 C15 125.3(2) . . ? O6 C16 C17 115.0(2) . . ? C15 C16 C17 119.7(2) . . ? O5 C9 C9 106.0(2) . 3_456 ? O5 C9 H9A 110.5 . . ? C9 C9 H9A 110.5 3_456 . ? O5 C9 H9B 110.5 . . ? C9 C9 H9B 110.5 3_456 . ? H9A C9 H9B 108.7 . . ? C5 C6 C7 119.9(2) . . ? C5 C6 H6 120.1 . . ? C7 C6 H6 120.1 . . ? N1 C19 N2 111.5(2) . . ? N1 C19 H19 124.3 . . ? N2 C19 H19 124.3 . . ? C20 C21 N2 106.9(2) . . ? C20 C21 H21 126.6 . . ? N2 C21 H21 126.6 . . ? O5 C5 C4 115.3(2) . . ? O5 C5 C6 124.8(2) . . ? C4 C5 C6 120.0(2) . . ? C4 C3 C8 119.3(2) . . ? C4 C3 C2 119.8(2) . . ? C8 C3 C2 120.6(2) . . ? O2 C1 O1 124.8(2) . . ? O2 C1 C7 118.6(2) . . ? O1 C1 C7 116.6(2) . . ? C8 C7 C6 119.3(2) . . ? C8 C7 C1 121.1(2) . . ? C6 C7 C1 119.5(2) . . ? O7 C10 O8 121.0(2) . . ? O7 C10 C12 121.2(2) . . ? O8 C10 C12 117.8(2) . . ? O7 C10 Ni2 65.46(12) . . ? O8 C10 Ni2 55.59(11) . . ? C12 C10 Ni2 172.8(2) . . ? C41 C40 C39 117.7(3) . . ? C41 C40 C43 119.2(3) . . ? C39 C40 C43 123.0(3) . . ? C24 C23 C28 118.4(3) . . ? C24 C23 C22 121.4(2) . . ? C28 C23 C22 120.1(3) . . ? C27 C26 C25 118.2(3) . . ? C27 C26 C29 120.8(3) . . ? C25 C26 C29 120.8(3) . . ? C21 C20 N1 109.3(2) . . ? C21 C20 H20 125.4 . . ? N1 C20 H20 125.4 . . ? C34 C35 N6 106.3(3) . . ? C34 C35 H35 126.8 . . ? N6 C35 H35 126.8 . . ? C37 C38 C39 121.1(3) . . ? C37 C38 H38 119.5 . . ? C39 C38 H38 119.5 . . ? C16 C15 C14 120.3(2) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C38 C37 C42 118.0(3) . . ? C38 C37 C36 121.1(3) . . ? C42 C37 C36 120.9(3) . . ? O6 C18 C18 105.9(3) . 3_355 ? O6 C18 H18A 110.6 . . ? C18 C18 H18A 110.6 3_355 . ? O6 C18 H18B 110.6 . . ? C18 C18 H18B 110.6 3_355 . ? H18A C18 H18B 108.7 . . ? C35 C34 N5 110.3(2) . . ? C35 C34 H34 124.9 . . ? N5 C34 H34 124.9 . . ? C12 C17 C16 120.2(2) . . ? C12 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? N5 C33 N6 112.1(2) . . ? N5 C33 H33 124.0 . . ? N6 C33 H33 124.0 . . ? C26 C27 C28 121.5(3) . . ? C26 C27 H27 119.2 . . ? C28 C27 H27 119.2 . . ? N2 C22 C23 112.9(2) . . ? N2 C22 H22A 109.0 . . ? C23 C22 H22A 109.0 . . ? N2 C22 H22B 109.0 . . ? C23 C22 H22B 109.0 . . ? H22A C22 H22B 107.8 . . ? N6 C36 C37 110.1(2) . . ? N6 C36 H36A 109.6 . . ? C37 C36 H36A 109.6 . . ? N6 C36 H36B 109.6 . . ? C37 C36 H36B 109.6 . . ? H36A C36 H36B 108.2 . . ? C7 C8 C3 120.9(2) . . ? C7 C8 H8 119.5 . . ? C3 C8 H8 119.5 . . ? C26 C25 C24 120.5(3) . . ? C26 C25 H25 119.8 . . ? C24 C25 H25 119.8 . . ? C23 C24 C25 121.3(3) . . ? C23 C24 H24 119.4 . . ? C25 C24 H24 119.4 . . ? C23 C28 C27 120.0(3) . . ? C23 C28 H28 120.0 . . ? C27 C28 H28 120.0 . . ? C42 C41 C40 121.1(3) . . ? C42 C41 H41 119.5 . . ? C40 C41 H41 119.5 . . ? C41 C42 C37 121.2(3) . . ? C41 C42 H42 119.4 . . ? C37 C42 H42 119.4 . . ? O9 C11 O10 119.5(2) . . ? O9 C11 C14 120.1(2) . . ? O10 C11 C14 120.4(2) . . ? O9 C11 Ni1 60.07(13) . 2_545 ? O10 C11 Ni1 59.46(13) . 2_545 ? C14 C11 Ni1 178.71(19) . 2_545 ? C30 N3 C31 106.5(2) . . ? C30 N3 C29 126.5(3) . . ? C31 N3 C29 126.9(3) . . ? N3 C29 C26 115.0(2) . . ? N3 C29 H29A 108.5 . . ? C26 C29 H29A 108.5 . . ? N3 C29 H29B 108.5 . . ? C26 C29 H29B 108.5 . . ? H29A C29 H29B 107.5 . . ? C31 C32 N4 109.8(3) . . ? C31 C32 H32 125.1 . . ? N4 C32 H32 125.1 . . ? N4 C30 N3 112.8(3) . . ? N4 C30 H30 123.6 . . ? N3 C30 H30 123.6 . . ? C32 C31 N3 107.0(3) . . ? C32 C31 H31 126.5 . . ? N3 C31 H31 126.5 . . ? C30 N4 C32 103.9(2) . . ? C30 N4 Ni1 129.3(2) . 4_566 ? C32 N4 Ni1 126.80(18) . 4_566 ? C44 N7 C45 106.6(2) . . ? C44 N7 C43 125.4(2) . . ? C45 N7 C43 127.8(2) . . ? C40 C39 C38 120.9(3) . . ? C40 C39 H39 119.5 . . ? C38 C39 H39 119.5 . . ? N7 C43 C40 114.4(2) . . ? N7 C43 H43A 108.7 . . ? C40 C43 H43A 108.7 . . ? N7 C43 H43B 108.7 . . ? C40 C43 H43B 108.7 . . ? H43A C43 H43B 107.6 . . ? N8 C44 N7 111.9(2) . . ? N8 C44 H44 124.1 . . ? N7 C44 H44 124.1 . . ? C45 C46 N8 109.3(3) . . ? C45 C46 H46 125.3 . . ? N8 C46 H46 125.3 . . ? C46 C45 N7 107.1(2) . . ? C46 C45 H45 126.5 . . ? N7 C45 H45 126.5 . . ? C44 N8 C46 105.1(2) . . ? C44 N8 Ni2 122.03(15) . 2_655 ? C46 N8 Ni2 132.9(2) . 2_655 ? C11 O10 Ni1 90.13(14) . 2_545 ? C11 O9 Ni1 89.78(14) . 2_545 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N5 Ni2 O8 C10 -82.58(15) . . . . ? N8 Ni2 O8 C10 -179.70(14) 2_645 . . . ? O3 Ni2 O8 C10 63.9(3) . . . . ? O4 Ni2 O8 C10 88.06(14) . . . . ? O7 Ni2 O8 C10 -1.09(13) . . . . ? C2 Ni2 O8 C10 81.12(16) . . . . ? N5 Ni2 O4 C2 -11.9(2) . . . . ? N8 Ni2 O4 C2 96.88(14) 2_645 . . . ? O8 Ni2 O4 C2 -169.52(13) . . . . ? O3 Ni2 O4 C2 1.01(13) . . . . ? O7 Ni2 O4 C2 -108.45(14) . . . . ? C10 Ni2 O4 C2 -138.49(14) . . . . ? N5 Ni2 O3 C2 173.66(14) . . . . ? N8 Ni2 O3 C2 -89.70(14) 2_645 . . . ? O8 Ni2 O3 C2 26.3(3) . . . . ? O4 Ni2 O3 C2 -1.00(13) . . . . ? O7 Ni2 O3 C2 83.06(15) . . . . ? C10 Ni2 O3 C2 68.01(18) . . . . ? N5 Ni2 O7 C10 106.81(15) . . . . ? N8 Ni2 O7 C10 4.3(2) 2_645 . . . ? O8 Ni2 O7 C10 1.11(14) . . . . ? O3 Ni2 O7 C10 -159.04(14) . . . . ? O4 Ni2 O7 C10 -97.55(15) . . . . ? C2 Ni2 O7 C10 -127.36(15) . . . . ? N1 Ni1 O1 C1 71.7(2) . . . . ? N4 Ni1 O1 C1 167.8(2) 4_565 . . . ? O1W Ni1 O1 C1 -17.49(19) . . . . ? O10 Ni1 O1 C1 -102.3(3) 2 . . . ? O9 Ni1 O1 C1 -98.69(19) 2 . . . ? C11 Ni1 O1 C1 -98.7(2) 2 . . . ? O1 Ni1 N1 C19 158.31(19) . . . . ? N4 Ni1 N1 C19 68.8(2) 4_565 . . . ? O1W Ni1 N1 C19 -113.4(2) . . . . ? O10 Ni1 N1 C19 -23.4(2) 2 . . . ? O9 Ni1 N1 C19 -45.5(3) 2 . . . ? C11 Ni1 N1 C19 -30.4(2) 2 . . . ? O1 Ni1 N1 C20 -27.7(2) . . . . ? N4 Ni1 N1 C20 -117.2(2) 4_565 . . . ? O1W Ni1 N1 C20 60.7(2) . . . . ? O10 Ni1 N1 C20 150.7(2) 2 . . . ? O9 Ni1 N1 C20 128.5(2) 2 . . . ? C11 Ni1 N1 C20 143.6(2) 2 . . . ? N8 Ni2 N5 C33 -31.5(2) 2_645 . . . ? O8 Ni2 N5 C33 -126.3(2) . . . . ? O3 Ni2 N5 C33 65.0(2) . . . . ? O4 Ni2 N5 C33 76.4(3) . . . . ? O7 Ni2 N5 C33 173.9(2) . . . . ? C2 Ni2 N5 C33 69.0(2) . . . . ? C10 Ni2 N5 C33 -157.1(2) . . . . ? N8 Ni2 N5 C34 164.2(2) 2_645 . . . ? O8 Ni2 N5 C34 69.3(2) . . . . ? O3 Ni2 N5 C34 -99.3(2) . . . . ? O4 Ni2 N5 C34 -87.9(3) . . . . ? O7 Ni2 N5 C34 9.6(2) . . . . ? C2 Ni2 N5 C34 -95.4(2) . . . . ? C10 Ni2 N5 C34 38.5(2) . . . . ? C15 C14 C13 C12 1.5(4) . . . . ? C11 C14 C13 C12 -175.9(2) . . . . ? C17 C12 C13 C14 -1.3(4) . . . . ? C10 C12 C13 C14 175.9(2) . . . . ? Ni2 O4 C2 O3 -1.7(2) . . . . ? Ni2 O4 C2 C3 175.4(2) . . . . ? Ni2 O3 C2 O4 1.8(2) . . . . ? Ni2 O3 C2 C3 -175.39(18) . . . . ? N5 Ni2 C2 O4 173.98(12) . . . . ? N8 Ni2 C2 O4 -84.93(14) 2_645 . . . ? O8 Ni2 C2 O4 13.46(17) . . . . ? O3 Ni2 C2 O4 -178.3(2) . . . . ? O7 Ni2 C2 O4 75.93(14) . . . . ? C10 Ni2 C2 O4 48.82(17) . . . . ? N5 Ni2 C2 O3 -7.74(17) . . . . ? N8 Ni2 C2 O3 93.35(14) 2_645 . . . ? O8 Ni2 C2 O3 -168.26(12) . . . . ? O4 Ni2 C2 O3 178.3(2) . . . . ? O7 Ni2 C2 O3 -105.78(14) . . . . ? C10 Ni2 C2 O3 -132.90(14) . . . . ? N5 Ni2 C2 C3 42.2(18) . . . . ? N8 Ni2 C2 C3 143.3(18) 2_645 . . . ? O8 Ni2 C2 C3 -118.3(18) . . . . ? O3 Ni2 C2 C3 50.0(18) . . . . ? O4 Ni2 C2 C3 -131.7(18) . . . . ? O7 Ni2 C2 C3 -55.8(18) . . . . ? C10 Ni2 C2 C3 -82.9(18) . . . . ? C18 O6 C16 C15 8.5(4) . . . . ? C18 O6 C16 C17 -170.6(2) . . . . ? C5 O5 C9 C9 173.5(2) . . . 3_456 ? C20 N1 C19 N2 -0.2(3) . . . . ? Ni1 N1 C19 N2 175.01(16) . . . . ? C21 N2 C19 N1 0.5(3) . . . . ? C22 N2 C19 N1 -178.2(2) . . . . ? C19 N2 C21 C20 -0.6(3) . . . . ? C22 N2 C21 C20 178.1(2) . . . . ? C9 O5 C5 C4 -164.8(2) . . . . ? C9 O5 C5 C6 14.6(3) . . . . ? C3 C4 C5 O5 177.3(2) . . . . ? C3 C4 C5 C6 -2.1(4) . . . . ? C7 C6 C5 O5 -179.4(2) . . . . ? C7 C6 C5 C4 -0.1(4) . . . . ? C5 C4 C3 C8 2.8(4) . . . . ? C5 C4 C3 C2 -170.5(2) . . . . ? O4 C2 C3 C4 -23.0(3) . . . . ? O3 C2 C3 C4 154.1(2) . . . . ? Ni2 C2 C3 C4 106.5(18) . . . . ? O4 C2 C3 C8 163.7(2) . . . . ? O3 C2 C3 C8 -19.1(3) . . . . ? Ni2 C2 C3 C8 -66.8(18) . . . . ? Ni1 O1 C1 O2 -3.3(3) . . . . ? Ni1 O1 C1 C7 176.69(14) . . . . ? C5 C6 C7 C8 1.5(3) . . . . ? C5 C6 C7 C1 178.0(2) . . . . ? O2 C1 C7 C8 179.2(2) . . . . ? O1 C1 C7 C8 -0.8(3) . . . . ? O2 C1 C7 C6 2.7(3) . . . . ? O1 C1 C7 C6 -177.3(2) . . . . ? Ni2 O7 C10 O8 -1.8(2) . . . . ? Ni2 O7 C10 C12 176.8(2) . . . . ? Ni2 O8 C10 O7 2.0(2) . . . . ? Ni2 O8 C10 C12 -176.61(18) . . . . ? C17 C12 C10 O7 13.0(4) . . . . ? C13 C12 C10 O7 -164.2(2) . . . . ? C17 C12 C10 O8 -168.4(2) . . . . ? C13 C12 C10 O8 14.4(3) . . . . ? C17 C12 C10 Ni2 168.8(12) . . . . ? C13 C12 C10 Ni2 -8.4(14) . . . . ? N5 Ni2 C10 O7 -74.96(15) . . . . ? N8 Ni2 C10 O7 -177.74(13) 2_645 . . . ? O8 Ni2 C10 O7 -178.1(2) . . . . ? O3 Ni2 C10 O7 29.3(2) . . . . ? O4 Ni2 C10 O7 85.38(15) . . . . ? C2 Ni2 C10 O7 62.56(17) . . . . ? N5 Ni2 C10 O8 103.15(14) . . . . ? N8 Ni2 C10 O8 0.36(17) 2_645 . . . ? O3 Ni2 C10 O8 -152.54(13) . . . . ? O4 Ni2 C10 O8 -96.51(14) . . . . ? O7 Ni2 C10 O8 178.1(2) . . . . ? C2 Ni2 C10 O8 -119.33(14) . . . . ? N5 Ni2 C10 C12 127.7(13) . . . . ? N8 Ni2 C10 C12 24.9(14) 2_645 . . . ? O8 Ni2 C10 C12 24.5(13) . . . . ? O3 Ni2 C10 C12 -128.0(13) . . . . ? O4 Ni2 C10 C12 -72.0(13) . . . . ? O7 Ni2 C10 C12 -157.3(14) . . . . ? C2 Ni2 C10 C12 -94.8(13) . . . . ? N2 C21 C20 N1 0.5(3) . . . . ? C19 N1 C20 C21 -0.2(3) . . . . ? Ni1 N1 C20 C21 -175.09(17) . . . . ? C33 N6 C35 C34 -0.6(3) . . . . ? C36 N6 C35 C34 -166.9(3) . . . . ? O6 C16 C15 C14 -178.6(2) . . . . ? C17 C16 C15 C14 0.5(4) . . . . ? C13 C14 C15 C16 -1.1(4) . . . . ? C11 C14 C15 C16 176.3(2) . . . . ? C39 C38 C37 C42 1.4(4) . . . . ? C39 C38 C37 C36 179.8(3) . . . . ? C16 O6 C18 C18 175.5(3) . . . 3_355 ? N6 C35 C34 N5 0.3(3) . . . . ? C33 N5 C34 C35 0.2(3) . . . . ? Ni2 N5 C34 C35 166.70(19) . . . . ? C13 C12 C17 C16 0.7(3) . . . . ? C10 C12 C17 C16 -176.4(2) . . . . ? O6 C16 C17 C12 178.8(2) . . . . ? C15 C16 C17 C12 -0.3(4) . . . . ? C34 N5 C33 N6 -0.6(3) . . . . ? Ni2 N5 C33 N6 -168.33(17) . . . . ? C35 N6 C33 N5 0.8(3) . . . . ? C36 N6 C33 N5 167.2(2) . . . . ? C25 C26 C27 C28 2.1(4) . . . . ? C29 C26 C27 C28 -172.6(2) . . . . ? C19 N2 C22 C23 93.2(3) . . . . ? C21 N2 C22 C23 -85.3(3) . . . . ? C24 C23 C22 N2 -83.4(3) . . . . ? C28 C23 C22 N2 99.9(3) . . . . ? C33 N6 C36 C37 -92.3(3) . . . . ? C35 N6 C36 C37 71.4(3) . . . . ? C38 C37 C36 N6 -115.9(3) . . . . ? C42 C37 C36 N6 62.5(3) . . . . ? C6 C7 C8 C3 -0.7(3) . . . . ? C1 C7 C8 C3 -177.2(2) . . . . ? C4 C3 C8 C7 -1.4(4) . . . . ? C2 C3 C8 C7 171.9(2) . . . . ? C27 C26 C25 C24 -1.6(4) . . . . ? C29 C26 C25 C24 173.1(2) . . . . ? C28 C23 C24 C25 2.1(4) . . . . ? C22 C23 C24 C25 -174.5(2) . . . . ? C26 C25 C24 C23 -0.5(4) . . . . ? C24 C23 C28 C27 -1.7(4) . . . . ? C22 C23 C28 C27 175.0(2) . . . . ? C26 C27 C28 C23 -0.4(4) . . . . ? C39 C40 C41 C42 1.2(4) . . . . ? C43 C40 C41 C42 -179.9(2) . . . . ? C40 C41 C42 C37 -0.6(4) . . . . ? C38 C37 C42 C41 -0.7(4) . . . . ? C36 C37 C42 C41 -179.1(3) . . . . ? C13 C14 C11 O9 6.0(4) . . . . ? C15 C14 C11 O9 -171.4(2) . . . . ? C13 C14 C11 O10 -174.4(2) . . . . ? C15 C14 C11 O10 8.3(4) . . . . ? C13 C14 C11 Ni1 -92(8) . . . 2_545 ? C15 C14 C11 Ni1 91(8) . . . 2_545 ? C30 N3 C29 C26 98.1(3) . . . . ? C31 N3 C29 C26 -86.7(4) . . . . ? C27 C26 C29 N3 -83.8(4) . . . . ? C25 C26 C29 N3 101.6(3) . . . . ? C31 N3 C30 N4 1.2(3) . . . . ? C29 N3 C30 N4 177.3(2) . . . . ? N4 C32 C31 N3 0.2(3) . . . . ? C30 N3 C31 C32 -0.8(3) . . . . ? C29 N3 C31 C32 -176.8(2) . . . . ? N3 C30 N4 C32 -1.1(3) . . . . ? N3 C30 N4 Ni1 -179.17(16) . . . 4_566 ? C31 C32 N4 C30 0.5(3) . . . . ? C31 C32 N4 Ni1 178.67(17) . . . 4_566 ? C41 C40 C39 C38 -0.5(4) . . . . ? C43 C40 C39 C38 -179.3(2) . . . . ? C37 C38 C39 C40 -0.8(4) . . . . ? C44 N7 C43 C40 -96.2(3) . . . . ? C45 N7 C43 C40 77.0(3) . . . . ? C41 C40 C43 N7 162.5(2) . . . . ? C39 C40 C43 N7 -18.7(4) . . . . ? C45 N7 C44 N8 -1.0(3) . . . . ? C43 N7 C44 N8 173.3(2) . . . . ? N8 C46 C45 N7 -0.7(3) . . . . ? C44 N7 C45 C46 1.0(3) . . . . ? C43 N7 C45 C46 -173.2(3) . . . . ? N7 C44 N8 C46 0.6(3) . . . . ? N7 C44 N8 Ni2 -179.24(15) . . . 2_655 ? C45 C46 N8 C44 0.0(3) . . . . ? C45 C46 N8 Ni2 179.89(19) . . . 2_655 ? O9 C11 O10 Ni1 -1.8(2) . . . 2_545 ? C14 C11 O10 Ni1 178.5(2) . . . 2_545 ? O10 C11 O9 Ni1 1.8(2) . . . 2_545 ? C14 C11 O9 Ni1 -178.5(2) . . . 2_545 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.405 _refine_diff_density_min -0.314 _refine_diff_density_rms 0.047 #============================================================================= data_compound-3 _database_code_depnum_ccdc_archive 'CCDC 834800' #TrackingRef '- CIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H31 Co2 N6 O10, 2.5(H2 O)' _chemical_formula_sum 'C39 H36 Co2 N6 O12.50' _chemical_formula_weight 906.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M p-1 _symmetry_space_group_name_hall '-P 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.6861(8) _cell_length_b 13.3872(10) _cell_length_c 13.4602(8) _cell_angle_alpha 91.588(5) _cell_angle_beta 100.888(5) _cell_angle_gamma 115.561(7) _cell_volume 2009.7(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2322 _cell_measurement_theta_min 2.9923 _cell_measurement_theta_max 25.2940 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.498 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 932 _exptl_absorpt_coefficient_mu 0.897 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.98452 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _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 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13200 _diffrn_reflns_av_R_equivalents 0.0574 _diffrn_reflns_av_sigmaI/netI 0.2336 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 25.35 _reflns_number_total 7336 _reflns_number_gt 2995 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^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 7336 _refine_ls_number_parameters 541 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1300 _refine_ls_R_factor_gt 0.0462 _refine_ls_wR_factor_ref 0.0663 _refine_ls_wR_factor_gt 0.0613 _refine_ls_goodness_of_fit_ref 0.797 _refine_ls_restrained_S_all 0.810 _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 Co2 Co 1.57937(7) 0.00961(6) 1.59650(5) 0.0340(2) Uani 1 1 d . . . Co1 Co 1.75711(6) 0.54076(5) 1.06451(5) 0.0325(2) Uani 1 1 d . . . O1 O 1.7339(3) 0.4180(3) 1.1533(2) 0.0403(10) Uani 1 1 d . . . O2 O 1.8961(3) 0.5646(3) 1.2341(2) 0.0475(11) Uani 1 1 d . . . O3 O 1.7027(3) 0.1119(2) 1.5186(2) 0.0401(10) Uani 1 1 d . . . N1 N 1.7222(4) 0.6599(3) 1.1251(3) 0.0374(12) Uani 1 1 d . . . N3 N 1.8978(4) 1.3117(3) 0.9893(3) 0.0390(12) Uani 1 1 d . . . N4 N 2.0893(4) 1.3996(3) 0.9881(3) 0.0402(12) Uani 1 1 d . . . N2 N 1.6434(4) 0.7761(4) 1.1383(4) 0.0438(12) Uani 1 1 d . . . N5 N 1.6800(4) -0.0583(3) 1.6726(3) 0.0377(12) Uani 1 1 d . . . C3 C 1.7792(4) 0.2407(4) 1.4042(3) 0.0324(13) Uani 1 1 d . . . C26 C 1.7190(4) 1.1436(4) 0.9949(4) 0.0373(14) Uani 1 1 d . . . C24 C 1.6228(5) 1.0337(5) 1.1167(4) 0.0476(16) Uani 1 1 d . . . H24 H 1.5886 1.0282 1.1729 0.057 Uiso 1 1 calc R . . C33 C 1.7967(5) -0.0234(5) 1.6960(4) 0.0522(17) Uani 1 1 d . . . H33 H 1.8517 0.0457 1.6838 0.063 Uiso 1 1 calc R . . C5 C 1.8479(4) 0.3946(4) 1.3056(3) 0.0300(13) Uani 1 1 d . . . C21 C 1.7276(5) 0.7970(5) 1.2251(4) 0.0550(18) Uani 1 1 d . . . H21 H 1.7489 0.8517 1.2793 0.066 Uiso 1 1 calc R . . C4 C 1.7542(4) 0.3009(4) 1.3253(3) 0.0354(14) Uani 1 1 d . . . H4 H 1.6764 0.2778 1.2877 0.042 Uiso 1 1 calc R . . N6 N 1.8282(5) -0.1003(4) 1.7404(3) 0.0604(15) Uani 1 1 d . . . C8 C 1.8943(5) 0.2746(4) 1.4553(3) 0.0408(15) Uani 1 1 d . . . H8 H 1.9102 0.2352 1.5071 0.049 Uiso 1 1 calc R . . C31 C 2.0769(5) 1.4007(5) 1.0867(4) 0.0561(17) Uani 1 1 d . . . H31 H 2.1392 1.4330 1.1442 0.067 Uiso 1 1 calc R . . C23 C 1.6252(4) 0.9422(5) 1.0729(4) 0.0410(15) Uani 1 1 d . . . C1 C 1.8247(5) 0.4641(5) 1.2267(4) 0.0363(14) Uani 1 1 d . . . C19 C 1.6438(5) 0.6940(4) 1.0807(4) 0.0412(15) Uani 1 1 d . . . H19 H 1.5944 0.6641 1.0162 0.049 Uiso 1 1 calc R . . C7 C 1.9896(4) 0.3665(4) 1.4325(3) 0.0375(15) Uani 1 1 d . . . C29 C 1.7695(4) 1.2535(4) 0.9525(4) 0.0472(16) Uani 1 1 d . . . H29A H 1.7503 1.2405 0.8787 0.057 Uiso 1 1 calc R . . H29B H 1.7332 1.2992 0.9728 0.057 Uiso 1 1 calc R . . C30 C 1.9797(5) 1.3445(4) 0.9333(4) 0.0422(16) Uani 1 1 d . . . H30 H 1.9613 1.3299 0.8626 0.051 Uiso 1 1 calc R . . C27 C 1.7208(5) 1.0516(5) 0.9507(4) 0.0535(17) Uani 1 1 d . . . H27 H 1.7545 1.0572 0.8942 0.064 Uiso 1 1 calc R . . C34 C 1.6319(5) -0.1634(4) 1.7024(4) 0.0564(18) Uani 1 1 d . . . H34 H 1.5506 -0.2093 1.6954 0.068 Uiso 1 1 calc R . . C28 C 1.6737(5) 0.9509(4) 0.9881(4) 0.0576(17) Uani 1 1 d . . . H28 H 1.6745 0.8887 0.9564 0.069 Uiso 1 1 calc R . . C6 C 1.9645(5) 0.4285(4) 1.3584(3) 0.0384(15) Uani 1 1 d . . . H6 H 2.0261 0.4926 1.3447 0.046 Uiso 1 1 calc R . . C25 C 1.6705(4) 1.1346(4) 1.0788(3) 0.0487(16) Uani 1 1 d . . . H25 H 1.6697 1.1969 1.1104 0.058 Uiso 1 1 calc R . . C32 C 1.9585(5) 1.3468(5) 1.0867(4) 0.0531(17) Uani 1 1 d . . . H32 H 1.9253 1.3360 1.1438 0.064 Uiso 1 1 calc R . . C20 C 1.7753(5) 0.7246(5) 1.2194(4) 0.0441(15) Uani 1 1 d . . . H20 H 1.8332 0.7191 1.2697 0.053 Uiso 1 1 calc R . . C37 C 1.9789(5) -0.0389(6) 1.9001(4) 0.0549(18) Uani 1 1 d . . . C22 C 1.5645(5) 0.8291(4) 1.1105(4) 0.0564(17) Uani 1 1 d . . . H22A H 1.5344 0.8387 1.1693 0.068 Uiso 1 1 calc R . . H22B H 1.4963 0.7798 1.0574 0.068 Uiso 1 1 calc R . . C2 C 1.6775(5) 0.1446(4) 1.4331(4) 0.0342(14) Uani 1 1 d . . . C39 C 1.9663(5) -0.0724(6) 2.0679(5) 0.073(2) Uani 1 1 d . . . H39 H 1.9428 -0.1224 2.1152 0.088 Uiso 1 1 calc R . . C38 C 1.9447(5) -0.1131(5) 1.9677(5) 0.072(2) Uani 1 1 d . . . H38 H 1.9076 -0.1895 1.9469 0.087 Uiso 1 1 calc R . . C35 C 1.7216(6) -0.1895(5) 1.7438(4) 0.070(2) Uani 1 1 d . . . H35 H 1.7126 -0.2557 1.7697 0.084 Uiso 1 1 calc R . . C36 C 1.9509(5) -0.0830(5) 1.7893(4) 0.078(2) Uani 1 1 d . . . H36A H 2.0086 -0.0303 1.7554 0.093 Uiso 1 1 calc R . . H36B H 1.9561 -0.1531 1.7834 0.093 Uiso 1 1 calc R . . O4 O 1.5764(3) 0.1037(3) 1.3729(2) 0.0392(10) Uani 1 1 d . . . O6 O 2.3390(3) 0.4092(3) 1.5269(2) 0.0562(11) Uani 1 1 d . . . O5 O 2.1020(3) 0.3897(3) 1.4885(3) 0.0547(12) Uani 1 1 d . . . C9 C 2.2040(5) 0.4861(4) 1.4717(4) 0.0588(18) Uani 1 1 d . . . H9A H 2.1914 0.5522 1.4785 0.071 Uiso 1 1 calc R . . H9B H 2.2158 0.4762 1.4036 0.071 Uiso 1 1 calc R . . C10 C 2.3125(5) 0.4983(5) 1.5510(4) 0.0570(18) Uani 1 1 d . . . H10A H 2.3804 0.5692 1.5503 0.068 Uiso 1 1 calc R . . H10B H 2.2955 0.4957 1.6184 0.068 Uiso 1 1 calc R . . C12 C 2.4845(4) 0.4632(4) 1.6926(3) 0.0364(14) Uani 1 1 d . . . H12 H 2.4753 0.5268 1.7075 0.044 Uiso 1 1 calc R . . C11 C 2.4213(5) 0.3939(4) 1.5987(4) 0.0387(15) Uani 1 1 d . . . C17 C 2.6200(4) 0.5048(4) 1.8624(3) 0.0345(15) Uani 1 1 d . . . C14 C 2.5751(4) 0.3426(4) 1.7363(3) 0.0333(14) Uani 1 1 d . . . H14 H 2.6266 0.3248 1.7828 0.040 Uiso 1 1 calc R . . C16 C 2.4378(4) 0.3012(4) 1.5751(4) 0.0389(15) Uani 1 1 d . . . H16 H 2.3967 0.2561 1.5133 0.047 Uiso 1 1 calc R . . C13 C 2.5596(4) 0.4355(4) 1.7613(3) 0.0325(14) Uani 1 1 d . . . C15 C 2.5160(4) 0.2757(4) 1.6443(4) 0.0344(14) Uani 1 1 d . . . C18 C 2.5304(4) 0.1728(4) 1.6182(4) 0.0348(14) Uani 1 1 d . . . O8 O 2.6445(3) 0.4524(2) 1.9352(2) 0.0380(10) Uani 1 1 d . . . O10 O 2.5995(3) 0.1487(3) 1.6835(2) 0.0483(11) Uani 1 1 d . . . O9 O 2.4715(3) 0.1130(3) 1.5361(2) 0.0482(11) Uani 1 1 d . . . O7 O 2.6450(3) 0.6031(3) 1.8712(2) 0.0585(12) Uani 1 1 d . . . O1W O 1.8320(4) -0.0139(4) 1.4410(3) 0.1135(17) Uani 1 1 d . . . O2W O 2.0794(5) 0.1541(5) 1.4882(5) 0.182(3) Uani 1 1 d . . . O3W O 2.1255(6) 0.7365(7) 1.3024(4) 0.113(4) Uani 0.50 1 d PU . . 