# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Rong Cao' _publ_contact_author_address ; State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter Chinese Academy of Sciences Fuzhou, Fujian, 350002, China ; _publ_contact_author_email rcao@fjirsm.ac.cn _publ_contact_author_fax +86-591-83796710 _publ_contact_author_phone +86-591-83796710 _publ_contact_letter ; Dear Sir, Please consider this CIF submission for publication in Dalton Transactions. All authors have seen and approved this submission. Best wishes Rong Cao ; _publ_section_title ; Synthesis, structural characterization and anion-sensing studies of metal(II) complexes based on 3, 3', 4, 4'-oxydiphthalate and N-donor ligands ; loop_ _publ_author_name 'Yun Gong' 'Rong Cao' # Attachment '- Dalton Trans-gy.cif' data_090925 _database_code_depnum_ccdc_archive 'CCDC 749220' #TrackingRef '- Dalton Trans-gy.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C80 H52 Cu4 N8 O31' _chemical_formula_weight 1875.46 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 '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 2(1)/n' 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 13.287(4) _cell_length_b 18.455(5) _cell_length_c 16.997(5) _cell_angle_alpha 90.00 _cell_angle_beta 103.840(4) _cell_angle_gamma 90.00 _cell_volume 4046.9(18) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9103 _cell_measurement_theta_min 3.1033 _cell_measurement_theta_max 27.4835 _exptl_crystal_description Prism _exptl_crystal_colour Blue _exptl_crystal_size_max 0.3500 _exptl_crystal_size_mid 0.2000 _exptl_crystal_size_min 0.1500 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.539 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1904 _exptl_absorpt_coefficient_mu 1.129 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8332 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 'Rigaku Mercury 70 diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31126 _diffrn_reflns_av_R_equivalents 0.0358 _diffrn_reflns_av_sigmaI/netI 0.0396 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 27.48 _reflns_number_total 9216 _reflns_number_gt 7584 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+5.4885P] 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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9216 _refine_ls_number_parameters 562 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0753 _refine_ls_R_factor_gt 0.0605 _refine_ls_wR_factor_ref 0.1716 _refine_ls_wR_factor_gt 0.1604 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.098 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.12997(3) 0.75466(2) 0.23873(3) 0.02617(13) Uani 1 1 d . . . Cu3 Cu 0.0000 0.0000 0.5000 0.0499(2) Uani 1 2 d S . . O1 O 0.17377(19) 0.69693(12) 0.33877(15) 0.0320(5) Uani 1 1 d . . . N4 N 0.2793(2) 0.76401(15) 0.23364(19) 0.0277(6) Uani 1 1 d . . . O2 O 0.1674(2) 0.61666(14) 0.24098(16) 0.0379(6) Uani 1 1 d . . . N3 N 0.0792(2) 0.80120(16) 0.12843(18) 0.0310(6) Uani 1 1 d . . . O5 O 0.2181(3) 0.42087(15) 0.55961(18) 0.0527(8) Uani 1 1 d . . . O4 O 0.1937(2) 0.45246(15) 0.23132(17) 0.0446(7) Uani 1 1 d . . . O9 O 0.0615(3) 0.09568(14) 0.51635(18) 0.0465(7) Uani 1 1 d . . . C1 C 0.1871(3) 0.57320(17) 0.3761(2) 0.0283(7) Uani 1 1 d . . . C21 C 0.0707(3) 0.9019(2) 0.0395(2) 0.0384(8) Uani 1 1 d . . . H21 H 0.0915 0.9489 0.0314 0.046 Uiso 1 1 calc R . . O3 O 0.0333(2) 0.48538(19) 0.23565(18) 0.0505(7) Uani 1 1 d . . . C11 C 0.1814(3) 0.22357(19) 0.5485(2) 0.0323(7) Uani 1 1 d . . . C28 C 0.6010(3) 0.7654(2) 0.2404(3) 0.0423(9) Uani 1 1 d . . . H28 H 0.6389 0.8034 0.2689 0.051 Uiso 1 1 calc R . . C37 C 0.1760(2) 0.63185(18) 0.3137(2) 0.0285(7) Uani 1 1 d . . . C2 C 0.1645(3) 0.50090(17) 0.3539(2) 0.0293(7) Uani 1 1 d . . . C3 C 0.1703(3) 0.44892(19) 0.4145(2) 0.0360(8) Uani 1 1 d . . . H3 H 0.1537 0.4009 0.4008 0.043 Uiso 1 1 calc R . . C10 C 0.0759(3) 0.21987(19) 0.5459(2) 0.0340(8) Uani 1 1 d . . . C18 C 0.0120(3) 0.7667(2) 0.0689(2) 0.0408(9) Uani 1 1 d . . . H18 H -0.0085 0.7201 0.0788 0.049 Uiso 1 1 calc R . . C5 C 0.2231(3) 0.54064(19) 0.5171(2) 0.0379(8) Uani 1 1 d . . . H5 H 0.2430 0.5537 0.5715 0.045 Uiso 1 1 calc R . . C23 C 0.3487(3) 0.7922(2) 0.2960(2) 0.0332(8) Uani 1 1 d . . . H23 H 0.3257 0.8108 0.3394 0.040 Uiso 1 1 calc R . . C20 C 0.0032(3) 0.8654(2) -0.0230(2) 0.0345(8) Uani 1 1 d . . . C38 C 0.0168(3) 0.1498(2) 0.5376(2) 0.0384(8) Uani 1 1 d . . . C26 C 0.4165(3) 0.7355(2) 0.1717(2) 0.0395(9) Uani 1 1 d . . . H26 H 0.4375 0.7148 0.1283 0.047 Uiso 1 1 calc R . . C39 C 0.1279(3) 0.4780(2) 0.2660(2) 0.0343(8) Uani 1 1 d . . . C25 C 0.4888(3) 0.7646(2) 0.2357(3) 0.0362(8) Uani 1 1 d . . . C27 C 0.3131(3) 0.7371(2) 0.1722(2) 0.0371(8) Uani 1 1 d . . . H27 H 0.2650 0.7186 0.1277 0.045 Uiso 1 1 calc R . . O6 O 0.2786(3) 0.12142(19) 0.6102(2) 0.0671(10) Uani 1 1 d . . . C6 C 0.2153(3) 0.59173(19) 0.4577(2) 0.0359(8) Uani 1 1 d . . . H6 H 0.2292 0.6400 0.4722 0.043 Uiso 1 1 calc R . . O8 O -0.0707(3) 0.14833(19) 0.5521(3) 0.0703(10) Uani 1 1 d . . . C24 C 0.4525(3) 0.7949(2) 0.2987(3) 0.0373(8) Uani 1 1 d . . . H24 H 0.4983 0.8168 0.3422 0.045 Uiso 1 1 calc R . . O10 O 0.1368(2) 0.86558(15) 0.30591(19) 0.0452(7) Uani 1 1 d . . . C8 C 0.0645(4) 0.3507(2) 0.5474(3) 0.0481(10) Uani 1 1 d . . . H8 H 0.0259 0.3928 0.5470 0.058 Uiso 1 1 calc R . . O7 O 0.2794(3) 0.1494(2) 0.4835(2) 0.0804(13) Uani 1 1 d . . . C12 C 0.2269(3) 0.2923(2) 0.5512(2) 0.0376(8) Uani 1 1 d . . . H12 H 0.2973 0.2967 0.5537 0.045 Uiso 1 1 calc R . . C40 C 0.2516(3) 0.1585(2) 0.5481(3) 0.0421(9) Uani 1 1 d . . . C7 C 0.1671(3) 0.35328(19) 0.5501(2) 0.0378(9) Uani 1 1 d . . . C4 C 0.2010(3) 0.4691(2) 0.4951(2) 0.0356(8) Uani 1 1 d . . . C22 C 0.1068(3) 0.8687(2) 0.1132(2) 0.0360(8) Uani 1 1 d . . . H22 H 0.1520 0.8940 0.1542 0.043 Uiso 1 1 calc R . . C19 C -0.0280(3) 0.7966(2) -0.0057(2) 0.0456(10) Uani 1 1 d . . . H19 H -0.0758 0.7710 -0.0447 0.055 Uiso 1 1 calc R . . C9 C 0.0191(3) 0.2830(2) 0.5454(3) 0.0454(10) Uani 1 1 d . . . H9 H -0.0512 0.2798 0.5438 0.054 Uiso 1 1 calc R . . C30 C -0.0281(3) 0.8932(2) -0.1063(2) 0.0403(9) Uani 1 1 d . . . H30 H -0.0888 0.8756 -0.1401 0.048 Uiso 1 1 calc R . . Cu2 Cu 0.5000 1.0000 0.5000 0.04095(19) Uani 1 2 d S . . O13 O 0.5840(3) 0.98253(18) 0.41292(18) 0.0537(8) Uani 1 1 d . . . O12 O 0.5755(2) 0.91390(17) 0.57279(18) 0.0483(7) Uani 1 1 d . . . O11 O 0.3818(3) 0.9292(2) 0.4333(2) 0.0739(11) Uani 1 1 d . . . C29 C 0.6525(3) 0.7181(3) 0.2086(3) 0.0496(11) Uani 1 1 d . . . H29 H 0.6171 0.6794 0.1794 0.059 Uiso 1 1 calc R . . O15 O 0.8345(4) 0.4580(3) 0.2695(4) 0.1114(18) Uani 1 1 d . . . O14 O 0.2039(5) -0.0465(4) 0.5313(5) 0.159(3) Uani 1 1 d . . . O16 O 0.7256(6) 0.1956(6) 0.5134(6) 0.103(3) Uani 0.50 1 d P . . N2 N 0.9791(2) 0.73761(16) 0.23756(19) 0.0324(6) Uani 1 1 d . . . C14 C 0.8273(3) 0.6639(2) 0.2189(3) 0.0478(10) Uani 1 1 d . . . H14 H 0.7980 0.6178 0.2125 0.057 Uiso 1 1 calc R . . C15 C 0.7653(3) 0.7241(2) 0.2177(3) 0.0415(9) Uani 1 1 d . . . C17 C 0.9187(3) 0.7957(2) 0.2367(3) 0.0401(9) Uani 1 1 d . . . H17 H 0.9494 0.8413 0.2428 0.048 Uiso 1 1 calc R . . C16 C 0.8137(3) 0.7910(2) 0.2273(3) 0.0467(10) Uani 1 1 d . . . H16 H 0.7748 0.8329 0.2273 0.056 Uiso 1 1 calc R . . C13 C 0.9336(3) 0.6723(2) 0.2299(3) 0.0401(9) Uani 1 1 d . . . H13 H 0.9747 0.6312 0.2320 0.048 Uiso 1 1 calc R . . N1 N -0.0013(3) 0.99056(17) -0.3836(2) 0.0400(8) Uani 1 1 d . . . C33 C -0.0806(3) 0.9482(2) -0.2800(2) 0.0395(8) Uani 1 1 d . . . H33 H -0.1387 0.9297 -0.2655 0.047 Uiso 1 1 calc R . . C32 C -0.0825(3) 0.9618(2) -0.3600(2) 0.0411(9) Uani 1 1 d . . . H32 H -0.1422 0.9507 -0.3993 0.049 Uiso 1 1 calc R . . C31 C 0.0256(3) 0.9418(2) -0.1353(2) 0.0426(9) Uani 1 1 d . . . H31 H 0.0784 0.9653 -0.0981 0.051 Uiso 1 1 calc R . . C36 C 0.0832(4) 1.0081(2) -0.3265(3) 0.0447(10) Uani 1 1 d . . . H36 H 0.1382 1.0303 -0.3420 0.054 Uiso 1 1 calc R . . C34 C 0.0103(3) 0.9627(2) -0.2211(2) 0.0390(9) Uani 1 1 d . . . C35 C 0.0918(3) 0.9946(2) -0.2458(3) 0.0450(10) Uani 1 1 d . . . H35 H 0.1522 1.0068 -0.2079 0.054 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0187(2) 0.0299(2) 0.0305(3) 0.00756(16) 0.00710(16) 0.00133(14) Cu3 0.0964(6) 0.0290(3) 0.0291(4) -0.0026(3) 0.0246(4) -0.0206(3) O1 0.0342(12) 0.0269(11) 0.0355(14) 0.0049(10) 0.0098(11) 0.0010(10) N4 0.0199(12) 0.0303(13) 0.0336(16) 0.0047(12) 0.0075(11) -0.0004(10) O2 0.0474(15) 0.0368(13) 0.0301(15) 0.0033(11) 0.0107(11) -0.0015(11) N3 0.0253(13) 0.0379(15) 0.0306(16) 0.0088(13) 0.0083(12) 0.0023(12) O5 0.077(2) 0.0326(14) 0.0392(17) 0.0108(12) -0.0043(15) -0.0159(14) O4 0.0516(16) 0.0441(15) 0.0385(16) -0.0076(12) 0.0115(13) 0.0081(13) O9 0.071(2) 0.0317(13) 0.0450(17) -0.0073(12) 0.0293(15) -0.0127(13) C1 0.0284(16) 0.0253(15) 0.0301(19) 0.0022(13) 0.0047(14) 0.0015(12) C21 0.044(2) 0.0353(18) 0.036(2) 0.0071(16) 0.0114(17) -0.0032(16) O3 0.0359(15) 0.076(2) 0.0363(17) -0.0053(15) 0.0024(12) -0.0057(14) C11 0.0396(19) 0.0308(16) 0.0271(19) 0.0042(14) 0.0092(15) -0.0012(14) C28 0.0234(17) 0.058(2) 0.047(2) -0.0013(19) 0.0105(16) -0.0052(16) C37 0.0208(14) 0.0316(16) 0.033(2) 0.0048(14) 0.0068(13) 0.0010(12) C2 0.0275(16) 0.0288(16) 0.0309(19) 0.0019(14) 0.0058(14) 0.0016(12) C3 0.046(2) 0.0256(16) 0.034(2) 0.0023(15) 0.0052(16) -0.0027(14) C10 0.0397(19) 0.0278(16) 0.037(2) 0.0050(15) 0.0130(16) -0.0034(14) C18 0.049(2) 0.0392(19) 0.035(2) 0.0047(17) 0.0096(18) -0.0070(17) C5 0.051(2) 0.0305(17) 0.028(2) -0.0002(15) 0.0008(17) -0.0014(16) C23 0.0248(16) 0.0384(18) 0.037(2) -0.0008(16) 0.0080(14) -0.0004(14) C20 0.0354(18) 0.0415(19) 0.0274(19) 0.0068(16) 0.0090(15) 0.0048(15) C38 0.044(2) 0.0371(19) 0.035(2) 0.0035(16) 0.0110(17) -0.0078(16) C26 0.0269(17) 0.057(2) 0.036(2) -0.0068(18) 0.0101(16) -0.0009(16) C39 0.041(2) 0.0323(17) 0.030(2) -0.0006(15) 0.0080(16) -0.0052(15) C25 0.0231(16) 0.0422(19) 0.045(2) 0.0003(17) 0.0117(15) -0.0015(14) C27 0.0251(17) 0.047(2) 0.039(2) -0.0044(17) 0.0075(15) -0.0024(15) O6 0.086(3) 0.062(2) 0.046(2) 0.0067(17) 0.0013(17) 0.0328(19) C6 0.043(2) 