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 Co2 0.0389(5) 0.0326(5) 0.0318(4) 0.0059(4) 0.0050(4) 0.0181(4) Co1 0.0350(5) 0.0292(5) 0.0314(4) 0.0043(4) 0.0045(4) 0.0136(4) O1 0.038(2) 0.043(2) 0.039(2) 0.0157(18) -0.0005(18) 0.0207(19) O2 0.050(3) 0.039(2) 0.053(2) 0.017(2) 0.0143(19) 0.018(2) O3 0.039(2) 0.040(2) 0.0361(19) 0.0124(18) 0.0043(17) 0.0142(18) N1 0.044(3) 0.030(3) 0.044(3) 0.005(2) 0.013(2) 0.020(2) N3 0.042(3) 0.045(3) 0.037(3) 0.012(2) 0.014(3) 0.023(2) N4 0.041(3) 0.044(3) 0.036(3) 0.007(2) 0.014(2) 0.018(2) N2 0.046(3) 0.031(3) 0.062(3) 0.005(3) 0.021(3) 0.021(3) N5 0.038(3) 0.037(3) 0.037(2) 0.006(2) -0.002(2) 0.019(2) C3 0.030(3) 0.038(3) 0.030(3) -0.001(3) -0.001(3) 0.019(3) C26 0.033(3) 0.042(4) 0.043(3) 0.013(3) 0.013(3) 0.021(3) C24 0.057(4) 0.054(4) 0.042(3) 0.007(3) 0.023(3) 0.030(3) C33 0.059(4) 0.055(4) 0.045(3) 0.011(3) 0.009(3) 0.028(4) C5 0.032(3) 0.032(3) 0.023(3) 0.009(2) 0.005(2) 0.011(3) C21 0.073(5) 0.039(4) 0.050(4) -0.003(3) 0.027(4) 0.018(4) C4 0.043(3) 0.046(3) 0.023(3) 0.003(3) 0.002(3) 0.028(3) N6 0.066(4) 0.063(4) 0.062(3) 0.012(3) 0.006(3) 0.040(3) C8 0.054(4) 0.044(4) 0.033(3) 0.019(3) 0.010(3) 0.028(3) C31 0.058(4) 0.065(4) 0.038(3) -0.009(3) 0.003(3) 0.026(4) C23 0.036(4) 0.042(4) 0.056(4) 0.010(3) 0.019(3) 0.025(3) C1 0.033(4) 0.054(4) 0.035(3) 0.013(3) 0.018(3) 0.026(3) C19 0.042(4) 0.033(4) 0.050(4) 0.007(3) 0.016(3) 0.015(3) C7 0.024(3) 0.046(4) 0.036(3) 0.003(3) -0.004(3) 0.014(3) C29 0.027(3) 0.047(4) 0.070(4) 0.019(3) 0.013(3) 0.017(3) C30 0.040(4) 0.045(4) 0.038(3) 0.013(3) 0.010(3) 0.014(3) C27 0.065(4) 0.060(4) 0.049(4) 0.011(4) 0.035(3) 0.030(4) C34 0.059(4) 0.042(4) 0.064(4) 0.015(3) 0.003(3) 0.023(3) C28 0.089(5) 0.047(4) 0.069(4) 0.008(3) 0.050(4) 0.046(4) C6 0.045(4) 0.034(3) 0.038(3) 0.019(3) 0.013(3) 0.017(3) C25 0.069(4) 0.038(4) 0.045(3) 0.007(3) 0.021(3) 0.025(3) C32 0.047(4) 0.071(5) 0.045(4) 0.000(3) 0.024(3) 0.025(4) C20 0.049(4) 0.046(4) 0.039(4) -0.004(3) 0.004(3) 0.026(3) C37 0.056(4) 0.068(5) 0.049(4) 0.018(4) 0.003(3) 0.037(4) C22 0.057(4) 0.046(4) 0.088(4) 0.023(4) 0.033(3) 0.036(3) C2 0.041(4) 0.030(3) 0.036(3) 0.011(3) 0.018(3) 0.014(3) C39 0.063(5) 0.060(5) 0.092(6) 0.042(5) 0.017(4) 0.021(4) C38 0.079(5) 0.063(5) 0.063(4) 0.012(4) -0.004(4) 0.030(4) C35 0.073(5) 0.045(4) 0.078(4) 0.025(4) 0.000(4) 0.018(4) C36 0.052(4) 0.108(6) 0.084(5) 0.003(4) -0.009(4) 0.056(4) O4 0.035(2) 0.042(2) 0.0348(19) 0.0099(18) 0.0020(18) 0.0141(19) O6 0.071(3) 0.070(3) 0.044(2) -0.005(2) -0.011(2) 0.057(2) O5 0.034(2) 0.050(3) 0.075(3) 0.026(2) 0.006(2) 0.014(2) C9 0.052(4) 0.055(4) 0.065(4) 0.008(4) -0.003(3) 0.025(4) C10 0.052(4) 0.060(4) 0.052(4) 0.006(3) -0.007(3) 0.027(4) C12 0.034(3) 0.033(3) 0.042(3) 0.004(3) 0.004(3) 0.016(3) C11 0.039(4) 0.044(4) 0.036(3) 0.009(3) 0.004(3) 0.023(3) C17 0.037(3) 0.036(4) 0.022(3) 0.002(3) 0.003(3) 0.009(3) C14 0.035(3) 0.042(4) 0.026(3) 0.012(3) 0.004(3) 0.021(3) C16 0.043(4) 0.040(4) 0.034(3) 0.005(3) 0.002(3) 0.021(3) C13 0.041(3) 0.028(3) 0.030(3) 0.009(3) 0.007(3) 0.017(3) C15 0.037(3) 0.039(4) 0.037(3) 0.005(3) 0.009(3) 0.025(3) C18 0.030(3) 0.034(3) 0.042(3) 0.007(3) 0.007(3) 0.016(3) O8 0.037(2) 0.039(2) 0.0293(18) 0.0015(18) -0.0056(16) 0.0145(18) O10 0.068(3) 0.039(2) 0.046(2) -0.0009(19) 0.004(2) 0.035(2) O9 0.059(3) 0.044(2) 0.037(2) -0.0097(19) 0.003(2) 0.023(2) O7 0.094(3) 0.027(2) 0.044(2) -0.0026(19) 0.001(2) 0.023(2) O1W 0.142(5) 0.107(4) 0.103(3) -0.021(3) 0.002(3) 0.078(4) O2W 0.133(5) 0.112(5) 0.302(7) -0.002(5) 0.010(5) 0.072(4) O3W 0.072(5) 0.134(7) 0.013(3) -0.008(4) 0.005(4) -0.061(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co2 N5 2.016(4) . ? Co2 O4 2.032(3) 2_858 ? Co2 O10 2.064(4) 1_455 ? Co2 O3 2.067(3) . ? Co2 O9 2.187(4) 2_958 ? Co2 O9 2.393(4) 1_455 ? Co2 Co2 2.9000(13) 2_858 ? Co1 O8 1.989(3) 1_454 ? Co1 O1 2.010(2) . ? Co1 N1 2.020(4) . ? Co1 N4 2.036(4) 2_977 ? O1 C1 1.267(5) . ? O2 C1 1.245(5) . ? O3 C2 1.276(4) . ? N1 C19 1.318(6) . ? N1 C20 1.388(6) . ? N3 C30 1.328(5) . ? N3 C32 1.343(5) . ? N3 C29 1.443(5) . ? N4 C30 1.311(5) . ? N4 C31 1.366(5) . ? N4 Co1 2.036(4) 2_977 ? N2 C19 1.330(6) . ? N2 C21 1.356(6) . ? N2 C22 1.459(6) . ? N5 C33 1.315(6) . ? N5 C34 1.376(5) . ? C3 C8 1.358(6) . ? C3 C4 1.421(5) . ? C3 C2 1.501(6) . ? C26 C27 1.363(7) . ? C26 C25 1.370(6) . ? C26 C29 1.508(6) . ? C24 C23 1.361(7) . ? C24 C25 1.378(6) . ? C24 H24 0.9300 . ? C33 N6 1.370(6) . ? C33 H33 0.9300 . ? C5 C6 1.380(6) . ? C5 C4 1.381(5) . ? C5 C1 1.501(5) . ? C21 C20 1.353(7) . ? C21 H21 0.9300 . ? C4 H4 0.9300 . ? N6 C35 1.374(6) . ? N6 C36 1.484(6) . ? C8 C7 1.396(6) . ? C8 H8 0.9300 . ? C31 C32 1.358(6) . ? C31 H31 0.9300 . ? C23 C28 1.380(6) . ? C23 C22 1.525(6) . ? C19 H19 0.9300 . ? C7 O5 1.377(5) . ? C7 C6 1.392(6) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 H30 0.9300 . ? C27 C28 1.372(6) . ? C27 H27 0.9300 . ? C34 C35 1.357(7) . ? C34 H34 0.9300 . ? C28 H28 0.9300 . ? C6 H6 0.9300 . ? C25 H25 0.9300 . ? C32 H32 0.9300 . ? C20 H20 0.9300 . ? C37 C38 1.354(6) . ? C37 C39 1.359(8) 2_959 ? C37 C36 1.506(7) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C2 O4 1.256(5) . ? C39 C37 1.359(8) 2_959 ? C39 C38 1.372(8) . ? C39 H39 0.9300 . ? C38 H38 0.9300 . ? C35 H35 0.9300 . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? O4 Co2 2.032(3) 2_858 ? O6 C11 1.371(5) . ? O6 C10 1.416(6) . ? O5 C9 1.440(5) . ? C9 C10 1.518(6) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C12 C13 1.375(6) . ? C12 C11 1.418(6) . ? C12 H12 0.9300 . ? C11 C16 1.384(7) . ? C17 O7 1.210(5) . ? C17 O8 1.289(5) . ? C17 C13 1.491(6) . ? C14 C15 1.382(6) . ? C14 C13 1.382(7) . ? C14 H14 0.9300 . ? C16 C15 1.389(6) . ? C16 H16 0.9300 . ? C15 C18 1.505(7) . ? C18 O9 1.243(5) . ? C18 O10 1.270(5) . ? O8 Co1 1.989(3) 1_656 ? O10 Co2 2.064(3) 1_655 ? O9 Co2 2.187(4) 2_958 ? O9 Co2 2.393(4) 1_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Co2 O4 94.53(14) . 2_858 ? N5 Co2 O10 110.39(15) . 1_455 ? O4 Co2 O10 98.87(14) 2_858 1_455 ? N5 Co2 O3 97.99(15) . . ? O4 Co2 O3 161.39(12) 2_858 . ? O10 Co2 O3 89.63(13) 1_455 . ? N5 Co2 O9 89.37(15) . 2_958 ? O4 Co2 O9 83.06(13) 2_858 2_958 ? O10 Co2 O9 159.82(12) 1_455 2_958 ? O3 Co2 O9 83.37(12) . 2_958 ? N5 Co2 O9 169.05(15) . 1_455 ? O4 Co2 O9 86.40(12) 2_858 1_455 ? O10 Co2 O9 58.75(12) 1_455 1_455 ? O3 Co2 O9 83.92(12) . 1_455 ? O9 Co2 O9 101.57(12) 2_958 1_455 ? N5 Co2 Co2 143.30(13) . 2_858 ? O4 Co2 Co2 81.78(9) 2_858 2_858 ? O10 Co2 Co2 106.25(10) 1_455 2_858 ? O3 Co2 Co2 79.95(8) . 2_858 ? O9 Co2 Co2 53.93(9) 2_958 2_858 ? O9 Co2 Co2 47.63(9) 1_455 2_858 ? O8 Co1 O1 99.98(13) 1_454 . ? O8 Co1 N1 115.64(16) 1_454 . ? O1 Co1 N1 111.64(14) . . ? O8 Co1 N4 97.71(15) 1_454 2_977 ? O1 Co1 N4 115.88(15) . 2_977 ? N1 Co1 N4 114.46(17) . 2_977 ? C1 O1 Co1 102.3(3) . . ? C2 O3 Co2 125.6(3) . . ? C19 N1 C20 105.2(5) . . ? C19 N1 Co1 126.2(4) . . ? C20 N1 Co1 128.6(4) . . ? C30 N3 C32 106.0(4) . . ? C30 N3 C29 126.8(4) . . ? C32 N3 C29 127.1(5) . . ? C30 N4 C31 104.9(4) . . ? C30 N4 Co1 126.5(4) . 2_977 ? C31 N4 Co1 128.5(4) . 2_977 ? C19 N2 C21 106.2(5) . . ? C19 N2 C22 125.0(5) . . ? C21 N2 C22 128.8(6) . . ? C33 N5 C34 105.4(4) . . ? C33 N5 Co2 131.1(3) . . ? C34 N5 Co2 123.2(4) . . ? C8 C3 C4 119.2(4) . . ? C8 C3 C2 121.3(4) . . ? C4 C3 C2 119.5(4) . . ? C27 C26 C25 118.9(5) . . ? C27 C26 C29 120.8(5) . . ? C25 C26 C29 120.3(5) . . ? C23 C24 C25 120.7(5) . . ? C23 C24 H24 119.6 . . ? C25 C24 H24 119.6 . . ? N5 C33 N6 112.4(5) . . ? N5 C33 H33 123.8 . . ? N6 C33 H33 123.8 . . ? C6 C5 C4 121.6(4) . . ? C6 C5 C1 118.0(4) . . ? C4 C5 C1 120.3(4) . . ? C20 C21 N2 108.2(6) . . ? C20 C21 H21 125.9 . . ? N2 C21 H21 125.9 . . ? C5 C4 C3 118.6(4) . . ? C5 C4 H4 120.7 . . ? C3 C4 H4 120.7 . . ? C33 N6 C35 105.1(5) . . ? C33 N6 C36 126.8(5) . . ? C35 N6 C36 127.3(5) . . ? C3 C8 C7 122.2(4) . . ? C3 C8 H8 118.9 . . ? C7 C8 H8 118.9 . . ? C32 C31 N4 108.5(5) . . ? C32 C31 H31 125.8 . . ? N4 C31 H31 125.8 . . ? C24 C23 C28 119.0(5) . . ? C24 C23 C22 120.4(5) . . ? C28 C23 C22 120.3(5) . . ? O2 C1 O1 121.8(4) . . ? O2 C1 C5 119.2(5) . . ? O1 C1 C5 118.9(5) . . ? N1 C19 N2 112.5(5) . . ? N1 C19 H19 123.8 . . ? N2 C19 H19 123.8 . . ? O5 C7 C6 125.4(4) . . ? O5 C7 C8 116.0(4) . . ? C6 C7 C8 118.6(5) . . ? N3 C29 C26 110.6(4) . . ? N3 C29 H29A 109.5 . . ? C26 C29 H29A 109.5 . . ? N3 C29 H29B 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 108.1 . . ? N4 C30 N3 112.9(4) . . ? N4 C30 H30 123.5 . . ? N3 C30 H30 123.5 . . ? C26 C27 C28 121.2(5) . . ? C26 C27 H27 119.4 . . ? C28 C27 H27 119.4 . . ? C35 C34 N5 109.5(5) . . ? C35 C34 H34 125.2 . . ? N5 C34 H34 125.2 . . ? C27 C28 C23 119.9(5) . . ? C27 C28 H28 120.1 . . ? C23 C28 H28 120.1 . . ? C5 C6 C7 119.7(4) . . ? C5 C6 H6 120.1 . . ? C7 C6 H6 120.1 . . ? C26 C25 C24 120.3(5) . . ? C26 C25 H25 119.8 . . ? C24 C25 H25 119.8 . . ? N3 C32 C31 107.7(5) . . ? N3 C32 H32 126.2 . . ? C31 C32 H32 126.2 . . ? C21 C20 N1 107.8(5) . . ? C21 C20 H20 126.1 . . ? N1 C20 H20 126.1 . . ? C38 C37 C39 120.1(6) . 2_959 ? C38 C37 C36 118.3(7) . . ? C39 C37 C36 121.6(6) 2_959 . ? N2 C22 C23 113.7(4) . . ? N2 C22 H22A 108.8 . . ? C23 C22 H22A 108.8 . . ? N2 C22 H22B 108.8 . . ? C23 C22 H22B 108.8 . . ? H22A C22 H22B 107.7 . . ? O4 C2 O3 125.6(4) . . ? O4 C2 C3 118.6(4) . . ? O3 C2 C3 115.8(4) . . ? C37 C39 C38 121.8(6) 2_959 . ? C37 C39 H39 119.1 2_959 . ? C38 C39 H39 119.1 . . ? C37 C38 C39 118.1(6) . . ? C37 C38 H38 121.0 . . ? C39 C38 H38 121.0 . . ? C34 C35 N6 107.5(5) . . ? C34 C35 H35 126.2 . . ? N6 C35 H35 126.2 . . ? N6 C36 C37 109.3(5) . . ? N6 C36 H36A 109.8 . . ? C37 C36 H36A 109.8 . . ? N6 C36 H36B 109.8 . . ? C37 C36 H36B 109.8 . . ? H36A C36 H36B 108.3 . . ? C2 O4 Co2 125.9(2) . 2_858 ? C11 O6 C10 117.0(4) . . ? C7 O5 C9 118.9(3) . . ? O5 C9 C10 107.4(4) . . ? O5 C9 H9A 110.2 . . ? C10 C9 H9A 110.2 . . ? O5 C9 H9B 110.2 . . ? C10 C9 H9B 110.2 . . ? H9A C9 H9B 108.5 . . ? O6 C10 C9 107.9(5) . . ? O6 C10 H10A 110.1 . . ? C9 C10 H10A 110.1 . . ? O6 C10 H10B 110.1 . . ? C9 C10 H10B 110.1 . . ? H10A C10 H10B 108.4 . . ? C13 C12 C11 119.4(5) . . ? C13 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? O6 C11 C16 114.9(5) . . ? O6 C11 C12 124.8(5) . . ? C16 C11 C12 120.3(5) . . ? O7 C17 O8 124.8(5) . . ? O7 C17 C13 120.3(4) . . ? O8 C17 C13 114.8(5) . . ? C15 C14 C13 121.8(5) . . ? C15 C14 H14 119.1 . . ? C13 C14 H14 119.1 . . ? C11 C16 C15 119.6(5) . . ? C11 C16 H16 120.2 . . ? C15 C16 H16 120.2 . . ? C12 C13 C14 119.4(5) . . ? C12 C13 C17 119.1(5) . . ? C14 C13 C17 121.4(4) . . ? C14 C15 C16 119.4(5) . . ? C14 C15 C18 121.8(5) . . ? C16 C15 C18 118.8(5) . . ? O9 C18 O10 122.7(5) . . ? O9 C18 C15 119.2(5) . . ? O10 C18 C15 118.1(5) . . ? C17 O8 Co1 118.6(3) . 1_656 ? C18 O10 Co2 96.3(3) . 1_655 ? C18 O9 Co2 159.2(4) . 2_958 ? C18 O9 Co2 82.1(3) . 1_655 ? Co2 O9 Co2 78.43(12) 2_958 1_655 ? 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 O8 Co1 O1 C1 163.5(3) 1_454 . . . ? N1 Co1 O1 C1 -73.7(4) . . . . ? N4 Co1 O1 C1 59.8(4) 2_977 . . . ? N5 Co2 O3 C2 152.9(4) . . . . ? O4 Co2 O3 C2 21.1(7) 2_858 . . . ? O10 Co2 O3 C2 -96.5(4) 1_455 . . . ? O9 Co2 O3 C2 64.5(4) 2_958 . . . ? O9 Co2 O3 C2 -37.9(4) 1_455 . . . ? Co2 Co2 O3 C2 10.1(4) 2_858 . . . ? O8 Co1 N1 C19 -10.0(4) 1_454 . . . ? O1 Co1 N1 C19 -123.5(3) . . . . ? N4 Co1 N1 C19 102.4(4) 2_977 . . . ? O8 Co1 N1 C20 171.5(4) 1_454 . . . ? O1 Co1 N1 C20 58.1(4) . . . . ? N4 Co1 N1 C20 -76.0(4) 2_977 . . . ? O4 Co2 N5 C33 -172.3(5) 2_858 . . . ? O10 Co2 N5 C33 -71.0(5) 1_455 . . . ? O3 Co2 N5 C33 21.5(5) . . . . ? O9 Co2 N5 C33 104.8(5) 2_958 . . . ? O9 Co2 N5 C33 -77.8(10) 1_455 . . . ? Co2 Co2 N5 C33 105.4(5) 2_858 . . . ? O4 Co2 N5 C34 14.8(4) 2_858 . . . ? O10 Co2 N5 C34 116.0(4) 1_455 . . . ? O3 Co2 N5 C34 -151.4(4) . . . . ? O9 Co2 N5 C34 -68.2(4) 2_958 . . . ? O9 Co2 N5 C34 109.2(8) 1_455 . . . ? Co2 Co2 N5 C34 -67.5(5) 2_858 . . . ? C34 N5 C33 N6 -0.3(6) . . . . ? Co2 N5 C33 N6 -174.2(3) . . . . ? C19 N2 C21 C20 -1.7(6) . . . . ? C22 N2 C21 C20 177.4(4) . . . . ? C6 C5 C4 C3 1.9(8) . . . . ? C1 C5 C4 C3 -176.8(4) . . . . ? C8 C3 C4 C5 -2.3(7) . . . . ? C2 C3 C4 C5 174.7(5) . . . . ? N5 C33 N6 C35 0.3(7) . . . . ? N5 C33 N6 C36 -170.7(5) . . . . ? C4 C3 C8 C7 -0.4(8) . . . . ? C2 C3 C8 C7 -177.3(5) . . . . ? C30 N4 C31 C32 -0.9(6) . . . . ? Co1 N4 C31 C32 -176.8(4) 2_977 . . . ? C25 C24 C23 C28 -1.5(8) . . . . ? C25 C24 C23 C22 -175.6(4) . . . . ? Co1 O1 C1 O2 5.3(6) . . . . ? Co1 O1 C1 C5 -173.4(4) . . . . ? C6 C5 C1 O2 -24.8(7) . . . . ? C4 C5 C1 O2 154.0(5) . . . . ? C6 C5 C1 O1 153.9(5) . . . . ? C4 C5 C1 O1 -27.3(7) . . . . ? C20 N1 C19 N2 0.7(5) . . . . ? Co1 N1 C19 N2 -178.0(3) . . . . ? C21 N2 C19 N1 0.6(6) . . . . ? C22 N2 C19 N1 -178.5(4) . . . . ? C3 C8 C7 O5 -178.4(5) . . . . ? C3 C8 C7 C6 3.4(8) . . . . ? C30 N3 C29 C26 121.3(5) . . . . ? C32 N3 C29 C26 -60.9(7) . . . . ? C27 C26 C29 N3 -82.5(6) . . . . ? C25 C26 C29 N3 97.4(5) . . . . ? C31 N4 C30 N3 1.0(6) . . . . ? Co1 N4 C30 N3 177.0(3) 2_977 . . . ? C32 N3 C30 N4 -0.7(6) . . . . ? C29 N3 C30 N4 177.4(5) . . . . ? C25 C26 C27 C28 0.8(8) . . . . ? C29 C26 C27 C28 -179.2(4) . . . . ? C33 N5 C34 C35 0.2(6) . . . . ? Co2 N5 C34 C35 174.7(4) . . . . ? C26 C27 C28 C23 -1.0(8) . . . . ? C24 C23 C28 C27 1.4(8) . . . . ? C22 C23 C28 C27 175.5(5) . . . . ? C4 C5 C6 C7 1.0(8) . . . . ? C1 C5 C6 C7 179.8(5) . . . . ? O5 C7 C6 C5 178.2(5) . . . . ? C8 C7 C6 C5 -3.6(8) . . . . ? C27 C26 C25 C24 -1.0(8) . . . . ? C29 C26 C25 C24 179.1(4) . . . . ? C23 C24 C25 C26 1.3(8) . . . . ? C30 N3 C32 C31 0.2(7) . . . . ? C29 N3 C32 C31 -178.0(5) . . . . ? N4 C31 C32 N3 0.4(7) . . . . ? N2 C21 C20 N1 2.1(6) . . . . ? C19 N1 C20 C21 -1.7(5) . . . . ? Co1 N1 C20 C21 177.0(3) . . . . ? C19 N2 C22 C23 -101.7(6) . . . . ? C21 N2 C22 C23 79.4(6) . . . . ? C24 C23 C22 N2 -126.1(6) . . . . ? C28 C23 C22 N2 59.8(7) . . . . ? Co2 O3 C2 O4 -15.0(8) . . . . ? Co2 O3 C2 C3 164.7(3) . . . . ? C8 C3 C2 O4 -167.2(5) . . . . ? C4 C3 C2 O4 15.9(7) . . . . ? C8 C3 C2 O3 13.1(7) . . . . ? C4 C3 C2 O3 -163.8(4) . . . . ? C39 C37 C38 C39 0.5(10) 2_959 . . . ? C36 C37 C38 C39 -177.5(5) . . . . ? C37 C39 C38 C37 -0.5(11) 2_959 . . . ? N5 C34 C35 N6 0.0(6) . . . . ? C33 N6 C35 C34 -0.1(6) . . . . ? C36 N6 C35 C34 170.7(5) . . . . ? C33 N6 C36 C37 88.3(7) . . . . ? C35 N6 C36 C37 -80.7(8) . . . . ? C38 C37 C36 N6 86.2(6) . . . . ? C39 C37 C36 N6 -91.8(7) 2_959 . . . ? O3 C2 O4 Co2 9.5(8) . . . 2_858 ? C3 C2 O4 Co2 -170.2(3) . . . 2_858 ? C6 C7 O5 C9 0.6(8) . . . . ? C8 C7 O5 C9 -177.6(5) . . . . ? C7 O5 C9 C10 173.8(5) . . . . ? C11 O6 C10 C9 -169.3(4) . . . . ? O5 C9 C10 O6 69.7(6) . . . . ? C10 O6 C11 C16 175.5(5) . . . . ? C10 O6 C11 C12 -2.6(7) . . . . ? C13 C12 C11 O6 176.0(4) . . . . ? C13 C12 C11 C16 -1.9(7) . . . . ? O6 C11 C16 C15 -177.7(4) . . . . ? C12 C11 C16 C15 0.4(7) . . . . ? C11 C12 C13 C14 2.1(7) . . . . ? C11 C12 C13 C17 -176.3(4) . . . . ? C15 C14 C13 C12 -0.8(7) . . . . ? C15 C14 C13 C17 177.6(4) . . . . ? O7 C17 C13 C12 -30.1(7) . . . . ? O8 C17 C13 C12 151.6(4) . . . . ? O7 C17 C13 C14 151.5(5) . . . . ? O8 C17 C13 C14 -26.7(7) . . . . ? C13 C14 C15 C16 -0.8(7) . . . . ? C13 C14 C15 C18 -178.3(4) . . . . ? C11 C16 C15 C14 0.9(7) . . . . ? C11 C16 C15 C18 178.5(5) . . . . ? C14 C15 C18 O9 177.2(4) . . . . ? C16 C15 C18 O9 -0.4(7) . . . . ? C14 C15 C18 O10 -0.4(7) . . . . ? C16 C15 C18 O10 -177.9(4) . . . . ? O7 C17 O8 Co1 -12.2(7) . . . 1_656 ? C13 C17 O8 Co1 166.0(3) . . . 1_656 ? O9 C18 O10 Co2 4.6(5) . . . 1_655 ? C15 C18 O10 Co2 -178.0(4) . . . 1_655 ? O10 C18 O9 Co2 -24.2(11) . . . 2_958 ? C15 C18 O9 Co2 158.4(6) . . . 2_958 ? O10 C18 O9 Co2 -4.0(4) . . . 1_655 ? C15 C18 O9 Co2 178.6(4) . . . 1_655 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.621 _refine_diff_density_min -0.534 _refine_diff_density_rms 0.061 #============================================================================= data_compound-4 _database_code_depnum_ccdc_archive 'CCDC 834801' #TrackingRef '- CIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H28 Co2 N9 O10, 5(H2 O)' _chemical_formula_sum 'C36 H38 Co2 N9 O15' _chemical_formula_weight 954.61 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 pbcn _symmetry_space_group_name_hall '-P 2n 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y, z-1/2' _cell_length_a 17.930(5) _cell_length_b 20.008(5) _cell_length_c 22.662(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 90.000(5) _cell_angle_gamma 90.000(5) _cell_volume 8130(4) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3229 _cell_measurement_theta_min 3.0450 _cell_measurement_theta_max 25.2936 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.560 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3928 _exptl_absorpt_coefficient_mu 0.898 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.95672 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27048 _diffrn_reflns_av_R_equivalents 0.1177 _diffrn_reflns_av_sigmaI/netI 0.1209 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 25.35 _reflns_number_total 7395 _reflns_number_gt 4192 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0504P)^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 7395 _refine_ls_number_parameters 559 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1333 _refine_ls_R_factor_gt 0.0629 _refine_ls_wR_factor_ref 0.1411 _refine_ls_wR_factor_gt 0.1167 _refine_ls_goodness_of_fit_ref 0.990 _refine_ls_restrained_S_all 0.990 _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 0.39186(4) 0.56652(3) 0.36378(3) 0.02484(19) Uani 1 1 d . . . Co2 Co 0.25890(4) 0.44158(3) 0.31688(3) 0.02255(19) Uani 1 1 d . . . C1 C 0.3160(3) 0.4680(2) 0.4440(2) 0.0253(12) Uani 1 1 d . . . C2 C 0.4320(3) 0.4572(3) 0.6461(2) 0.0312(13) Uani 1 1 d . . . C3 C 0.3656(3) 0.4471(3) 0.6057(2) 0.0305(13) Uani 1 1 d . . . C4 C 0.3003(3) 0.4193(3) 0.6273(2) 0.0328(14) Uani 1 1 d . . . H4 H 0.2964 0.4096 0.6673 0.039 Uiso 1 1 calc R . . C5 C 0.2414(3) 0.4058(3) 0.5907(2) 0.0329(13) Uani 1 1 d . . . C6 C 0.2469(3) 0.4203(3) 0.5304(2) 0.0378(14) Uani 1 1 d . . . H6 H 0.2075 0.4101 0.5052 0.045 Uiso 1 1 calc R . . C7 C 0.3099(3) 0.4493(3) 0.5084(2) 0.0297(13) Uani 1 1 d . . . C8 C 0.3696(3) 0.4627(3) 0.5467(2) 0.0318(13) Uani 1 1 d . . . H8 H 0.4126 0.4826 0.5320 0.038 Uiso 1 1 calc R . . C9 C 0.1713(3) 0.3548(3) 0.6674(2) 0.0400(15) Uani 1 1 d . . . H9A H 0.1720 0.3921 0.6948 0.048 Uiso 1 1 calc R . . H9B H 0.2134 0.3260 0.6760 0.048 Uiso 1 1 calc R . . C10 C 0.0996(3) 0.3167(3) 0.6731(3) 0.0388(15) Uani 1 1 d . . . H10A H 0.0936 0.2869 0.6397 0.047 Uiso 1 1 calc R . . H10B H 0.1003 0.2900 0.7088 0.047 Uiso 1 1 calc R . . C11 C -0.0312(3) 0.3368(2) 0.6760(2) 0.0209(11) Uani 1 1 d . . . C12 C -0.0898(3) 0.3819(2) 0.6751(2) 0.0241(12) Uani 1 1 d . . . H12 H -0.0798 0.4275 0.6765 0.029 Uiso 1 1 calc R . . C13 C -0.1631(3) 0.3601(2) 0.6721(2) 0.0229(12) Uani 1 1 d . . . C14 C -0.1770(3) 0.2918(2) 0.6714(2) 0.0246(12) Uani 1 1 d . . . H14 H -0.2257 0.2764 0.6677 0.030 Uiso 1 1 calc R . . C15 C -0.1190(3) 0.2464(2) 0.6763(2) 0.0220(12) Uani 1 1 d . . . C16 C -0.0459(3) 0.2688(2) 0.6783(2) 0.0229(12) Uani 1 1 d . . . H16 H -0.0069 0.2384 0.6811 0.027 Uiso 1 1 calc R . . C17 C -0.1348(3) 0.1720(2) 0.6791(2) 0.0290(13) Uani 1 1 d . . . C18 C -0.2252(3) 0.4102(2) 0.6694(2) 0.0226(12) Uani 1 1 d . . . C19 C 0.4714(3) 0.6422(3) 0.4619(3) 0.0406(15) Uani 1 1 d . . . H19 H 0.4992 0.6038 0.4691 0.049 Uiso 1 1 calc R . . C20 C 0.3935(4) 0.7073(3) 0.4303(3) 0.0553(18) Uani 1 1 d . . . H20 H 0.3532 0.7246 0.4094 0.066 Uiso 1 1 calc R . . C21 C 0.5408(4) 0.7174(3) 0.5297(3) 0.0557(19) Uani 1 1 d . . . H21A H 0.5620 0.6771 0.5467 0.067 Uiso 1 1 calc R . . H21B H 0.5184 0.7429 0.5615 0.067 Uiso 1 1 calc R . . C22 C 0.6030(3) 0.7584(3) 0.5021(2) 0.0376(14) Uani 1 1 d . . . C23 C 0.6395(4) 0.7366(3) 0.4525(3) 0.0534(18) Uani 1 1 d . . . H23 H 0.6263 0.6960 0.4354 0.064 Uiso 1 1 calc R . . C24 C 0.6958(4) 0.7748(3) 0.4278(3) 0.0513(18) Uani 1 1 d . . . H24 H 0.7193 0.7603 0.3936 0.062 Uiso 1 1 calc R . . C25 C 0.7172(3) 0.8337(3) 0.4535(2) 0.0358(14) Uani 1 1 d . . . C26 C 0.6811(3) 0.8548(3) 0.5031(2) 0.0418(15) Uani 1 1 d . . . H26 H 0.6950 0.8948 0.5209 0.050 Uiso 1 1 calc R . . C27 C 0.6244(3) 0.8175(3) 0.5272(2) 0.0415(16) Uani 1 1 d . . . H27 H 0.6003 0.8326 0.5610 0.050 Uiso 1 1 calc R . . C28 C 0.7774(4) 0.8765(3) 0.4259(2) 0.0496(17) Uani 1 1 d . . . H28A H 0.7900 0.9128 0.4524 0.060 Uiso 1 1 calc R . . H28B H 0.8219 0.8497 0.4200 0.060 Uiso 1 1 calc R . . C29 C 0.7854(3) 0.9014(3) 0.3169(3) 0.0422(15) Uani 1 1 d . . . H29 H 0.8305 0.8801 0.3095 0.051 Uiso 1 1 calc R . . C30 C 0.6877(3) 0.9558(3) 0.3090(3) 0.0452(16) Uani 1 1 d . . . H30 H 0.6497 0.9813 0.2926 0.054 Uiso 1 1 calc R . . C31 C 0.1077(3) 0.4211(3) 0.3762(2) 0.0333(13) Uani 1 1 d . . . H31 H 0.1216 0.4522 0.4046 0.040 Uiso 1 1 calc R . . C32 C 0.1070(4) 0.3574(3) 0.3041(3) 0.062(2) Uani 1 1 d . . . H32 H 0.1219 0.3349 0.2702 0.075 Uiso 1 1 calc R . . C33 C -0.0192(3) 0.3918(3) 0.4169(3) 0.0443(16) Uani 1 1 d . . . H33A H -0.0223 0.3496 0.4379 0.053 Uiso 1 1 calc R . . H33B H -0.0655 0.3980 0.3955 0.053 Uiso 1 1 calc R . . C34 C -0.0097(3) 0.4472(3) 0.4602(3) 0.0357(14) Uani 1 1 d . . . C35 C -0.0385(3) 0.5107(3) 0.4483(3) 0.0422(15) Uani 1 1 d . . . H35 H -0.0648 0.5181 0.4136 0.051 Uiso 1 1 calc R . . C36 C -0.0282(3) 0.5624(3) 0.4873(3) 0.0430(15) Uani 1 1 d . . . H36 H -0.0471 0.6044 0.4784 0.052 Uiso 1 1 calc R . . N1 N 0.4154(3) 0.6451(2) 0.42411(19) 0.0360(12) Uani 1 1 d . . . N2 N 0.4323(3) 0.7438(3) 0.4681(3) 0.0650(17) Uani 1 1 d . . . N3 N 0.4832(3) 0.6989(3) 0.4878(2) 0.0414(13) Uani 1 1 d . . . N4 N 0.7529(3) 0.9043(2) 0.3687(2) 0.0395(12) Uani 1 1 d . . . N5 N 0.6889(3) 0.9396(3) 0.3645(2) 0.0507(14) Uani 1 1 d . . . N6 N 0.7454(2) 0.9329(2) 0.27687(18) 0.0321(11) Uani 1 1 d . . . N7 N 0.1499(2) 0.4022(2) 0.33121(19) 0.0307(11) Uani 1 1 d . . . N8 N 0.0414(3) 0.3475(3) 0.3292(3) 0.0657(18) Uani 1 1 d . . . N9 N 0.0434(2) 0.3896(2) 0.3750(2) 0.0339(11) Uani 1 1 d . . . O1 O 0.3695(2) 0.5052(2) 0.43157(16) 0.0445(11) Uani 1 1 d . . . O2 O 0.2685(2) 0.44662(19) 0.40872(15) 0.0372(9) Uani 1 1 d . . . O1W O 0.37124(17) 0.48606(15) 0.30161(14) 0.0228(8) Uani 1 1 d . . . O3 O 0.4951(2) 0.46648(19) 0.62256(15) 0.0367(9) Uani 1 1 d . . . O2W O 0.4265(2) 0.62838(19) 0.29374(16) 0.0438(10) Uani 1 1 d . . . O4 O 0.4205(2) 0.4528(2) 0.70071(17) 0.0517(12) Uani 1 1 d . . . O3W O 0.4507(3) 0.6152(3) 0.6180(3) 0.100(2) Uani 1 1 d . . . O5 O 0.1755(2) 0.3787(2) 0.60792(17) 0.0522(12) Uani 1 1 d . . . O4W O 0.4626(3) 0.2796(2) 0.6774(2) 0.0831(16) Uani 1 1 d . . . O6 O 0.03911(18) 0.36322(16) 0.67508(16) 0.0318(9) Uani 1 1 d . . . O5W O 0.3202(4) 0.2751(4) 0.7358(3) 0.140(3) Uani 1 1 d . . . O7 O -0.0801(2) 0.13330(18) 0.6777(2) 0.0593(13) Uani 1 1 d . . . O8 O -0.20047(19) 0.15463(16) 0.68455(17) 0.0342(9) Uani 1 1 d . . . O9 O -0.2868(2) 0.39110(18) 0.64975(17) 0.0393(10) Uani 1 1 d . . . O10 O -0.2097(2) 0.46710(16) 0.68754(17) 0.0363(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0209(4) 0.0312(4) 0.0225(4) -0.0005(3) -0.0012(3) -0.0040(3) Co2 0.0189(4) 0.0215(3) 0.0272(4) -0.0011(3) -0.0022(3) 0.0025(3) C1 0.023(3) 0.028(3) 0.024(3) 0.003(2) 0.002(3) 0.005(3) C2 0.034(4) 0.033(3) 0.026(3) -0.002(2) -0.003(3) 0.003(3) C3 0.025(3) 0.034(3) 0.033(3) -0.001(2) 0.002(3) -0.005(3) C4 0.025(3) 0.045(3) 0.029(3) 0.007(3) 0.002(3) -0.002(3) C5 0.014(3) 0.053(4) 0.031(3) 0.001(3) 0.003(3) -0.004(3) C6 0.027(3) 0.051(4) 0.035(3) 0.009(3) -0.006(3) -0.001(3) C7 0.027(3) 0.035(3) 0.027(3) 0.008(2) 0.006(3) 0.004(3) C8 0.037(4) 0.036(3) 0.022(3) 0.003(2) 0.003(3) 0.000(3) C9 0.025(3) 0.058(4) 0.037(4) 0.015(3) -0.002(3) -0.003(3) C10 0.031(4) 0.048(4) 0.037(3) 0.009(3) 0.001(3) -0.005(3) C11 0.015(3) 0.024(3) 0.024(3) 0.002(2) 0.001(2) -0.003(2) C12 0.030(3) 0.018(2) 0.024(3) 0.003(2) -0.001(2) -0.006(2) C13 0.018(3) 0.024(3) 0.027(3) 0.000(2) 0.005(2) -0.004(2) C14 0.017(3) 0.032(3) 0.025(3) -0.005(2) 0.000(2) -0.004(2) C15 0.023(3) 0.020(3) 0.024(3) 0.001(2) 0.003(2) -0.003(2) C16 0.017(3) 0.031(3) 0.021(3) 0.005(2) 0.005(2) 0.003(2) C17 0.030(3) 0.022(3) 0.035(3) 0.001(2) 0.001(3) -0.007(3) C18 0.017(3) 0.026(3) 0.024(3) 0.003(2) 0.002(2) -0.002(2) C19 0.038(4) 0.047(4) 0.037(4) -0.003(3) 0.002(3) -0.003(3) C20 0.045(4) 0.047(4) 0.074(5) -0.015(4) -0.018(4) 0.003(3) C21 0.060(5) 0.079(5) 0.029(4) -0.006(3) -0.010(3) -0.035(4) C22 0.038(4) 0.049(4) 0.025(3) 0.003(3) -0.004(3) -0.010(3) C23 0.061(5) 0.043(4) 0.056(4) -0.019(3) 0.019(4) -0.006(3) C24 0.055(5) 0.057(4) 0.041(4) -0.015(3) 0.020(3) -0.003(4) C25 0.029(3) 0.049(4) 0.029(3) 0.008(3) -0.001(3) -0.008(3) C26 0.046(4) 0.049(4) 0.030(4) -0.003(3) -0.001(3) -0.016(3) C27 0.045(4) 0.055(4) 0.024(3) -0.007(3) 0.004(3) -0.018(3) C28 0.046(4) 0.074(5) 0.029(4) 0.006(3) -0.002(3) -0.015(4) C29 0.041(4) 0.048(4) 0.037(4) 0.007(3) 0.013(3) 0.007(3) C30 0.044(4) 0.041(4) 0.051(4) 0.006(3) 0.013(3) -0.001(3) C31 0.031(3) 0.036(3) 0.033(3) -0.007(2) -0.002(3) -0.006(3) C32 0.057(5) 0.072(5) 0.059(5) -0.035(4) 0.023(4) -0.029(4) C33 0.019(3) 0.056(4) 0.058(4) -0.007(3) 0.009(3) -0.009(3) C34 0.019(3) 0.043(3) 0.045(4) -0.005(3) 0.006(3) 0.001(3) C35 0.034(4) 0.055(4) 0.038(4) 0.000(3) 0.003(3) 0.003(3) C36 0.034(4) 0.035(3) 0.060(4) 0.004(3) 0.005(3) 0.005(3) N1 0.031(3) 0.043(3) 0.034(3) -0.010(2) -0.006(2) -0.006(2) N2 0.063(4) 0.056(4) 0.076(4) -0.028(3) -0.017(3) 0.000(3) N3 0.043(3) 0.047(3) 0.034(3) -0.008(2) 0.000(2) -0.017(3) N4 0.038(3) 0.053(3) 0.028(3) 0.009(2) 0.006(2) -0.008(3) N5 0.052(4) 0.062(3) 0.038(3) 0.004(3) 0.016(3) 0.007(3) N6 0.029(3) 0.037(3) 0.030(3) 0.004(2) 0.007(2) 0.003(2) N7 0.020(3) 0.033(3) 0.039(3) -0.011(2) 0.000(2) -0.002(2) N8 0.060(4) 0.075(4) 0.062(4) -0.031(3) 0.016(3) -0.039(3) N9 0.018(3) 0.038(3) 0.046(3) -0.006(2) 0.003(2) -0.010(2) O1 0.039(3) 0.064(3) 0.031(2) 0.0131(19) -0.0039(19) -0.024(2) O2 0.033(2) 0.057(2) 0.021(2) 0.0043(18) -0.0050(17) -0.015(2) O1W 0.021(2) 0.0252(18) 0.0220(19) -0.0032(14) -0.0012(15) -0.0014(15) O3 0.021(2) 0.056(3) 0.033(2) -0.0025(18) 0.0000(18) -0.0044(19) O2W 0.044(3) 0.054(3) 0.033(2) 0.0058(19) 0.0041(19) -0.016(2) O4 0.047(3) 0.082(3) 0.025(2) -0.006(2) -0.001(2) -0.002(2) O3W 0.060(4) 0.096(4) 0.143(5) 0.047(4) -0.040(3) -0.026(3) O5 0.030(3) 0.087(3) 0.040(3) 0.023(2) -0.002(2) -0.019(2) O4W 0.073(4) 0.067(3) 0.109(4) -0.023(3) -0.004(3) 0.003(3) O6 0.015(2) 0.030(2) 0.050(3) 0.0000(17) 0.0002(17) -0.0039(17) O5W 0.123(6) 0.178(7) 0.118(6) 0.004(5) 0.017(5) 0.053(5) O7 0.026(2) 0.025(2) 0.127(4) 0.006(2) 0.016(3) 0.0038(19) O8 0.021(2) 0.0216(18) 0.060(3) 0.0031(17) 0.0029(19) -0.0095(16) O9 0.024(2) 0.033(2) 0.061(3) -0.0133(19) -0.009(2) 0.0060(18) O10 0.027(2) 0.0186(18) 0.064(3) -0.0099(18) -0.0136(19) 0.0052(17) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1 2.007(4) . ? Co1 O9 2.088(4) 5_566 ? Co1 O2W 2.107(4) . ? Co1 N1 2.126(4) . ? Co1 O3 2.155(4) 5_666 ? Co1 O1W 2.171(3) . ? Co2 O10 2.031(3) 5_566 ? Co2 O8 2.058(3) 3_556 ? Co2 O2 2.091(3) . ? Co2 N7 2.132(4) . ? Co2 N6 2.145(4) 6_556 ? Co2 O1W 2.229(3) . ? C1 O2 1.244(6) . ? C1 O1 1.246(6) . ? C1 C7 1.511(7) . ? C2 O4 1.258(6) . ? C2 O3 1.264(6) . ? C2 C3 1.515(7) . ? C3 C8 1.375(7) . ? C3 C4 1.385(7) . ? C4 C5 1.369(7) . ? C4 H4 0.9300 . ? C5 O5 1.357(6) . ? C5 C6 1.401(7) . ? C6 C7 1.364(7) . ? C6 H6 0.9300 . ? C7 C8 1.405(7) . ? C8 H8 0.9300 . ? C9 O5 1.432(6) . ? C9 C10 1.501(7) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 O6 1.430(6) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 O6 1.366(5) . ? C11 C12 1.386(7) . ? C11 C16 1.387(6) . ? C12 C13 1.386(7) . ? C12 H12 0.9300 . ? C13 C14 1.389(6) . ? C13 C18 1.500(7) . ? C14 C15 1.384(7) . ? C14 H14 0.9300 . ? C15 C16 1.386(6) . ? C15 C17 1.516(6) . ? C16 H16 0.9300 . ? C17 O8 1.234(6) . ? C17 O7 1.251(6) . ? C18 O10 1.242(6) . ? C18 O9 1.252(6) . ? C19 N3 1.296(7) . ? C19 N1 1.322(7) . ? C19 H19 0.9300 . ? C20 N1 1.311(7) . ? C20 N2 1.324(8) . ? C20 H20 0.9300 . ? C21 N3 1.452(7) . ? C21 C22 1.519(8) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C27 1.367(7) . ? C22 C23 1.372(8) . ? C23 C24 1.384(8) . ? C23 H23 0.9300 . ? C24 C25 1.371(8) . ? C24 H24 0.9300 . ? C25 C26 1.364(8) . ? C25 C28 1.514(8) . ? C26 C27 1.373(8) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 N4 1.477(7) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 N4 1.312(7) . ? C29 N6 1.318(7) . ? C29 H29 0.9300 . ? C30 N5 1.300(7) . ? C30 N6 1.344(7) . ? C30 H30 0.9300 . ? C31 N9 1.314(6) . ? C31 N7 1.325(6) . ? C31 H31 0.9300 . ? C32 N8 1.320(7) . ? C32 N7 1.332(7) . ? C32 H32 0.9300 . ? C33 N9 1.471(7) . ? C33 C34 1.490(8) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C36 1.383(8) 5_566 ? C34 C35 1.398(8) . ? C35 C36 1.373(8) . ? C35 H35 0.9300 . ? C36 C34 1.383(8) 5_566 ? C36 H36 0.9300 . ? N2 N3 1.356(7) . ? N4 N5 1.351(7) . ? N6 Co2 2.145(4) 6_666 ? N8 N9 1.339(6) . ? O3 Co1 2.155(4) 5_666 ? O8 Co2 2.058(3) 3_456 ? O9 Co1 2.088(4) 5_566 ? O10 Co2 2.031(3) 5_566 ? 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 O9 100.42(16) . 5_566 ? O1 Co1 O2W 174.32(16) . . ? O9 Co1 O2W 85.22(16) 5_566 . ? O1 Co1 N1 89.99(17) . . ? O9 Co1 N1 88.43(16) 5_566 . ? O2W Co1 N1 89.51(17) . . ? O1 Co1 O3 83.71(15) . 5_666 ? O9 Co1 O3 173.85(15) 5_566 5_666 ? O2W Co1 O3 90.62(15) . 5_666 ? N1 Co1 O3 87.01(16) . 5_666 ? O1 Co1 O1W 90.53(14) . . ? O9 Co1 O1W 93.00(13) 5_566 . ? O2W Co1 O1W 89.82(14) . . ? N1 Co1 O1W 178.36(15) . . ? O3 Co1 O1W 91.50(13) 5_666 . ? O10 Co2 O8 173.73(14) 5_566 3_556 ? O10 Co2 O2 92.38(15) 5_566 . ? O8 Co2 O2 91.81(15) 3_556 . ? O10 Co2 N7 86.68(16) 5_566 . ? O8 Co2 N7 88.92(15) 3_556 . ? O2 Co2 N7 86.66(15) . . ? O10 Co2 N6 88.54(16) 5_566 6_556 ? O8 Co2 N6 87.07(16) 3_556 6_556 ? O2 Co2 N6 177.43(15) . 6_556 ? N7 Co2 N6 90.99(17) . 6_556 ? O10 Co2 O1W 91.47(13) 5_566 . ? O8 Co2 O1W 92.93(13) 3_556 . ? O2 Co2 O1W 93.48(13) . . ? N7 Co2 O1W 178.14(15) . . ? N6 Co2 O1W 88.90(14) 6_556 . ? O2 C1 O1 125.9(5) . . ? O2 C1 C7 119.1(5) . . ? O1 C1 C7 115.0(5) . . ? O4 C2 O3 124.9(5) . . ? O4 C2 C3 117.1(5) . . ? O3 C2 C3 117.9(5) . . ? C8 C3 C4 118.6(5) . . ? C8 C3 C2 121.0(5) . . ? C4 C3 C2 120.3(5) . . ? C5 C4 C3 121.1(5) . . ? C5 C4 H4 119.5 . . ? C3 C4 H4 119.5 . . ? O5 C5 C4 125.1(5) . . ? O5 C5 C6 115.1(5) . . ? C4 C5 C6 119.8(5) . . ? C7 C6 C5 120.1(5) . . ? C7 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? C6 C7 C8 119.2(5) . . ? C6 C7 C1 121.2(5) . . ? C8 C7 C1 119.6(5) . . ? C3 C8 C7 121.1(5) . . ? C3 C8 H8 119.4 . . ? C7 C8 H8 119.4 . . ? O5 C9 C10 107.2(4) . . ? O5 C9 H9A 110.3 . . ? C10 C9 H9A 110.3 . . ? O5 C9 H9B 110.3 . . ? C10 C9 H9B 110.3 . . ? H9A C9 H9B 108.5 . . ? O6 C10 C9 108.7(5) . . ? O6 C10 H10A 109.9 . . ? C9 C10 H10A 109.9 . . ? O6 C10 H10B 109.9 . . ? C9 C10 H10B 109.9 . . ? H10A C10 H10B 108.3 . . ? O6 C11 C12 116.6(4) . . ? O6 C11 C16 123.7(4) . . ? C12 C11 C16 119.7(4) . . ? C11 C12 C13 121.0(4) . . ? C11 C12 H12 119.5 . . ? C13 C12 H12 119.5 . . ? C12 C13 C14 118.7(4) . . ? C12 C13 C18 119.7(4) . . ? C14 C13 C18 121.6(4) . . ? C15 C14 C13 120.6(5) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C14 C15 C16 120.1(4) . . ? C14 C15 C17 120.4(5) . . ? C16 C15 C17 119.5(4) . . ? C15 C16 C11 119.7(4) . . ? C15 C16 H16 120.1 . . ? C11 C16 H16 120.1 . . ? O8 C17 O7 125.2(5) . . ? O8 C17 C15 117.3(5) . . ? O7 C17 C15 117.4(5) . . ? O10 C18 O9 126.5(5) . . ? O10 C18 C13 115.7(4) . . ? O9 C18 C13 117.8(4) . . ? N3 C19 N1 112.2(5) . . ? N3 C19 H19 123.9 . . ? N1 C19 H19 123.9 . . ? N1 C20 N2 115.8(6) . . ? N1 C20 H20 122.1 . . ? N2 C20 H20 122.1 . . ? N3 C21 C22 112.9(5) . . ? N3 C21 H21A 109.0 . . ? C22 C21 H21A 109.0 . . ? N3 C21 H21B 109.0 . . ? C22 C21 H21B 109.0 . . ? H21A C21 H21B 107.8 . . ? C27 C22 C23 118.8(5) . . ? C27 C22 C21 120.1(5) . . ? C23 C22 C21 121.0(5) . . ? C22 C23 C24 120.2(6) . . ? C22 C23 H23 119.9 . . ? C24 C23 H23 119.9 . . ? C25 C24 C23 120.5(5) . . ? C25 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C26 C25 C24 118.9(5) . . ? C26 C25 C28 120.4(5) . . ? C24 C25 C28 120.7(5) . . ? C25 C26 C27 120.7(5) . . ? C25 C26 H26 119.6 . . ? C27 C26 H26 119.6 . . ? C22 C27 C26 120.8(5) . . ? C22 C27 H27 119.6 . . ? C26 C27 H27 119.6 . . ? N4 C28 C25 111.3(5) . . ? N4 C28 H28A 109.4 . . ? C25 C28 H28A 109.4 . . ? N4 C28 H28B 109.4 . . ? C25 C28 H28B 109.4 . . ? H28A C28 H28B 108.0 . . ? N4 C29 N6 110.7(5) . . ? N4 C29 H29 124.7 . . ? N6 C29 H29 124.7 . . ? N5 C30 N6 115.3(6) . . ? N5 C30 H30 122.4 . . ? N6 C30 H30 122.4 . . ? N9 C31 N7 110.5(5) . . ? N9 C31 H31 124.7 . . ? N7 C31 H31 124.7 . . ? N8 C32 N7 114.7(5) . . ? N8 C32 H32 122.7 . . ? N7 C32 H32 122.7 . . ? N9 C33 C34 111.1(4) . . ? N9 C33 H33A 109.4 . . ? C34 C33 H33A 109.4 . . ? N9 C33 H33B 109.4 . . ? C34 C33 H33B 109.4 . . ? H33A C33 H33B 108.0 . . ? C36 C34 C35 118.2(5) 5_566 . ? C36 C34 C33 121.3(5) 5_566 . ? C35 C34 C33 120.5(6) . . ? C36 C35 C34 120.7(6) . . ? C36 C35 H35 119.6 . . ? C34 C35 H35 119.6 . . ? C35 C36 C34 121.1(5) . 5_566 ? C35 C36 H36 119.5 . . ? C34 C36 H36 119.5 5_566 . ? C20 N1 C19 101.6(5) . . ? C20 N1 Co1 135.3(4) . . ? C19 N1 Co1 122.3(4) . . ? C20 N2 N3 101.6(5) . . ? C19 N3 N2 108.7(5) . . ? C19 N3 C21 129.5(6) . . ? N2 N3 C21 121.7(5) . . ? C29 N4 N5 109.7(5) . . ? C29 N4 C28 129.5(6) . . ? N5 N4 C28 120.8(5) . . ? C30 N5 N4 102.2(5) . . ? C29 N6 C30 102.0(5) . . ? C29 N6 Co2 131.2(4) . 6_666 ? C30 N6 Co2 126.6(4) . 6_666 ? C31 N7 C32 102.5(5) . . ? C31 N7 Co2 122.4(4) . . ? C32 N7 Co2 135.1(4) . . ? C32 N8 N9 102.5(5) . . ? C31 N9 N8 109.9(5) . . ? C31 N9 C33 130.0(5) . . ? N8 N9 C33 120.0(4) . . ? C1 O1 Co1 133.8(3) . . ? C1 O2 Co2 135.5(3) . . ? Co1 O1W Co2 110.44(13) . . ? C2 O3 Co1 137.4(3) . 5_666 ? C5 O5 C9 116.8(4) . . ? C11 O6 C10 116.6(4) . . ? C17 O8 Co2 126.9(3) . 3_456 ? C18 O9 Co1 136.5(3) . 5_566 ? C18 O10 Co2 135.3(3) . 5_566 ? 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 C2 C3 C8 168.2(5) . . . . ? O3 C2 C3 C8 -15.0(7) . . . . ? O4 C2 C3 C4 -14.4(7) . . . . ? O3 C2 C3 C4 162.5(5) . . . . ? C8 C3 C4 C5 1.7(8) . . . . ? C2 C3 C4 C5 -175.8(5) . . . . ? C3 C4 C5 O5 -180.0(5) . . . . ? C3 C4 C5 C6 0.0(8) . . . . ? O5 C5 C6 C7 178.3(5) . . . . ? C4 C5 C6 C7 -1.7(8) . . . . ? C5 C6 C7 C8 1.6(8) . . . . ? C5 C6 C7 C1 -177.4(5) . . . . ? O2 C1 C7 C6 -12.4(8) . . . . ? O1 C1 C7 C6 166.9(5) . . . . ? O2 C1 C7 C8 168.6(5) . . . . ? O1 C1 C7 C8 -12.0(7) . . . . ? C4 C3 C8 C7 -1.8(8) . . . . ? C2 C3 C8 C7 175.7(5) . . . . ? C6 C7 C8 C3 0.2(8) . . . . ? C1 C7 C8 C3 179.2(5) . . . . ? O5 C9 C10 O6 -74.5(6) . . . . ? O6 C11 C12 C13 175.8(4) . . . . ? C16 C11 C12 C13 -4.7(7) . . . . ? C11 C12 C13 C14 1.6(7) . . . . ? C11 C12 C13 C18 -178.2(4) . . . . ? C12 C13 C14 C15 2.7(7) . . . . ? C18 C13 C14 C15 -177.5(5) . . . . ? C13 C14 C15 C16 -3.9(7) . . . . ? C13 C14 C15 C17 176.4(4) . . . . ? C14 C15 C16 C11 0.7(7) . . . . ? C17 C15 C16 C11 -179.6(4) . . . . ? O6 C11 C16 C15 -177.0(4) . . . . ? C12 C11 C16 C15 3.5(7) . . . . ? C14 C15 C17 O8 -8.9(7) . . . . ? C16 C15 C17 O8 171.3(5) . . . . ? C14 C15 C17 O7 173.2(5) . . . . ? C16 C15 C17 O7 -6.5(7) . . . . ? C12 C13 C18 O10 -20.9(7) . . . . ? C14 C13 C18 O10 159.4(5) . . . . ? C12 C13 C18 O9 159.5(5) . . . . ? C14 C13 C18 O9 -20.2(7) . . . . ? N3 C21 C22 C27 128.6(6) . . . . ? N3 C21 C22 C23 -52.6(9) . . . . ? C27 C22 C23 C24 -1.5(10) . . . . ? C21 C22 C23 C24 179.8(6) . . . . ? C22 C23 C24 C25 1.8(10) . . . . ? C23 C24 C25 C26 -1.2(10) . . . . ? C23 C24 C25 C28 -178.4(6) . . . . ? C24 C25 C26 C27 0.2(9) . . . . ? C28 C25 C26 C27 177.5(6) . . . . ? C23 C22 C27 C26 0.5(9) . . . . ? C21 C22 C27 C26 179.2(6) . . . . ? C25 C26 C27 C22 0.2(9) . . . . ? C26 C25 C28 N4 -110.5(6) . . . . ? C24 C25 C28 N4 66.7(8) . . . . ? N9 C33 C34 C36 -89.2(7) . . . 5_566 ? N9 C33 C34 C35 90.1(6) . . . . ? C36 C34 C35 C36 1.0(9) 5_566 . . . ? C33 C34 C35 C36 -178.3(5) . . . . ? C34 C35 C36 C34 -1.0(10) . . . 5_566 ? N2 C20 N1 C19 1.2(8) . . . . ? N2 C20 N1 Co1 -167.9(5) . . . . ? N3 C19 N1 C20 -1.3(7) . . . . ? N3 C19 N1 Co1 169.7(4) . . . . ? O1 Co1 N1 C20 -128.6(6) . . . . ? O9 Co1 N1 C20 -28.2(6) 5_566 . . . ? O2W Co1 N1 C20 57.0(6) . . . . ? O3 Co1 N1 C20 147.7(6) 5_666 . . . ? O1W Co1 N1 C20 123(5) . . . . ? O1 Co1 N1 C19 63.9(5) . . . . ? O9 Co1 N1 C19 164.4(4) 5_566 . . . ? O2W Co1 N1 C19 -110.4(5) . . . . ? O3 Co1 N1 C19 -19.8(4) 5_666 . . . ? O1W Co1 N1 C19 -45(6) . . . . ? N1 C20 N2 N3 -0.7(8) . . . . ? N1 C19 N3 N2 1.0(7) . . . . ? N1 C19 N3 C21 -176.9(5) . . . . ? C20 N2 N3 C19 -0.2(7) . . . . ? C20 N2 N3 C21 177.9(5) . . . . ? C22 C21 N3 C19 102.9(7) . . . . ? C22 C21 N3 N2 -74.8(8) . . . . ? N6 C29 N4 N5 -0.9(7) . . . . ? N6 C29 N4 C28 -179.7(5) . . . . ? C25 C28 N4 C29 -127.0(6) . . . . ? C25 C28 N4 N5 54.4(7) . . . . ? N6 C30 N5 N4 0.8(7) . . . . ? C29 N4 N5 C30 0.1(6) . . . . ? C28 N4 N5 C30 179.0(5) . . . . ? N4 C29 N6 C30 1.3(6) . . . . ? N4 C29 N6 Co2 -174.2(4) . . . 6_666 ? N5 C30 N6 C29 -1.3(7) . . . . ? N5 C30 N6 Co2 174.4(4) . . . 6_666 ? N9 C31 N7 C32 -0.6(7) . . . . ? N9 C31 N7 Co2 179.9(3) . . . . ? N8 C32 N7 C31 0.0(8) . . . . ? N8 C32 N7 Co2 179.3(5) . . . . ? O10 Co2 N7 C31 -58.9(4) 5_566 . . . ? O8 Co2 N7 C31 125.6(4) 3_556 . . . ? O2 Co2 N7 C31 33.7(4) . . . . ? N6 Co2 N7 C31 -147.4(4) 6_556 . . . ? O1W Co2 N7 C31 -61(5) . . . . ? O10 Co2 N7 C32 121.9(6) 5_566 . . . ? O8 Co2 N7 C32 -53.6(6) 3_556 . . . ? O2 Co2 N7 C32 -145.5(6) . . . . ? N6 Co2 N7 C32 33.4(6) 6_556 . . . ? O1W Co2 N7 C32 120(4) . . . . ? N7 C32 N8 N9 0.6(8) . . . . ? N7 C31 N9 N8 1.1(7) . . . . ? N7 C31 N9 C33 176.7(5) . . . . ? C32 N8 N9 C31 -1.0(7) . . . . ? C32 N8 N9 C33 -177.1(6) . . . . ? C34 C33 N9 C31 11.3(9) . . . . ? C34 C33 N9 N8 -173.4(5) . . . . ? O2 C1 O1 Co1 19.7(9) . . . . ? C7 C1 O1 Co1 -159.6(4) . . . . ? O9 Co1 O1 C1 39.9(5) 5_566 . . . ? O2W Co1 O1 C1 -146.7(14) . . . . ? N1 Co1 O1 C1 128.3(5) . . . . ? O3 Co1 O1 C1 -144.7(5) 5_666 . . . ? O1W Co1 O1 C1 -53.2(5) . . . . ? O1 C1 O2 Co2 13.8(9) . . . . ? C7 C1 O2 Co2 -167.0(3) . . . . ? O10 Co2 O2 C1 -89.1(5) 5_566 . . . ? O8 Co2 O2 C1 95.5(5) 3_556 . . . ? N7 Co2 O2 C1 -175.6(5) . . . . ? N6 Co2 O2 C1 160(3) 6_556 . . . ? O1W Co2 O2 C1 2.5(5) . . . . ? O1 Co1 O1W Co2 54.31(17) . . . . ? O9 Co1 O1W Co2 -46.15(16) 5_566 . . . ? O2W Co1 O1W Co2 -131.36(16) . . . . ? N1 Co1 O1W Co2 163(5) . . . . ? O3 Co1 O1W Co2 138.03(15) 5_666 . . . ? O10 Co2 O1W Co1 52.53(16) 5_566 . . . ? O8 Co2 O1W Co1 -131.94(16) 3_556 . . . ? O2 Co2 O1W Co1 -39.95(16) . . . . ? N7 Co2 O1W Co1 54(4) . . . . ? N6 Co2 O1W Co1 141.04(17) 6_556 . . . ? O4 C2 O3 Co1 39.1(8) . . . 5_666 ? C3 C2 O3 Co1 -137.5(4) . . . 5_666 ? C4 C5 O5 C9 -8.3(8) . . . . ? C6 C5 O5 C9 171.7(5) . . . . ? C10 C9 O5 C5 -170.1(5) . . . . ? C12 C11 O6 C10 -177.0(4) . . . . ? C16 C11 O6 C10 3.5(7) . . . . ? C9 C10 O6 C11 175.5(4) . . . . ? O7 C17 O8 Co2 -7.6(8) . . . 3_456 ? C15 C17 O8 Co2 174.7(3) . . . 3_456 ? O10 C18 O9 Co1 -0.8(9) . . . 5_566 ? C13 C18 O9 Co1 178.8(3) . . . 5_566 ? O9 C18 O10 Co2 -13.3(8) . . . 5_566 ? C13 C18 O10 Co2 167.1(3) . . . 5_566 ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.772 _refine_diff_density_min -0.383 _refine_diff_density_rms 0.084 #============================================================================= data_compound-5 _database_code_depnum_ccdc_archive 'CCDC 834802' #TrackingRef '- CIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C29 H36 N4 Ni2 O15, 2(H2 O)' _chemical_formula_sum 'C29 H40 N4 Ni2 O17' _chemical_formula_weight 834.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M c2/m _symmetry_space_group_name_hall '-C 2y' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 13.2776(4) _cell_length_b 22.1202(6) _cell_length_c 14.2690(4) _cell_angle_alpha 90.00 _cell_angle_beta 112.540(4) _cell_angle_gamma 90.00 _cell_volume 3870.72(19) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4199 _cell_measurement_theta_min 3.0743 _cell_measurement_theta_max 25.2956 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.431 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1736 _exptl_absorpt_coefficient_mu 1.047 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.99329 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _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 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7517 _diffrn_reflns_av_R_equivalents 0.0213 _diffrn_reflns_av_sigmaI/netI 0.0423 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.22 _diffrn_reflns_theta_max 25.35 _reflns_number_total 3545 _reflns_number_gt 2640 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1100P)^2^+3.1982P] 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 3545 _refine_ls_number_parameters 321 _refine_ls_number_restraints 462 _refine_ls_R_factor_all 0.0761 _refine_ls_R_factor_gt 0.0607 _refine_ls_wR_factor_ref 0.1836 _refine_ls_wR_factor_gt 0.1770 _refine_ls_goodness_of_fit_ref 1.148 _refine_ls_restrained_S_all 1.148 _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 0.7500 0.7500 0.5000 0.0318(3) Uani 1 2 d S . . Ni2 Ni 1.01481(6) 1.0000 0.91185(5) 0.0275(3) Uani 1 2 d S . . O2 O 0.6083(3) 0.71337(19) 0.6448(3) 0.0566(10) Uani 1 1 d . . . O5 O 0.5956(3) 0.78519(19) 0.9826(3) 0.0552(10) Uani 1 1 d . . . O3 O 0.8984(3) 0.93611(19) 0.8691(3) 0.0605(11) Uani 1 1 d . . . C5 C 0.6471(4) 0.7995(2) 0.9185(3) 0.0406(8) Uani 1 1 d U . . O4 O 0.8757(3) 0.93652(16) 1.0151(3) 0.0499(9) Uani 1 1 d . . . C8 C 0.7603(4) 0.8368(2) 0.8022(4) 0.0418(8) Uani 1 1 d U . . H8 H 0.7976 0.8496 0.7623 0.050 Uiso 1 1 calc R . . C4 C 0.7176(4) 0.8478(2) 0.9495(3) 0.0392(8) Uani 1 1 d U . . H4 H 0.7269 0.8677 1.0096 0.047 Uiso 1 1 calc R . . C3 C 0.7750(4) 0.8669(2) 0.8910(3) 0.0388(8) Uani 1 1 d U . . C6 C 0.6337(4) 0.7682(2) 0.8304(4) 0.0438(9) Uani 1 1 d U . . H6 H 0.5878 0.7348 0.8110 0.053 Uiso 1 1 calc R . . O1 O 0.7332(4) 0.7759(2) 0.6287(3) 0.0788(15) Uani 1 1 d . . . C9 C 0.5241(4) 0.7353(2) 0.9600(4) 0.0404(9) Uani 1 1 d U . . H9A H 0.5635 0.6980 0.9625 0.048 Uiso 1 1 calc R . . H9B H 0.4673 0.7395 0.8929 0.048 Uiso 1 1 calc R . . C7 C 0.6901(4) 0.7877(2) 0.7717(4) 0.0428(8) Uani 1 1 d U . . C1 C 0.6759(4) 0.7562(2) 0.6739(4) 0.0484(10) Uani 1 1 d U . . C2 C 0.8550(4) 0.9173(2) 0.9278(4) 0.0394(9) Uani 1 1 d U . . N1 N 0.6671(10) 0.8189(6) 0.4079(9) 0.042(3) Uani 0.50 1 d P . . N1' N 0.6420(9) 0.8220(5) 0.4401(9) 0.041(2) Uani 0.50 1 d P . . N2 N 0.5638(7) 0.9000(3) 0.3456(5) 0.113(3) Uani 1 1 d . . . C14 C 0.5691(9) 1.0000 0.2735(8) 0.0849(17) Uani 1 2 d SU . . C12' C 0.6263(13) 0.8523(7) 0.3562(13) 0.0783(17) Uani 0.50 1 d PU . . C12 C 0.6577(12) 0.8734(6) 0.4366(11) 0.0778(17) Uani 0.50 1 d PU . . C10 C 0.6086(13) 0.8159(7) 0.3110(11) 0.0802(18) Uani 0.50 1 d PU . . C10' C 0.5665(12) 0.8450(6) 0.4786(11) 0.0751(16) Uani 0.50 1 d PU . . C11 C 0.5600(13) 0.8699(7) 0.2755(12) 0.0828(17) Uani 0.50 1 d PU . . C11' C 0.5067(12) 0.8912(6) 0.4132(11) 0.0783(17) Uani 0.50 1 d PU . . C13 C 0.5528(12) 0.9655(6) 0.3568(11) 0.0811(17) Uani 0.50 1 d PU . . C13' C 0.5071(13) 0.9342(6) 0.2529(11) 0.0811(17) Uani 0.50 1 d PU . . O1W O 0.6139(3) 0.69102(15) 0.4628(2) 0.0424(8) Uani 1 1 d . . . O2W O 0.5000 0.9136(4) 0.0000 0.138(4) Uani 1 2 d S . . O3W O 0.6515(8) 1.0000 0.0125(16) 0.215(8) Uani 1 2 d S . . O6 O 1.0493(5) 1.0000 0.7880(5) 0.0669(14) Uani 1 2 d SU . . C16 C 1.0749(8) 1.0000 0.6468(7) 0.0294(17) Uani 0.60 2 d SPU . . C16' C 1.0923(17) 0.9615(10) 0.6653(16) 0.033(2) Uani 0.20 1 d PU . . C15 C 1.0728(18) 1.0640(11) 0.7529(17) 0.032(2) Uani 0.20 1 d PU . . C15' C 1.0556(12) 1.0351(8) 0.7300(11) 0.031(2) Uani 0.30 1 d PU . . O5W O 0.8120(15) 0.9223(7) 0.6017(16) 0.164(7) Uani 0.50 1 d P . . O4W O 0.7281(11) 0.9720(6) 0.6485(10) 0.135(6) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0316(5) 0.0414(5) 0.0287(4) -0.0046(3) 0.0185(3) -0.0028(3) Ni2 0.0238(4) 0.0369(5) 0.0248(4) 0.000 0.0125(3) 0.000 O2 0.058(2) 0.079(3) 0.0411(19) -0.0229(18) 0.0290(17) -0.032(2) O5 0.053(2) 0.084(3) 0.0455(19) -0.0277(19) 0.0383(17) -0.0300(19) O3 0.054(2) 0.080(3) 0.056(2) -0.025(2) 0.0309(18) -0.037(2) C5 0.0333(15) 0.0588(17) 0.0377(15) -0.0157(15) 0.0226(13) -0.0129(14) O4 0.055(2) 0.052(2) 0.0418(19) -0.0155(16) 0.0172(16) -0.0213(17) C8 0.0348(16) 0.0588(18) 0.0394(16) -0.0130(15) 0.0227(14) -0.0134(15) C4 0.0326(15) 0.0543(18) 0.0364(16) -0.0154(15) 0.0194(13) -0.0091(15) C3 0.0313(15) 0.0545(18) 0.0364(16) -0.0120(15) 0.0193(13) -0.0114(15) C6 0.0372(16) 0.0610(18) 0.0409(16) -0.0162(16) 0.0235(14) -0.0180(15) O1 0.086(3) 0.122(4) 0.058(2) -0.053(3) 0.060(2) -0.064(3) C9 0.0344(19) 0.057(2) 0.0381(19) -0.0074(18) 0.0229(16) -0.0085(18) C7 0.0362(16) 0.0615(18) 0.0387(16) -0.0165(15) 0.0234(14) -0.0155(15) C1 0.0448(18) 0.0649(19) 0.0428(17) -0.0168(16) 0.0246(15) -0.0174(17) C2 0.0298(16) 0.0502(19) 0.0417(18) -0.0097(17) 0.0175(15) -0.0079(16) N1 0.036(6) 0.053(6) 0.046(6) -0.019(5) 0.024(4) -0.006(5) N1' 0.034(6) 0.035(5) 0.056(7) -0.004(5) 0.021(5) 0.005(4) N2 0.190(8) 0.064(4) 0.074(4) 0.019(3) 0.039(5) 0.063(5) C14 0.093(3) 0.068(3) 0.076(3) 0.000 0.013(3) 0.000 C12' 0.084(3) 0.064(3) 0.072(3) -0.002(2) 0.014(3) 0.004(2) C12 0.084(3) 0.065(3) 0.071(3) -0.002(2) 0.015(3) 0.005(2) C10 0.086(3) 0.065(3) 0.072(3) -0.004(2) 0.011(3) 0.007(2) C10' 0.080(3) 0.065(3) 0.070(3) -0.004(2) 0.017(3) 0.003(2) C11 0.089(3) 0.066(3) 0.074(3) -0.003(2) 0.010(3) 0.004(2) C11' 0.085(3) 0.065(3) 0.073(3) -0.003(2) 0.016(3) 0.004(2) C13 0.088(3) 0.066(3) 0.075(3) -0.002(2) 0.014(3) 0.005(2) C13' 0.088(3) 0.065(3) 0.074(3) -0.002(2) 0.012(3) 0.004(2) O1W 0.0385(18) 0.054(2) 0.0385(17) -0.0112(15) 0.0191(14) -0.0090(15) O2W 0.152(8) 0.083(5) 0.230(12) 0.000 0.130(9) 0.000 O3W 0.079(6) 0.134(9) 0.46(3) 0.000 0.132(11) 0.000 O6 0.0662(17) 0.0702(17) 0.0653(17) 0.000 0.0263(10) 0.000 C16 0.0306(18) 0.0308(19) 0.0287(18) 0.000 0.0134(11) 0.000 C16' 0.033(2) 0.034(2) 0.032(2) 0.0001(10) 0.0136(11) 0.0002(10) C15 0.032(2) 0.032(2) 0.031(2) 0.0004(10) 0.0130(11) -0.0006(10) C15' 0.036(3) 0.036(3) 0.029(3) 0.009(3) 0.021(3) -0.002(3) O5W 0.193(16) 0.098(9) 0.25(2) -0.047(11) 0.139(16) -0.016(10) O4W 0.110(9) 0.134(11) 0.120(10) 0.036(8) -0.002(7) -0.041(7) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O1 2.016(3) . ? Ni1 O1 2.016(3) 7_666 ? Ni1 N1 2.037(14) . ? Ni1 N1 2.037(14) 7_666 ? Ni1 N1' 2.093(11) . ? Ni1 N1' 2.093(11) 7_666 ? Ni1 O1W 2.125(3) 7_666 ? Ni1 O1W 2.125(3) . ? Ni2 O6 1.989(6) . ? Ni2 O4 2.002(3) 5_777 ? Ni2 O4 2.002(3) 2_757 ? Ni2 O3 2.009(3) . ? Ni2 O3 2.009(3) 6_575 ? Ni2 Ni2 2.6910(14) 5_777 ? O2 C1 1.262(6) . ? O5 C5 1.373(6) . ? O5 C9 1.411(6) . ? O3 C2 1.255(6) . ? C5 C4 1.376(7) . ? C5 C6 1.385(7) . ? O4 C2 1.243(6) . ? O4 Ni2 2.002(3) 5_777 ? C8 C3 1.378(6) . ? C8 C7 1.389(7) . ? C8 H8 0.9300 . ? C4 C3 1.394(6) . ? C4 H4 0.9300 . ? C3 C2 1.490(7) . ? C6 C7 1.390(7) . ? C6 H6 0.9300 . ? O1 C1 1.249(7) . ? C9 C9 1.508(9) 2_657 ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C7 C1 1.506(7) . ? N1 N1' 0.667(10) . ? N1 C12' 1.037(18) . ? N1 C12 1.295(18) . ? N1 C10 1.302(19) . ? N1' C12 1.161(18) . ? N1' C12' 1.32(2) . ? N1' C10' 1.411(19) . ? N1' C10 1.728(19) . ? N2 C11 1.186(16) . ? N2 C12' 1.315(18) . ? N2 C11' 1.450(18) . ? N2 C13' 1.457(15) . ? N2 C13 1.472(16) . ? N2 C12 1.532(15) . ? C14 C13 1.497(19) 6_575 ? C14 C13 1.497(19) . ? C14 C13' 1.643(15) . ? C14 C13' 1.643(15) 6_575 ? C12' C10 1.002(17) . ? C12' C12 1.158(19) . ? C12' C11 1.22(2) . ? C12 C10' 1.67(2) . ? C12 C11' 1.94(2) . ? C10 C11 1.36(2) . ? C10' C11' 1.407(19) . ? C11 C13' 1.56(2) . ? C11' C13 2.02(2) . ? C13 C13 1.53(3) 6_575 ? C13 C13' 1.54(2) . ? O6 C15' 1.160(14) . ? O6 C15' 1.160(14) 6_575 ? O6 C15 1.57(2) 6_575 ? O6 C15 1.57(2) . ? C16 C16' 0.90(2) 6_575 ? C16 C16' 0.90(2) . ? C16 C15' 1.520(18) 6_575 ? C16 C15' 1.520(18) . ? C16' C15' 1.20(3) 6_575 ? C16' C15 1.48(3) 6_575 ? C16' C16' 1.70(4) 6_575 ? C16' C15' 2.02(3) . ? C15 C15' 0.71(2) . ? C15 C16' 1.48(3) 6_575 ? C15' C16' 1.20(3) 6_575 ? C15' C15' 1.55(3) 6_575 ? O4W O4W 1.24(3) 6_575 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ni1 O1 180.00(7) . 