0.0262(16) 0.034(2) 0.0014(15) 0.0000(16) 0.0001(14) O8 0.0509(19) 0.061(2) 0.106(3) 0.002(2) 0.033(2) -0.0157(16) C24 0.0243(16) 0.0406(19) 0.045(2) -0.0075(17) 0.0044(15) -0.0030(14) O10 0.0411(15) 0.0405(14) 0.0556(19) -0.0080(13) 0.0149(13) -0.0025(12) C8 0.057(3) 0.0314(19) 0.057(3) 0.0041(18) 0.016(2) 0.0066(17) O7 0.096(3) 0.088(3) 0.072(3) 0.021(2) 0.050(2) 0.048(2) C12 0.0362(19) 0.043(2) 0.034(2) 0.0047(16) 0.0092(16) -0.0068(16) C40 0.039(2) 0.041(2) 0.045(2) 0.0026(18) 0.0071(18) 0.0083(16) C7 0.056(2) 0.0263(16) 0.030(2) 0.0064(14) 0.0098(17) -0.0054(15) C4 0.0386(19) 0.0318(17) 0.034(2) 0.0101(15) 0.0038(16) -0.0013(15) C22 0.0335(18) 0.0414(19) 0.033(2) 0.0065(16) 0.0074(15) -0.0058(15) C19 0.050(2) 0.052(2) 0.030(2) 0.0016(18) 0.0016(18) -0.0121(19) C9 0.041(2) 0.0362(19) 0.061(3) 0.0035(19) 0.017(2) 0.0032(16) C30 0.043(2) 0.048(2) 0.029(2) 0.0068(17) 0.0058(16) 0.0042(17) Cu2 0.0452(4) 0.0408(4) 0.0354(4) -0.0018(3) 0.0070(3) 0.0009(3) O13 0.061(2) 0.0637(19) 0.0359(17) 0.0002(15) 0.0108(14) 0.0200(16) O12 0.0552(18) 0.0520(17) 0.0372(17) 0.0041(13) 0.0102(13) 0.0119(14) O11 0.101(3) 0.066(2) 0.045(2) -0.0050(17) -0.0006(19) -0.034(2) C29 0.0225(17) 0.054(2) 0.073(3) -0.005(2) 0.0128(19) -0.0032(16) O15 0.083(3) 0.133(5) 0.137(5) -0.001(4) 0.063(3) 0.005(3) O14 0.125(5) 0.142(6) 0.172(7) 0.011(5) -0.040(5) -0.034(4) O16 0.058(5) 0.138(9) 0.117(8) 0.061(7) 0.030(5) 0.025(5) N2 0.0206(13) 0.0407(16) 0.0365(17) 0.0087(13) 0.0083(12) 0.0001(11) C14 0.0296(19) 0.044(2) 0.072(3) -0.002(2) 0.017(2) -0.0047(16) C15 0.0224(17) 0.050(2) 0.055(3) 0.0009(19) 0.0137(17) 0.0000(15) C17 0.0281(17) 0.0380(19) 0.057(3) 0.0024(18) 0.0150(17) -0.0005(15) C16 0.0291(19) 0.046(2) 0.068(3) 0.001(2) 0.0186(19) 0.0045(16) C13 0.0287(18) 0.0360(18) 0.058(3) 0.0063(18) 0.0147(17) 0.0026(14) N1 0.058(2) 0.0337(16) 0.0291(18) 0.0002(13) 0.0130(15) -0.0109(14) C33 0.042(2) 0.042(2) 0.036(2) 0.0045(17) 0.0100(17) -0.0025(16) C32 0.050(2) 0.039(2) 0.033(2) 0.0049(16) 0.0068(17) -0.0047(17) C31 0.042(2) 0.055(2) 0.029(2) 0.0045(18) 0.0052(16) -0.0008(18) C36 0.053(2) 0.046(2) 0.037(2) 0.0039(18) 0.0156(19) -0.0119(18) C34 0.049(2) 0.0392(19) 0.030(2) 0.0082(16) 0.0112(17) 0.0042(16) C35 0.043(2) 0.054(2) 0.036(2) 0.0044(18) 0.0040(18) -0.0085(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1 1.973(2) . ? Cu1 N4 2.013(3) . ? Cu1 N2 2.024(3) 1_455 ? Cu1 N3 2.026(3) . ? Cu1 O10 2.335(3) . ? Cu3 O9 1.938(3) 3_556 ? Cu3 O9 1.938(3) . ? Cu3 N1 1.990(3) 3_565 ? Cu3 N1 1.990(3) 1_546 ? O1 C37 1.277(4) . ? N4 C27 1.329(5) . ? N4 C23 1.333(5) . ? O2 C37 1.246(4) . ? N3 C18 1.339(5) . ? N3 C22 1.341(5) . ? O5 C4 1.388(4) . ? O5 C7 1.410(4) . ? O4 C39 1.258(5) . ? O9 C38 1.258(5) . ? C1 C6 1.390(5) . ? C1 C2 1.400(5) . ? C1 C37 1.498(5) . ? C21 C22 1.375(5) . ? C21 C20 1.390(6) . ? C21 H21 0.9300 . ? O3 C39 1.247(5) . ? C11 C10 1.393(5) . ? C11 C12 1.401(5) . ? C11 C40 1.522(5) . ? C28 C29 1.303(6) . ? C28 C25 1.474(5) . ? C28 H28 0.9300 . ? C2 C3 1.397(5) . ? C2 C39 1.516(5) . ? C3 C4 1.383(6) . ? C3 H3 0.9300 . ? C10 C9 1.387(5) . ? C10 C38 1.503(5) . ? C18 C19 1.369(6) . ? C18 H18 0.9300 . ? C5 C6 1.368(5) . ? C5 C4 1.385(5) . ? C5 H5 0.9300 . ? C23 C24 1.370(5) . ? C23 H23 0.9300 . ? C20 C19 1.388(6) . ? C20 C30 1.470(5) . ? C38 O8 1.245(5) . ? C26 C27 1.377(5) . ? C26 C25 1.377(6) . ? C26 H26 0.9300 . ? C25 C24 1.392(5) . ? C27 H27 0.9300 . ? O6 C40 1.237(5) . ? C6 H6 0.9300 . ? C24 H24 0.9300 . ? C8 C7 1.355(6) . ? C8 C9 1.383(6) . ? C8 H8 0.9300 . ? O7 C40 1.251(5) . ? C12 C7 1.375(6) . ? C12 H12 0.9300 . ? C22 H22 0.9300 . ? C19 H19 0.9300 . ? C9 H9 0.9300 . ? C30 C31 1.314(6) . ? C30 H30 0.9300 . ? Cu2 O13 2.081(3) . ? Cu2 O13 2.081(3) 3_676 ? Cu2 O12 2.114(3) . ? Cu2 O12 2.114(3) 3_676 ? Cu2 O11 2.146(3) . ? Cu2 O11 2.146(3) 3_676 ? C29 C15 1.473(5) . ? C29 H29 0.9300 . ? N2 C17 1.338(5) . ? N2 C13 1.341(5) . ? N2 Cu1 2.024(3) 1_655 ? C14 C15 1.382(6) . ? C14 C13 1.389(5) . ? C14 H14 0.9300 . ? C15 C16 1.384(6) . ? C17 C16 1.368(5) . ? C17 H17 0.9300 . ? C16 H16 0.9300 . ? C13 H13 0.9300 . ? N1 C36 1.336(6) . ? N1 C32 1.347(5) . ? N1 Cu3 1.990(3) 1_564 ? C33 C32 1.377(6) . ? C33 C34 1.399(6) . ? C33 H33 0.9300 . ? C32 H32 0.9300 . ? C31 C34 1.475(5) . ? C31 H31 0.9300 . ? C36 C35 1.370(6) . ? C36 H36 0.9300 . ? C34 C35 1.383(6) . ? C35 H35 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu1 N4 89.59(11) . . ? O1 Cu1 N2 90.68(11) . 1_455 ? N4 Cu1 N2 175.02(13) . 1_455 ? O1 Cu1 N3 172.35(11) . . ? N4 Cu1 N3 92.15(11) . . ? N2 Cu1 N3 86.95(12) 1_455 . ? O1 Cu1 O10 94.76(11) . . ? N4 Cu1 O10 91.27(11) . . ? N2 Cu1 O10 93.66(11) 1_455 . ? N3 Cu1 O10 92.65(12) . . ? O9 Cu3 O9 180.00(6) 3_556 . ? O9 Cu3 N1 92.34(12) 3_556 3_565 ? O9 Cu3 N1 87.66(12) . 3_565 ? O9 Cu3 N1 87.66(12) 3_556 1_546 ? O9 Cu3 N1 92.34(12) . 