7_666 ? O1 Ni1 N1 98.9(3) . . ? O1 Ni1 N1 81.1(3) 7_666 . ? O1 Ni1 N1 81.1(3) . 7_666 ? O1 Ni1 N1 98.9(3) 7_666 7_666 ? N1 Ni1 N1 180.000(3) . 7_666 ? O1 Ni1 N1' 81.8(4) . . ? O1 Ni1 N1' 98.2(4) 7_666 . ? N1 Ni1 N1' 18.5(3) . . ? N1 Ni1 N1' 161.5(3) 7_666 . ? O1 Ni1 N1' 98.2(4) . 7_666 ? O1 Ni1 N1' 81.8(4) 7_666 7_666 ? N1 Ni1 N1' 161.5(3) . 7_666 ? N1 Ni1 N1' 18.5(3) 7_666 7_666 ? N1' Ni1 N1' 180.000(3) . 7_666 ? O1 Ni1 O1W 88.80(14) . 7_666 ? O1 Ni1 O1W 91.20(14) 7_666 7_666 ? N1 Ni1 O1W 84.2(3) . 7_666 ? N1 Ni1 O1W 95.8(3) 7_666 7_666 ? N1' Ni1 O1W 91.1(3) . 7_666 ? N1' Ni1 O1W 88.9(3) 7_666 7_666 ? O1 Ni1 O1W 91.20(14) . . ? O1 Ni1 O1W 88.80(14) 7_666 . ? N1 Ni1 O1W 95.8(3) . . ? N1 Ni1 O1W 84.2(3) 7_666 . ? N1' Ni1 O1W 88.9(3) . . ? N1' Ni1 O1W 91.1(3) 7_666 . ? O1W Ni1 O1W 180.0 7_666 . ? O6 Ni2 O4 95.39(16) . 5_777 ? O6 Ni2 O4 95.39(16) . 2_757 ? O4 Ni2 O4 89.1(2) 5_777 2_757 ? O6 Ni2 O3 98.22(16) . . ? O4 Ni2 O3 166.37(15) 5_777 . ? O4 Ni2 O3 89.15(18) 2_757 . ? O6 Ni2 O3 98.22(16) . 6_575 ? O4 Ni2 O3 89.15(17) 5_777 6_575 ? O4 Ni2 O3 166.37(15) 2_757 6_575 ? O3 Ni2 O3 89.4(3) . 6_575 ? O6 Ni2 Ni2 175.48(18) . 5_777 ? O4 Ni2 Ni2 81.41(11) 5_777 5_777 ? O4 Ni2 Ni2 81.41(11) 2_757 5_777 ? O3 Ni2 Ni2 84.97(11) . 5_777 ? O3 Ni2 Ni2 84.97(11) 6_575 5_777 ? C5 O5 C9 119.4(3) . . ? C2 O3 Ni2 121.8(3) . . ? O5 C5 C4 114.6(4) . . ? O5 C5 C6 124.4(4) . . ? C4 C5 C6 121.0(4) . . ? C2 O4 Ni2 126.8(3) . 5_777 ? C3 C8 C7 120.5(4) . . ? C3 C8 H8 119.8 . . ? C7 C8 H8 119.8 . . ? C5 C4 C3 120.3(4) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? C8 C3 C4 119.1(4) . . ? C8 C3 C2 121.0(4) . . ? C4 C3 C2 119.8(4) . . ? C5 C6 C7 118.7(4) . . ? C5 C6 H6 120.7 . . ? C7 C6 H6 120.7 . . ? C1 O1 Ni1 132.4(3) . . ? O5 C9 C9 105.7(3) . 2_657 ? O5 C9 H9A 110.6 . . ? C9 C9 H9A 110.6 2_657 . ? O5 C9 H9B 110.6 . . ? C9 C9 H9B 110.6 2_657 . ? H9A C9 H9B 108.7 . . ? C8 C7 C6 120.5(4) . . ? C8 C7 C1 118.8(4) . . ? C6 C7 C1 120.7(4) . . ? O1 C1 O2 126.1(5) . . ? O1 C1 C7 115.7(4) . . ? O2 C1 C7 118.2(5) . . ? O4 C2 O3 125.0(4) . . ? O4 C2 C3 117.6(4) . . ? O3 C2 C3 117.5(4) . . ? N1' N1 C12' 99(2) . . ? N1' N1 C12 63.4(18) . . ? C12' N1 C12 58.3(12) . . ? N1' N1 C10 119(2) . . ? C12' N1 C10 49.1(10) . . ? C12 N1 C10 107.1(13) . . ? N1' N1 Ni1 85.4(19) . . ? C12' N1 Ni1 175.3(13) . . ? C12 N1 Ni1 125.8(10) . . ? C10 N1 Ni1 127.0(10) . . ? N1 N1' C12 86(2) . . ? N1 N1' C12' 51.1(19) . . ? C12 N1' C12' 55.3(10) . . ? N1 N1' C10' 157(2) . . ? C12 N1' C10' 80.2(12) . . ? C12' N1' C10' 106.3(12) . . ? N1 N1' C10 41.2(17) . . ? C12 N1' C10 90.4(12) . . ? C12' N1' C10 35.3(8) . . ? C10' N1' C10 120.9(11) . . ? N1 N1' Ni1 76.1(18) . . ? C12 N1' Ni1 131.0(11) . . ? C12' N1' Ni1 127.1(11) . . ? C10' N1' Ni1 126.4(10) . . ? C10 N1' Ni1 103.4(7) . . ? C11 N2 C12' 57.9(10) . . ? C11 N2 C11' 128.5(13) . . ? C12' N2 C11' 106.5(10) . . ? C11 N2 C13' 71.7(9) . . ? C12' N2 C13' 127.2(11) . . ? C11' N2 C13' 116.9(11) . . ? C11 N2 C13 132.1(11) . . ? C12' N2 C13 149.6(12) . . ? C11' N2 C13 87.7(10) . . ? C13' N2 C13 63.2(8) . . ? C11 N2 C12 104.9(10) . . ? C12' N2 C12 47.2(8) . . ? C11' N2 C12 81.3(9) . . ? C13' N2 C12 159.7(12) . . ? C13 N2 C12 111.6(9) . . ? C13 C14 C13 61.3(12) 6_575 . ? C13 C14 C13' 112.2(11) 6_575 . ? C13 C14 C13' 58.3(8) . . ? C13 C14 C13' 58.3(8) 6_575 6_575 ? C13 C14 C13' 112.2(11) . 6_575 ? C13' C14 C13' 124.8(13) . 6_575 ? C10 C12' N1 79.4(16) . . ? C10 C12' C12 150(2) . . ? N1 C12' C12 72.0(14) . . ? C10 C12' C11 75.0(15) . . ? N1 C12' C11 153.3(18) . . ? C12 C12' C11 131.7(19) . . ? C10 C12' N2 126.1(17) . . ? N1 C12' N2 142.0(18) . . ? C12 C12' N2 76.3(13) . . ? C11 C12' N2 55.7(11) . . ? C10 C12' N1' 95.4(16) . . ? N1 C12' N1' 30.0(8) . . ? C12 C12' N1' 55.5(11) . . ? C11 C12' N1' 146.1(18) . . ? N2 C12' N1' 112.8(14) . . ? C12' C12 N1' 69.2(13) . . ? C12' C12 N1 49.7(10) . . ? N1' C12 N1 30.9(6) . . ? C12' C12 N2 56.5(11) . . ? N1' C12 N2 108.2(12) . . ? N1 C12 N2 103.6(11) . . ? C12' C12 C10' 99.7(14) . . ? N1' C12 C10' 56.5(10) . . ? N1 C12 C10' 86.3(11) . . ? N2 C12 C10' 89.0(10) . . ? C12' C12 C11' 87.4(13) . . ? N1' C12 C11' 90.9(12) . . ? N1 C12 C11' 110.6(12) . . ? N2 C12 C11' 47.5(7) . . ? C10' C12 C11' 45.1(8) . . ? C12' C10 N1 51.5(12) . . ? C12' C10 C11 59.6(13) . . ? N1 C10 C11 110.8(14) . . ? C12' C10 N1' 49.4(13) . . ? N1 C10 N1' 19.7(6) . . ? C11 C10 N1' 102.7(12) . . ? C11' C10' N1' 108.0(14) . . ? C11' C10' C12 77.9(11) . . ? N1' C10' C12 43.3(8) . . ? N2 C11 C12' 66.4(12) . . ? N2 C11 C10 108.6(13) . . ? C12' C11 C10 45.3(10) . . ? N2 C11 C13' 62.2(9) . . ? C12' C11 C13' 126.3(15) . . ? C10 C11 C13' 170.8(16) . . ? C10' C11' N2 103.4(12) . . ? C10' C11' C12 57.0(9) . . ? N2 C11' C12 51.2(7) . . ? C10' C11' C13 132.3(12) . . ? N2 C11' C13 46.6(7) . . ? C12 C11' C13 77.5(9) . . ? N2 C13 C14 111.4(11) . . ? N2 C13 C13 170.0(8) . 6_575 ? C14 C13 C13 59.3(6) . 6_575 ? N2 C13 C13' 57.9(8) . . ? C14 C13 C13' 65.6(9) . . ? C13 C13 C13' 116.8(7) 6_575 . ? N2 C13 C11' 45.7(7) . . ? C14 C13 C11' 152.5(10) . . ? C13 C13 C11' 144.3(6) 6_575 . ? C13' C13 C11' 87.1(10) . . ? N2 C13' C13 58.9(8) . . ? N2 C13' C11 46.1(7) . . ? C13 C13' C11 103.4(11) . . ? N2 C13' C14 104.4(9) . . ? C13 C13' C14 56.1(8) . . ? C11 C13' C14 127.9(12) . . ? C15' O6 C15' 84.0(18) . 6_575 ? C15' O6 C15 107.4(14) . 6_575 ? C15' O6 C15 25.0(10) 6_575 6_575 ? C15' O6 C15 25.0(10) . . ? C15' O6 C15 107.4(14) 6_575 . ? C15 O6 C15 128.4(18) 6_575 . ? C15' O6 Ni2 137.5(9) . . ? C15' O6 Ni2 137.5(9) 6_575 . ? C15 O6 Ni2 115.1(9) 6_575 . ? C15 O6 Ni2 115.1(9) . . ? C16' C16 C16' 144(3) 6_575 . ? C16' C16 C15' 110.9(18) 6_575 6_575 ? C16' C16 C15' 52.1(16) . 6_575 ? C16' C16 C15' 52.1(17) 6_575 . ? C16' C16 C15' 110.9(18) . . ? C15' C16 C15' 61.4(12) 6_575 . ? C16 C16' C15' 92(2) . 6_575 ? C16 C16' C15 120(2) . 6_575 ? C15' C16' C15 28.5(11) 6_575 6_575 ? C16 C16' C16' 18.0(15) . 6_575 ? C15' C16' C16' 86.4(13) 6_575 6_575 ? C15 C16' C16' 112.4(13) 6_575 6_575 ? C16 C16' C15' 44.6(14) . . ? C15' C16' C15' 50.0(14) 6_575 . ? C15 C16' C15' 76.7(14) 6_575 . ? C16' C16' C15' 36.3(7) 6_575 . ? C15' C15 C16' 53(2) . 6_575 ? C15' C15 O6 43.2(19) . . ? C16' C15 O6 92.6(17) 6_575 . ? C15 C15' O6 112(3) . . ? C15 C15' C16' 98(3) . 6_575 ? O6 C15' C16' 138.8(19) . 6_575 ? C15 C15' C16 134(3) . . ? O6 C15' C16 107.1(13) . . ? C16' C15' C16 36.1(12) 6_575 . ? C15 C15' C15' 154(2) . 6_575 ? O6 C15' C15' 48.0(9) . 6_575 ? C16' C15' C15' 93.6(13) 6_575 6_575 ? C16 C15' C15' 59.3(6) . 6_575 ? C15 C15' C16' 147(3) . . ? O6 C15' C16' 83.2(12) . . ? C16' C15' C16' 57.3(17) 6_575 . ? C16 C15' C16' 24.5(7) . . ? C15' C15' C16' 36.3(7) 6_575 . ? 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 Ni2 O3 C2 175.5(4) . . . . ? O4 Ni2 O3 C2 -2.3(10) 5_777 . . . ? O4 Ni2 O3 C2 80.2(4) 2_757 . . . ? O3 Ni2 O3 C2 -86.2(4) 6_575 . . . ? Ni2 Ni2 O3 C2 -1.2(4) 5_777 . . . ? C9 O5 C5 C4 -178.0(5) . . . . ? C9 O5 C5 C6 0.4(8) . . . . ? O5 C5 C4 C3 -180.0(5) . . . . ? C6 C5 C4 C3 1.5(8) . . . . ? C7 C8 C3 C4 -0.8(8) . . . . ? C7 C8 C3 C2 176.3(5) . . . . ? C5 C4 C3 C8 0.0(7) . . . . ? C5 C4 C3 C2 -177.1(5) . . . . ? O5 C5 C6 C7 179.5(5) . . . . ? C4 C5 C6 C7 -2.1(8) . . . . ? O1 Ni1 O1 C1 -34(100) 7_666 . . . ? N1 Ni1 O1 C1 106.2(7) . . . . ? N1 Ni1 O1 C1 -73.8(7) 7_666 . . . ? N1' Ni1 O1 C1 98.9(7) . . . . ? N1' Ni1 O1 C1 -81.1(7) 7_666 . . . ? O1W Ni1 O1 C1 -169.8(7) 7_666 . . . ? O1W Ni1 O1 C1 10.2(7) . . . . ? C5 O5 C9 C9 -175.8(4) . . . 2_657 ? C3 C8 C7 C6 0.1(8) . . . . ? C3 C8 C7 C1 179.8(5) . . . . ? C5 C6 C7 C8 1.4(8) . . . . ? C5 C6 C7 C1 -178.3(5) . . . . ? Ni1 O1 C1 O2 -2.2(11) . . . . ? Ni1 O1 C1 C7 178.1(4) . . . . ? C8 C7 C1 O1 2.8(8) . . . . ? C6 C7 C1 O1 -177.5(6) . . . . ? C8 C7 C1 O2 -176.9(5) . . . . ? C6 C7 C1 O2 2.8(8) . . . . ? Ni2 O4 C2 O3 -1.9(8) 5_777 . . . ? Ni2 O4 C2 C3 176.2(3) 5_777 . . . ? Ni2 O3 C2 O4 2.2(8) . . . . ? Ni2 O3 C2 C3 -175.9(3) . . . . ? C8 C3 C2 O4 -169.8(5) . . . . ? C4 C3 C2 O4 7.2(7) . . . . ? C8 C3 C2 O3 8.4(7) . . . . ? C4 C3 C2 O3 -174.5(5) . . . . ? O1 Ni1 N1 N1' -23.3(18) . . . . ? O1 Ni1 N1 N1' 156.7(18) 7_666 . . . ? N1 Ni1 N1 N1' 165(100) 7_666 . . . ? N1' Ni1 N1 N1' 180.000(9) 7_666 . . . ? O1W Ni1 N1 N1' -111.2(18) 7_666 . . . ? O1W Ni1 N1 N1' 68.8(18) . . . . ? O1 Ni1 N1 C12' 180(100) . . . . ? O1 Ni1 N1 C12' 0(17) 7_666 . . . ? N1 Ni1 N1 C12' 8(100) 7_666 . . . ? N1' Ni1 N1 C12' -157(18) . . . . ? N1' Ni1 N1 C12' 23(18) 7_666 . . . ? O1W Ni1 N1 C12' 92(17) 7_666 . . . ? O1W Ni1 N1 C12' -88(17) . . . . ? O1 Ni1 N1 C12 28.9(13) . . . . ? O1 Ni1 N1 C12 -151.1(13) 7_666 . . . ? N1 Ni1 N1 C12 -143(100) 7_666 . . . ? N1' Ni1 N1 C12 52.3(17) . . . . ? N1' Ni1 N1 C12 -127.7(17) 7_666 . . . ? O1W Ni1 N1 C12 -58.9(13) 7_666 . . . ? O1W Ni1 N1 C12 121.1(13) . . . . ? O1 Ni1 N1 C10 -146.7(13) . . . . ? O1 Ni1 N1 C10 33.3(13) 7_666 . . . ? N1 Ni1 N1 C10 41(100) 7_666 . . . ? N1' Ni1 N1 C10 -123(3) . . . . ? N1' Ni1 N1 C10 57(3) 7_666 . . . ? O1W Ni1 N1 C10 125.4(13) 7_666 . . . ? O1W Ni1 N1 C10 -54.6(13) . . . . ? C12' N1 N1' C12 -47.7(16) . . . . ? C10 N1 N1' C12 -96(2) . . . . ? Ni1 N1 N1' C12 134.2(9) . . . . ? C12 N1 N1' C12' 47.7(16) . . . . ? C10 N1 N1' C12' -47.9(16) . . . . ? Ni1 N1 N1' C12' -178.1(14) . . . . ? C12' N1 N1' C10' 3(7) . . . . ? C12 N1 N1' C10' 51(5) . . . . ? C10 N1 N1' C10' -44(7) . . . . ? Ni1 N1 N1' C10' -175(5) . . . . ? C12' N1 N1' C10 47.9(16) . . . . ? C12 N1 N1' C10 96(2) . . . . ? Ni1 N1 N1' C10 -130.3(19) . . . . ? C12' N1 N1' Ni1 178.1(14) . . . . ? C12 N1 N1' Ni1 -134.2(8) . . . . ? C10 N1 N1' Ni1 130.3(19) . . . . ? O1 Ni1 N1' N1 156.7(18) . . . . ? O1 Ni1 N1' N1 -23.3(18) 7_666 . . . ? N1 Ni1 N1' N1 180.000(9) 7_666 . . . ? N1' Ni1 N1' N1 0(100) 7_666 . . . ? O1W Ni1 N1' N1 68.1(18) 7_666 . . . ? O1W Ni1 N1' N1 -111.9(18) . . . . ? O1 Ni1 N1' C12 85.3(16) . . . . ? O1 Ni1 N1' C12 -94.7(16) 7_666 . . . ? N1 Ni1 N1' C12 -71(2) . . . . ? N1 Ni1 N1' C12 109(2) 7_666 . . . ? N1' Ni1 N1' C12 0(100) 7_666 . . . ? O1W Ni1 N1' C12 -3.3(16) 7_666 . . . ? O1W Ni1 N1' C12 176.7(16) . . . . ? O1 Ni1 N1' C12' 158.6(12) . . . . ? O1 Ni1 N1' C12' -21.4(12) 7_666 . . . ? N1 Ni1 N1' C12' 1.8(14) . . . . ? N1 Ni1 N1' C12' -178.2(14) 7_666 . . . ? N1' Ni1 N1' C12' 0(100) 7_666 . . . ? O1W Ni1 N1' C12' 69.9(12) 7_666 . . . ? O1W Ni1 N1' C12' -110.1(12) . . . . ? O1 Ni1 N1' C10' -25.8(10) . . . . ? O1 Ni1 N1' C10' 154.2(10) 7_666 . . . ? N1 Ni1 N1' C10' 177(3) . . . . ? N1 Ni1 N1' C10' -3(3) 7_666 . . . ? N1' Ni1 N1' C10' 0(100) 7_666 . . . ? O1W Ni1 N1' C10' -114.5(11) 7_666 . . . ? O1W Ni1 N1' C10' 65.5(11) . . . . ? O1 Ni1 N1' C10 -172.2(8) . . . . ? O1 Ni1 N1' C10 7.8(8) 7_666 . . . ? N1 Ni1 N1' C10 31.1(16) . . . . ? N1 Ni1 N1' C10 -148.9(16) 7_666 . . . ? N1' Ni1 N1' C10 0(100) 7_666 . . . ? O1W Ni1 N1' C10 99.2(7) 7_666 . . . ? O1W Ni1 N1' C10 -80.8(7) . . . . ? N1' N1 C12' C10 -121(2) . . . . ? C12 N1 C12' C10 -172(2) . . . . ? Ni1 N1 C12' C10 35(17) . . . . ? N1' N1 C12' C12 51(2) . . . . ? C10 N1 C12' C12 172(2) . . . . ? Ni1 N1 C12' C12 -153(17) . . . . ? N1' N1 C12' C11 -105(5) . . . . ? C12 N1 C12' C11 -156(5) . . . . ? C10 N1 C12' C11 16(4) . . . . ? Ni1 N1 C12' C11 52(20) . . . . ? N1' N1 C12' N2 16(4) . . . . ? C12 N1 C12' N2 -35(2) . . . . ? C10 N1 C12' N2 137(3) . . . . ? Ni1 N1 C12' N2 173(15) . . . . ? C12 N1 C12' N1' -51(2) . . . . ? C10 N1 C12' N1' 121(2) . . . . ? Ni1 N1 C12' N1' 156(18) . . . . ? C11 N2 C12' C10 -28(2) . . . . ? C11' N2 C12' C10 98(2) . . . . ? C13' N2 C12' C10 -47(3) . . . . ? C13 N2 C12' C10 -148(2) . . . . ? C12 N2 C12' C10 158(3) . . . . ? C11 N2 C12' N1 -152(3) . . . . ? C11' N2 C12' N1 -27(3) . . . . ? C13' N2 C12' N1 -172(2) . . . . ? C13 N2 C12' N1 88(3) . . . . ? C12 N2 C12' N1 34(2) . . . . ? C11 N2 C12' C12 173.8(18) . . . . ? C11' N2 C12' C12 -60.7(13) . . . . ? C13' N2 C12' C12 154.4(15) . . . . ? C13 N2 C12' C12 54(3) . . . . ? C11' N2 C12' C11 125.5(14) . . . . ? C13' N2 C12' C11 -19.4(17) . . . . ? C13 N2 C12' C11 -120(2) . . . . ? C12 N2 C12' C11 -173.8(18) . . . . ? C11 N2 C12' N1' -143.5(18) . . . . ? C11' N2 C12' N1' -18.0(16) . . . . ? C13' N2 C12' N1' -162.9(12) . . . . ? C13 N2 C12' N1' 97(2) . . . . ? C12 N2 C12' N1' 42.7(13) . . . . ? N1 N1' C12' C10 58(2) . . . . ? C12 N1' C12' C10 174(2) . . . . ? C10' N1' C12' C10 -120.8(17) . . . . ? Ni1 N1' C12' C10 55.5(19) . . . . ? C12 N1' C12' N1 116(3) . . . . ? C10' N1' C12' N1 -179(3) . . . . ? C10 N1' C12' N1 -58(2) . . . . ? Ni1 N1' C12' N1 -2.3(17) . . . . ? N1 N1' C12' C12 -116(3) . . . . ? C10' N1' C12' C12 65.2(14) . . . . ? C10 N1' C12' C12 -174(2) . . . . ? Ni1 N1' C12' C12 -118.5(15) . . . . ? N1 N1' C12' C11 129(4) . . . . ? C12 N1' C12' C11 -115(3) . . . . ? C10' N1' C12' C11 -50(3) . . . . ? C10 N1' C12' C11 71(3) . . . . ? Ni1 N1' C12' C11 126(3) . . . . ? N1 N1' C12' N2 -169(2) . . . . ? C12 N1' C12' N2 -53.1(14) . . . . ? C10' N1' C12' N2 12.1(16) . . . . ? C10 N1' C12' N2 133(2) . . . . ? Ni1 N1' C12' N2 -171.6(9) . . . . ? C10 C12' C12 N1' -12(4) . . . . ? N1 C12' C12 N1' -28.1(10) . . . . ? C11 C12' C12 N1' 137(2) . . . . ? N2 C12' C12 N1' 130.6(13) . . . . ? C10 C12' C12 N1 16(4) . . . . ? C11 C12' C12 N1 166(3) . . . . ? N2 C12' C12 N1 158.8(16) . . . . ? N1' C12' C12 N1 28.1(10) . . . . ? C10 C12' C12 N2 -143(5) . . . . ? N1 C12' C12 N2 -158.8(16) . . . . ? C11 C12' C12 N2 7(2) . . . . ? N1' C12' C12 N2 -130.6(13) . . . . ? C10 C12' C12 C10' -61(5) . . . . ? N1 C12' C12 C10' -76.6(13) . . . . ? C11 C12' C12 C10' 89(2) . . . . ? N2 C12' C12 C10' 82.2(11) . . . . ? N1' C12' C12 C10' -48.4(10) . . . . ? C10 C12' C12 C11' -104(4) . . . . ? N1 C12' C12 C11' -120.1(13) . . . . ? C11 C12' C12 C11' 45(2) . . . . ? N2 C12' C12 C11' 38.7(8) . . . . ? N1' C12' C12 C11' -92.0(11) . . . . ? N1 N1' C12 C12' 44(2) . . . . ? C10' N1' C12 C12' -117.9(13) . . . . ? C10 N1' C12 C12' 3.5(12) . . . . ? Ni1 N1' C12 C12' 111.7(16) . . . . ? C12' N1' C12 N1 -44(2) . . . . ? C10' N1' C12 N1 -162(2) . . . . ? C10 N1' C12 N1 -41.0(17) . . . . ? Ni1 N1' C12 N1 67.3(18) . . . . ? N1 N1' C12 N2 86(2) . . . . ? C12' N1' C12 N2 41.8(12) . . . . ? C10' N1' C12 N2 -76.1(12) . . . . ? C10 N1' C12 N2 45.2(13) . . . . ? Ni1 N1' C12 N2 153.5(10) . . . . ? N1 N1' C12 C10' 162(2) . . . . ? C12' N1' C12 C10' 117.9(13) . . . . ? C10 N1' C12 C10' 121.3(10) . . . . ? Ni1 N1' C12 C10' -130.4(16) . . . . ? N1 N1' C12 C11' 131.3(19) . . . . ? C12' N1' C12 C11' 86.9(12) . . . . ? C10' N1' C12 C11' -31.0(9) . . . . ? C10 N1' C12 C11' 90.3(9) . . . . ? Ni1 N1' C12 C11' -161.4(11) . . . . ? N1' N1 C12 C12' -121(3) . . . . ? C10 N1 C12 C12' -6.3(16) . . . . ? Ni1 N1 C12 C12' 177.3(17) . . . . ? C12' N1 C12 N1' 121(3) . . . . ? C10 N1 C12 N1' 115(2) . . . . ? Ni1 N1 C12 N1' -61.9(18) . . . . ? N1' N1 C12 N2 -103(2) . . . . ? C12' N1 C12 N2 18.1(14) . . . . ? C10 N1 C12 N2 11.8(16) . . . . ? Ni1 N1 C12 N2 -164.6(8) . . . . ? N1' N1 C12 C10' -14.7(19) . . . . ? C12' N1 C12 C10' 106.1(15) . . . . ? C10 N1 C12 C10' 99.8(13) . . . . ? Ni1 N1 C12 C10' -76.6(12) . . . . ? N1' N1 C12 C11' -53(2) . . . . ? C12' N1 C12 C11' 67.5(15) . . . . ? C10 N1 C12 C11' 61.1(16) . . . . ? Ni1 N1 C12 C11' -115.2(11) . . . . ? C11 N2 C12 C12' -5.4(16) . . . . ? C11' N2 C12 C12' 122.2(14) . . . . ? C13' N2 C12 C12' -83(3) . . . . ? C13 N2 C12 C12' -153.8(15) . . . . ? C11 N2 C12 N1' -53.7(18) . . . . ? C12' N2 C12 N1' -48.3(14) . . . . ? C11' N2 C12 N1' 73.9(14) . . . . ? C13' N2 C12 N1' -131(2) . . . . ? C13 N2 C12 N1' 157.9(14) . . . . ? C11 N2 C12 N1 -21.9(17) . . . . ? C12' N2 C12 N1 -16.5(13) . . . . ? C11' N2 C12 N1 105.7(13) . . . . ? C13' N2 C12 N1 -99(3) . . . . ? C13 N2 C12 N1 -170.3(13) . . . . ? C11 N2 C12 C10' -107.8(13) . . . . ? C12' N2 C12 C10' -102.4(14) . . . . ? C11' N2 C12 C10' 19.8(9) . . . . ? C13' N2 C12 C10' 175(2) . . . . ? C13 N2 C12 C10' 103.8(11) . . . . ? C11 N2 C12 C11' -127.6(13) . . . . ? C12' N2 C12 C11' -122.2(14) . . . . ? C13' N2 C12 C11' 155(3) . . . . ? C13 N2 C12 C11' 84.0(11) . . . . ? C12 C12' C10 N1 -16(4) . . . . ? C11 C12' C10 N1 -172.4(19) . . . . ? N2 C12' C10 N1 -149(3) . . . . ? N1' C12' C10 N1 -25.5(9) . . . . ? N1 C12' C10 C11 172.4(19) . . . . ? C12 C12' C10 C11 157(5) . . . . ? N2 C12' C10 C11 23.6(19) . . . . ? N1' C12' C10 C11 146.9(17) . . . . ? N1 C12' C10 N1' 25.5(9) . . . . ? C12 C12' C10 N1' 10(4) . . . . ? C11 C12' C10 N1' -146.9(17) . . . . ? N2 C12' C10 N1' -123(3) . . . . ? N1' N1 C10 C12' 76(3) . . . . ? C12 N1 C10 C12' 7.1(18) . . . . ? Ni1 N1 C10 C12' -176.6(18) . . . . ? N1' N1 C10 C11 69(3) . . . . ? C12' N1 C10 C11 -7.0(17) . . . . ? C12 N1 C10 C11 0(2) . . . . ? Ni1 N1 C10 C11 176.5(11) . . . . ? C12' N1 C10 N1' -76(3) . . . . ? C12 N1 C10 N1' -69(2) . . . . ? Ni1 N1 C10 N1' 108(3) . . . . ? N1 N1' C10 C12' -88(3) . . . . ? C12 N1' C10 C12' -4.9(18) . . . . ? C10' N1' C10 C12' 73.8(19) . . . . ? Ni1 N1' C10 C12' -137.5(17) . . . . ? C12 N1' C10 N1 83(3) . . . . ? C12' N1' C10 N1 88(3) . . . . ? C10' N1' C10 N1 162(3) . . . . ? Ni1 N1' C10 N1 -50(2) . . . . ? N1 N1' C10 C11 -117(3) . . . . ? C12 N1' C10 C11 -33.8(15) . . . . ? C12' N1' C10 C11 -28.9(16) . . . . ? C10' N1' C10 C11 45.0(17) . . . . ? Ni1 N1' C10 C11 -166.4(11) . . . . ? N1 N1' C10' C11' -4(6) . . . . ? C12 N1' C10' C11' 48.4(13) . . . . ? C12' N1' C10' C11' -0.9(15) . . . . ? C10 N1' C10' C11' -36.2(16) . . . . ? Ni1 N1' C10' C11' -177.2(9) . . . . ? N1 N1' C10' C12 -52(6) . . . . ? C12' N1' C10' C12 -49.2(10) . . . . ? C10 N1' C10' C12 -84.5(13) . . . . ? Ni1 N1' C10' C12 134.4(14) . . . . ? C12' C12 C10' C11' -76.4(14) . . . . ? N1' C12 C10' C11' -133.4(13) . . . . ? N1 C12 C10' C11' -124.4(12) . . . . ? N2 C12 C10' C11' -20.7(9) . . . . ? C12' C12 C10' N1' 57.0(13) . . . . ? N1 C12 C10' N1' 9.0(11) . . . . ? N2 C12 C10' N1' 112.7(12) . . . . ? C11' C12 C10' N1' 133.4(13) . . . . ? C11' N2 C11 C12' -85.9(15) . . . . ? C13' N2 C11 C12' 163.8(14) . . . . ? C13 N2 C11 C12' 143.6(17) . . . . ? C12 N2 C11 C12' 4.7(14) . . . . ? C12' N2 C11 C10 17.1(13) . . . . ? C11' N2 C11 C10 -68.8(19) . . . . ? C13' N2 C11 C10 -179.1(17) . . . . ? C13 N2 C11 C10 160.7(14) . . . . ? C12 N2 C11 C10 21.8(18) . . . . ? C12' N2 C11 C13' -163.8(14) . . . . ? C11' N2 C11 C13' 110.3(14) . . . . ? C13 N2 C11 C13' -20.2(16) . . . . ? C12 N2 C11 C13' -159.1(12) . . . . ? C10 C12' C11 N2 156.9(19) . . . . ? N1 C12' C11 N2 140(5) . . . . ? C12 C12' C11 N2 -8(2) . . . . ? N1' C12' C11 N2 80(3) . . . . ? N1 C12' C11 C10 -17(4) . . . . ? C12 C12' C11 C10 -165(3) . . . . ? N2 C12' C11 C10 -156.9(19) . . . . ? N1' C12' C11 C10 -77(3) . . . . ? C10 C12' C11 C13' 175(2) . . . . ? N1 C12' C11 C13' 158(4) . . . . ? C12 C12' C11 C13' 10(4) . . . . ? N2 C12' C11 C13' 17.8(16) . . . . ? N1' C12' C11 C13' 98(3) . . . . ? C12' C10 C11 N2 -22.3(18) . . . . ? N1 C10 C11 N2 -16(2) . . . . ? N1' C10 C11 N2 2.8(18) . . . . ? N1 C10 C11 C12' 6.3(16) . . . . ? N1' C10 C11 C12' 25.1(14) . . . . ? C12' C10 C11 C13' -27(10) . . . . ? N1 C10 C11 C13' -21(11) . . . . ? N1' C10 C11 C13' -2(11) . . . . ? N1' C10' C11' N2 -9.1(14) . . . . ? C12 C10' C11' N2 22.6(10) . . . . ? N1' C10' C11' C12 -31.6(9) . . . . ? N1' C10' C11' C13 -51.5(18) . . . . ? C12 C10' C11' C13 -19.9(16) . . . . ? C11 N2 C11' C10' 77.7(15) . . . . ? C12' N2 C11' C10' 16.0(14) . . . . ? C13' N2 C11' C10' 165.1(10) . . . . ? C13 N2 C11' C10' -136.7(11) . . . . ? C12 N2 C11' C10' -24.4(11) . . . . ? C11 N2 C11' C12 102.1(13) . . . . ? C12' N2 C11' C12 40.4(9) . . . . ? C13' N2 C11' C12 -170.5(11) . . . . ? C13 N2 C11' C12 -112.3(9) . . . . ? C11 N2 C11' C13 -145.6(14) . . . . ? C12' N2 C11' C13 152.7(12) . . . . ? C13' N2 C11' C13 -58.3(9) . . . . ? C12 N2 C11' C13 112.3(9) . . . . ? C12' C12 C11' C10' 106.5(14) . . . . ? N1' C12 C11' C10' 37.3(11) . . . . ? N1 C12 C11' C10' 61.7(13) . . . . ? N2 C12 C11' C10' 151.4(12) . . . . ? C12' C12 C11' N2 -44.9(11) . . . . ? N1' C12 C11' N2 -114.1(12) . . . . ? N1 C12 C11' N2 -89.7(13) . . . . ? C10' C12 C11' N2 -151.4(12) . . . . ? C12' C12 C11' C13 -88.4(12) . . . . ? N1' C12 C11' C13 -157.6(12) . . . . ? N1 C12 C11' C13 -133.2(12) . . . . ? N2 C12 C11' C13 -43.5(7) . . . . ? C10' C12 C11' C13 165.1(11) . . . . ? C11 N2 C13 C14 -18(2) . . . . ? C12' N2 C13 C14 79(2) . . . . ? C11' N2 C13 C14 -161.6(11) . . . . ? C13' N2 C13 C14 -39.7(11) . . . . ? C12 N2 C13 C14 118.7(12) . . . . ? C11 N2 C13 C13 -39(5) . . . 6_575 ? C12' N2 C13 C13 58(5) . . . 6_575 ? C11' N2 C13 C13 177(4) . . . 6_575 ? C13' N2 C13 C13 -61(4) . . . 6_575 ? C12 N2 C13 C13 98(4) . . . 6_575 ? C11 N2 C13 C13' 21.5(18) . . . . ? C12' N2 C13 C13' 119(2) . . . . ? C11' N2 C13 C13' -121.9(11) . . . . ? C12 N2 C13 C13' 158.5(13) . . . . ? C11 N2 C13 C11' 143.4(19) . . . . ? C12' N2 C13 C11' -120(2) . . . . ? C13' N2 C13 C11' 121.9(11) . . . . ? C12 N2 C13 C11' -79.7(10) . . . . ? C13 C14 C13 N2 -175.8(7) 6_575 . . . ? C13' C14 C13 N2 36.5(10) . . . . ? C13' C14 C13 N2 154.7(10) 6_575 . . . ? C13' C14 C13 C13 -147.7(8) . . . 6_575 ? C13' C14 C13 C13 -29.5(6) 6_575 . . 6_575 ? C13 C14 C13 C13' 147.7(8) 6_575 . . . ? C13' C14 C13 C13' 118.2(14) 6_575 . . . ? C13 C14 C13 C11' 155(2) 6_575 . . . ? C13' C14 C13 C11' 7(2) . . . . ? C13' C14 C13 C11' 125(2) 6_575 . . . ? C10' C11' C13 N2 64.6(16) . . . . ? C12 C11' C13 N2 47.6(8) . . . . ? C10' C11' C13 C14 104(3) . . . . ? N2 C11' C13 C14 40(2) . . . . ? C12 C11' C13 C14 87(2) . . . . ? C10' C11' C13 C13 -114.6(15) . . . 6_575 ? N2 C11' C13 C13 -179.2(10) . . . 6_575 ? C12 C11' C13 C13 -131.6(9) . . . 6_575 ? C10' C11' C13 C13' 110.7(17) . . . . ? N2 C11' C13 C13' 46.1(9) . . . . ? C12 C11' C13 C13' 93.7(10) . . . . ? C11 N2 C13' C13 -163.3(14) . . . . ? C12' N2 C13' C13 -146.1(16) . . . . ? C11' N2 C13' C13 72.1(12) . . . . ? C12 N2 C13' C13 -80(3) . . . . ? C12' N2 C13' C11 17.2(15) . . . . ? C11' N2 C13' C11 -124.5(14) . . . . ? C13 N2 C13' C11 163.3(14) . . . . ? C12 N2 C13' C11 83(3) . . . . ? C11 N2 C13' C14 -129.3(14) . . . . ? C12' N2 C13' C14 -112.0(14) . . . . ? C11' N2 C13' C14 106.2(12) . . . . ? C13 N2 C13' C14 34.0(10) . . . . ? C12 N2 C13' C14 -46(3) . . . . ? C14 C13 C13' N2 139.2(12) . . . . ? C13 C13 C13' N2 170.2(9) 6_575 . . . ? C11' C13 C13' N2 -37.5(8) . . . . ? N2 C13 C13' C11 -12.3(11) . . . . ? C14 C13 C13' C11 126.9(13) . . . . ? C13 C13 C13' C11 158.0(9) 6_575 . . . ? C11' C13 C13' C11 -49.8(12) . . . . ? N2 C13 C13' C14 -139.2(12) . . . . ? C13 C13 C13' C14 31.0(8) 6_575 . . . ? C11' C13 C13' C14 -176.7(10) . . . . ? C12' C11 C13' N2 -18.5(17) . . . . ? C10 C11 C13' N2 5(10) . . . . ? N2 C11 C13' C13 14.6(13) . . . . ? C12' C11 C13' C13 -4(2) . . . . ? C10 C11 C13' C13 20(11) . . . . ? N2 C11 C13' C14 71.8(16) . . . . ? C12' C11 C13' C14 53(3) . . . . ? C10 C11 C13' C14 77(11) . . . . ? C13 C14 C13' N2 -65.7(13) 6_575 . . . ? C13 C14 C13' N2 -35.3(10) . . . . ? C13' C14 C13' N2 -131.7(10) 6_575 . . . ? C13 C14 C13' C13 -30.5(9) 6_575 . . . ? C13' C14 C13' C13 -96.5(15) 6_575 . . . ? C13 C14 C13' C11 -110.7(16) 6_575 . . . ? C13 C14 C13' C11 -80.2(16) . . . . ? C13' C14 C13' C11 -176.7(10) 6_575 . . . ? O4 Ni2 O6 C15' -53.1(13) 5_777 . . . ? O4 Ni2 O6 C15' -142.7(13) 2_757 . . . ? O3 Ni2 O6 C15' 127.4(13) . . . . ? O3 Ni2 O6 C15' 36.8(13) 6_575 . . . ? Ni2 Ni2 O6 C15' -97.9(13) 5_777 . . . ? O4 Ni2 O6 C15' 142.7(13) 5_777 . . 6_575 ? O4 Ni2 O6 C15' 53.1(13) 2_757 . . 6_575 ? O3 Ni2 O6 C15' -36.8(13) . . . 6_575 ? O3 Ni2 O6 C15' -127.4(13) 6_575 . . 6_575 ? Ni2 Ni2 O6 C15' 97.9(13) 5_777 . . 6_575 ? O4 Ni2 O6 C15 128.7(9) 5_777 . . 6_575 ? O4 Ni2 O6 C15 39.2(9) 2_757 . . 6_575 ? O3 Ni2 O6 C15 -50.7(10) . . . 6_575 ? O3 Ni2 O6 C15 -141.3(9) 6_575 . . 6_575 ? Ni2 Ni2 O6 C15 84.0(9) 5_777 . . 6_575 ? O4 Ni2 O6 C15 -39.2(9) 5_777 . . . ? O4 Ni2 O6 C15 -128.7(9) 2_757 . . . ? O3 Ni2 O6 C15 141.3(9) . . . . ? O3 Ni2 O6 C15 50.7(9) 6_575 . . . ? Ni2 Ni2 O6 C15 -84.0(9) 5_777 . . . ? C16' C16 C16' C15' 72(5) 6_575 . . 6_575 ? C15' C16 C16' C15' 18.7(18) . . . 6_575 ? C16' C16 C16' C15 69(6) 6_575 . . 6_575 ? C15' C16 C16' C15 -3.7(15) 6_575 . . 6_575 ? C15' C16 C16' C15 15(3) . . . 6_575 ? C15' C16 C16' C16' -72(5) 6_575 . . 6_575 ? C15' C16 C16' C16' -54(5) . . . 6_575 ? C16' C16 C16' C15' 54(5) 6_575 . . . ? C15' C16 C16' C15' -18.7(18) 6_575 . . . ? C15' O6 C15 C15' 21(2) 6_575 . . . ? C15 O6 C15 C15' 37(4) 6_575 . . . ? Ni2 O6 C15 C15' -157(2) . . . . ? C15' O6 C15 C16' -23(2) . . . 6_575 ? C15' O6 C15 C16' -1.5(16) 6_575 . . 6_575 ? C15 O6 C15 C16' 14(3) 6_575 . . 6_575 ? Ni2 O6 C15 C16' 179.8(10) . . . 6_575 ? C16' C15 C15' O6 151(3) 6_575 . . . ? O6 C15 C15' C16' -151(3) . . . 6_575 ? C16' C15 C15' C16 5(2) 6_575 . . . ? O6 C15 C15' C16 -146(4) . . . . ? C16' C15 C15' C15' 115(5) 6_575 . . 6_575 ? O6 C15 C15' C15' -36(4) . . . 6_575 ? C16' C15 C15' C16' 39(4) 6_575 . . . ? O6 C15 C15' C16' -112(5) . . . . ? C15' O6 C15' C15 -160(2) 6_575 . . . ? C15 O6 C15' C15 -151(3) 6_575 . . . ? Ni2 O6 C15' C15 31(3) . . . . ? C15' O6 C15' C16' -26(3) 6_575 . . 6_575 ? C15 O6 C15' C16' -17(3) 6_575 . . 6_575 ? C15 O6 C15' C16' 133(4) . . . 6_575 ? Ni2 O6 C15' C16' 164(2) . . . 6_575 ? C15' O6 C15' C16 -4.8(16) 6_575 . . . ? C15 O6 C15' C16 4.1(14) 6_575 . . . ? C15 O6 C15' C16 155(3) . . . . ? Ni2 O6 C15' C16 -174.1(6) . . . . ? C15 O6 C15' C15' 8.9(10) 6_575 . . 6_575 ? C15 O6 C15' C15' 160(2) . . . 6_575 ? Ni2 O6 C15' C15' -169.3(17) . . . 6_575 ? C15' O6 C15' C16' -10.0(12) 6_575 . . . ? C15 O6 C15' C16' -1.1(12) 6_575 . . . ? C15 O6 C15' C16' 150(3) . . . . ? Ni2 O6 C15' C16' -179.4(10) . . . . ? C16' C16 C15' C15 -9(4) 6_575 . . . ? C16' C16 C15' C15 134(4) . . . . ? C15' C16 C15' C15 151(3) 6_575 . . . ? C16' C16 C15' O6 -156(2) 6_575 . . . ? C16' C16 C15' O6 -13(2) . . . . ? C15' C16 C15' O6 4.1(14) 6_575 . . . ? C16' C16 C15' C16' 143(4) . . . 6_575 ? C15' C16 C15' C16' 160.0(19) 6_575 . . 6_575 ? C16' C16 C15' C15' -160.0(19) 6_575 . . 6_575 ? C16' C16 C15' C15' -16.8(16) . . . 6_575 ? C16' C16 C15' C16' -143(4) 6_575 . . . ? C15' C16 C15' C16' 16.8(16) 6_575 . . . ? C16 C16' C15' C15 -72(5) . . . . ? C15' C16' C15' C15 133(4) 6_575 . . . ? C15 C16' C15' C15 121(5) 6_575 . . . ? C16' C16' C15' C15 -47(4) 6_575 . . . ? C16 C16' C15' O6 168(2) . . . . ? C15' C16' C15' O6 12.6(15) 6_575 . . . ? C15 C16' C15' O6 1.2(12) 6_575 . . . ? C16' C16' C15' O6 -167.4(15) 6_575 . . . ? C16 C16' C15' C16' -25(2) . . . 6_575 ? C15' C16' C15' C16' 180.000(2) 6_575 . . 6_575 ? C15 C16' C15' C16' 168.6(12) 6_575 . . 6_575 ? C15' C16' C15' C16 -155(2) 6_575 . . . ? C15 C16' C15' C16 -167(2) 6_575 . . . ? C16' C16' C15' C16 25(2) 6_575 . . . ? C16 C16' C15' C15' 155(2) . . . 6_575 ? C15 C16' C15' C15' -11.4(12) 6_575 . . 6_575 ? C16' C16' C15' C15' 180.000(18) 6_575 . . 6_575 ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 0.965 _refine_diff_density_min -1.226 _refine_diff_density_rms 0.102 #============================================================================= data_compound-6 _database_code_depnum_ccdc_archive 'CCDC 834803' #TrackingRef '- CIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H24 N4 O12 Zn3' _chemical_formula_sum 'C27 H24 N4 O12 Zn3' _chemical_formula_weight 792.61 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 _symmetry_space_group_name_hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.536(5) _cell_length_b 10.243(5) _cell_length_c 15.501(5) _cell_angle_alpha 89.398(5) _cell_angle_beta 76.990(5) _cell_angle_gamma 88.190(5) _cell_volume 1474.5(12) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2520 _cell_measurement_theta_min 3.0641 _cell_measurement_theta_max 29.2239 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.785 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 800 _exptl_absorpt_coefficient_mu 2.492 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.96157 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9418 _diffrn_reflns_av_R_equivalents 0.0408 _diffrn_reflns_av_sigmaI/netI 0.0854 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 25.35 _reflns_number_total 5373 _reflns_number_gt 3707 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXS-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0412P)^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 5373 _refine_ls_number_parameters 415 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0866 _refine_ls_R_factor_gt 0.0517 _refine_ls_wR_factor_ref 0.1183 _refine_ls_wR_factor_gt 0.1014 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.001 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 Zn3 Zn 0.09115(6) 0.12418(6) 0.31701(4) 0.03303(19) Uani 1 1 d . . . Zn2 Zn 0.22301(6) -0.06799(5) 0.43773(4) 0.03285(19) Uani 1 1 d . . . Zn1 Zn 0.93079(6) -0.70512(6) 1.18206(4) 0.03398(19) Uani 1 1 d . . . O11 O 0.9233(4) -0.7884(3) 1.2966(3) 0.0386(9) Uani 1 1 d . . . O6 O 0.4293(4) -0.5983(3) 0.6885(3) 0.0474(11) Uani 1 1 d . . . C26 C 0.5120(6) 0.0571(6) 1.3745(4) 0.0504(17) Uani 1 1 d . . . H26 H 0.4946 0.1183 1.4199 0.061 Uiso 1 1 calc R . . C17 C 0.2442(5) -0.3074(5) 0.4798(4) 0.0340(13) Uani 1 1 d . . . O7 O 0.2326(5) -0.2993(4) 0.4026(3) 0.0531(11) Uani 1 1 d . . . O8 O 0.2392(4) -0.2055(3) 0.5279(2) 0.0368(9) Uani 1 1 d . . . O2 O 0.8518(4) -0.6373(4) 1.0294(3) 0.0543(12) Uani 1 1 d . . . O5 O 0.4430(4) -0.5996(4) 0.8629(3) 0.0522(11) Uani 1 1 d . . . C3 C 0.3627(5) -0.7625(5) 1.0750(4) 0.0366(14) Uani 1 1 d . . . N3 N 0.6163(5) -0.0579(4) 1.2605(3) 0.0383(12) Uani 1 1 d . . . C7 C 0.4702(6) -0.6535(6) 0.9387(4) 0.0411(14) Uani 1 1 d . . . C4 C 0.4953(5) -0.7677(5) 1.0981(4) 0.0358(14) Uani 1 1 d . . . H4 H 0.5049 -0.8089 1.1503 0.043 Uiso 1 1 calc R . . N2 N 0.9924(5) -0.3081(4) 1.1762(4) 0.0448(13) Uani 1 1 d . . . C15 C 0.2676(6) -0.4378(5) 0.5200(4) 0.0323(13) Uani 1 1 d . . . O1 O 0.7580(4) -0.7551(4) 1.1462(3) 0.0509(11) Uani 1 1 d . . . C13 C 0.2439(5) -0.6712(4) 0.5165(4) 0.0299(13) Uani 1 1 d . . . C11 C 0.3604(6) -0.5756(5) 0.6211(4) 0.0349(13) Uani 1 1 d . . . C5 C 0.6136(5) -0.7112(5) 1.0432(4) 0.0377(14) Uani 1 1 d . . . O3 O 0.2449(4) -0.8574(4) 1.2100(3) 0.0514(11) Uani 1 1 d . . . C12 C 0.3132(6) -0.6845(5) 0.5852(4) 0.0332(13) Uani 1 1 d . . . H12 H 0.3284 -0.7671 0.6075 0.040 Uiso 1 1 calc R . . C16 C 0.3364(5) -0.4501(5) 0.5896(4) 0.0324(13) Uani 1 1 d . . . H16 H 0.3659 -0.3768 0.6147 0.039 Uiso 1 1 calc R . . C14 C 0.2210(6) -0.5464(5) 0.4828(4) 0.0349(13) Uani 1 1 d . . . H14 H 0.1751 -0.5366 0.4361 0.042 Uiso 1 1 calc R . . O4 O 0.1118(3) -0.7923(4) 1.1156(3) 0.0421(10) Uani 1 1 d . . . N1 N 0.9702(5) -0.5184(4) 1.1966(3) 0.0406(12) Uani 1 1 d . . . N4 N 0.4169(4) -0.0335(4) 1.3603(3) 0.0367(11) Uani 1 1 d . . . C1 C 0.7534(6) -0.6999(6) 1.0735(4) 0.0378(14) Uani 1 1 d . . . O12 O 0.0750(4) -0.0464(3) 0.3697(2) 0.0369(9) Uani 1 1 d . . . C10 C 0.4896(7) -0.4911(6) 0.7261(4) 0.0488(16) Uani 1 1 d . . . H10A H 0.4150 -0.4261 0.7496 0.059 Uiso 1 1 calc R . . H10B H 0.5626 -0.4501 0.6812 0.059 Uiso 1 1 calc R . . C8 C 0.3503(6) -0.7044(5) 0.9962(4) 0.0369(14) Uani 1 1 d . . . H8 H 0.2611 -0.6990 0.9814 0.044 Uiso 1 1 calc R . . C6 C 0.6010(6) -0.6554(5) 0.9631(4) 0.0387(14) Uani 1 1 d . . . H6 H 0.6808 -0.6193 0.9258 0.046 Uiso 1 1 calc R . . C20 C 1.0226(6) -0.4660(6) 1.2647(5) 0.0521(17) Uani 1 1 d . . . H20 H 1.0438 -0.5132 1.3120 0.063 Uiso 1 1 calc R . . C2 C 0.2296(6) -0.8082(5) 1.1375(4) 0.0366(14) Uani 1 1 d . . . C9 C 0.5551(6) -0.5461(6) 0.7993(4) 0.0516(17) Uani 1 1 d . . . H9A H 0.6278 -0.6129 0.7762 0.062 Uiso 1 1 calc R . . H9B H 0.5999 -0.4775 0.8253 0.062 Uiso 1 1 calc R . . C27 C 0.6341(6) 0.0429(6) 1.3121(5) 0.0519(18) Uani 1 1 d . . . H27 H 0.7156 0.0929 1.3057 0.062 Uiso 1 1 calc R . . C23 C 0.8753(6) -0.0876(6) 1.1920(5) 0.0548(19) Uani 1 1 d . . . H23A H 0.8840 -0.0939 1.2530 0.066 Uiso 1 1 calc R . . H23B H 0.8940 0.0017 1.1724 0.066 Uiso 1 1 calc R . . C24 C 0.7237(6) -0.1187(6) 1.1875(5) 0.0548(18) Uani 1 1 d . . . H24A H 0.7058 -0.0879 1.1314 0.066 Uiso 1 1 calc R . . H24B H 0.7133 -0.2127 1.1899 0.066 Uiso 1 1 calc R . . C21 C 1.0384(7) -0.3360(6) 1.2523(5) 0.0537(17) Uani 1 1 d . . . H21 H 1.0731 -0.2780 1.2876 0.064 Uiso 1 1 calc R . . C22 C 0.9880(6) -0.1780(5) 1.1355(5) 0.0545(19) Uani 1 1 d . . . H22A H 0.9666 -0.1869 1.0776 0.065 Uiso 1 1 calc R . . H22B H 1.0818 -0.1398 1.1275 0.065 Uiso 1 1 calc R . . C19 C 0.9537(6) -0.4181(5) 1.1450(4) 0.0420(15) Uani 1 1 d . . . H19 H 0.9195 -0.4239 1.0936 0.050 Uiso 1 1 calc R . . C25 C 0.4838(6) -0.1015(5) 1.2913(4) 0.0406(15) Uani 1 1 d . . . H25 H 0.4445 -0.1705 1.2671 0.049 Uiso 1 1 calc R . . C18 C 0.1982(5) -0.7864(5) 0.4732(4) 0.0301(12) Uani 1 1 d . . . O10 O 0.1999(4) -0.8980(3) 0.5102(2) 0.0355(9) Uani 1 1 d . . . O9 O 0.1655(5) -0.7659(3) 0.4001(3) 0.0511(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn3 0.0347(4) 0.0344(3) 0.0321(4) 0.0076(3) -0.0122(3) -0.0023(3) Zn2 0.0336(3) 0.0284(3) 0.0369(4) 0.0078(3) -0.0088(3) -0.0006(3) Zn1 0.0261(3) 0.0407(4) 0.0368(4) 0.0063(3) -0.0110(3) -0.0003(3) O11 0.037(2) 0.046(2) 0.034(2) 0.0082(18) -0.0122(18) 0.0077(18) O6 0.077(3) 0.033(2) 0.043(3) 0.0021(19) -0.037(2) 0.000(2) C26 0.035(3) 0.051(4) 0.063(5) -0.013(3) -0.003(3) -0.012(3) C17 0.031(3) 0.038(3) 0.034(4) 0.010(3) -0.008(3) -0.007(3) O7 0.092(3) 0.038(2) 0.037(3) 0.007(2) -0.032(2) 0.002(2) O8 0.051(2) 0.0243(18) 0.034(2) 0.0035(17) -0.0079(18) 0.0025(17) O2 0.030(2) 0.087(3) 0.046(3) 0.006(2) -0.0069(19) -0.017(2) O5 0.041(2) 0.083(3) 0.038(3) 0.022(2) -0.018(2) -0.015(2) C3 0.026(3) 0.048(3) 0.037(4) 0.007(3) -0.009(3) -0.006(3) N3 0.031(2) 0.034(2) 0.046(3) -0.001(2) -0.001(2) -0.003(2) C7 0.040(3) 0.054(3) 0.033(4) 0.006(3) -0.015(3) -0.008(3) C4 0.024(3) 0.048(3) 0.036(4) 0.001(3) -0.010(2) 0.006(3) N2 0.039(3) 0.036(3) 0.058(4) -0.006(3) -0.008(3) -0.002(2) C15 0.040(3) 0.026(3) 0.033(4) 0.003(2) -0.012(3) 0.003(2) O1 0.034(2) 0.076(3) 0.051(3) 0.019(2) -0.026(2) -0.012(2) C13 0.031(3) 0.024(3) 0.034(4) 0.007(2) -0.004(2) -0.003(2) C11 0.045(3) 0.032(3) 0.030(4) 0.006(2) -0.014(3) 0.003(3) C5 0.030(3) 0.046(3) 0.040(4) 0.002(3) -0.013(3) -0.007(3) O3 0.031(2) 0.079(3) 0.043(3) 0.023(2) -0.0063(19) -0.005(2) C12 0.046(3) 0.026(3) 0.033(4) 0.006(2) -0.018(3) -0.004(2) C16 0.034(3) 0.030(3) 0.034(4) 0.000(2) -0.009(3) -0.004(2) C14 0.043(3) 0.038(3) 0.025(3) -0.003(2) -0.011(3) 0.006(3) O4 0.0170(18) 0.069(3) 0.040(3) 0.004(2) -0.0077(17) 0.0056(18) N1 0.047(3) 0.041(3) 0.037(3) 0.003(2) -0.016(2) 0.002(2) N4 0.032(2) 0.038(2) 0.039(3) 0.004(2) -0.007(2) -0.004(2) C1 0.027(3) 0.049(3) 0.037(4) -0.006(3) -0.007(3) 0.004(3) O12 0.041(2) 0.0313(18) 0.044(3) 0.0095(18) -0.0203(18) -0.0053(17) C10 0.061(4) 0.046(3) 0.045(4) -0.006(3) -0.025(3) 0.004(3) C8 0.031(3) 0.049(3) 0.034(4) 0.001(3) -0.014(3) -0.001(3) C6 0.028(3) 0.054(3) 0.032(4) 0.005(3) -0.002(3) -0.010(3) C20 0.052(4) 0.060(4) 0.050(5) 0.000(3) -0.022(3) -0.009(3) C2 0.031(3) 0.043(3) 0.036(4) 0.001(3) -0.008(3) -0.005(3) C9 0.050(4) 0.061(4) 0.048(4) 0.006(3) -0.021(3) -0.006(3) C27 0.044(4) 0.043(3) 0.068(5) -0.006(3) -0.008(3) -0.017(3) C23 0.041(3) 0.043(3) 0.075(5) -0.009(3) -0.001(3) -0.003(3) C24 0.048(4) 0.063(4) 0.052(5) -0.008(3) -0.010(3) 0.002(3) C21 0.053(4) 0.059(4) 0.054(5) -0.013(3) -0.022(3) -0.006(3) C22 0.044(4) 0.043(3) 0.068(5) -0.008(3) 0.006(3) -0.003(3) C19 0.040(3) 0.042(3) 0.042(4) 0.003(3) -0.007(3) 0.005(3) C25 0.041(3) 0.039(3) 0.042(4) -0.005(3) -0.008(3) -0.006(3) C18 0.030(3) 0.027(3) 0.033(4) 0.003(2) -0.008(2) 0.003(2) O10 0.043(2) 0.0256(18) 0.038(2) 0.0016(17) -0.0080(18) -0.0005(17) O9 0.083(3) 0.032(2) 0.051(3) 0.006(2) -0.041(2) -0.012(2) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn3 O11 1.896(4) 1_464 ? Zn3 O12 1.917(3) . ? Zn3 O3 1.963(4) 1_564 ? Zn3 O9 1.980(4) 1_565 ? Zn3 Zn2 3.1278(12) . ? Zn2 O12 1.949(4) . ? Zn2 O8 2.001(4) . ? Zn2 N4 2.004(4) 1_554 ? Zn2 O10 2.061(3) 1_565 ? Zn2 O7 2.431(4) . ? Zn2 C17 2.544(5) . ? Zn1 O1 1.938(4) . ? Zn1 O11 1.950(4) . ? Zn1 N1 1.985(5) . ? Zn1 O4 1.990(4) 1_655 ? O11 Zn3 1.896(4) 1_646 ? O6 C11 1.368(7) . ? O6 C10 1.441(6) . ? C26 C27 1.341(8) . ? C26 N4 1.371(7) . ? C26 H26 0.9300 . ? C17 O7 1.228(7) . ? C17 O8 1.283(6) . ? C17 C15 1.500(7) . ? O2 C1 1.224(6) . ? O5 C7 1.367(7) . ? O5 C9 1.402(6) . ? C3 C8 1.380(8) . ? C3 C4 1.389(7) . ? C3 C2 1.497(7) . ? N3 C25 1.336(6) . ? N3 C27 1.351(7) . ? N3 C24 1.474(7) . ? C7 C6 1.382(8) . ? C7 C8 1.394(7) . ? C4 C5 1.390(7) . ? C4 H4 0.9300 . ? N2 C19 1.325(7) . ? N2 C21 1.372(8) . ? N2 C22 1.472(7) . ? C15 C16 1.384(8) . ? C15 C14 1.388(7) . ? O1 C1 1.265(7) . ? C13 C12 1.378(7) . ? C13 C14 1.405(7) . ? C13 C18 1.487(7) . ? C11 C12 1.384(7) . ? C11 C16 1.401(7) . ? C5 C6 1.389(8) . ? C5 C1 1.518(8) . ? O3 C2 1.262(7) . ? O3 Zn3 1.963(4) 1_546 ? C12 H12 0.9300 . ? C16 H16 0.9300 . ? C14 H14 0.9300 . ? O4 C2 1.251(6) . ? O4 Zn1 1.990(4) 1_455 ? N1 C19 1.323(7) . ? N1 C20 1.387(8) . ? N4 C25 1.310(7) . ? N4 Zn2 2.004(4) 1_556 ? C10 C9 1.508(8) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C8 H8 0.9300 . ? C6 H6 0.9300 . ? C20 C21 1.351(8) . ? C20 H20 0.9300 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C27 H27 0.9300 . ? C23 C24 1.507(8) . ? C23 C22 1.519(8) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C21 H21 0.9300 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C19 H19 0.9300 . ? C25 H25 0.9300 . ? C18 O9 1.255(6) . ? C18 O10 1.275(6) . ? O10 Zn2 2.061(3) 1_545 ? O9 Zn3 1.980(4) 1_545 ? 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 O11 Zn3 O12 119.01(15) 1_464 . ? O11 Zn3 O3 107.92(17) 1_464 1_564 ? O12 Zn3 O3 115.72(17) . 1_564 ? O11 Zn3 O9 106.68(17) 1_464 1_565 ? O12 Zn3 O9 105.21(16) . 1_565 ? O3 Zn3 O9 100.15(18) 1_564 1_565 ? O11 Zn3 Zn2 146.95(11) 1_464 . ? O12 Zn3 Zn2 36.33(11) . . ? O3 Zn3 Zn2 104.43(13) 1_564 . ? O9 Zn3 Zn2 73.62(12) 1_565 . ? O12 Zn2 O8 128.01(14) . . ? O12 Zn2 N4 109.95(18) . 1_554 ? O8 Zn2 N4 110.53(17) . 1_554 ? O12 Zn2 O10 102.78(15) . 1_565 ? O8 Zn2 O10 102.90(15) . 1_565 ? N4 Zn2 O10 97.42(16) 1_554 1_565 ? O12 Zn2 O7 87.52(14) . . ? O8 Zn2 O7 58.27(14) . . ? N4 Zn2 O7 94.40(16) 1_554 . ? O10 Zn2 O7 160.54(15) 1_565 . ? O12 Zn2 C17 109.17(16) . . ? O8 Zn2 C17 29.84(17) . . ? N4 Zn2 C17 103.22(17) 1_554 . ? O10 Zn2 C17 132.66(17) 1_565 . ? O7 Zn2 C17 28.45(15) . . ? O12 Zn2 Zn3 35.65(9) . . ? O8 Zn2 Zn3 161.10(11) . . ? N4 Zn2 Zn3 87.75(14) 1_554 . ? O10 Zn2 Zn3 78.51(11) 1_565 . ? O7 Zn2 Zn3 117.48(11) . . ? C17 Zn2 Zn3 143.50(14) . . ? O1 Zn1 O11 106.00(16) . . ? O1 Zn1 N1 120.80(19) . . ? O11 Zn1 N1 106.41(19) . . ? O1 Zn1 O4 114.81(18) . 1_655 ? O11 Zn1 O4 97.96(15) . 1_655 ? N1 Zn1 O4 107.99(17) . 1_655 ? Zn3 O11 Zn1 118.86(18) 1_646 . ? C11 O6 C10 119.9(4) . . ? C27 C26 N4 108.7(6) . . ? C27 C26 H26 125.7 . . ? N4 C26 H26 125.7 . . ? O7 C17 O8 121.5(5) . . ? O7 C17 C15 120.5(5) . . ? O8 C17 C15 118.0(5) . . ? O7 C17 Zn2 70.7(3) . . ? O8 C17 Zn2 50.9(2) . . ? C15 C17 Zn2 168.3(4) . . ? C17 O7 Zn2 80.9(3) . . ? C17 O8 Zn2 99.3(3) . . ? C7 O5 C9 120.1(4) . . ? C8 C3 C4 119.6(5) . . ? C8 C3 C2 118.9(5) . . ? C4 C3 C2 121.2(5) . . ? C25 N3 C27 107.6(5) . . ? C25 N3 C24 124.3(5) . . ? C27 N3 C24 127.9(5) . . ? O5 C7 C6 125.9(5) . . ? O5 C7 C8 114.6(5) . . ? C6 C7 C8 119.5(6) . . ? C5 C4 C3 119.9(5) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C19 N2 C21 108.6(5) . . ? C19 N2 C22 125.6(6) . . ? C21 N2 C22 125.7(5) . . ? C16 C15 C14 121.3(5) . . ? C16 C15 C17 121.6(5) . . ? C14 C15 C17 117.0(5) . . ? C1 O1 Zn1 109.3(3) . . ? C12 C13 C14 119.8(5) . . ? C12 C13 C18 121.9(4) . . ? C14 C13 C18 118.3(5) . . ? O6 C11 C12 116.2(4) . . ? O6 C11 C16 123.0(5) . . ? C12 C11 C16 120.8(5) . . ? C6 C5 C4 120.0(5) . . ? C6 C5 C1 119.5(5) . . ? C4 C5 C1 120.3(5) . . ? C2 O3 Zn3 125.5(4) . 1_546 ? C13 C12 C11 120.3(5) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C15 C16 C11 118.5(5) . . ? C15 C16 H16 120.8 . . ? C11 C16 H16 120.8 . . ? C15 C14 C13 119.4(5) . . ? C15 C14 H14 120.3 . . ? C13 C14 H14 120.3 . . ? C2 O4 Zn1 128.9(4) . 1_455 ? C19 N1 C20 105.1(5) . . ? C19 N1 Zn1 128.7(4) . . ? C20 N1 Zn1 126.2(4) . . ? C25 N4 C26 106.3(4) . . ? C25 N4 Zn2 126.8(3) . 1_556 ? C26 N4 Zn2 126.6(4) . 1_556 ? O2 C1 O1 123.9(5) . . ? O2 C1 C5 120.1(6) . . ? O1 C1 C5 116.0(5) . . ? Zn3 O12 Zn2 108.02(15) . . ? O6 C10 C9 107.4(5) . . ? O6 C10 H10A 110.2 . . ? C9 C10 H10A 110.2 . . ? O6 C10 H10B 110.2 . . ? C9 C10 H10B 110.2 . . ? H10A C10 H10B 108.5 . . ? C3 C8 C7 120.7(5) . . ? C3 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? C7 C6 C5 120.1(5) . . ? C7 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C21 C20 N1 109.9(6) . . ? C21 C20 H20 125.1 . . ? N1 C20 H20 125.1 . . ? O4 C2 O3 124.8(5) . . ? O4 C2 C3 118.2(5) . . ? O3 C2 C3 117.0(5) . . ? O5 C9 C10 107.1(5) . . ? O5 C9 H9A 110.3 . . ? C10 C9 H9A 110.3 . . ? O5 C9 H9B 110.3 . . ? C10 C9 H9B 110.3 . . ? H9A C9 H9B 108.6 . . ? C26 C27 N3 106.9(5) . . ? C26 C27 H27 126.5 . . ? N3 C27 H27 126.5 . . ? C24 C23 C22 113.0(5) . . ? C24 C23 H23A 109.0 . . ? C22 C23 H23A 109.0 . . ? C24 C23 H23B 109.0 . . ? C22 C23 H23B 109.0 . . ? H23A C23 H23B 107.8 . . ? N3 C24 C23 111.9(5) . . ? N3 C24 H24A 109.2 . . ? C23 C24 H24A 109.2 . . ? N3 C24 H24B 109.2 . . ? C23 C24 H24B 109.2 . . ? H24A C24 H24B 107.9 . . ? C20 C21 N2 105.2(5) . . ? C20 C21 H21 127.4 . . ? N2 C21 H21 127.4 . . ? N2 C22 C23 111.8(5) . . ? N2 C22 H22A 109.2 . . ? C23 C22 H22A 109.2 . . ? N2 C22 H22B 109.2 . . ? C23 C22 H22B 109.2 . . ? H22A C22 H22B 107.9 . . ? N1 C19 N2 111.1(6) . . ? N1 C19 H19 124.4 . . ? N2 C19 H19 124.4 . . ? N4 C25 N3 110.5(5) . . ? N4 C25 H25 124.8 . . ? N3 C25 H25 124.8 . . ? O9 C18 O10 124.8(5) . . ? O9 C18 C13 116.4(4) . . ? O10 C18 C13 118.8(5) . . ? C18 O10 Zn2 121.4(4) . 1_545 ? C18 O9 Zn3 134.2(3) . 1_545 ? 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 O11 Zn3 Zn2 O12 53.9(3) 1_464 . . . ? O3 Zn3 Zn2 O12 -114.0(2) 1_564 . . . ? O9 Zn3 Zn2 O12 149.5(2) 1_565 . . . ? O11 Zn3 Zn2 O8 18.1(4) 1_464 . . . ? O12 Zn3 Zn2 O8 -35.8(4) . . . . ? O3 Zn3 Zn2 O8 -149.8(4) 1_564 . . . ? O9 Zn3 Zn2 O8 113.6(4) 1_565 . . . ? O11 Zn3 Zn2 N4 -176.3(3) 1_464 . . 