1_546 ? N1 Cu3 N1 180.000(1) 3_565 1_546 ? C37 O1 Cu1 104.2(2) . . ? C27 N4 C23 118.1(3) . . ? C27 N4 Cu1 121.6(2) . . ? C23 N4 Cu1 120.1(2) . . ? C18 N3 C22 117.4(3) . . ? C18 N3 Cu1 120.8(2) . . ? C22 N3 Cu1 121.8(3) . . ? C4 O5 C7 119.5(3) . . ? C38 O9 Cu3 123.5(3) . . ? C6 C1 C2 119.6(3) . . ? C6 C1 C37 119.1(3) . . ? C2 C1 C37 121.3(3) . . ? C22 C21 C20 120.1(3) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C10 C11 C12 117.9(3) . . ? C10 C11 C40 125.1(3) . . ? C12 C11 C40 117.0(3) . . ? C29 C28 C25 126.5(4) . . ? C29 C28 H28 116.7 . . ? C25 C28 H28 116.7 . . ? O2 C37 O1 122.6(3) . . ? O2 C37 C1 120.7(3) . . ? O1 C37 C1 116.7(3) . . ? C3 C2 C1 119.0(3) . . ? C3 C2 C39 119.0(3) . . ? C1 C2 C39 122.0(3) . . ? C4 C3 C2 119.8(3) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C9 C10 C11 120.1(3) . . ? C9 C10 C38 116.8(3) . . ? C11 C10 C38 123.0(3) . . ? N3 C18 C19 123.3(4) . . ? N3 C18 H18 118.4 . . ? C19 C18 H18 118.4 . . ? C6 C5 C4 118.9(4) . . ? C6 C5 H5 120.5 . . ? C4 C5 H5 120.5 . . ? N4 C23 C24 122.7(3) . . ? N4 C23 H23 118.6 . . ? C24 C23 H23 118.6 . . ? C19 C20 C21 116.9(3) . . ? C19 C20 C30 119.6(4) . . ? C21 C20 C30 123.3(4) . . ? O8 C38 O9 124.6(4) . . ? O8 C38 C10 119.4(4) . . ? O9 C38 C10 116.0(3) . . ? C27 C26 C25 119.7(4) . . ? C27 C26 H26 120.1 . . ? C25 C26 H26 120.1 . . ? O3 C39 O4 126.3(4) . . ? O3 C39 C2 115.5(3) . . ? O4 C39 C2 118.1(3) . . ? C26 C25 C24 117.4(3) . . ? C26 C25 C28 123.5(4) . . ? C24 C25 C28 119.1(4) . . ? N4 C27 C26 122.6(4) . . ? N4 C27 H27 118.7 . . ? C26 C27 H27 118.7 . . ? C5 C6 C1 121.5(3) . . ? C5 C6 H6 119.3 . . ? C1 C6 H6 119.3 . . ? C23 C24 C25 119.4(4) . . ? C23 C24 H24 120.3 . . ? C25 C24 H24 120.3 . . ? C7 C8 C9 117.5(4) . . ? C7 C8 H8 121.2 . . ? C9 C8 H8 121.2 . . ? C7 C12 C11 119.8(4) . . ? C7 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? O6 C40 O7 126.1(4) . . ? O6 C40 C11 119.0(4) . . ? O7 C40 C11 114.8(4) . . ? C8 C7 C12 123.0(3) . . ? C8 C7 O5 119.2(4) . . ? C12 C7 O5 117.5(4) . . ? C3 C4 C5 121.2(3) . . ? C3 C4 O5 124.3(3) . . ? C5 C4 O5 114.4(3) . . ? N3 C22 C21 122.6(4) . . ? N3 C22 H22 118.7 . . ? C21 C22 H22 118.7 . . ? C18 C19 C20 119.7(4) . . ? C18 C19 H19 120.1 . . ? C20 C19 H19 120.1 . . ? C8 C9 C10 121.6(4) . . ? C8 C9 H9 119.2 . . ? C10 C9 H9 119.2 . . ? C31 C30 C20 123.1(4) . . ? C31 C30 H30 118.5 . . ? C20 C30 H30 118.5 . . ? O13 Cu2 O13 180.000(1) . 3_676 ? O13 Cu2 O12 92.28(12) . . ? O13 Cu2 O12 87.72(12) 3_676 . ? O13 Cu2 O12 87.72(12) . 3_676 ? O13 Cu2 O12 92.28(12) 3_676 3_676 ? O12 Cu2 O12 180.000(1) . 3_676 ? O13 Cu2 O11 88.79(15) . . ? O13 Cu2 O11 91.21(15) 3_676 . ? O12 Cu2 O11 92.09(14) . . ? O12 Cu2 O11 87.91(14) 3_676 . ? O13 Cu2 O11 91.21(15) . 3_676 ? O13 Cu2 O11 88.79(15) 3_676 3_676 ? O12 Cu2 O11 87.91(14) . 3_676 ? O12 Cu2 O11 92.09(14) 3_676 3_676 ? O11 Cu2 O11 180.00(16) . 3_676 ? C28 C29 C15 121.8(4) . . ? C28 C29 H29 119.1 . . ? C15 C29 H29 119.1 . . ? C17 N2 C13 117.6(3) . . ? C17 N2 Cu1 117.7(2) . 1_655 ? C13 N2 Cu1 124.3(2) . 1_655 ? C15 C14 C13 119.7(4) . . ? C15 C14 H14 120.2 . . ? C13 C14 H14 120.2 . . ? C14 C15 C16 117.2(3) . . ? C14 C15 C29 121.9(4) . . ? C16 C15 C29 120.9(4) . . ? N2 C17 C16 122.9(4) . . ? N2 C17 H17 118.6 . . ? C16 C17 H17 118.6 . . ? C17 C16 C15 120.2(4) . . ? C17 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? N2 C13 C14 122.4(4) . . ? N2 C13 H13 118.8 . . ? C14 C13 H13 118.8 . . ? C36 N1 C32 118.2(3) . . ? C36 N1 Cu3 119.7(3) . 1_564 ? C32 N1 Cu3 121.9(3) . 1_564 ? C32 C33 C34 118.7(4) . . ? C32 C33 H33 120.6 . . ? C34 C33 H33 120.6 . . ? N1 C32 C33 122.6(4) . . ? N1 C32 H32 118.7 . . ? C33 C32 H32 118.7 . . ? C30 C31 C34 126.2(4) . . ? C30 C31 H31 116.9 . . ? C34 C31 H31 116.9 . . ? N1 C36 C35 122.5(4) . . ? N1 C36 H36 118.8 . . ? C35 C36 H36 118.8 . . ? C35 C34 C33 117.9(4) . . ? C35 C34 C31 118.7(4) . . ? C33 C34 C31 123.3(4) . . ? C36 C35 C34 119.9(4) . . ? C36 C35 H35 120.1 . . ? C34 C35 H35 120.1 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.861 _refine_diff_density_min -1.297 _refine_diff_density_rms 0.090 #===END data_041801 _database_code_depnum_ccdc_archive 'CCDC 787892' #TrackingRef '- Dalton Trans-gy.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H14 Mn2 N2 O11' _chemical_formula_weight 664.29 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' Mn Mn 0.3368 0.7283 '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' 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 16.348(4) _cell_length_b 22.823(5) _cell_length_c 14.011(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.558(3) _cell_angle_gamma 90.00 _cell_volume 5218(2) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5611 _cell_measurement_theta_min 2.3034 _cell_measurement_theta_max 27.4565 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.1400 _exptl_crystal_size_mid 0.1200 _exptl_crystal_size_min 0.0300 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.691 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2672 _exptl_absorpt_coefficient_mu 1.038 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8880 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 'Rigaku Saturn 70 diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16528 _diffrn_reflns_av_R_equivalents 0.0289 _diffrn_reflns_av_sigmaI/netI 0.0255 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 25.01 _reflns_number_total 4580 _reflns_number_gt 4059 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1031P)^2^+12.3593P] 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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4580 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0626 _refine_ls_R_factor_gt 0.0546 _refine_ls_wR_factor_ref 0.1744 _refine_ls_wR_factor_gt 0.1612 _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_restrained_S_all 1.106 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C24 C 0.0981(2) 0.36415(16) 0.5598(3) 0.0345(8) Uani 1 1 d . . . Mn1 Mn 0.25711(3) 0.41446(3) 0.57426(5) 0.0366(2) Uani 1 1 d . . . O7 O 0.16251(18) 0.35126(14) 0.6054(2) 0.0516(8) Uani 1 1 d . . . O2 O 0.2590(2) 0.46943(13) 0.3431(2) 0.0559(9) Uani 1 1 d . . . O1 O 0.2777(2) 0.38803(14) 0.4279(2) 0.0497(8) Uani 1 1 d . . . C10 C 0.2662(2) 0.41481(16) 0.3514(3) 0.0358(9) Uani 1 1 d . . . O3 O 0.1035(2) 0.40625(17) 0.2833(3) 0.0619(10) Uani 1 1 d . . . O4 O 0.4363(2) 0.30474(13) 0.1405(3) 0.0592(9) Uani 1 1 d . . . O6 O 0.2133(2) 0.45198(15) 0.7089(3) 0.0586(9) Uani 1 1 d . . . C25 C 0.0194(2) 0.33952(16) 0.5931(3) 0.0325(8) Uani 1 1 d . . . N2 N 0.3852(2) 0.45265(17) 0.6080(3) 0.0456(9) Uani 1 1 d . . . O8 O 0.0965(2) 0.39555(19) 0.4882(3) 0.0715(11) Uani 1 1 d . . . O5 O 0.2238(2) 0.50344(14) 0.5198(2) 0.0568(8) Uani 1 1 d . . . C6 C 0.3481(3) 0.35500(18) 0.2423(3) 0.0443(10) Uani 1 1 d . . . H6 H 0.3906 0.3556 0.2896 0.053 Uiso 1 1 calc R . . C27 C -0.0445(2) 0.37626(17) 0.6189(3) 0.0374(9) Uani 1 1 d . . . C2 C 0.2090(2) 0.37738(17) 0.1885(3) 0.0392(9) Uani 1 1 d . . . C9 C 0.1250(2) 0.40083(16) 0.2015(3) 0.0347(8) Uani 1 1 d . . . C5 C 0.3596(3) 0.32884(19) 0.1553(4) 0.0486(11) Uani 1 1 d . . . N1 N 0.3443(2) 0.33796(16) 0.6142(3) 0.0437(8) Uani 1 1 d . . . C1 C 0.2726(2) 0.38064(17) 0.2595(3) 0.0395(9) Uani 1 1 d . . . C16 C 0.4248(3) 0.3515(2) 0.6198(3) 0.0469(11) Uani 1 1 d . . . C26 C 0.0104(2) 0.27936(17) 0.6007(3) 0.0378(9) Uani 1 1 d . . . H26 H 0.0525 0.2547 0.5841 0.045 Uiso 1 1 calc R . . O9 O -0.0831(3) 0.4131(2) 0.3717(3) 0.0884(15) Uani 1 1 d . . . C8 C 0.4390(3) 0.24410(18) 0.1330(3) 0.0432(10) Uani 1 1 d . . . C3 C 0.2228(3) 0.3515(2) 0.1003(4) 0.0536(12) Uani 1 1 d . . . H3 H 0.1808 0.3507 0.0524 0.064 Uiso 1 1 calc R . . C15 C 0.4467(3) 0.4123(2) 0.6181(3) 0.0475(11) Uani 1 1 d . . . C19 C 0.5905(3) 0.3839(4) 0.6350(4) 0.083(2) Uani 1 1 d . . . H19 H 0.6456 0.3943 0.6404 0.100 Uiso 1 1 calc R . . C4 C 0.2977(3) 0.3271(2) 0.0833(4) 0.0557(12) Uani 1 1 d . . . H4 H 0.3064 0.3099 0.0246 0.067 Uiso 1 1 calc R . . C28 C -0.1143(3) 0.35178(19) 0.6523(4) 0.0497(11) Uani 1 1 d . . . H28 H -0.1560 0.3763 0.6706 0.060 Uiso 1 1 calc R . . C17 C 0.4864(3) 0.3077(3) 0.6286(3) 0.0626(15) Uani 1 1 d . . . C14 C 0.5300(3) 0.4290(3) 0.6269(4) 0.0680(16) Uani 1 1 d . . . C20 C 0.3227(3) 0.2817(2) 0.6186(4) 0.0543(12) Uani 1 1 d . . . H20 H 0.2673 0.2722 0.6154 0.065 Uiso 1 1 calc R . . C7 C 0.3760(3) 0.2081(2) 0.1592(4) 0.0539(12) Uani 1 1 d . . . H7 H 0.3282 0.2240 0.1809 0.065 Uiso 1 1 calc R . . C21 C 0.3806(4) 0.2361(2) 0.6281(4) 0.0682(15) Uani 1 1 d . . . H21 H 0.3636 0.1973 0.6310 0.082 Uiso 1 1 calc R . . C11 C 0.4045(3) 0.5092(2) 0.6098(4) 0.0624(13) Uani 1 1 d . . . H11 H 0.3626 0.5367 0.6042 0.075 Uiso 1 1 calc R . . C22 C 0.4605(4) 0.2494(3) 0.6327(4) 0.0705(17) Uani 1 1 d . . . H22 H 0.4992 0.2196 0.6388 0.085 Uiso 1 1 calc R . . C13 C 0.5474(4) 0.4891(4) 0.6279(4) 0.083(2) Uani 1 1 d . . . H13 H 0.6015 0.5017 0.6341 0.100 Uiso 1 1 calc R . . C23 C 0.0376(3) 0.55843(18) 0.3814(3) 0.0430(10) Uani 1 1 d . . . C18 C 0.5703(4) 0.3269(4) 0.6351(4) 0.084(2) Uani 1 1 d . . . H18 H 0.6118 0.2990 0.6396 0.101 Uiso 1 1 calc R . . C12 C 0.4860(5) 0.5287(3) 0.6199(5) 0.085(2) Uani 1 1 d . . . H12 H 0.4976 0.5686 0.6211 0.102 Uiso 1 1 calc R . . Mn2 Mn 0.03391(4) 0.44515(3) 0.38616(5) 0.0386(2) Uani 1 1 d . . . O10 O 0.0137(7) 0.5306(3) 0.4527(6) 0.084(3) Uani 0.50 1 d P . . O11 O 0.0761(7) 0.5298(3) 0.3255(8) 0.079(3) Uani 0.50 1 d P . . O11' O 0.0912(4) 0.5277(3) 0.3957(6) 0.0449(15) Uani 0.50 1 d P . . O10' O -0.0377(4) 0.5362(2) 0.3510(5) 0.0448(14) 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 C24 0.032(2) 0.0271(17) 0.045(2) 0.0010(16) 0.0107(17) -0.0014(15) Mn1 0.0287(4) 0.0365(4) 0.0449(4) 0.0055(3) 0.0048(3) -0.0038(2) O7 0.0294(16) 0.0580(19) 0.067(2) 0.0077(16) -0.0025(14) -0.0106(13) O2 0.082(2) 0.0378(16) 0.0475(18) -0.0012(14) 0.0016(17) 0.0071(15) O1 0.0504(19) 0.0559(18) 0.0434(17) 0.0092(15) 0.0073(14) 0.0116(15) C10 0.0273(19) 0.036(2) 0.044(2) 0.0017(17) -0.0012(16) -0.0001(15) O3 0.050(2) 0.083(2) 0.055(2) 0.0053(18) 0.0204(16) 0.0205(17) O4 0.0418(18) 0.0399(16) 0.098(3) -0.0082(17) 0.0226(18) 0.0100(13) O6 0.061(2) 0.059(2) 0.059(2) -0.0137(16) 0.0236(17) -0.0098(16) C25 0.0298(19) 0.0329(19) 0.0349(19) 0.0016(15) 