1_554 ? O12 Zn3 Zn2 N4 129.8(2) . . . 1_554 ? O3 Zn3 Zn2 N4 15.85(18) 1_564 . . 1_554 ? O9 Zn3 Zn2 N4 -80.70(19) 1_565 . . 1_554 ? O11 Zn3 Zn2 O10 -78.2(2) 1_464 . . 1_565 ? O12 Zn3 Zn2 O10 -132.1(2) . . . 1_565 ? O3 Zn3 Zn2 O10 113.89(16) 1_564 . . 1_565 ? O9 Zn3 Zn2 O10 17.34(16) 1_565 . . 1_565 ? O11 Zn3 Zn2 O7 90.0(2) 1_464 . . . ? O12 Zn3 Zn2 O7 36.0(2) . . . . ? O3 Zn3 Zn2 O7 -77.94(18) 1_564 . . . ? O9 Zn3 Zn2 O7 -174.49(18) 1_565 . . . ? O11 Zn3 Zn2 C17 74.4(3) 1_464 . . . ? O12 Zn3 Zn2 C17 20.5(3) . . . . ? O3 Zn3 Zn2 C17 -93.5(2) 1_564 . . . ? O9 Zn3 Zn2 C17 169.9(2) 1_565 . . . ? O1 Zn1 O11 Zn3 134.3(2) . . . 1_646 ? N1 Zn1 O11 Zn3 -96.0(2) . . . 1_646 ? O4 Zn1 O11 Zn3 15.5(2) 1_655 . . 1_646 ? O12 Zn2 C17 O7 42.5(4) . . . . ? O8 Zn2 C17 O7 177.2(5) . . . . ? N4 Zn2 C17 O7 -74.5(3) 1_554 . . . ? O10 Zn2 C17 O7 172.2(3) 1_565 . . . ? Zn3 Zn2 C17 O7 30.0(4) . . . . ? O12 Zn2 C17 O8 -134.8(3) . . . . ? N4 Zn2 C17 O8 108.3(3) 1_554 . . . ? O10 Zn2 C17 O8 -5.0(4) 1_565 . . . ? O7 Zn2 C17 O8 -177.2(5) . . . . ? Zn3 Zn2 C17 O8 -147.2(2) . . . . ? O12 Zn2 C17 C15 -153.9(18) . . . . ? O8 Zn2 C17 C15 -19.1(17) . . . . ? N4 Zn2 C17 C15 89.2(18) 1_554 . . . ? O10 Zn2 C17 C15 -24.1(19) 1_565 . . . ? O7 Zn2 C17 C15 164(2) . . . . ? Zn3 Zn2 C17 C15 -166.3(17) . . . . ? O8 C17 O7 Zn2 2.5(5) . . . . ? C15 C17 O7 Zn2 -176.2(5) . . . . ? O12 Zn2 O7 C17 -140.3(3) . . . . ? O8 Zn2 O7 C17 -1.6(3) . . . . ? N4 Zn2 O7 C17 109.8(3) 1_554 . . . ? O10 Zn2 O7 C17 -17.5(6) 1_565 . . . ? Zn3 Zn2 O7 C17 -160.4(3) . . . . ? O7 C17 O8 Zn2 -3.1(6) . . . . ? C15 C17 O8 Zn2 175.7(4) . . . . ? O12 Zn2 O8 C17 58.4(4) . . . . ? N4 Zn2 O8 C17 -80.7(3) 1_554 . . . ? O10 Zn2 O8 C17 176.2(3) 1_565 . . . ? O7 Zn2 O8 C17 1.6(3) . . . . ? Zn3 Zn2 O8 C17 84.0(4) . . . . ? C9 O5 C7 C6 3.7(9) . . . . ? C9 O5 C7 C8 -179.5(5) . . . . ? C8 C3 C4 C5 1.8(8) . . . . ? C2 C3 C4 C5 -172.7(5) . . . . ? O7 C17 C15 C16 153.7(5) . . . . ? O8 C17 C15 C16 -25.1(7) . . . . ? Zn2 C17 C15 C16 -8(2) . . . . ? O7 C17 C15 C14 -24.4(7) . . . . ? O8 C17 C15 C14 156.8(5) . . . . ? Zn2 C17 C15 C14 173.5(16) . . . . ? O11 Zn1 O1 C1 177.5(4) . . . . ? N1 Zn1 O1 C1 56.6(4) . . . . ? O4 Zn1 O1 C1 -75.6(4) 1_655 . . . ? C10 O6 C11 C12 176.2(5) . . . . ? C10 O6 C11 C16 -4.3(8) . . . . ? C3 C4 C5 C6 -3.2(8) . . . . ? C3 C4 C5 C1 171.7(5) . . . . ? C14 C13 C12 C11 0.0(8) . . . . ? C18 C13 C12 C11 176.9(5) . . . . ? O6 C11 C12 C13 -179.4(5) . . . . ? C16 C11 C12 C13 1.1(8) . . . . ? C14 C15 C16 C11 1.0(8) . . . . ? C17 C15 C16 C11 -177.1(5) . . . . ? O6 C11 C16 C15 179.0(5) . . . . ? C12 C11 C16 C15 -1.6(8) . . . . ? C16 C15 C14 C13 0.1(8) . . . . ? C17 C15 C14 C13 178.3(5) . . . . ? C12 C13 C14 C15 -0.6(8) . . . . ? C18 C13 C14 C15 -177.7(5) . . . . ? O1 Zn1 N1 C19 -42.8(6) . . . . ? O11 Zn1 N1 C19 -163.5(5) . . . . ? O4 Zn1 N1 C19 92.2(5) 1_655 . . . ? O1 Zn1 N1 C20 137.5(5) . . . . ? O11 Zn1 N1 C20 16.8(5) . . . . ? O4 Zn1 N1 C20 -87.5(5) 1_655 . . . ? C27 C26 N4 C25 1.1(7) . . . . ? C27 C26 N4 Zn2 174.9(4) . . . 1_556 ? Zn1 O1 C1 O2 7.5(7) . . . . ? Zn1 O1 C1 C5 -170.6(4) . . . . ? C6 C5 C1 O2 3.1(8) . . . . ? C4 C5 C1 O2 -171.8(5) . . . . ? C6 C5 C1 O1 -178.7(5) . . . . ? C4 C5 C1 O1 6.3(8) . . . . ? O11 Zn3 O12 Zn2 -149.74(17) 1_464 . . . ? O3 Zn3 O12 Zn2 79.2(2) 1_564 . . . ? O9 Zn3 O12 Zn2 -30.3(2) 1_565 . . . ? O8 Zn2 O12 Zn3 166.08(15) . . . . ? N4 Zn2 O12 Zn3 -54.7(2) 1_554 . . . ? O10 Zn2 O12 Zn3 48.2(2) 1_565 . . . ? O7 Zn2 O12 Zn3 -148.50(19) . . . . ? C17 Zn2 O12 Zn3 -167.28(18) . . . . ? C11 O6 C10 C9 179.0(5) . . . . ? C4 C3 C8 C7 1.5(8) . . . . ? C2 C3 C8 C7 176.1(5) . . . . ? O5 C7 C8 C3 179.6(5) . . . . ? C6 C7 C8 C3 -3.4(9) . . . . ? O5 C7 C6 C5 178.6(5) . . . . ? C8 C7 C6 C5 1.9(9) . . . . ? C4 C5 C6 C7 1.4(9) . . . . ? C1 C5 C6 C7 -173.6(5) . . . . ? C19 N1 C20 C21 -0.8(7) . . . . ? Zn1 N1 C20 C21 178.9(4) . . . . ? Zn1 O4 C2 O3 51.9(8) 1_455 . . . ? Zn1 O4 C2 C3 -126.3(5) 1_455 . . . ? Zn3 O3 C2 O4 -17.9(8) 1_546 . . . ? Zn3 O3 C2 C3 160.3(4) 1_546 . . . ? C8 C3 C2 O4 0.4(8) . . . . ? C4 C3 C2 O4 174.9(5) . . . . ? C8 C3 C2 O3 -178.0(5) . . . . ? C4 C3 C2 O3 -3.5(8) . . . . ? C7 O5 C9 C10 -178.1(5) . . . . ? O6 C10 C9 O5 -61.8(6) . . . . ? N4 C26 C27 N3 -1.3(8) . . . . ? C25 N3 C27 C26 1.0(7) . . . . ? C24 N3 C27 C26 -174.6(6) . . . . ? C25 N3 C24 C23 -156.1(6) . . . . ? C27 N3 C24 C23 18.9(9) . . . . ? C22 C23 C24 N3 163.3(5) . . . . ? N1 C20 C21 N2 1.1(7) . . . . ? C19 N2 C21 C20 -1.0(7) . . . . ? C22 N2 C21 C20 179.5(5) . . . . ? C19 N2 C22 C23 112.3(7) . . . . ? C21 N2 C22 C23 -68.3(8) . . . . ? C24 C23 C22 N2 -74.8(8) . . . . ? C20 N1 C19 N2 0.1(6) . . . . ? Zn1 N1 C19 N2 -179.6(4) . . . . ? C21 N2 C19 N1 0.6(7) . . . . ? C22 N2 C19 N1 180.0(5) . . . . ? C26 N4 C25 N3 -0.5(7) . . . . ? Zn2 N4 C25 N3 -174.2(4) 1_556 . . . ? C27 N3 C25 N4 -0.3(7) . . . . ? C24 N3 C25 N4 175.5(5) . . . . ? C12 C13 C18 O9 -164.8(5) . . . . ? C14 C13 C18 O9 12.2(7) . . . . ? C12 C13 C18 O10 12.6(7) . . . . ? C14 C13 C18 O10 -170.4(5) . . . . ? O9 C18 O10 Zn2 23.2(7) . . . 1_545 ? C13 C18 O10 Zn2 -154.0(3) . . . 1_545 ? O10 C18 O9 Zn3 6.0(9) . . . 1_545 ? C13 C18 O9 Zn3 -176.8(4) . . . 1_545 ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.686 _refine_diff_density_min -0.511 _refine_diff_density_rms 0.100 #============================================================================= data_compound-7 _database_code_depnum_ccdc_archive 'CCDC 834804' #TrackingRef '- CIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H15 N6 Ni O5, 3(H2 O)' _chemical_formula_sum 'C16 H21 N6 Ni O8' _chemical_formula_weight 484.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'p 21/c' _symmetry_space_group_name_hall '-P 2ybc ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 6.6602(3) _cell_length_b 16.2245(7) _cell_length_c 18.3730(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.984(4) _cell_angle_gamma 90.00 _cell_volume 1985.06(16) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2722 _cell_measurement_theta_min 3.3438 _cell_measurement_theta_max 29.2090 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.620 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1004 _exptl_absorpt_coefficient_mu 1.037 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.97669 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _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 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8018 _diffrn_reflns_av_R_equivalents 0.0344 _diffrn_reflns_av_sigmaI/netI 0.0485 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.35 _diffrn_reflns_theta_max 25.35 _reflns_number_total 3562 _reflns_number_gt 2808 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXS-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0692P)^2^+0.2869P] 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 3562 _refine_ls_number_parameters 298 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0598 _refine_ls_R_factor_gt 0.0440 _refine_ls_wR_factor_ref 0.1231 _refine_ls_wR_factor_gt 0.1133 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 1.49119(5) 0.31940(2) 1.25185(2) 0.01807(16) Uani 1 1 d . . . C1 C 1.1914(4) 0.22491(19) 1.34144(17) 0.0211(7) Uani 1 1 d . . . O5 O 0.6963(3) 0.06694(12) 1.47056(14) 0.0274(6) Uani 1 1 d . . . C11 C 1.2413(5) 0.2102(2) 1.1459(2) 0.0329(8) Uani 1 1 d . . . H11 H 1.1822 0.1807 1.1833 0.039 Uiso 1 1 calc R . . C2 C 1.2027(4) -0.0860(2) 1.33386(17) 0.0206(7) Uani 1 1 d . . . O2 O 1.0834(3) 0.28714(14) 1.35184(13) 0.0307(6) Uani 1 1 d . . . O1 O 1.3593(3) 0.22589(13) 1.30981(12) 0.0257(5) Uani 1 1 d . . . O4 O 1.0923(3) -0.14848(14) 1.33901(13) 0.0309(6) Uani 1 1 d . . . O3 O 1.3762(3) -0.08624(13) 1.30699(12) 0.0230(5) Uani 1 1 d . . . N3 N 1.1942(4) 0.2017(2) 1.07585(16) 0.0325(7) Uani 1 1 d . . . C7 C 1.1144(4) 0.14280(19) 1.36577(16) 0.0187(7) Uani 1 1 d . . . N1 N 1.3840(4) 0.26630(17) 1.15532(14) 0.0256(6) Uani 1 1 d . . . C6 C 0.9445(4) 0.1394(2) 1.40823(18) 0.0217(7) Uani 1 1 d . . . H6 H 0.8846 0.1879 1.4237 0.026 Uiso 1 1 calc R . . C3 C 1.1195(4) -0.00544(19) 1.36101(17) 0.0192(7) Uani 1 1 d . . . N2 N 1.3078(4) 0.2542(2) 1.03567(17) 0.0385(8) Uani 1 1 d . . . C10 C 1.4195(5) 0.2912(2) 1.08639(19) 0.0309(8) Uani 1 1 d . . . H10 H 1.5147 0.3311 1.0755 0.037 Uiso 1 1 calc R . . C5 C 0.8633(4) 0.06418(18) 1.42776(18) 0.0211(7) Uani 1 1 d . . . C4 C 0.9482(4) -0.00807(19) 1.40337(17) 0.0205(7) Uani 1 1 d . . . H4 H 0.8911 -0.0585 1.4152 0.025 Uiso 1 1 calc R . . C9 C 0.5910(4) -0.0096(2) 1.47833(18) 0.0242(7) Uani 1 1 d . . . H9A H 0.6748 -0.0497 1.5035 0.029 Uiso 1 1 calc R . . H9B H 0.5527 -0.0316 1.4310 0.029 Uiso 1 1 calc R . . C8 C 1.2039(4) 0.06948(18) 1.34266(17) 0.0190(7) Uani 1 1 d . . . H8 H 1.3196 0.0711 1.3151 0.023 Uiso 1 1 calc R . . C14 C 0.6849(5) 0.1023(3) 1.0395(2) 0.0394(9) Uani 1 1 d . . . H14A H 0.7259 0.0488 1.0580 0.047 Uiso 1 1 calc R . . H14B H 0.5551 0.1153 1.0597 0.047 Uiso 1 1 calc R . . C12 C 1.0473(5) 0.1478(3) 1.0404(2) 0.0433(10) Uani 1 1 d . . . H12A H 1.0789 0.0909 1.0521 0.052 Uiso 1 1 calc R . . H12B H 1.0550 0.1543 0.9880 0.052 Uiso 1 1 calc R . . C13 C 0.8371(5) 0.1669(2) 1.0642(2) 0.0401(9) Uani 1 1 d . . . H13A H 0.7972 0.2201 1.0446 0.048 Uiso 1 1 calc R . . H13B H 0.8360 0.1707 1.1169 0.048 Uiso 1 1 calc R . . N4 N 0.6661(4) 0.09847(19) 0.96017(16) 0.0319(7) Uani 1 1 d . . . C16 C 0.5713(5) 0.1486(2) 0.91366(19) 0.0319(8) Uani 1 1 d . . . H16 H 0.4974 0.1946 0.9272 0.038 Uiso 1 1 calc R . . N5 N 0.7578(6) 0.0384(2) 0.9221(2) 0.0588(10) Uani 1 1 d . . . C15 C 0.7118(7) 0.0573(3) 0.8541(2) 0.0535(12) Uani 1 1 d . . . H15 H 0.7558 0.0266 0.8146 0.064 Uiso 1 1 calc R . . N6 N 0.5956(4) 0.12471(18) 0.84654(15) 0.0264(6) Uani 1 1 d . . . O1W O 1.7524(3) 0.24556(14) 1.25047(12) 0.0278(5) Uani 1 1 d . . . O2W O 1.2318(3) 0.39329(14) 1.25706(13) 0.0279(5) Uani 1 1 d . . . O3W O 0.6355(12) 0.0713(4) 1.2089(4) 0.0563(16) Uani 0.50 1 d PU . . O4W O 1.801(2) 0.0658(7) 1.2062(7) 0.054(3) Uani 0.25 1 d PU . . O5W O 0.523(3) 0.0615(12) 1.2455(13) 0.107(7) Uani 0.25 1 d PU . . 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 0.0153(2) 0.0168(2) 0.0222(3) 0.00250(16) 0.00188(16) -0.00227(15) C1 0.0212(14) 0.0208(17) 0.0213(16) -0.0008(13) 0.0006(12) -0.0005(14) O5 0.0237(11) 0.0201(12) 0.0391(14) -0.0027(10) 0.0176(10) -0.0047(9) C11 0.0304(17) 0.035(2) 0.033(2) -0.0010(17) 0.0004(15) -0.0096(16) C2 0.0197(15) 0.0210(17) 0.0210(17) -0.0015(13) -0.0005(12) 0.0002(13) O2 0.0303(11) 0.0205(12) 0.0419(15) 0.0055(11) 0.0157(10) 0.0050(10) O1 0.0191(10) 0.0218(12) 0.0366(13) 0.0043(10) 0.0099(9) -0.0022(9) O4 0.0263(11) 0.0207(13) 0.0463(15) -0.0067(11) 0.0140(10) -0.0058(10) O3 0.0142(10) 0.0241(12) 0.0309(13) -0.0040(10) 0.0080(9) 0.0010(9) N3 0.0290(14) 0.0374(17) 0.0308(17) -0.0075(14) -0.0047(12) -0.0045(13) C7 0.0167(13) 0.0191(16) 0.0205(16) 0.0004(13) 0.0035(12) -0.0029(12) N1 0.0241(12) 0.0264(16) 0.0261(15) -0.0003(12) -0.0017(11) -0.0014(12) C6 0.0186(14) 0.0201(17) 0.0266(17) -0.0039(14) 0.0040(12) 0.0007(13) C3 0.0173(14) 0.0199(16) 0.0207(16) -0.0023(13) 0.0046(12) -0.0005(12) N2 0.0421(16) 0.0417(19) 0.0317(17) -0.0013(15) -0.0017(14) -0.0010(15) C10 0.0349(17) 0.0264(18) 0.031(2) 0.0030(16) -0.0005(15) 0.0017(16) C5 0.0157(14) 0.0217(17) 0.0259(17) -0.0026(13) 0.0060(12) -0.0023(12) C4 0.0194(14) 0.0170(16) 0.0252(17) 0.0013(13) 0.0036(12) -0.0037(12) C9 0.0225(14) 0.0202(17) 0.0302(19) -0.0008(14) 0.0086(14) -0.0074(13) C8 0.0143(13) 0.0223(17) 0.0204(16) -0.0010(13) 0.0036(12) 0.0008(12) C14 0.0399(19) 0.051(2) 0.027(2) 0.0052(18) -0.0019(16) -0.0095(18) C12 0.0371(19) 0.041(2) 0.052(3) -0.013(2) -0.0134(18) -0.0001(17) C13 0.0411(19) 0.046(2) 0.033(2) -0.0090(19) -0.0011(16) -0.0035(18) N4 0.0327(14) 0.0352(16) 0.0277(16) 0.0001(14) -0.0027(12) -0.0029(14) C16 0.0320(17) 0.033(2) 0.030(2) 0.0000(17) -0.0021(15) 0.0095(16) N5 0.094(3) 0.043(2) 0.038(2) -0.0038(17) -0.015(2) 0.033(2) C15 0.088(3) 0.040(2) 0.032(2) -0.0068(18) -0.011(2) 0.033(2) N6 0.0250(13) 0.0262(16) 0.0280(16) -0.0010(12) -0.0008(11) 0.0023(12) O1W 0.0222(10) 0.0251(12) 0.0361(14) 0.0037(10) 0.0023(10) 0.0025(9) O2W 0.0220(10) 0.0236(12) 0.0381(14) 0.0057(11) 0.0040(10) 0.0030(9) O3W 0.082(4) 0.044(3) 0.043(3) 0.007(2) 0.012(3) -0.011(3) O4W 0.072(5) 0.043(5) 0.045(5) -0.001(4) 0.002(4) 0.005(4) O5W 0.109(8) 0.101(8) 0.111(8) -0.008(5) -0.010(5) 0.002(5) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O1 2.059(2) . ? Ni1 N6 2.071(3) 4_666 ? Ni1 O3 2.080(2) 2_857 ? Ni1 N1 2.087(3) . ? Ni1 O2W 2.106(2) . ? Ni1 O1W 2.113(2) . ? C1 O2 1.256(4) . ? C1 O1 1.269(3) . ? C1 C7 1.498(4) . ? O5 C5 1.374(4) . ? O5 C9 1.434(4) . ? C11 N1 1.326(4) . ? C11 N3 1.326(4) . ? C11 H11 0.9300 . ? C2 O4 1.257(4) . ? C2 O3 1.265(3) . ? C2 C3 1.507(4) . ? O3 Ni1 2.080(2) 2_847 ? N3 N2 1.365(4) . ? N3 C12 1.459(4) . ? C7 C6 1.387(4) . ? C7 C8 1.400(4) . ? N1 C10 1.354(4) . ? C6 C5 1.384(4) . ? C6 H6 0.9300 . ? C3 C8 1.383(4) . ? C3 C4 1.393(4) . ? N2 C10 1.326(5) . ? C10 H10 0.9300 . ? C5 C4 1.380(4) . ? C4 H4 0.9300 . ? C9 C9 1.494(5) 3_658 ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C8 H8 0.9300 . ? C14 N4 1.461(5) . ? C14 C13 1.522(5) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C12 C13 1.506(5) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? N4 C16 1.332(5) . ? N4 N5 1.351(5) . ? C16 N6 1.306(4) . ? C16 H16 0.9300 . ? N5 C15 1.318(6) . ? C15 N6 1.346(5) . ? C15 H15 0.9300 . ? N6 Ni1 2.071(3) 4_465 ? O3W O5W 1.03(2) . ? O3W O4W 1.105(14) 1_455 ? O4W O3W 1.105(14) 1_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ni1 N6 91.62(10) . 4_666 ? O1 Ni1 O3 179.80(9) . 2_857 ? N6 Ni1 O3 88.56(10) 4_666 2_857 ? O1 Ni1 N1 89.58(10) . . ? N6 Ni1 N1 178.42(11) 4_666 . ? O3 Ni1 N1 90.24(10) 2_857 . ? O1 Ni1 O2W 92.19(8) . . ? N6 Ni1 O2W 88.66(10) 4_666 . ? O3 Ni1 O2W 87.74(8) 2_857 . ? N1 Ni1 O2W 90.27(10) . . ? O1 Ni1 O1W 86.97(8) . . ? N6 Ni1 O1W 89.64(10) 4_666 . ? O3 Ni1 O1W 93.10(8) 2_857 . ? N1 Ni1 O1W 91.45(10) . . ? O2W Ni1 O1W 178.08(9) . . ? O2 C1 O1 124.8(3) . . ? O2 C1 C7 118.0(2) . . ? O1 C1 C7 117.2(3) . . ? C5 O5 C9 115.5(2) . . ? N1 C11 N3 110.8(3) . . ? N1 C11 H11 124.6 . . ? N3 C11 H11 124.6 . . ? O4 C2 O3 124.5(3) . . ? O4 C2 C3 117.1(2) . . ? O3 C2 C3 118.4(3) . . ? C1 O1 Ni1 129.29(19) . . ? C2 O3 Ni1 127.19(19) . 2_847 ? C11 N3 N2 109.7(3) . . ? C11 N3 C12 129.9(3) . . ? N2 N3 C12 120.5(3) . . ? C6 C7 C8 119.5(3) . . ? C6 C7 C1 119.4(3) . . ? C8 C7 C1 121.0(2) . . ? C11 N1 C10 102.6(3) . . ? C11 N1 Ni1 129.0(2) . . ? C10 N1 Ni1 127.5(2) . . ? C5 C6 C7 120.5(3) . . ? C5 C6 H6 119.8 . . ? C7 C6 H6 119.8 . . ? C8 C3 C4 120.2(3) . . ? C8 C3 C2 121.9(2) . . ? C4 C3 C2 117.9(3) . . ? C10 N2 N3 102.2(3) . . ? N2 C10 N1 114.7(3) . . ? N2 C10 H10 122.7 . . ? N1 C10 H10 122.7 . . ? O5 C5 C4 123.6(3) . . ? O5 C5 C6 116.3(2) . . ? C4 C5 C6 120.0(3) . . ? C5 C4 C3 120.0(3) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? O5 C9 C9 106.0(3) . 3_658 ? O5 C9 H9A 110.5 . . ? C9 C9 H9A 110.5 3_658 . ? O5 C9 H9B 110.5 . . ? C9 C9 H9B 110.5 3_658 . ? H9A C9 H9B 108.7 . . ? C3 C8 C7 119.7(3) . . ? C3 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? N4 C14 C13 111.9(3) . . ? N4 C14 H14A 109.2 . . ? C13 C14 H14A 109.2 . . ? N4 C14 H14B 109.2 . . ? C13 C14 H14B 109.2 . . ? H14A C14 H14B 107.9 . . ? N3 C12 C13 111.5(3) . . ? N3 C12 H12A 109.3 . . ? C13 C12 H12A 109.3 . . ? N3 C12 H12B 109.3 . . ? C13 C12 H12B 109.3 . . ? H12A C12 H12B 108.0 . . ? C12 C13 C14 112.9(3) . . ? C12 C13 H13A 109.0 . . ? C14 C13 H13A 109.0 . . ? C12 C13 H13B 109.0 . . ? C14 C13 H13B 109.0 . . ? H13A C13 H13B 107.8 . . ? C16 N4 N5 108.8(3) . . ? C16 N4 C14 130.2(3) . . ? N5 N4 C14 121.0(3) . . ? N6 C16 N4 111.0(3) . . ? N6 C16 H16 124.5 . . ? N4 C16 H16 124.5 . . ? C15 N5 N4 103.0(3) . . ? N5 C15 N6 114.2(4) . . ? N5 C15 H15 122.9 . . ? N6 C15 H15 122.9 . . ? C16 N6 C15 103.0(3) . . ? C16 N6 Ni1 128.1(2) . 4_465 ? C15 N6 Ni1 128.8(3) . 4_465 ? O5W O3W O4W 139.0(15) . 1_455 ? 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 C1 O1 Ni1 -10.7(5) . . . . ? C7 C1 O1 Ni1 167.2(2) . . . . ? N6 Ni1 O1 C1 81.7(3) 4_666 . . . ? O3 Ni1 O1 C1 -77(28) 2_857 . . . ? N1 Ni1 O1 C1 -97.2(3) . . . . ? O2W Ni1 O1 C1 -7.0(3) . . . . ? O1W Ni1 O1 C1 171.3(3) . . . . ? O4 C2 O3 Ni1 11.7(5) . . . 2_847 ? C3 C2 O3 Ni1 -167.6(2) . . . 2_847 ? N1 C11 N3 N2 -0.3(4) . . . . ? N1 C11 N3 C12 180.0(3) . . . . ? O2 C1 C7 C6 -9.8(4) . . . . ? O1 C1 C7 C6 172.2(3) . . . . ? O2 C1 C7 C8 166.3(3) . . . . ? O1 C1 C7 C8 -11.7(4) . . . . ? N3 C11 N1 C10 0.1(4) . . . . ? N3 C11 N1 Ni1 170.0(2) . . . . ? O1 Ni1 N1 C11 16.6(3) . . . . ? N6 Ni1 N1 C11 -123(3) 4_666 . . . ? O3 Ni1 N1 C11 -163.4(3) 2_857 . . . ? O2W Ni1 N1 C11 -75.6(3) . . . . ? O1W Ni1 N1 C11 103.5(3) . . . . ? O1 Ni1 N1 C10 -175.9(3) . . . . ? N6 Ni1 N1 C10 45(3) 4_666 . . . ? O3 Ni1 N1 C10 4.1(3) 2_857 . . . ? O2W Ni1 N1 C10 91.9(3) . . . . ? O1W Ni1 N1 C10 -89.0(3) . . . . ? C8 C7 C6 C5 0.0(5) . . . . ? C1 C7 C6 C5 176.1(3) . . . . ? O4 C2 C3 C8 -164.2(3) . . . . ? O3 C2 C3 C8 15.2(4) . . . . ? O4 C2 C3 C4 13.3(4) . . . . ? O3 C2 C3 C4 -167.3(3) . . . . ? C11 N3 N2 C10 0.4(4) . . . . ? C12 N3 N2 C10 -179.9(3) . . . . ? N3 N2 C10 N1 -0.3(4) . . . . ? C11 N1 C10 N2 0.1(4) . . . . ? Ni1 N1 C10 N2 -169.9(2) . . . . ? C9 O5 C5 C4 -10.8(5) . . . . ? C9 O5 C5 C6 168.1(3) . . . . ? C7 C6 C5 O5 179.3(3) . . . . ? C7 C6 C5 C4 -1.7(5) . . . . ? O5 C5 C4 C3 -179.1(3) . . . . ? C6 C5 C4 C3 2.1(5) . . . . ? C8 C3 C4 C5 -0.6(5) . . . . ? C2 C3 C4 C5 -178.2(3) . . . . ? C5 O5 C9 C9 -175.8(3) . . . 3_658 ? C4 C3 C8 C7 -1.1(5) . . . . ? C2 C3 C8 C7 176.3(3) . . . . ? C6 C7 C8 C3 1.4(5) . . . . ? C1 C7 C8 C3 -174.6(3) . . . . ? C11 N3 C12 C13 62.3(5) . . . . ? N2 N3 C12 C13 -117.4(4) . . . . ? N3 C12 C13 C14 -169.4(3) . . . . ? N4 C14 C13 C12 -63.7(5) . . . . ? C13 C14 N4 C16 -76.7(5) . . . . ? C13 C14 N4 N5 101.2(4) . . . . ? N5 N4 C16 N6 0.0(4) . . . . ? C14 N4 C16 N6 178.1(3) . . . . ? C16 N4 N5 C15 0.3(5) . . . . ? C14 N4 N5 C15 -178.0(4) . . . . ? N4 N5 C15 N6 -0.6(5) . . . . ? N4 C16 N6 C15 -0.4(4) . . . . ? N4 C16 N6 Ni1 -177.8(2) . . . 4_465 ? N5 C15 N6 C16 0.6(5) . . . . ? N5 C15 N6 Ni1 178.1(3) . . . 4_465 ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.719 _refine_diff_density_min -0.322 _refine_diff_density_rms 0.081 #============================================================================= data_compound-8 _database_code_depnum_ccdc_archive 'CCDC 834805' #TrackingRef '- CIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H30 N12 O10 Zn2, 3(H2 O)' _chemical_formula_sum 'C32 H36 N12 O13 Zn2' _chemical_formula_weight 927.47 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 'p 21/n' _symmetry_space_group_name_hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.088(5) _cell_length_b 16.376(5) _cell_length_c 18.092(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 101.446(5) _cell_angle_gamma 90.000(5) _cell_volume 3801(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1753 _cell_measurement_theta_min 2.8048 _cell_measurement_theta_max 29.1369 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.621 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1904 _exptl_absorpt_coefficient_mu 1.344 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.98372 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14999 _diffrn_reflns_av_R_equivalents 0.0683 _diffrn_reflns_av_sigmaI/netI 0.1196 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.81 _diffrn_reflns_theta_max 25.35 _reflns_number_total 6920 _reflns_number_gt 3880 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0240P)^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 mconstr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6920 _refine_ls_number_parameters 532 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1319 _refine_ls_R_factor_gt 0.0605 _refine_ls_wR_factor_ref 0.1076 _refine_ls_wR_factor_gt 0.0866 _refine_ls_goodness_of_fit_ref 0.985 _refine_ls_restrained_S_all 0.986 _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 0.40146(4) 0.20157(4) 0.18385(3) 0.03684(18) Uani 1 1 d . . . Zn2 Zn 0.44739(4) 0.28433(4) -0.30769(3) 0.03776(18) Uani 1 1 d . . . C1 C 0.3349(4) 0.2523(3) 0.0436(3) 0.0434(14) Uani 1 1 d . . . C2 C 0.3166(4) 0.3600(3) -0.2171(3) 0.0382(13) Uani 1 1 d . . . C3 C 0.2794(4) 0.3627(3) -0.1429(2) 0.0317(12) Uani 1 1 d . . . C4 C 0.3243(4) 0.3107(3) -0.0848(2) 0.0348(12) Uani 1 1 d . . . H4 H 0.3796 0.2771 -0.0903 0.042 Uiso 1 1 calc R . . C5 C 0.2866(4) 0.3091(3) -0.0188(2) 0.0342(12) Uani 1 1 d . . . C6 C 0.2060(4) 0.3607(3) -0.0093(3) 0.0358(13) Uani 1 1 d . . . H6 H 0.1819 0.3598 0.0357 0.043 Uiso 1 1 calc R . . C7 C 0.1612(4) 0.4133(3) -0.0664(3) 0.0334(12) Uani 1 1 d . . . C8 C 0.1992(4) 0.4136(3) -0.1332(2) 0.0334(12) Uani 1 1 d . . . H8 H 0.1699 0.4488 -0.1719 0.040 Uiso 1 1 calc R . . C9 C 0.0449(3) 0.4704(3) 0.0062(2) 0.0352(13) Uani 1 1 d . . . H9A H 0.1004 0.4897 0.0462 0.042 Uiso 1 1 calc R . . H9B H 0.0223 0.4172 0.0203 0.042 Uiso 1 1 calc R . . C10 C 0.3054(5) 0.1546(4) 0.2889(3) 0.0462(15) Uani 1 1 d . . . C11 C 0.3804(5) 0.2061(3) 0.5661(3) 0.0445(14) Uani 1 1 d . . . C12 C 0.2806(4) 0.1396(3) 0.3665(3) 0.0375(13) Uani 1 1 d . . . C13 C 0.3406(4) 0.1748(3) 0.4299(3) 0.0383(13) Uani 1 1 d . . . H13 H 0.3987 0.2059 0.4257 0.046 Uiso 1 1 calc R . . C14 C 0.3145(4) 0.1641(3) 0.5001(3) 0.0368(13) Uani 1 1 d . . . C15 C 0.2293(4) 0.1165(3) 0.5062(3) 0.0419(14) Uani 1 1 d . . . H15 H 0.2111 0.1096 0.5529 0.050 Uiso 1 1 calc R . . C16 C 0.1713(4) 0.0793(3) 0.4433(3) 0.0462(15) Uani 1 1 d . . . C17 C 0.1980(4) 0.0912(3) 0.3730(3) 0.0465(15) Uani 1 1 d . . . H17 H 0.1594 0.0659 0.3304 0.056 Uiso 1 1 calc R . . C18 C 0.0481(4) 0.0254(4) 0.5098(3) 0.0563(17) Uani 1 1 d . . . H18A H 0.0318 0.0794 0.5262 0.068 Uiso 1 1 calc R . . H18B H 0.0985 0.0000 0.5497 0.068 Uiso 1 1 calc R . . C19 C 0.5228(4) 0.0606(4) 0.1311(3) 0.0446(14) Uani 1 1 d . . . H19 H 0.5343 0.0872 0.0881 0.054 Uiso 1 1 calc R . . C20 C 0.4769(4) 0.0310(4) 0.2323(3) 0.0429(14) Uani 1 1 d . . . H20 H 0.4480 0.0357 0.2751 0.051 Uiso 1 1 calc R . . C21 C 0.6100(4) -0.0736(4) 0.1136(3) 0.0584(17) Uani 1 1 d . . . H21A H 0.6104 -0.0547 0.0628 0.070 Uiso 1 1 calc R . . H21B H 0.5733 -0.1253 0.1097 0.070 Uiso 1 1 calc R . . C22 C 0.7223(4) -0.0872(4) 0.1547(3) 0.0522(15) Uani 1 1 d . . . H22A H 0.7568 -0.1226 0.1244 0.063 Uiso 1 1 calc R . . H22B H 0.7585 -0.0352 0.1598 0.063 Uiso 1 1 calc R . . C23 C 0.7310(4) -0.1242(4) 0.2312(3) 0.0570(16) Uani 1 1 d . . . H23A H 0.7058 -0.0856 0.2642 0.068 Uiso 1 1 calc R . . H23B H 0.6876 -0.1727 0.2275 0.068 Uiso 1 1 calc R . . C24 C 0.8859(4) -0.2169(4) 0.2730(3) 0.0649(18) Uani 1 1 d D . . H24 H 0.8520 -0.2663 0.2603 0.078 Uiso 1 1 calc R . . C25 C 0.9965(5) -0.1298(4) 0.3119(4) 0.079(2) Uani 1 1 d D . . H25 H 1.0598 -0.1051 0.3323 0.095 Uiso 1 1 calc R . . C26 C 0.6144(4) 0.2031(3) -0.1917(3) 0.0474(14) Uani 1 1 d . . . H26 H 0.5921 0.2268 -0.1510 0.057 Uiso 1 1 calc R . . N8 N 0.7061(4) 0.1295(4) -0.2562(3) 0.0783(17) Uani 1 1 d . . . C28 C 0.7687(4) 0.1216(4) -0.1216(3) 0.0594(17) Uani 1 1 d . . . H28A H 0.7691 0.1564 -0.0782 0.071 Uiso 1 1 calc R . . H28B H 0.8380 0.1227 -0.1331 0.071 Uiso 1 1 calc R . . C29 C 0.7431(4) 0.0356(3) -0.1023(3) 0.0446(14) Uani 1 1 d . . . H29A H 0.7259 0.0038 -0.1484 0.054 Uiso 1 1 calc R . . H29B H 0.6822 0.0363 -0.0792 0.054 Uiso 1 1 calc R . . C30 C 0.8332(4) -0.0056(4) -0.0486(3) 0.0582(17) Uani 1 1 d . . . H30A H 0.8664 0.0336 -0.0112 0.070 Uiso 1 1 calc R . . H30B H 0.8065 -0.0500 -0.0223 0.070 Uiso 1 1 calc R . . C31 C 0.9279(4) -0.1127(4) -0.1069(3) 0.0472(14) Uani 1 1 d . . . H31 H 0.8957 -0.1582 -0.0911 0.057 Uiso 1 1 calc R . . C32 C 1.0208(4) -0.0362(4) -0.1576(3) 0.0525(15) Uani 1 1 d . . . H32 H 1.0687 -0.0186 -0.1859 0.063 Uiso 1 1 calc R . . N1 N 0.4733(3) 0.0925(3) 0.1816(2) 0.0373(11) Uani 1 1 d . . . N2 N 0.5237(3) -0.0348(3) 0.2166(3) 0.0482(12) Uani 1 1 d . . . N3 N 0.5532(3) -0.0144(3) 0.1507(2) 0.0439(11) Uani 1 1 d . . . N4 N 0.8401(3) -0.1463(3) 0.2639(2) 0.0481(12) Uani 1 1 d . . . N5 N 0.9098(4) -0.0886(3) 0.2900(3) 0.0866(19) Uani 1 1 d . . . N6 N 0.9851(3) -0.2103(3) 0.3023(2) 0.0426(11) Uani 1 1 d . . . N7 N 0.5704(3) 0.2151(3) -0.2613(3) 0.0481(12) Uani 1 1 d . . . C27 C 0.6302(5) 0.1695(4) -0.3001(4) 0.074(2) Uani 1 1 d . . . H27 H 0.6182 0.1670 -0.3524 0.089 Uiso 1 1 calc R . . N9 N 0.6946(3) 0.1535(3) -0.1856(3) 0.0499(12) Uani 1 1 d . . . N10 N 0.9099(3) -0.0374(3) -0.0896(2) 0.0440(12) Uani 1 1 d . . . N11 N 0.9705(4) 0.0141(3) -0.1221(3) 0.0579(13) Uani 1 1 d . . . N12 N 0.9984(3) -0.1152(3) -0.1504(2) 0.0381(11) Uani 1 1 d . . . O1 O 0.2986(2) 0.2526(2) 0.10346(18) 0.0449(9) Uani 1 1 d . . . O2 O 0.4098(3) 0.2083(3) 0.03621(19) 0.0639(12) Uani 1 1 d . . . O3 O 0.3943(3) 0.3133(2) -0.21807(17) 0.0478(10) Uani 1 1 d . . . O4 O 0.2679(3) 0.3981(2) -0.27164(18) 0.0544(11) Uani 1 1 d . . . O5 O 0.0806(2) 0.4653(2) -0.06329(17) 0.0427(9) Uani 1 1 d . . . O6 O 0.3786(3) 0.2041(3) 0.28767(19) 0.0630(11) Uani 1 1 d . . . O7 O 0.2574(3) 0.1188(3) 0.2337(2) 0.0660(12) Uani 1 1 d . . . O8 O 0.4709(3) 0.2249(3) 0.5641(2) 0.0684(13) Uani 1 1 d . . . O9 O 0.3380(3) 0.2215(2) 0.62285(19) 0.0507(10) Uani 1 1 d . . . O10 O 0.0876(3) 0.0300(3) 0.4423(2) 0.0650(12) Uani 1 1 d . . . O1W O 0.2298(4) 0.3959(4) -0.4309(3) 0.1147(19) Uani 1 1 d . . . O2W O 0.5902(4) 0.2122(4) -0.0139(3) 0.124(2) Uani 1 1 d . . . O3W O 1.0702(5) 0.1784(5) -0.0804(5) 0.202(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0395(3) 0.0399(4) 0.0318(3) 0.0061(3) 0.0088(3) 0.0023(3) Zn2 0.0419(4) 0.0372(4) 0.0390(3) -0.0014(3) 0.0197(3) -0.0006(3) C1 0.045(3) 0.049(4) 0.038(3) 0.002(3) 0.011(3) 0.009(3) C2 0.048(3) 0.039(4) 0.030(3) -0.004(3) 0.015(3) -0.014(3) C3 0.039(3) 0.029(3) 0.027(3) 0.000(2) 0.009(2) 0.001(3) C4 0.035(3) 0.037(3) 0.034(3) 0.000(2) 0.011(2) 0.011(3) C5 0.039(3) 0.034(3) 0.031(3) -0.002(2) 0.010(2) 0.010(3) C6 0.045(3) 0.039(3) 0.028(3) 0.007(2) 0.018(2) 0.007(3) C7 0.036(3) 0.037(3) 0.030(3) 0.000(2) 0.012(2) 0.007(3) C8 0.038(3) 0.031(3) 0.030(3) 0.007(2) 0.004(2) 0.003(3) C9 0.037(3) 0.037(3) 0.036(3) 0.007(2) 0.017(2) 0.007(2) C10 0.050(4) 0.044(4) 0.049(4) 0.010(3) 0.021(3) 0.021(3) C11 0.056(4) 0.031(3) 0.049(3) -0.006(3) 0.016(3) -0.001(3) C12 0.049(3) 0.031(3) 0.036(3) 0.005(2) 0.017(3) 0.001(3) C13 0.040(3) 0.029(3) 0.050(3) 0.001(3) 0.019(3) 0.003(3) C14 0.041(3) 0.036(3) 0.038(3) -0.001(2) 0.018(2) 0.001(3) C15 0.050(3) 0.046(4) 0.035(3) -0.001(3) 0.021(3) -0.006(3) C16 0.049(4) 0.051(4) 0.039(3) 0.005(3) 0.012(3) -0.009(3) C17 0.048(3) 0.053(4) 0.038(3) -0.003(3) 0.005(3) -0.002(3) C18 0.045(3) 0.078(5) 0.049(4) 0.006(3) 0.018(3) -0.019(3) C19 0.041(3) 0.050(4) 0.045(3) 0.008(3) 0.012(3) 0.004(3) C20 0.035(3) 0.045(4) 0.050(3) 0.008(3) 0.011(3) 0.005(3) C21 0.053(4) 0.059(4) 0.062(4) -0.020(3) 0.008(3) 0.010(3) C22 0.045(3) 0.055(4) 0.060(4) -0.006(3) 0.018(3) 0.006(3) C23 0.042(3) 0.054(4) 0.080(4) 0.012(3) 0.025(3) 0.010(3) C24 0.050(4) 0.031(4) 0.110(5) -0.011(4) 0.006(4) 0.001(3) C25 0.063(4) 0.040(4) 0.119(6) -0.002(4) -0.018(4) 0.000(4) C26 0.046(3) 0.035(3) 0.062(4) 0.002(3) 0.014(3) -0.002(3) N8 0.084(4) 0.080(4) 0.082(4) 0.010(3) 0.043(3) 0.032(4) C28 0.041(3) 0.050(4) 0.081(4) -0.001(3) -0.002(3) 0.003(3) C29 0.037(3) 0.047(4) 0.050(3) -0.010(3) 0.009(3) 0.002(3) C30 0.060(4) 0.072(5) 0.047(3) -0.003(3) 0.019(3) 0.021(4) C31 0.049(4) 0.044(4) 0.051(4) 0.005(3) 0.016(3) 0.007(3) C32 0.041(3) 0.046(4) 0.074(4) 0.005(3) 0.022(3) 0.004(3) N1 0.033(2) 0.038(3) 0.041(3) 0.006(2) 0.009(2) 0.005(2) N2 0.042(3) 0.042(3) 0.062(3) 0.009(2) 0.013(2) 0.005(2) N3 0.037(3) 0.044(3) 0.050(3) -0.003(2) 0.007(2) 0.002(2) N4 0.043(3) 0.043(3) 0.062(3) 0.003(3) 0.021(2) 0.001(3) N5 0.078(4) 0.053(4) 0.114(5) -0.005(3) -0.018(4) 0.012(4) N6 0.037(3) 0.041(3) 0.049(3) -0.003(2) 0.005(2) -0.003(2) N7 0.051(3) 0.041(3) 0.058(3) 0.010(3) 0.024(2) 0.008(3) C27 0.091(5) 0.076(5) 0.065(4) 0.017(4) 0.040(4) 0.041(4) N9 0.042(3) 0.040(3) 0.068(3) 0.000(3) 0.012(3) 0.000(3) N10 0.042(3) 0.047(3) 0.042(3) -0.006(2) 0.005(2) 0.012(3) N11 0.046(3) 0.041(3) 0.090(4) -0.006(3) 0.021(3) 0.002(3) N12 0.038(3) 0.036(3) 0.043(3) 0.000(2) 0.016(2) 0.003(2) O1 0.042(2) 0.060(3) 0.035(2) 0.0138(18) 0.0147(16) 0.0168(19) O2 0.073(3) 0.077(3) 0.049(2) 0.020(2) 0.029(2) 0.040(3) O3 0.056(2) 0.056(3) 0.038(2) 0.0008(18) 0.0235(17) 0.016(2) O4 0.066(2) 0.070(3) 0.030(2) 0.018(2) 0.0174(18) 0.014(2) O5 0.044(2) 0.052(3) 0.037(2) 0.0096(17) 0.0206(16) 0.0177(19) O6 0.093(3) 0.059(3) 0.048(2) 0.005(2) 0.040(2) -0.002(3) O7 0.063(3) 0.098(4) 0.040(2) 0.002(2) 0.015(2) 0.013(3) O8 0.052(3) 0.083(4) 0.075(3) -0.030(2) 0.025(2) -0.026(3) O9 0.056(2) 0.052(3) 0.048(2) -0.0070(19) 0.0205(18) -0.006(2) O10 0.054(2) 0.091(4) 0.055(3) -0.005(2) 0.022(2) -0.034(2) O1W 0.104(4) 0.155(6) 0.094(4) -0.017(3) 0.042(3) -0.007(4) O2W 0.097(4) 0.158(6) 0.129(4) -0.001(4) 0.052(3) 0.004(4) O3W 0.145(6) 0.129(7) 0.356(11) -0.048(6) 0.109(6) -0.017(5) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O6 1.960(3) . ? Zn1 O1 1.962(3) . ? Zn1 N1 2.022(4) . ? Zn1 N6 2.050(4) 2_655 ? Zn1 C10 2.594(6) . ? Zn2 O3 1.946(3) . ? Zn2 O9 1.993(3) 1_554 ? Zn2 N12 1.999(4) 2_654 ? Zn2 N7 2.011(4) . ? C1 O2 1.245(6) . ? C1 O1 1.266(6) . ? C1 C5 1.502(7) . ? C2 O4 1.233(6) . ? C2 O3 1.274(6) . ? C2 C3 1.517(6) . ? C3 C8 1.378(6) . ? C3 C4 1.390(6) . ? C4 C5 1.380(6) . ? C4 H4 0.9300 . ? C5 C6 1.389(6) . ? C6 C7 1.382(6) . ? C6 H6 0.9300 . ? C7 O5 1.366(5) . ? C7 C8 1.396(6) . ? C8 H8 0.9300 . ? C9 O5 1.428(5) . ? C9 C9 1.505(8) 3_565 ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 O7 1.219(6) . ? C10 O6 1.259(6) . ? C10 C12 1.524(7) . ? C11 O8 1.230(6) . ? C11 O9 1.285(6) . ? C11 C14 1.495(7) . ? C12 C17 1.363(7) . ? C12 C13 1.382(6) . ? C13 C14 1.389(6) . ? C13 H13 0.9300 . ? C14 C15 1.383(6) . ? C15 C16 1.379(7) . ? C15 H15 0.9300 . ? C16 O10 1.358(6) . ? C16 C17 1.398(7) . ? C17 H17 0.9300 . ? C18 O10 1.419(6) . ? C18 C18 1.493(9) 3_556 ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 N3 1.317(6) . ? C19 N1 1.329(6) . ? C19 H19 0.9300 . ? C20 N2 1.299(6) . ? C20 N1 1.356(6) . ? C20 H20 0.9300 . ? C21 N3 1.463(6) . ? C21 C22 1.526(6) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.494(7) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 N4 1.479(6) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 N4 1.297(7) . ? C24 N6 1.306(6) . ? C24 H24 0.9300 . ? C25 N5 1.311(7) . ? C25 N6 1.335(7) . ? C25 H25 0.9300 . ? C26 N7 1.291(6) . ? C26 N9 1.315(6) . ? C26 H26 0.9300 . ? N8 C27 1.316(7) . ? N8 N9 1.373(6) . ? C28 N9 1.452(6) . ? C28 C29 1.505(7) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C30 1.529(7) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 N10 1.458(6) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 N10 1.305(6) . ? C31 N12 1.327(6) . ? C31 H31 0.9300 . ? C32 N11 1.302(7) . ? C32 N12 1.338(6) . ? C32 H32 0.9300 . ? N2 N3 1.366(6) . ? N4 N5 1.332(6) . ? N6 Zn1 2.050(4) 2_645 ? N7 C27 1.371(7) . ? C27 H27 0.9300 . ? N10 N11 1.368(6) . ? N12 Zn2 1.999(4) 2_644 ? O9 Zn2 1.993(3) 1_556 ? 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 Zn1 O1 119.24(16) . . ? O6 Zn1 N1 101.41(17) . . ? O1 Zn1 N1 127.94(15) . . ? O6 Zn1 N6 96.43(18) . 2_655 ? O1 Zn1 N6 99.46(16) . 2_655 ? N1 Zn1 N6 107.21(17) . 2_655 ? O6 Zn1 C10 27.91(16) . . ? O1 Zn1 C10 107.95(16) . . ? N1 Zn1 C10 92.74(17) . . ? N6 Zn1 C10 124.30(19) 2_655 . ? O3 Zn2 O9 108.71(15) . 1_554 ? O3 Zn2 N12 109.11(17) . 2_654 ? O9 Zn2 N12 116.74(15) 1_554 2_654 ? O3 Zn2 N7 100.30(17) . . ? O9 Zn2 N7 112.78(17) 1_554 . ? N12 Zn2 N7 107.89(17) 2_654 . ? O2 C1 O1 122.1(5) . . ? O2 C1 C5 120.1(5) . . ? O1 C1 C5 117.8(5) . . ? O4 C2 O3 125.4(5) . . ? O4 C2 C3 119.2(5) . . ? O3 C2 C3 115.3(5) . . ? C8 C3 C4 119.5(4) . . ? C8 C3 C2 121.1(4) . . ? C4 C3 C2 119.3(5) . . ? C5 C4 C3 119.7(5) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C4 C5 C6 120.5(4) . . ? C4 C5 C1 119.5(5) . . ? C6 C5 C1 120.0(4) . . ? C7 C6 C5 120.4(4) . . ? C7 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? O5 C7 C6 125.1(4) . . ? O5 C7 C8 116.4(4) . . ? C6 C7 C8 118.6(5) . . ? C3 C8 C7 121.3(4) . . ? C3 C8 H8 119.3 . . ? C7 C8 H8 119.3 . . ? O5 C9 C9 106.7(4) . 3_565 ? O5 C9 H9A 110.4 . . ? C9 C9 H9A 110.4 3_565 . ? O5 C9 H9B 110.4 . . ? C9 C9 H9B 110.4 3_565 . ? H9A C9 H9B 108.6 . . ? O7 C10 O6 124.5(5) . . ? O7 C10 C12 120.5(6) . . ? O6 C10 C12 115.0(5) . . ? O7 C10 Zn1 77.8(3) . . ? O6 C10 Zn1 46.8(3) . . ? C12 C10 Zn1 161.1(5) . . ? O8 C11 O9 123.0(5) . . ? O8 C11 C14 119.8(5) . . ? O9 C11 C14 117.1(5) . . ? C17 C12 C13 120.1(5) . . ? C17 C12 C10 119.4(5) . . ? C13 C12 C10 120.5(5) . . ? C12 C13 C14 120.2(5) . . ? C12 C13 H13 119.9 . . ? C14 C13 H13 119.9 . . ? C15 C14 C13 119.5(5) . . ? C15 C14 C11 122.8(5) . . ? C13 C14 C11 117.6(5) . . ? C16 C15 C14 120.2(5) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? O10 C16 C15 125.7(5) . . ? O10 C16 C17 114.7(5) . . ? C15 C16 C17 119.6(5) . . ? C12 C17 C16 120.3(5) . . ? C12 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? O10 C18 C18 105.1(5) . 3_556 ? O10 C18 H18A 110.7 . . ? C18 C18 H18A 110.7 3_556 . ? O10 C18 H18B 110.7 . . ? C18 C18 H18B 110.7 3_556 . ? H18A C18 H18B 108.8 . . ? N3 C19 N1 110.2(5) . . ? N3 C19 H19 124.9 . . ? N1 C19 H19 124.9 . . ? N2 C20 N1 115.1(5) . . ? N2 C20 H20 122.5 . . ? N1 C20 H20 122.5 . . ? N3 C21 C22 113.6(4) . . ? N3 C21 H21A 108.8 . . ? C22 C21 H21A 108.8 . . ? N3 C21 H21B 108.8 . . ? C22 C21 H21B 108.8 . . ? H21A C21 H21B 107.7 . . ? C23 C22 C21 113.6(5) . . ? C23 C22 H22A 108.8 . . ? C21 C22 H22A 108.8 . . ? C23 C22 H22B 108.8 . . ? C21 C22 H22B 108.8 . . ? H22A C22 H22B 107.7 . . ? N4 C23 C22 111.1(4) . . ? N4 C23 H23A 109.4 . . ? C22 C23 H23A 109.4 . . ? N4 C23 H23B 109.4 . . ? C22 C23 H23B 109.4 . . ? H23A C23 H23B 108.0 . . ? N4 C24 N6 112.1(5) . . ? N4 C24 H24 124.0 . . ? N6 C24 H24 124.0 . . ? N5 C25 N6 113.6(5) . . ? N5 C25 H25 123.2 . . ? N6 C25 H25 123.2 . . ? N7 C26 N9 111.8(5) . . ? N7 C26 H26 124.1 . . ? N9 C26 H26 124.1 . . ? C27 N8 N9 102.1(5) . . ? N9 C28 C29 112.2(4) . . ? N9 C28 H28A 109.2 . . ? C29 C28 H28A 109.2 . . ? N9 C28 H28B 109.2 . . ? C29 C28 H28B 109.2 . . ? H28A C28 H28B 107.9 . . ? C28 C29 C30 112.4(4) . . ? C28 C29 H29A 109.1 . . ? C30 C29 H29A 109.1 . . ? C28 C29 H29B 109.1 . . ? C30 C29 H29B 109.1 . . ? H29A C29 H29B 107.9 . . ? N10 C30 C29 110.9(4) . . ? N10 C30 H30A 109.5 . . ? C29 C30 H30A 109.5 . . ? N10 C30 H30B 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 108.1 . . ? N10 C31 N12 110.6(5) . . ? N10 C31 H31 124.7 . . ? N12 C31 H31 124.7 . . ? N11 C32 N12 115.0(5) . . ? N11 C32 H32 122.5 . . ? N12 C32 H32 122.5 . . ? C19 N1 C20 102.5(5) . . ? C19 N1 Zn1 130.8(4) . . ? C20 N1 Zn1 126.6(4) . . ? C20 N2 N3 102.4(4) . . ? C19 N3 N2 109.9(4) . . ? C19 N3 C21 130.4(5) . . ? N2 N3 C21 119.8(5) . . ? C24 N4 N5 108.7(4) . . ? C24 N4 C23 130.9(5) . . ? N5 N4 C23 120.5(5) . . ? C25 N5 N4 103.5(5) . . ? C24 N6 C25 102.1(4) . . ? C24 N6 Zn1 129.0(4) . 2_645 ? C25 N6 Zn1 128.4(4) . 2_645 ? C26 N7 C27 103.1(5) . . ? C26 N7 Zn2 131.1(4) . . ? C27 N7 Zn2 125.8(4) . . ? N8 C27 N7 113.7(6) . . ? N8 C27 H27 123.2 . . ? N7 C27 H27 123.2 . . ? C26 N9 N8 109.3(5) . . ? C26 N9 C28 133.3(5) . . ? N8 N9 C28 117.3(5) . . ? C31 N10 N11 109.3(5) . . ? C31 N10 C30 129.4(5) . . ? N11 N10 C30 121.0(5) . . ? C32 N11 N10 102.4(5) . . ? C31 N12 C32 102.7(5) . . ? C31 N12 Zn2 126.2(4) . 2_644 ? C32 N12 Zn2 131.1(4) . 2_644 ? C1 O1 Zn1 108.3(3) . . ? C2 O3 Zn2 125.1(3) . . ? C7 O5 C9 117.6(3) . . ? C10 O6 Zn1 105.3(4) . . ? C11 O9 Zn2 103.6(3) . 1_556 ? C16 O10 C18 116.8(4) . . ? 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 C2 C3 C8 -7.0(7) . . . . ? O3 C2 C3 C8 176.9(4) . . . . ? O4 C2 C3 C4 170.6(5) . . . . ? O3 C2 C3 C4 -5.5(7) . . . . ? C8 C3 C4 C5 1.6(7) . . . . ? C2 C3 C4 C5 -176.0(4) . . . . ? C3 C4 C5 C6 -1.7(7) . . . . ? C3 C4 C5 C1 179.4(4) . . . . ? O2 C1 C5 C4 1.6(8) . . . . ? O1 C1 C5 C4 179.8(5) . . . . ? O2 C1 C5 C6 -177.3(5) . . . . ? O1 C1 C5 C6 0.9(7) . . . . ? C4 C5 C6 C7 1.1(7) . . . . ? C1 C5 C6 C7 179.9(5) . . . . ? C5 C6 C7 O5 178.8(4) . . . . ? C5 C6 C7 C8 -0.3(7) . . . . ? C4 C3 C8 C7 -0.8(7) . . . . ? C2 C3 C8 C7 176.7(4) . . . . ? O5 C7 C8 C3 -179.0(4) . . . . ? C6 C7 C8 C3 0.2(7) . . . . ? O6 Zn1 C10 O7 176.3(6) . . . . ? O1 Zn1 C10 O7 57.3(3) . . . . ? N1 Zn1 C10 O7 -74.2(3) . . . . ? N6 Zn1 C10 O7 172.8(3) 2_655 . . . ? O1 Zn1 C10 O6 -119.1(3) . . . . ? N1 Zn1 C10 O6 109.5(4) . . . . ? N6 Zn1 C10 O6 -3.6(4) 2_655 . . . ? O6 Zn1 C10 C12 -16.8(10) . . . . ? O1 Zn1 C10 C12 -135.8(11) . . . . ? N1 Zn1 C10 C12 92.7(11) . . . . ? N6 Zn1 C10 C12 -20.4(12) 2_655 . . . ? O7 C10 C12 C17 -5.8(8) . . . . ? O6 C10 C12 C17 175.7(5) . . . . ? Zn1 C10 C12 C17 -170.9(9) . . . . ? O7 C10 C12 C13 174.5(5) . . . . ? O6 C10 C12 C13 -4.0(7) . . . . ? Zn1 C10 C12 C13 9.4(14) . . . . ? C17 C12 C13 C14 -2.8(7) . . . . ? C10 C12 C13 C14 176.8(5) . . . . ? C12 C13 C14 C15 1.3(7) . . . . ? C12 C13 C14 C11 -178.0(5) . . . . ? O8 C11 C14 C15 156.6(5) . . . . ? O9 C11 C14 C15 -23.8(8) . . . . ? O8 C11 C14 C13 -24.1(8) . . . . ? O9 C11 C14 C13 155.4(5) . . . . ? C13 C14 C15 C16 0.7(8) . . . . ? C11 C14 C15 C16 179.9(5) . . . . ? C14 C15 C16 O10 178.6(5) . . . . ? C14 C15 C16 C17 -1.1(8) . . . . ? C13 C12 C17 C16 2.3(8) . . . . ? C10 C12 C17 C16 -177.3(5) . . . . ? O10 C16 C17 C12 179.8(5) . . . . ? C15 C16 C17 C12 -0.4(8) . . . . ? N3 C21 C22 C23 64.3(7) . . . . ? C21 C22 C23 N4 172.2(5) . . . . ? N9 C28 C29 C30 166.2(5) . . . . ? C28 C29 C30 N10 -81.5(6) . . . . ? N3 C19 N1 C20 0.0(5) . . . . ? N3 C19 N1 Zn1 -176.8(3) . . . . ? N2 C20 N1 C19 -0.2(6) . . . . ? N2 C20 N1 Zn1 176.8(3) . . . . ? O6 Zn1 N1 C19 -168.4(4) . . . . ? O1 Zn1 N1 C19 49.5(5) . . . . ? N6 Zn1 N1 C19 -67.9(4) 2_655 . . . ? C10 Zn1 N1 C19 164.9(4) . . . . ? O6 Zn1 N1 C20 15.5(4) . . . . ? O1 Zn1 N1 C20 -126.6(4) . . . . ? N6 Zn1 N1 C20 116.0(4) 2_655 . . . ? C10 Zn1 N1 C20 -11.2(4) . . . . ? N1 C20 N2 N3 0.3(6) . . . . ? N1 C19 N3 N2 0.1(6) . . . . ? N1 C19 N3 C21 -179.9(4) . . . . ? C20 N2 N3 C19 -0.2(5) . . . . ? C20 N2 N3 C21 179.8(4) . . . . ? C22 C21 N3 C19 108.2(6) . . . . ? C22 C21 N3 N2 -71.8(6) . . . . ? N6 C24 N4 N5 -1.9(7) . . . . ? N6 C24 N4 C23 177.9(5) . . . . ? C22 C23 N4 C24 -105.8(7) . . . . ? C22 C23 N4 N5 74.0(7) . . . . ? N6 C25 N5 N4 -1.0(8) . . . . ? C24 N4 N5 C25 1.7(7) . . . . ? C23 N4 N5 C25 -178.2(5) . . . . ? N4 C24 N6 C25 1.2(7) . . . . ? N4 C24 N6 Zn1 -171.1(4) . . . 2_645 ? N5 C25 N6 C24 -0.1(8) . . . . ? N5 C25 N6 Zn1 172.3(4) . . . 2_645 ? N9 C26 N7 C27 -0.8(6) . . . . ? N9 C26 N7 Zn2 -179.2(4) . . . . ? O3 Zn2 N7 C26 -10.4(5) . . . . ? O9 Zn2 N7 C26 -125.9(5) 1_554 . . . ? N12 Zn2 N7 C26 103.7(5) 2_654 . . . ? O3 Zn2 N7 C27 171.4(5) . . . . ? O9 Zn2 N7 C27 55.9(5) 1_554 . . . ? N12 Zn2 N7 C27 -74.5(5) 2_654 . . . ? N9 N8 C27 N7 -1.7(7) . . . . ? C26 N7 C27 N8 1.6(7) . . . . ? Zn2 N7 C27 N8 -179.9(4) . . . . ? N7 C26 N9 N8 -0.2(6) . . . . ? N7 C26 N9 C28 179.7(5) . . . . ? C27 N8 N9 C26 1.1(6) . . . . ? C27 N8 N9 C28 -178.8(5) . . . . ? C29 C28 N9 C26 100.9(7) . . . . ? C29 C28 N9 N8 -79.2(6) . . . . ? N12 C31 N10 N11 -0.2(6) . . . . ? N12 C31 N10 C30 174.6(4) . . . . ? C29 C30 N10 C31 -105.3(6) . . . . ? C29 C30 N10 N11 68.9(6) . . . . ? N12 C32 N11 N10 -0.4(6) . . . . ? C31 N10 N11 C32 0.3(6) . . . . ? C30 N10 N11 C32 -174.9(4) . . . . ? N10 C31 N12 C32 -0.1(5) . . . . ? N10 C31 N12 Zn2 -179.9(3) . . . 2_644 ? N11 C32 N12 C31 0.3(6) . . . . ? N11 C32 N12 Zn2 -179.9(3) . . . 2_644 ? O2 C1 O1 Zn1 16.1(6) . . . . ? C5 C1 O1 Zn1 -162.1(4) . . . . ? O6 Zn1 O1 C1 172.4(3) . . . . ? N1 Zn1 O1 C1 -51.2(4) . . . . ? N6 Zn1 O1 C1 69.4(4) 2_655 . . . ? C10 Zn1 O1 C1 -159.7(4) . . . . ? O4 C2 O3 Zn2 -5.2(7) . . . . ? C3 C2 O3 Zn2 170.6(3) . . . . ? O9 Zn2 O3 C2 -63.8(4) 1_554 . . . ? N12 Zn2 O3 C2 64.5(4) 2_654 . . . ? N7 Zn2 O3 C2 177.7(4) . . . . ? C6 C7 O5 C9 5.1(7) . . . . ? C8 C7 O5 C9 -175.8(4) . . . . ? C9 C9 O5 C7 -178.6(5) 3_565 . . . ? O7 C10 O6 Zn1 -4.3(7) . . . . ? C12 C10 O6 Zn1 174.1(3) . . . . ? O1 Zn1 O6 C10 72.4(4) . . . . ? N1 Zn1 O6 C10 -73.9(4) . . . . ? N6 Zn1 O6 C10 177.0(3) 2_655 . . . ? O8 C11 O9 Zn2 3.9(7) . . . 1_556 ? C14 C11 O9 Zn2 -175.6(4) . . . 1_556 ? C15 C16 O10 C18 9.0(8) . . . . ? C17 C16 O10 C18 -171.2(5) . . . . ? C18 C18 O10 C16 174.6(6) 3_556 . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.455 _refine_diff_density_min -0.335 _refine_diff_density_rms 0.079 #============================================================================= data_compound-9 _database_code_depnum_ccdc_archive 'CCDC 834806' #TrackingRef '- CIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C13 H15 Co N3 O7, 1.5(H2 O)' _chemical_formula_sum 'C13 H18 Co N3 O8.50' _chemical_formula_weight 411.23 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' 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' _symmetry_space_group_name_hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.731(5) _cell_length_b 10.120(5) _cell_length_c 10.597(5) _cell_angle_alpha 67.258(5) _cell_angle_beta 62.830(5) _cell_angle_gamma 75.866(5) _cell_volume 853.3(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1348 _cell_measurement_theta_min 3.3436 _cell_measurement_theta_max 29.1063 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.601 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 424 _exptl_absorpt_coefficient_mu 1.056 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.73791 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5380 _diffrn_reflns_av_R_equivalents 0.0561 _diffrn_reflns_av_sigmaI/netI 0.1106 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.35 _diffrn_reflns_theta_max 25.35 _reflns_number_total 3110 _reflns_number_gt 1945 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXS-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0793P)^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 3110 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1162 _refine_ls_R_factor_gt 0.0691 _refine_ls_wR_factor_ref 0.1864 _refine_ls_wR_factor_gt 0.1566 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.010 _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 0.55065(10) 0.37289(8) 0.22735(9) 0.0397(3) Uani 1 1 d . . . O3 O 0.5696(5) 1.1461(4) 0.2391(5) 0.0459(11) Uani 1 1 d . . . O4 O 0.3805(4) 1.2976(4) 0.1988(4) 0.0432(10) Uani 1 1 d . . . C3 C 0.3907(6) 1.0617(5) 0.1967(6) 0.0330(13) Uani 1 1 d . . . O1 O 0.4546(5) 0.5824(4) 0.1890(4) 0.0445(10) Uani 1 1 d . . . O5 O 0.1114(5) 1.0497(4) 0.0662(6) 0.0651(14) Uani 1 1 d . . . C5 C 0.3973(6) 0.8155(5) 0.2120(6) 0.0333(13) Uani 1 1 d . . . O2 O 0.5309(6) 0.6226(4) 0.3367(5) 0.0570(13) Uani 1 1 d . . . C2 C 0.4494(7) 1.1746(6) 0.2125(6) 0.0357(13) Uani 1 1 d . . . C8 C 0.2752(7) 1.1005(6) 0.1430(7) 0.0407(15) Uani 1 1 d . . . H8 H 0.2327 1.1951 0.1216 0.049 Uiso 1 1 calc R . . C4 C 0.4511(7) 0.9190(5) 0.2317(6) 0.0351(13) Uani 1 1 d . . . H4 H 0.5277 0.8924 0.2684 0.042 Uiso 1 1 calc R . . C7 C 0.2231(7) 0.9974(6) 0.1211(7) 0.0406(15) Uani 1 1 d . . . C1 C 0.4660(7) 0.6624(6) 0.2499(6) 0.0370(14) Uani 1 1 d . . . C6 C 0.2841(7) 0.8566(6) 0.1550(7) 0.0389(14) Uani 1 1 d . . . H6 H 0.2494 0.7884 0.1397 0.047 Uiso 1 1 calc R . . N3 N 0.9216(7) 0.3652(8) 0.3305(7) 0.0688(18) Uani 1 1 d . . . C9 C 0.0559(7) 0.9539(6) 0.0339(8) 0.0501(17) Uani 1 1 d . . . H9A H 0.0040 0.8783 0.1245 0.060 Uiso 1 1 calc R . . H9B H 0.1406 0.9104 -0.0362 0.060 Uiso 1 1 calc R . . N1 N 0.7556(7) 0.3629(6) 0.2457(7) 0.0537(15) Uani 1 1 d . . . C12 C 0.9953(10) 0.3675(11) 0.4206(10) 0.086(3) Uani 1 1 d . . . H12A H 0.9595 0.2912 0.5156 0.103 Uiso 1 1 calc R . . H12B H 