0.0032(15) -0.0042(15) N2 0.0353(19) 0.054(2) 0.047(2) -0.0006(17) 0.0037(15) -0.0097(16) O8 0.052(2) 0.088(3) 0.077(3) 0.048(2) 0.0251(18) 0.0109(19) O5 0.068(2) 0.0414(17) 0.060(2) 0.0007(15) -0.0047(17) 0.0043(15) C6 0.037(2) 0.041(2) 0.055(3) -0.0032(19) 0.0027(19) 0.0066(17) C27 0.033(2) 0.031(2) 0.048(2) -0.0009(17) 0.0074(17) -0.0015(15) C2 0.030(2) 0.037(2) 0.050(2) -0.0099(18) 0.0012(17) 0.0062(16) C9 0.030(2) 0.0336(19) 0.041(2) -0.0058(17) 0.0036(17) 0.0035(15) C5 0.042(2) 0.041(2) 0.064(3) -0.004(2) 0.015(2) 0.0086(18) N1 0.038(2) 0.048(2) 0.045(2) 0.0049(16) 0.0030(15) 0.0057(15) C1 0.034(2) 0.0314(19) 0.054(2) -0.0014(18) 0.0029(18) 0.0055(15) C16 0.037(2) 0.070(3) 0.034(2) 0.003(2) 0.0028(17) 0.012(2) C26 0.031(2) 0.0306(19) 0.052(2) 0.0035(17) 0.0059(17) -0.0029(15) O9 0.057(2) 0.156(5) 0.050(2) 0.008(2) -0.0142(18) -0.048(3) C8 0.037(2) 0.035(2) 0.058(3) -0.0035(19) 0.0059(19) 0.0052(17) C3 0.046(3) 0.063(3) 0.051(3) -0.013(2) 0.003(2) 0.010(2) C15 0.032(2) 0.077(3) 0.034(2) -0.001(2) 0.0011(17) -0.007(2) C19 0.029(3) 0.165(7) 0.057(3) -0.001(4) 0.002(2) 0.008(4) C4 0.054(3) 0.058(3) 0.057(3) -0.015(2) 0.010(2) 0.015(2) C28 0.038(2) 0.041(2) 0.072(3) 0.001(2) 0.021(2) 0.0009(18) C17 0.050(3) 0.098(4) 0.040(3) 0.006(3) 0.008(2) 0.031(3) C14 0.034(3) 0.128(5) 0.042(3) -0.006(3) 0.004(2) -0.018(3) C20 0.062(3) 0.045(2) 0.055(3) 0.009(2) 0.006(2) 0.006(2) C7 0.039(2) 0.047(2) 0.078(3) -0.004(2) 0.023(2) 0.0076(19) C21 0.093(5) 0.052(3) 0.060(3) 0.005(2) 0.008(3) 0.025(3) C11 0.057(3) 0.062(3) 0.068(3) -0.005(3) 0.004(2) -0.023(2) C22 0.082(4) 0.081(4) 0.049(3) 0.006(3) 0.008(3) 0.044(3) C13 0.047(3) 0.134(6) 0.068(4) -0.017(4) 0.003(3) -0.041(4) C23 0.050(3) 0.037(2) 0.045(2) -0.0026(18) 0.020(2) -0.002(2) C18 0.049(3) 0.151(7) 0.054(3) 0.002(4) 0.005(3) 0.041(4) C12 0.076(4) 0.097(5) 0.082(4) -0.019(4) 0.011(3) -0.050(4) Mn2 0.0338(4) 0.0316(4) 0.0503(4) 0.0010(3) 0.0018(3) -0.0012(2) O10 0.157(9) 0.037(3) 0.066(5) -0.013(3) 0.059(5) -0.027(4) O11 0.113(8) 0.042(4) 0.090(6) 0.003(5) 0.060(6) 0.011(4) O11' 0.033(3) 0.028(3) 0.073(5) 0.002(3) -0.006(3) 0.006(2) O10' 0.038(3) 0.035(3) 0.061(4) -0.003(3) 0.004(3) -0.005(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C24 O8 1.232(5) . ? C24 O7 1.232(5) . ? C24 C25 1.506(5) . ? Mn1 O7 2.179(3) . ? Mn1 O1 2.183(3) . ? Mn1 O5 2.225(3) . ? Mn1 O6 2.231(3) . ? Mn1 N2 2.291(4) . ? Mn1 N1 2.301(4) . ? O2 C10 1.257(5) . ? O1 C10 1.238(5) . ? C10 C1 1.514(6) . ? O3 C9 1.226(5) . ? O3 Mn2 2.088(3) . ? O4 C8 1.389(5) . ? O4 C5 1.395(5) . ? C25 C26 1.386(5) . ? C25 C27 1.404(5) . ? N2 C11 1.327(7) . ? N2 C15 1.365(6) . ? O8 Mn2 2.046(4) . ? C6 C5 1.381(6) . ? C6 C1 1.400(6) . ? C27 C28 1.378(6) . ? C27 C23 1.495(6) 5_566 ? C2 C1 1.396(6) . ? C2 C3 1.401(6) . ? C2 C9 1.496(5) . ? C9 O9 1.230(5) 2 ? C5 C4 1.385(7) . ? N1 C20 1.335(6) . ? N1 C16 1.349(6) . ? C16 C17 1.418(7) . ? C16 C15 1.433(7) . ? C26 C8 1.386(6) 8_456 ? O9 C9 1.230(5) 2 ? O9 Mn2 2.046(4) . ? C8 C7 1.384(6) . ? C8 C26 1.386(6) 8 ? C3 C4 1.377(7) . ? C15 C14 1.412(7) . ? C19 C18 1.341(11) . ? C19 C14 1.428(10) . ? C28 C7 1.380(6) 8_456 ? C17 C22 1.399(9) . ? C17 C18 1.437(9) . ? C14 C13 1.399(10) . ? C20 C21 1.407(7) . ? C7 C28 1.380(6) 8 ? C21 C22 1.339(9) . ? C11 C12 1.404(8) . ? C13 C12 1.351(11) . ? C23 O11' 1.130(7) . ? C23 O11 1.223(8) . ? C23 O10 1.266(8) . ? C23 O10' 1.374(7) . ? C23 C27 1.495(6) 5_566 ? C23 Mn2 2.587(4) . ? Mn2 O11' 2.105(6) . ? Mn2 O10 2.195(7) . ? Mn2 O11 2.236(8) . ? Mn2 O10' 2.421(6) . ? Mn2 O10 2.496(7) 5_566 ? O10 O11' 1.540(11) . ? O10 O10' 1.614(12) . ? O10 Mn2 2.496(7) 5_566 ? O11 O11' 0.999(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O8 C24 O7 122.4(4) . . ? O8 C24 C25 119.6(4) . . ? O7 C24 C25 118.0(3) . . ? O7 Mn1 O1 99.08(13) . . ? O7 Mn1 O5 120.74(13) . . ? O1 Mn1 O5 88.77(12) . . ? O7 Mn1 O6 79.37(13) . . ? O1 Mn1 O6 167.65(14) . . ? O5 Mn1 O6 81.68(13) . . ? O7 Mn1 N2 149.53(13) . . ? O1 Mn1 N2 96.13(13) . . ? O5 Mn1 N2 85.69(14) . . ? O6 Mn1 N2 90.97(14) . . ? O7 Mn1 N1 83.44(13) . . ? O1 Mn1 N1 83.65(12) . . ? O5 Mn1 N1 155.60(14) . . ? O6 Mn1 N1 108.20(14) . . ? N2 Mn1 N1 72.17(14) . . ? C24 O7 Mn1 109.4(3) . . ? C10 O1 Mn1 130.8(3) . . ? O1 C10 O2 125.3(4) . . ? O1 C10 C1 117.9(3) . . ? O2 C10 C1 116.3(4) . . ? C9 O3 Mn2 152.6(3) . . ? C8 O4 C5 115.9(3) . . ? C26 C25 C27 119.3(3) . . ? C26 C25 C24 119.3(3) . . ? C27 C25 C24 121.4(3) . . ? C11 N2 C15 118.8(4) . . ? C11 N2 Mn1 125.9(4) . . ? C15 N2 Mn1 115.0(3) . . ? C24 O8 Mn2 151.1(3) . . ? C5 C6 C1 120.2(4) . . ? C28 C27 C25 119.3(4) . . ? C28 C27 C23 118.0(4) . 5_566 ? C25 C27 C23 122.5(3) . 5_566 ? C1 C2 C3 119.9(4) . . ? C1 C2 C9 122.8(4) . . ? C3 C2 C9 117.3(4) . . ? O3 C9 O9 125.4(4) . 2 ? O3 C9 C2 118.0(4) . . ? O9 C9 C2 116.6(4) 2 . ? C6 C5 C4 121.4(4) . . ? C6 C5 O4 118.3(4) . . ? C4 C5 O4 120.2(4) . . ? C20 N1 C16 118.5(4) . . ? C20 N1 Mn1 125.5(3) . . ? C16 N1 Mn1 115.3(3) . . ? C2 C1 C6 118.7(4) . . ? C2 C1 C10 123.1(3) . . ? C6 C1 C10 118.0(4) . . ? N1 C16 C17 121.9(5) . . ? N1 C16 C15 117.7(4) . . ? C17 C16 C15 120.4(5) . . ? C25 C26 C8 120.2(4) . 