1.1064 0.3491 0.3702 0.103 Uiso 1 1 calc R . . C10 C 0.9038(16) 0.3922(19) 0.1212(19) 0.078(7) Uiso 0.66(4) 1 d P A 1 C10' C 0.872(4) 0.301(5) 0.202(4) 0.093(14) Uiso 0.34(4) 1 d P A 2 N2 N 1.0078(13) 0.3959(13) 0.1714(13) 0.078(5) Uiso 0.64(2) 1 d P A 1 N2' N 0.977(4) 0.271(4) 0.269(4) 0.154(15) Uiso 0.36(2) 1 d P A 2 C13 C 0.9635(11) 0.5009(11) 0.4475(12) 0.100(3) Uani 1 1 d . . . H13A H 0.8522 0.5219 0.4931 0.120 Uiso 1 1 calc R A . H13B H 1.0044 0.5766 0.3530 0.120 Uiso 1 1 calc R . . C11 C 0.7785(9) 0.3660(12) 0.3551(10) 0.097(3) Uani 1 1 d . A . O1W O 0.6816(5) 0.4254(4) -0.0124(5) 0.0463(10) Uani 1 1 d . . . O2W O 0.4192(5) 0.3140(5) 0.4590(5) 0.0564(12) Uani 1 1 d . . . O3W O 0.2717(7) 0.0670(6) 0.6046(7) 0.108(2) Uani 1 1 d . . . O4W O 0.0581(17) -0.0100(19) 0.533(2) 0.158(8) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0568(6) 0.0232(4) 0.0596(6) -0.0145(4) -0.0409(5) 0.0001(3) O3 0.058(3) 0.028(2) 0.073(3) -0.018(2) -0.043(2) -0.0024(19) O4 0.057(3) 0.026(2) 0.067(3) -0.021(2) -0.042(2) 0.0046(19) C3 0.048(3) 0.023(3) 0.037(3) -0.012(2) -0.021(3) -0.007(3) O1 0.071(3) 0.027(2) 0.060(3) -0.019(2) -0.045(2) 0.0021(19) O5 0.082(3) 0.038(2) 0.130(4) -0.043(3) -0.085(3) 0.017(2) C5 0.045(3) 0.023(3) 0.040(3) -0.012(2) -0.024(3) -0.001(2) O2 0.099(4) 0.031(2) 0.074(3) -0.021(2) -0.065(3) 0.006(2) C2 0.049(4) 0.024(3) 0.043(3) -0.011(3) -0.025(3) -0.006(3) C8 0.052(4) 0.028(3) 0.059(4) -0.020(3) -0.035(3) 0.003(3) C4 0.050(3) 0.022(3) 0.044(4) -0.011(3) -0.030(3) 0.000(3) C7 0.046(3) 0.035(3) 0.058(4) -0.017(3) -0.036(3) 0.000(3) C1 0.059(4) 0.025(3) 0.041(3) -0.011(3) -0.032(3) -0.004(3) C6 0.052(4) 0.027(3) 0.057(4) -0.019(3) -0.033(3) -0.002(3) N3 0.056(4) 0.097(5) 0.092(5) -0.056(4) -0.047(4) 0.008(3) C9 0.060(4) 0.040(4) 0.076(5) -0.025(3) -0.044(4) -0.003(3) N1 0.056(3) 0.057(3) 0.080(4) -0.041(3) -0.044(3) 0.007(3) C12 0.076(5) 0.125(8) 0.101(7) -0.060(6) -0.061(5) 0.009(5) C13 0.091(6) 0.124(8) 0.158(9) -0.091(7) -0.091(6) 0.028(6) C11 0.063(5) 0.174(10) 0.095(7) -0.062(7) -0.058(5) 0.008(6) O1W 0.061(3) 0.040(2) 0.053(3) -0.020(2) -0.031(2) -0.004(2) O2W 0.085(3) 0.052(3) 0.052(3) -0.018(2) -0.041(3) -0.011(2) O3W 0.129(5) 0.074(4) 0.114(5) 0.022(4) -0.075(4) -0.029(4) O4W 0.129(15) 0.111(12) 0.169(18) -0.011(12) -0.030(12) -0.019(12) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1 2.061(4) . ? Co1 N1 2.066(5) . ? Co1 O2W 2.095(4) . ? Co1 O4 2.160(4) 1_545 ? Co1 O1W 2.166(4) . ? Co1 O3 2.216(4) 1_545 ? O3 C2 1.267(7) . ? O3 Co1 2.216(4) 1_565 ? O4 C2 1.250(6) . ? O4 Co1 2.160(4) 1_565 ? C3 C8 1.391(7) . ? C3 C4 1.392(7) . ? C3 C2 1.488(7) . ? O1 C1 1.265(6) . ? O5 C7 1.363(7) . ? O5 C9 1.425(7) . ? C5 C6 1.394(8) . ? C5 C4 1.396(7) . ? C5 C1 1.506(7) . ? O2 C1 1.235(6) . ? C8 C7 1.397(7) . ? C8 H8 0.9300 . ? C4 H4 0.9300 . ? C7 C6 1.378(8) . ? C6 H6 0.9300 . ? N3 N2' 1.24(3) . ? N3 C11 1.293(9) . ? N3 N2 1.440(12) . ? N3 C12 1.441(9) . ? C9 C9 1.506(12) 2_575 ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? N1 C10' 1.14(3) . ? N1 C11 1.289(9) . ? N1 C10 1.441(16) . ? C12 C13 1.418(12) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C10 N2 1.355(16) . ? C10' N2' 1.41(4) . ? C10' C11 1.76(3) . ? N2' C11 1.91(3) . ? C13 C13 1.564(15) 2_766 ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? O4W O4W 1.53(3) 2_556 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 N1 108.91(19) . . ? O1 Co1 O2W 93.93(17) . . ? N1 Co1 O2W 93.9(2) . . ? O1 Co1 O4 94.12(15) . 1_545 ? N1 Co1 O4 156.22(18) . 1_545 ? O2W Co1 O4 90.32(16) . 1_545 ? O1 Co1 O1W 87.59(16) . . ? N1 Co1 O1W 87.9(2) . . ? O2W Co1 O1W 177.14(15) . . ? O4 Co1 O1W 87.15(15) 1_545 . ? O1 Co1 O3 153.73(15) . 1_545 ? N1 Co1 O3 96.84(19) . 1_545 ? O2W Co1 O3 89.33(16) . 1_545 ? O4 Co1 O3 59.77(14) 1_545 1_545 ? O1W Co1 O3 88.25(15) . 1_545 ? C2 O3 Co1 88.6(3) . 1_565 ? C2 O4 Co1 91.6(3) . 1_565 ? C8 C3 C4 119.6(5) . . ? C8 C3 C2 119.1(5) . . ? C4 C3 C2 121.3(5) . . ? C1 O1 Co1 120.7(4) . . ? C7 O5 C9 118.3(4) . . ? C6 C5 C4 119.5(5) . . ? C6 C5 C1 121.6(5) . . ? C4 C5 C1 118.9(5) . . ? O4 C2 O3 120.0(5) . . ? O4 C2 C3 120.0(5) . . ? O3 C2 C3 120.0(5) . . ? C3 C8 C7 120.1(5) . . ? C3 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C3 C4 C5 120.3(5) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? O5 C7 C6 125.7(5) . . ? O5 C7 C8 114.2(5) . . ? C6 C7 C8 120.1(5) . . ? O2 C1 O1 123.9(5) . . ? O2 C1 C5 118.8(5) . . ? O1 C1 C5 117.3(5) . . ? C7 C6 C5 120.4(5) . . ? C7 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? N2' N3 C11 98.1(17) . . ? N2' N3 N2 56.6(16) . . ? C11 N3 N2 105.9(7) . . ? N2' N3 C12 115.1(18) . . ? C11 N3 C12 133.1(7) . . ? N2 N3 C12 119.7(7) . . ? O5 C9 C9 105.0(6) . 2_575 ? O5 C9 H9A 110.7 . . ? C9 C9 H9A 110.7 2_575 . ? O5 C9 H9B 110.7 . . ? C9 C9 H9B 110.7 2_575 . ? H9A C9 H9B 108.8 . . ? C10' N1 C11 92.7(17) . . ? C10' N1 C10 42.8(19) . . ? C11 N1 C10 103.3(8) . . ? C10' N1 Co1 131.2(17) . . ? C11 N1 Co1 129.9(6) . . ? C10 N1 Co1 124.8(7) . . ? C13 C12 N3 112.3(7) . . ? C13 C12 H12A 109.1 . . ? N3 C12 H12A 109.1 . . ? C13 C12 H12B 109.1 . . ? N3 C12 H12B 109.1 . . ? H12A C12 H12B 107.9 . . ? N2 C10 N1 109.0(12) . . ? N1 C10' N2' 120(3) . . ? N1 C10' C11 47.1(12) . . ? N2' C10' C11 73(2) . . ? C10 N2 N3 104.5(11) . . ? N3 N2' C10' 97(3) . . ? N3 N2' C11 42.0(11) . . ? C10' N2' C11 61.7(18) . . ? C12 C13 C13 111.8(10) . 2_766 ? C12 C13 H13A 109.3 . . ? C13 C13 H13A 109.3 2_766 . ? C12 C13 H13B 109.3 . . ? C13 C13 H13B 109.3 2_766 . ? H13A C13 H13B 107.9 . . ? N1 C11 N3 115.6(8) . . ? N1 C11 C10' 40.2(11) . . ? N3 C11 C10' 79.8(12) . . ? N1 C11 N2' 85.1(12) . . ? N3 C11 N2' 39.9(11) . . ? C10' C11 N2' 45.0(13) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Co1 O1 C1 -35.8(5) . . . . ? O2W Co1 O1 C1 59.6(4) . . . . ? O4 Co1 O1 C1 150.2(4) 1_545 . . . ? O1W Co1 O1 C1 -122.8(4) . . . . ? O3 Co1 O1 C1 156.1(4) 1_545 . . . ? Co1 O4 C2 O3 2.3(6) 1_565 . . . ? Co1 O4 C2 C3 -177.4(5) 1_565 . . . ? Co1 O3 C2 O4 -2.3(5) 1_565 . . . ? Co1 O3 C2 C3 177.5(5) 1_565 . . . ? C8 C3 C2 O4 10.4(8) . . . . ? C4 C3 C2 O4 -170.9(5) . . . . ? C8 C3 C2 O3 -169.3(5) . . . . ? C4 C3 C2 O3 9.4(9) . . . . ? C4 C3 C8 C7 -1.5(9) . . . . ? C2 C3 C8 C7 177.2(5) . . . . ? C8 C3 C4 C5 0.5(9) . . . . ? C2 C3 C4 C5 -178.2(5) . . . . ? C6 C5 C4 C3 0.9(9) . . . . ? C1 C5 C4 C3 179.6(5) . . . . ? C9 O5 C7 C6 -3.0(10) . . . . ? C9 O5 C7 C8 177.3(6) . . . . ? C3 C8 C7 O5 -179.2(5) . . . . ? C3 C8 C7 C6 1.1(9) . . . . ? Co1 O1 C1 O2 -1.3(8) . . . . ? Co1 O1 C1 C5 178.0(4) . . . . ? C6 C5 C1 O2 -159.9(6) . . . . ? C4 C5 C1 O2 21.4(9) . . . . ? C6 C5 C1 O1 20.7(8) . . . . ? C4 C5 C1 O1 -157.9(5) . . . . ? O5 C7 C6 C5 -179.4(6) . . . . ? C8 C7 C6 C5 0.3(9) . . . . ? C4 C5 C6 C7 -1.3(9) . . . . ? C1 C5 C6 C7 -180.0(5) . . . . ? C7 O5 C9 C9 -176.1(6) . . . 2_575 ? O1 Co1 N1 C10' -139(3) . . . . ? O2W Co1 N1 C10' 125(3) . . . . ? O4 Co1 N1 C10' 26(3) 1_545 . . . ? O1W Co1 N1 C10' -53(3) . . . . ? O3 Co1 N1 C10' 35(3) 1_545 . . . ? O1 Co1 N1 C11 76.3(8) . . . . ? O2W Co1 N1 C11 -19.2(8) . . . . ? O4 Co1 N1 C11 -118.8(8) 1_545 . . . ? O1W Co1 N1 C11 163.0(8) . . . . ? O3 Co1 N1 C11 -109.0(8) 1_545 . . . ? O1 Co1 N1 C10 -84.7(9) . . . . ? O2W Co1 N1 C10 179.8(8) . . . . ? O4 Co1 N1 C10 80.2(10) 1_545 . . . ? O1W Co1 N1 C10 2.0(8) . . . . ? O3 Co1 N1 C10 90.0(9) 1_545 . . . ? N2' N3 C12 C13 160.8(19) . . . . ? C11 N3 C12 C13 -68.7(14) . . . . ? N2 N3 C12 C13 96.4(10) . . . . ? C10' N1 C10 N2 -73(3) . . . . ? C11 N1 C10 N2 6.2(14) . . . . ? Co1 N1 C10 N2 171.3(8) . . . . ? C11 N1 C10' N2' -5(4) . . . . ? C10 N1 C10' N2' 102(5) . . . . ? Co1 N1 C10' N2' -158(2) . . . . ? C10 N1 C10' C11 107(2) . . . . ? Co1 N1 C10' C11 -153(2) . . . . ? N1 C10 N2 N3 1.2(14) . . . . ? N2' N3 N2 C10 81(2) . . . . ? C11 N3 N2 C10 -8.2(13) . . . . ? C12 N3 N2 C10 -176.9(10) . . . . ? C11 N3 N2' C10' 32(3) . . . . ? N2 N3 N2' C10' -72(3) . . . . ? C12 N3 N2' C10' 178(2) . . . . ? N2 N3 N2' C11 -103.8(13) . . . . ? C12 N3 N2' C11 145.9(14) . . . . ? N1 C10' N2' N3 -20(5) . . . . ? C11 C10' N2' N3 -23.5(19) . . . . ? N1 C10' N2' C11 4(3) . . . . ? N3 C12 C13 C13 176.9(10) . . . 2_766 ? C10' N1 C11 N3 29(2) . . . . ? C10 N1 C11 N3 -12.5(13) . . . . ? Co1 N1 C11 N3 -176.5(6) . . . . ? C10 N1 C11 C10' -42.0(19) . . . . ? Co1 N1 C11 C10' 154(2) . . . . ? C10' N1 C11 N2' 3(2) . . . . ? C10 N1 C11 N2' -39.0(14) . . . . ? Co1 N1 C11 N2' 156.9(12) . . . . ? N2' N3 C11 N1 -44(2) . . . . ? N2 N3 C11 N1 13.5(12) . . . . ? C12 N3 C11 N1 -179.9(9) . . . . ? N2' N3 C11 C10' -25(2) . . . . ? N2 N3 C11 C10' 32.4(16) . . . . ? C12 N3 C11 C10' -161.0(17) . . . . ? N2 N3 C11 N2' 57.5(17) . . . . ? C12 N3 C11 N2' -136(2) . . . . ? N2' C10' C11 N1 176(4) . . . . ? N1 C10' C11 N3 -153(2) . . . . ? N2' C10' C11 N3 23(2) . . . . ? N1 C10' C11 N2' -176(4) . . . . ? N3 N2' C11 N1 141.1(17) . . . . ? C10' N2' C11 N1 -3(2) . . . . ? C10' N2' C11 N3 -144(3) . . . . ? N3 N2' C11 C10' 144(3) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.648 _refine_diff_density_min -0.513 _refine_diff_density_rms 0.094 #============================================================================= data_compound-10 _database_code_depnum_ccdc_archive 'CCDC 834807' #TrackingRef '- CIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H18 N6 O5, 0.5(H2 O)' _chemical_formula_sum 'C17 H18 N6 O5.50 Zn' _chemical_formula_weight 459.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 2/c' _symmetry_space_group_name_hall '-C 2yc' 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 21.092(5) _cell_length_b 15.132(5) _cell_length_c 12.318(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 100.208(5) _cell_angle_gamma 90.000(5) _cell_volume 3869(2) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 972 _cell_measurement_theta_min 3.1673 _cell_measurement_theta_max 29.0038 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.578 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1888 _exptl_absorpt_coefficient_mu 1.316 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.40566 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8500 _diffrn_reflns_av_R_equivalents 0.1154 _diffrn_reflns_av_sigmaI/netI 0.1697 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.17 _diffrn_reflns_theta_max 25.35 _reflns_number_total 3541 _reflns_number_gt 1628 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXS-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0283P)^2^+5.6095P] 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 3541 _refine_ls_number_parameters 271 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.2149 _refine_ls_R_factor_gt 0.0996 _refine_ls_wR_factor_ref 0.1817 _refine_ls_wR_factor_gt 0.1502 _refine_ls_goodness_of_fit_ref 1.144 _refine_ls_restrained_S_all 1.155 _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 0.63298(4) 0.20364(7) 0.54675(9) 0.0600(4) Uani 1 1 d . . . C6 C 0.8195(3) 0.0345(6) 0.5736(7) 0.058(3) Uani 1 1 d . . . H6 H 0.8092 0.0754 0.5169 0.069 Uiso 1 1 calc R . . O5 O 0.9185(3) 0.0150(4) 0.5145(5) 0.080(2) Uani 1 1 d . . . N3 N 0.4435(3) 0.1176(6) 0.5172(8) 0.076(3) Uani 1 1 d . . . C5 C 0.7771(3) 0.0186(6) 0.6429(7) 0.048(2) Uani 1 1 d . . . O2 O 0.6887(3) 0.0781(5) 0.7114(6) 0.089(2) Uani 1 1 d . . . O1 O 0.7020(2) 0.1183(4) 0.5470(6) 0.0686(19) Uani 1 1 d . . . C1 C 0.7164(4) 0.0725(6) 0.6337(9) 0.055(3) Uani 1 1 d . . . C7 C 0.8789(3) -0.0105(6) 0.5872(8) 0.057(3) Uani 1 1 d . . . C13 C 0.3329(4) 0.1665(7) 0.4523(8) 0.070(3) Uani 1 1 d . . . H13A H 0.2887 0.1550 0.4598 0.084 Uiso 1 1 calc R . . H13B H 0.3383 0.1467 0.3796 0.084 Uiso 1 1 calc R . . O3 O 0.8212(3) -0.1962(4) 0.8637(6) 0.080(2) Uani 1 1 d . . . N5 N 0.4102(3) 0.3219(6) 0.2706(7) 0.078(3) Uani 1 1 d . . . N4 N 0.3476(3) 0.2949(6) 0.2660(7) 0.071(2) Uani 1 1 d . . . C4 C 0.7911(3) -0.0471(6) 0.7218(7) 0.053(2) Uani 1 1 d . . . H4 H 0.7622 -0.0586 0.7690 0.063 Uiso 1 1 calc R . . N6 N 0.3712(3) 0.2536(5) 0.1082(6) 0.056(2) Uani 1 1 d . . . C3 C 0.8476(4) -0.0960(6) 0.7315(8) 0.057(3) Uani 1 1 d . . . C8 C 0.8921(4) -0.0751(6) 0.6655(8) 0.061(3) Uani 1 1 d . . . H8 H 0.9311 -0.1052 0.6744 0.073 Uiso 1 1 calc R . . N2 N 0.4576(4) 0.0810(6) 0.4223(9) 0.097(3) Uani 1 1 d . . . C2 C 0.8632(6) -0.1714(7) 0.8106(9) 0.080(3) Uani 1 1 d . . . N1 N 0.5442(3) 0.1500(5) 0.5199(7) 0.066(2) Uani 1 1 d . . . C12 C 0.3767(4) 0.1138(7) 0.5373(9) 0.085(3) Uani 1 1 d . . . H12A H 0.3750 0.1370 0.6101 0.102 Uiso 1 1 calc R . . H12B H 0.3624 0.0528 0.5348 0.102 Uiso 1 1 calc R . . C14 C 0.3449(4) 0.2637(7) 0.4609(8) 0.070(3) Uani 1 1 d . . . H14A H 0.3273 0.2867 0.5228 0.083 Uiso 1 1 calc R . . H14B H 0.3910 0.2742 0.4757 0.083 Uiso 1 1 calc R . . C11 C 0.4944(4) 0.1572(6) 0.5703(8) 0.067(3) Uani 1 1 d . . . H11 H 0.4954 0.1873 0.6364 0.081 Uiso 1 1 calc R . . O4 O 0.9154(4) -0.2092(5) 0.8182(7) 0.124(3) Uani 1 1 d . . . C10 C 0.5198(4) 0.1003(6) 0.4293(10) 0.080(3) Uani 1 1 d . . . H10 H 0.5443 0.0818 0.3777 0.095 Uiso 1 1 calc R . . C17 C 0.4217(4) 0.2973(7) 0.1751(9) 0.072(3) Uani 1 1 d . . . H17 H 0.4609 0.3081 0.1529 0.086 Uiso 1 1 calc R . . C9 C 0.9822(4) -0.0221(7) 0.5371(9) 0.086(3) Uani 1 1 d . . . H9A H 0.9807 -0.0853 0.5236 0.104 Uiso 1 1 calc R . . H9B H 1.0021 -0.0116 0.6132 0.104 Uiso 1 1 calc R . . C16 C 0.3278(4) 0.2548(6) 0.1706(9) 0.067(3) Uani 1 1 d . . . H16 H 0.2871 0.2300 0.1505 0.081 Uiso 1 1 calc R . . C15 C 0.3158(4) 0.3131(7) 0.3586(9) 0.085(3) Uani 1 1 d . . . H15A H 0.2707 0.2973 0.3389 0.102 Uiso 1 1 calc R . . H15B H 0.3182 0.3760 0.3740 0.102 Uiso 1 1 calc R . . O1W O 0.6238(8) 0.0505(13) 0.2919(15) 0.155(7) Uani 0.50 1 d PU . . 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 0.0382(5) 0.0658(8) 0.0715(8) -0.0045(7) -0.0027(4) 0.0009(6) C6 0.046(5) 0.064(7) 0.059(7) 0.006(5) 0.001(4) 0.001(5) O5 0.051(3) 0.100(6) 0.095(6) 0.017(4) 0.026(3) 0.024(4) N3 0.044(4) 0.083(7) 0.097(7) 0.003(6) -0.002(5) -0.011(4) C5 0.042(5) 0.049(6) 0.050(6) -0.001(5) -0.003(4) -0.004(4) O2 0.060(4) 0.111(6) 0.101(6) 0.012(5) 0.031(4) 0.020(4) O1 0.050(3) 0.071(5) 0.079(5) 0.007(4) -0.004(3) 0.027(3) C1 0.034(5) 0.058(7) 0.067(8) -0.006(6) -0.003(5) -0.004(5) C7 0.036(4) 0.067(7) 0.068(7) 0.001(6) 0.012(4) 0.007(5) C13 0.038(5) 0.089(8) 0.080(8) 0.006(6) -0.001(5) -0.010(5) O3 0.090(4) 0.057(5) 0.087(6) 0.007(4) 0.002(4) -0.019(4) N5 0.051(5) 0.099(8) 0.076(7) -0.002(6) -0.007(4) -0.001(4) N4 0.052(4) 0.091(6) 0.064(6) -0.002(5) -0.004(4) 0.019(5) C4 0.039(4) 0.050(6) 0.065(7) 0.002(5) -0.002(4) -0.003(4) N6 0.036(4) 0.068(5) 0.060(5) 0.010(4) -0.006(4) 0.008(4) C3 0.049(5) 0.052(7) 0.067(7) -0.008(6) -0.001(5) -0.016(5) C8 0.050(5) 0.041(6) 0.083(8) 0.003(6) -0.010(5) 0.009(5) N2 0.060(5) 0.106(8) 0.122(9) -0.013(7) 0.009(5) -0.001(5) C2 0.078(7) 0.071(9) 0.077(9) 0.001(7) -0.023(6) -0.017(7) N1 0.042(4) 0.070(6) 0.084(7) -0.002(5) 0.006(4) -0.006(4) C12 0.056(5) 0.093(9) 0.109(9) -0.005(7) 0.022(6) -0.026(6) C14 0.072(6) 0.074(8) 0.060(7) -0.003(6) 0.005(5) 0.007(6) C11 0.048(5) 0.081(8) 0.068(7) 0.007(6) -0.004(5) -0.004(5) O4 0.101(5) 0.111(7) 0.153(8) 0.059(6) -0.002(5) 0.039(5) C10 0.054(6) 0.064(8) 0.121(10) -0.021(7) 0.017(6) 0.005(5) C17 0.047(5) 0.094(8) 0.069(8) 0.003(7) -0.002(5) -0.015(6) C9 0.063(6) 0.089(8) 0.115(10) 0.018(7) 0.035(5) 0.006(6) C16 0.041(5) 0.080(8) 0.071(8) -0.002(6) -0.014(5) 0.013(5) C15 0.068(6) 0.090(9) 0.097(9) -0.009(7) 0.020(6) 0.028(6) O1W 0.181(10) 0.166(11) 0.137(10) 0.005(8) 0.079(8) 0.057(8) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O1 1.947(5) . ? Zn1 N1 2.014(7) . ? Zn1 O3 2.017(6) 4_656 ? Zn1 N6 2.040(7) 2_655 ? Zn1 O4 2.480(8) 4_656 ? Zn1 C2 2.573(12) 4_656 ? C6 C5 1.364(10) . ? C6 C7 1.409(10) . ? C6 H6 0.9300 . ? O5 C7 1.382(9) . ? O5 C9 1.438(9) . ? N3 C11 1.300(10) . ? N3 N2 1.373(10) . ? N3 C12 1.473(10) . ? C5 C4 1.385(10) . ? C5 C1 1.504(11) . ? O2 C1 1.209(10) . ? O1 C1 1.264(10) . ? C7 C8 1.367(11) . ? C13 C12 1.497(12) . ? C13 C14 1.494(12) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? O3 C2 1.249(11) . ? O3 Zn1 2.017(6) 4_646 ? N5 C17 1.296(11) . ? N5 N4 1.374(9) . ? N4 C16 1.322(11) . ? N4 C15 1.449(11) . ? C4 C3 1.390(10) . ? C4 H4 0.9300 . ? N6 C16 1.296(10) . ? N6 C17 1.392(10) . ? N6 Zn1 2.040(7) 2_655 ? C3 C8 1.382(11) . ? C3 C2 1.499(13) . ? C8 H8 0.9300 . ? N2 C10 1.331(10) . ? C2 O4 1.230(11) . ? C2 Zn1 2.573(12) 4_646 ? N1 C11 1.316(9) . ? N1 C10 1.369(11) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C14 C15 1.499(12) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C11 H11 0.9300 . ? O4 Zn1 2.480(8) 4_646 ? C10 H10 0.9300 . ? C17 H17 0.9300 . ? C9 C9 1.445(16) 5_756 ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C16 H16 0.9300 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn1 N1 114.0(3) . . ? O1 Zn1 O3 102.2(3) . 4_656 ? N1 Zn1 O3 137.2(3) . 4_656 ? O1 Zn1 N6 99.0(3) . 2_655 ? N1 Zn1 N6 96.4(3) . 2_655 ? O3 Zn1 N6 99.8(3) 4_656 2_655 ? O1 Zn1 O4 138.5(3) . 4_656 ? N1 Zn1 O4 81.0(3) . 4_656 ? O3 Zn1 O4 56.5(2) 4_656 4_656 ? N6 Zn1 O4 118.4(3) 2_655 4_656 ? O1 Zn1 C2 123.6(3) . 4_656 ? N1 Zn1 C2 108.9(4) . 4_656 ? O3 Zn1 C2 28.4(3) 4_656 4_656 ? N6 Zn1 C2 110.9(3) 2_655 4_656 ? O4 Zn1 C2 28.1(3) 4_656 4_656 ? C5 C6 C7 120.6(9) . . ? C5 C6 H6 119.7 . . ? C7 C6 H6 119.7 . . ? C7 O5 C9 114.6(7) . . ? C11 N3 N2 109.2(8) . . ? C11 N3 C12 131.4(10) . . ? N2 N3 C12 119.1(8) . . ? C6 C5 C4 119.0(8) . . ? C6 C5 C1 120.1(9) . . ? C4 C5 C1 121.0(8) . . ? C1 O1 Zn1 115.6(6) . . ? O2 C1 O1 123.6(9) . . ? O2 C1 C5 120.1(10) . . ? O1 C1 C5 115.7(9) . . ? C8 C7 O5 125.9(8) . . ? C8 C7 C6 119.6(8) . . ? O5 C7 C6 114.4(9) . . ? C12 C13 C14 113.6(8) . . ? C12 C13 H13A 108.9 . . ? C14 C13 H13A 108.9 . . ? C12 C13 H13B 108.9 . . ? C14 C13 H13B 108.9 . . ? H13A C13 H13B 107.7 . . ? C2 O3 Zn1 101.4(7) . 4_646 ? C17 N5 N4 102.1(8) . . ? C16 N4 N5 108.8(8) . . ? C16 N4 C15 132.1(8) . . ? N5 N4 C15 119.1(9) . . ? C3 C4 C5 121.0(8) . . ? C3 C4 H4 119.5 . . ? C5 C4 H4 119.5 . . ? C16 N6 C17 100.8(8) . . ? C16 N6 Zn1 130.0(6) . 2_655 ? C17 N6 Zn1 129.2(6) . 2_655 ? C4 C3 C8 119.2(9) . . ? C4 C3 C2 123.2(9) . . ? C8 C3 C2 117.5(9) . . ? C7 C8 C3 120.3(8) . . ? C7 C8 H8 119.9 . . ? C3 C8 H8 119.9 . . ? C10 N2 N3 102.5(9) . . ? O4 C2 O3 122.0(11) . . ? O4 C2 C3 119.6(11) . . ? O3 C2 C3 118.3(10) . . ? O4 C2 Zn1 71.8(7) . 4_646 ? O3 C2 Zn1 50.2(5) . 4_646 ? C3 C2 Zn1 168.6(8) . 4_646 ? C11 N1 C10 102.4(7) . . ? C11 N1 Zn1 133.3(7) . . ? C10 N1 Zn1 124.0(6) . . ? N3 C12 C13 110.6(8) . . ? N3 C12 H12A 109.5 . . ? C13 C12 H12A 109.5 . . ? N3 C12 H12B 109.5 . . ? C13 C12 H12B 109.5 . . ? H12A C12 H12B 108.1 . . ? C15 C14 C13 113.1(8) . . ? C15 C14 H14A 109.0 . . ? C13 C14 H14A 109.0 . . ? C15 C14 H14B 109.0 . . ? C13 C14 H14B 109.0 . . ? H14A C14 H14B 107.8 . . ? N3 C11 N1 112.4(9) . . ? N3 C11 H11 123.8 . . ? N1 C11 H11 123.8 . . ? C2 O4 Zn1 80.1(7) . 4_646 ? N2 C10 N1 113.4(9) . . ? N2 C10 H10 123.3 . . ? N1 C10 H10 123.3 . . ? N5 C17 N6 115.3(8) . . ? N5 C17 H17 122.3 . . ? N6 C17 H17 122.3 . . ? O5 C9 C9 105.7(10) . 5_756 ? O5 C9 H9A 110.6 . . ? C9 C9 H9A 110.6 5_756 . ? O5 C9 H9B 110.6 . . ? C9 C9 H9B 110.6 5_756 . ? H9A C9 H9B 108.7 . . ? N6 C16 N4 112.9(8) . . ? N6 C16 H16 123.5 . . ? N4 C16 H16 123.5 . . ? N4 C15 C14 112.9(7) . . ? N4 C15 H15A 109.0 . . ? C14 C15 H15A 109.0 . . ? N4 C15 H15B 109.0 . . ? C14 C15 H15B 109.0 . . ? H15A C15 H15B 107.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C7 C6 C5 C4 -4.7(12) . . . . ? C7 C6 C5 C1 174.8(7) . . . . ? N1 Zn1 O1 C1 -77.3(6) . . . . ? O3 Zn1 O1 C1 79.4(6) 4_656 . . . ? N6 Zn1 O1 C1 -178.5(6) 2_655 . . . ? O4 Zn1 O1 C1 26.8(8) 4_656 . . . ? C2 Zn1 O1 C1 58.9(7) 4_656 . . . ? Zn1 O1 C1 O2 2.1(11) . . . . ? Zn1 O1 C1 C5 -169.4(5) . . . . ? C6 C5 C1 O2 -158.1(8) . . . . ? C4 C5 C1 O2 21.4(12) . . . . ? C6 C5 C1 O1 13.7(11) . . . . ? C4 C5 C1 O1 -166.9(8) . . . . ? C9 O5 C7 C8 -9.7(13) . . . . ? C9 O5 C7 C6 172.3(8) . . . . ? C5 C6 C7 C8 4.7(13) . . . . ? C5 C6 C7 O5 -177.1(7) . . . . ? C17 N5 N4 C16 1.7(11) . . . . ? C17 N5 N4 C15 -178.3(9) . . . . ? C6 C5 C4 C3 0.5(12) . . . . ? C1 C5 C4 C3 -179.0(7) . . . . ? C5 C4 C3 C8 3.8(12) . . . . ? C5 C4 C3 C2 -176.1(8) . . . . ? O5 C7 C8 C3 -178.3(8) . . . . ? C6 C7 C8 C3 -0.4(13) . . . . ? C4 C3 C8 C7 -3.8(13) . . . . ? C2 C3 C8 C7 176.1(8) . . . . ? C11 N3 N2 C10 2.3(11) . . . . ? C12 N3 N2 C10 177.0(8) . . . . ? Zn1 O3 C2 O4 2.6(12) 4_646 . . . ? Zn1 O3 C2 C3 179.8(7) 4_646 . . . ? C4 C3 C2 O4 -176.7(9) . . . . ? C8 C3 C2 O4 3.4(14) . . . . ? C4 C3 C2 O3 6.1(14) . . . . ? C8 C3 C2 O3 -173.8(8) . . . . ? C4 C3 C2 Zn1 7(4) . . . 4_646 ? C8 C3 C2 Zn1 -173(3) . . . 4_646 ? O1 Zn1 N1 C11 130.9(8) . . . . ? O3 Zn1 N1 C11 -14.5(10) 4_656 . . . ? N6 Zn1 N1 C11 -126.3(8) 2_655 . . . ? O4 Zn1 N1 C11 -8.5(8) 4_656 . . . ? C2 Zn1 N1 C11 -11.6(9) 4_656 . . . ? O1 Zn1 N1 C10 -56.5(8) . . . . ? O3 Zn1 N1 C10 158.2(7) 4_656 . . . ? N6 Zn1 N1 C10 46.3(8) 2_655 . . . ? O4 Zn1 N1 C10 164.1(8) 4_656 . . . ? C2 Zn1 N1 C10 161.1(7) 4_656 . . . ? C11 N3 C12 C13 108.7(12) . . . . ? N2 N3 C12 C13 -64.6(12) . . . . ? C14 C13 C12 N3 -68.0(11) . . . . ? C12 C13 C14 C15 162.9(8) . . . . ? N2 N3 C11 N1 -0.9(11) . . . . ? C12 N3 C11 N1 -174.8(9) . . . . ? C10 N1 C11 N3 -0.8(11) . . . . ? Zn1 N1 C11 N3 173.0(6) . . . . ? O3 C2 O4 Zn1 -2.1(10) . . . 4_646 ? C3 C2 O4 Zn1 -179.2(9) . . . 4_646 ? N3 N2 C10 N1 -2.9(12) . . . . ? C11 N1 C10 N2 2.4(11) . . . . ? Zn1 N1 C10 N2 -172.2(7) . . . . ? N4 N5 C17 N6 -1.5(12) . . . . ? C16 N6 C17 N5 0.8(11) . . . . ? Zn1 N6 C17 N5 179.9(6) 2_655 . . . ? C7 O5 C9 C9 -172.0(10) . . . 5_756 ? C17 N6 C16 N4 0.5(10) . . . . ? Zn1 N6 C16 N4 -178.7(6) 2_655 . . . ? N5 N4 C16 N6 -1.4(11) . . . . ? C15 N4 C16 N6 178.6(9) . . . . ? C16 N4 C15 C14 113.7(11) . . . . ? N5 N4 C15 C14 -66.3(11) . . . . ? C13 C14 C15 N4 -69.3(10) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.865 _refine_diff_density_min -0.430 _refine_diff_density_rms 0.086 #=========================END