8_456 ? C9 O9 Mn2 129.3(3) 2 . ? C7 C8 C26 120.9(4) . 8 ? C7 C8 O4 122.9(4) . . ? C26 C8 O4 116.2(4) 8 . ? C4 C3 C2 121.1(5) . . ? N2 C15 C14 121.7(5) . . ? N2 C15 C16 118.2(4) . . ? C14 C15 C16 120.1(5) . . ? C18 C19 C14 122.0(6) . . ? C3 C4 C5 118.7(4) . . ? C27 C28 C7 121.7(4) . 8_456 ? C22 C17 C16 117.3(5) . . ? C22 C17 C18 125.3(6) . . ? C16 C17 C18 117.4(6) . . ? C13 C14 C15 117.4(6) . . ? C13 C14 C19 124.5(6) . . ? C15 C14 C19 118.1(6) . . ? N1 C20 C21 122.5(5) . . ? C28 C7 C8 118.6(4) 8 . ? C22 C21 C20 119.0(6) . . ? N2 C11 C12 122.3(6) . . ? C21 C22 C17 120.7(5) . . ? C12 C13 C14 120.4(5) . . ? O11' C23 O11 50.1(6) . . ? O11' C23 O10 79.8(7) . . ? O11 C23 O10 115.6(6) . . ? O11' C23 O10' 119.7(5) . . ? O11 C23 O10' 95.2(7) . . ? O10 C23 O10' 75.2(6) . . ? O11' C23 C27 124.1(5) . 5_566 ? O11 C23 C27 119.3(5) . 5_566 ? O10 C23 C27 122.0(4) . 5_566 ? O10' C23 C27 115.7(4) . 5_566 ? O11' C23 Mn2 52.8(3) . . ? O11 C23 Mn2 59.8(4) . . ? O10 C23 Mn2 57.9(3) . . ? O10' C23 Mn2 67.5(3) . . ? C27 C23 Mn2 176.8(3) 5_566 . ? C19 C18 C17 122.0(6) . . ? C13 C12 C11 119.4(6) . . ? O9 Mn2 O8 107.15(17) . . ? O9 Mn2 O3 108.99(18) . . ? O8 Mn2 O3 88.66(15) . . ? O9 Mn2 O11' 137.4(2) . . ? O8 Mn2 O11' 104.5(2) . . ? O3 Mn2 O11' 99.5(2) . . ? O9 Mn2 O10 101.3(3) . . ? O8 Mn2 O10 106.0(3) . . ? O3 Mn2 O10 140.7(2) . . ? O11' Mn2 O10 41.9(3) . . ? O9 Mn2 O11 125.4(3) . . ? O8 Mn2 O11 126.2(4) . . ? O3 Mn2 O11 84.9(2) . . ? O11' Mn2 O11 26.4(3) . . ? O10 Mn2 O11 56.8(3) . . ? O9 Mn2 O10' 81.4(2) . . ? O8 Mn2 O10' 146.2(2) . . ? O3 Mn2 O10' 120.11(18) . . ? O11' Mn2 O10' 56.7(2) . . ? O10 Mn2 O10' 40.6(3) . . ? O11 Mn2 O10' 48.5(3) . . ? O9 Mn2 O10 80.0(3) . 5_566 ? O8 Mn2 O10 70.2(3) . 5_566 ? O3 Mn2 O10 158.8(3) . 5_566 ? O11' Mn2 O10 84.6(3) . 5_566 ? O10 Mn2 O10 49.8(3) . 5_566 ? O11 Mn2 O10 105.8(3) . 5_566 ? O10' Mn2 O10 79.6(3) . 5_566 ? O9 Mn2 C23 112.21(19) . . ? O8 Mn2 C23 124.02(17) . . ? O3 Mn2 C23 113.10(14) . . ? O11' Mn2 C23 25.29(19) . . ? O10 Mn2 C23 29.3(2) . . ? O11 Mn2 C23 28.2(2) . . ? O10' Mn2 C23 31.62(17) . . ? O10 Mn2 C23 79.09(18) 5_566 . ? C23 O10 O11' 46.2(4) . . ? C23 O10 O10' 55.4(5) . . ? O11' O10 O10' 86.8(5) . . ? C23 O10 Mn2 92.8(4) . . ? O11' O10 Mn2 65.9(3) . . ? O10' O10 Mn2 77.3(3) . . ? C23 O10 Mn2 137.0(5) . 5_566 ? O11' O10 Mn2 142.3(7) . 5_566 ? O10' O10 Mn2 127.3(6) . 5_566 ? Mn2 O10 Mn2 130.2(3) . 5_566 ? O11' O11 C23 60.1(6) . . ? O11' O11 Mn2 69.5(6) . . ? C23 O11 Mn2 92.0(5) . . ? O11 O11' C23 69.8(7) . . ? O11 O11' O10 110.3(9) . . ? C23 O11' O10 54.0(5) . . ? O11 O11' Mn2 84.2(7) . . ? C23 O11' Mn2 101.9(4) . . ? O10 O11' Mn2 72.2(3) . . ? C23 O10' O10 49.4(4) . . ? C23 O10' Mn2 80.9(3) . . ? O10 O10' Mn2 62.2(3) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.179 _refine_diff_density_min -0.577 _refine_diff_density_rms 0.113 #===END data_051201 _database_code_depnum_ccdc_archive 'CCDC 787893' #TrackingRef '- Dalton Trans-gy.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H16 Co N2 O10' _chemical_formula_weight 599.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 24.319(7) _cell_length_b 11.905(3) _cell_length_c 8.666(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.750(6) _cell_angle_gamma 90.00 _cell_volume 2485.9(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3175 _cell_measurement_theta_min 3.0588 _cell_measurement_theta_max 27.4603 _exptl_crystal_description Prism _exptl_crystal_colour Blue _exptl_crystal_size_max 0.4500 _exptl_crystal_size_mid 0.4000 _exptl_crystal_size_min 0.2500 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.601 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1220 _exptl_absorpt_coefficient_mu 0.757 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8758 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 'Rigaku Mercury 70 diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9451 _diffrn_reflns_av_R_equivalents 0.0219 _diffrn_reflns_av_sigmaI/netI 0.0212 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 27.47 _reflns_number_total 2740 _reflns_number_gt 2510 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0432P)^2^+6.1956P] 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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2740 _refine_ls_number_parameters 188 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0419 _refine_ls_R_factor_gt 0.0384 _refine_ls_wR_factor_ref 0.1003 _refine_ls_wR_factor_gt 0.0978 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.0000 0.5000 0.0000 0.01566(13) Uani 1 2 d S . . O1 O 0.03358(6) 0.65532(12) 0.06032(17) 0.0211(3) Uani 1 1 d . . . O6 O 0.0000 0.45102(17) 0.2500 0.0196(4) Uani 1 2 d S . . O5 O 0.0000 1.04831(17) 0.2500 0.0258(5) Uani 1 2 d S . . O2 O 0.07754(7) 0.69809(14) -0.1430(2) 0.0305(4) Uani 1 1 d . . . N1 N -0.08043(7) 0.56829(14) -0.0140(2) 0.0202(4) Uani 1 1 d . . . C7 C 0.06300(8) 0.71836(16) -0.0139(2) 0.0188(4) Uani 1 1 d . . . C6 C 0.03445(9) 0.88514(17) 0.1214(3) 0.0206(4) Uani 1 1 d . . . H6 H 0.0000 0.8504 0.1146 0.025 Uiso 1 1 calc R . . C2 C 0.12959(9) 0.88431(18) 0.0715(3) 0.0227(4) Uani 1 1 d . . . C1 C 0.07780(8) 0.83051(16) 0.0636(2) 0.0190(4) Uani 1 1 d . . . O4 O 0.21812(9) 0.88423(19) -0.0134(4) 0.0664(8) Uani 1 1 d . . . O3 O 0.18573(8) 0.72167(17) 0.0594(3) 0.0504(5) Uani 1 1 d . . . C8 C 0.18029(9) 0.8270(2) 0.0303(3) 0.0310(5) Uani 1 1 d . . . C4 C 0.09176(9) 1.04730(18) 0.1900(3) 0.0260(5) Uani 1 1 d . . . H4 H 0.0962 1.1200 0.2289 0.031 Uiso 1 1 calc R . . C12 C -0.17612(10) 0.5702(2) -0.1210(3) 0.0381(6) Uani 1 1 d . . . H12 H -0.2048 0.5380 -0.1882 0.046 Uiso 1 1 calc R . . C9 C -0.08982(9) 0.65824(19) 0.0708(3) 0.0261(5) Uani 1 1 d . . . H9 H -0.0603 0.6888 0.1368 0.031 Uiso 1 1 calc R . . C10 C -0.14124(10) 0.7077(2) 0.0650(3) 0.0331(6) Uani 1 1 d . . . H10 H -0.1460 0.7707 0.1253 0.040 Uiso 1 1 calc R . . C5 C 0.04164(9) 0.99103(16) 0.1894(3) 0.0202(4) Uani 1 1 d . . . C14 C -0.24266(10) 0.7077(3) -0.0408(3) 0.0421(7) Uani 1 1 d . . . H14 H -0.2702 0.6734 -0.1098 0.050 Uiso 1 1 calc R . . C11 C -0.18621(9) 0.6625(2) -0.0322(3) 0.0319(5) Uani 1 1 d . . . C13 C -0.12324(9) 0.5259(2) -0.1094(3) 0.0307(5) Uani 1 1 d . . . H13 H -0.1171 0.4641 -0.1705 0.037 Uiso 1 1 calc R . . C3 C 0.13503(10) 0.99336(18) 0.1317(3) 0.0267(5) Uani 1 1 d . . . H3 H 0.1687 1.0307 0.1327 0.032 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.01231(19) 0.01353(19) 0.0214(2) -0.00034(13) 0.00324(15) 0.00103(12) O1 0.0222(7) 0.0162(7) 0.0259(8) -0.0018(6) 0.0073(6) -0.0032(5) O6 0.0210(10) 0.0195(10) 0.0189(10) 0.000 0.0043(8) 0.000 O5 0.0303(11) 0.0147(9) 0.0361(13) 0.000 0.0181(10) 0.000 O2 0.0371(9) 0.0271(8) 0.0305(9) -0.0089(7) 0.0166(7) -0.0101(7) N1 0.0149(8) 0.0212(8) 0.0247(9) 0.0003(7) 0.0033(7) 0.0037(6) C7 0.0155(9) 0.0160(9) 0.0249(11) -0.0014(8) 0.0029(8) 0.0002(7) C6 0.0202(9) 0.0174(9) 0.0251(11) -0.0001(8) 0.0067(8) -0.0025(7) C2 0.0207(10) 0.0222(10) 0.0260(11) -0.0014(8) 0.0065(8) -0.0027(8) C1 0.0199(9) 0.0171(9) 0.0207(10) 0.0000(8) 0.0047(8) -0.0020(7) O4 0.0399(11) 0.0418(11) 0.128(2) 0.0085(13) 0.0506(14) 0.0000(9) O3 0.0382(11) 0.0337(10) 0.0821(16) 0.0031(10) 0.0187(10) 0.0054(8) C8 0.0193(10) 0.0330(12) 0.0416(14) -0.0090(10) 0.0072(10) -0.0033(9) C4 0.0314(12) 0.0181(10) 0.0298(12) -0.0051(8) 0.0089(9) -0.0066(8) C12 0.0190(11) 0.0450(15) 0.0474(16) -0.0168(12) -0.0058(10) 0.0066(10) C9 0.0186(10) 0.0298(11) 0.0294(12) -0.0043(9) 0.0018(9) 0.0044(8) C10 0.0254(11) 0.0365(13) 0.0372(14) -0.0120(10) 0.0031(10) 0.0120(10) C5 0.0231(10) 0.0176(9) 0.0213(11) 0.0013(7) 0.0083(8) 0.0011(7) C14 0.0207(11) 0.0540(16) 0.0488(17) -0.0149(13) -0.0046(11) 0.0154(11) C11 0.0186(10) 0.0406(13) 0.0360(13) -0.0061(10) 0.0019(9) 0.0105(9) C13 0.0209(11) 0.0307(11) 0.0396(14) -0.0117(10) 0.0006(10) 0.0054(9) C3 0.0232(11) 0.0239(11) 0.0342(13) -0.0052(9) 0.0082(9) -0.0083(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1 2.0601(14) . ? Co1 O1 2.0601(14) 5_565 ? Co1 N1 2.1066(17) 5_565 ? Co1 N1 2.1066(17) . ? Co1 O6 2.2435(8) . ? Co1 O6 2.2435(8) 5_565 ? O1 C7 1.270(2) . ? O6 Co1 2.2435(8) 2 ? O5 C5 1.382(2) . ? O5 C5 1.382(2) 2 ? O2 C7 1.242(3) . ? N1 C9 1.335(3) . ? N1 C13 1.338(3) . ? C7 C1 1.516(3) . ? C6 C1 1.388(3) . ? C6 C5 1.392(3) . ? C6 H6 0.9300 . ? C2 C3 1.399(3) . ? C2 C1 1.406(3) . ? C2 C8 1.494(3) . ? O4 C8 1.244(3) . ? O3 C8 1.282(3) . ? C4 C3 1.385(3) . ? C4 C5 1.390(3) . ? C4 H4 0.9300 . ? C12 C13 1.381(3) . ? C12 C11 1.382(3) . ? C12 H12 0.9300 . ? C9 C10 1.377(3) . ? C9 H9 0.9300 . ? C10 C11 1.396(3) . ? C10 H10 0.9300 . ? C14 C14 1.309(5) 7_465 ? C14 C11 1.467(3) . ? C14 H14 0.9300 . ? C13 H13 0.9300 . ? C3 H3 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 O1 180.00(7) . 5_565 ? O1 Co1 N1 89.92(6) . 5_565 ? O1 Co1 N1 90.08(6) 5_565 5_565 ? O1 Co1 N1 90.08(6) . . ? O1 Co1 N1 89.92(6) 5_565 . ? N1 Co1 N1 180.00(4) 5_565 . ? O1 Co1 O6 92.28(6) . . ? O1 Co1 O6 87.72(6) 5_565 . ? N1 Co1 O6 88.00(5) 5_565 . ? N1 Co1 O6 92.00(5) . . ? O1 Co1 O6 87.72(6) . 5_565 ? O1 Co1 O6 92.28(6) 5_565 5_565 ? N1 Co1 O6 92.00(5) 5_565 5_565 ? N1 Co1 O6 88.00(5) . 5_565 ? O6 Co1 O6 180.00(10) . 5_565 ? C7 O1 Co1 129.28(13) . . ? Co1 O6 Co1 149.87(10) 2 . ? C5 O5 C5 120.9(2) . 2 ? C9 N1 C13 117.76(18) . . ? C9 N1 Co1 120.27(14) . . ? C13 N1 Co1 121.94(15) . . ? O2 C7 O1 126.14(19) . . ? O2 C7 C1 119.40(18) . . ? O1 C7 C1 114.37(18) . . ? C1 C6 C5 121.25(19) . . ? C1 C6 H6 119.4 . . ? C5 C6 H6 119.4 . . ? C3 C2 C1 118.7(2) . . ? C3 C2 C8 118.27(19) . . ? C1 C2 C8 122.88(19) . . ? C6 C1 C2 119.19(19) . . ? C6 C1 C7 115.21(18) . . ? C2 C1 C7 125.46(19) . . ? O4 C8 O3 122.3(2) . . ? O4 C8 C2 119.4(2) . . ? O3 C8 C2 117.8(2) . . ? C3 C4 C5 118.96(19) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? C13 C12 C11 119.8(2) . . ? C13 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? N1 C9 C10 123.0(2) . . ? N1 C9 H9 118.5 . . ? C10 C9 H9 118.5 . . ? C9 C10 C11 119.4(2) . . ? C9 C10 H10 120.3 . . ? C11 C10 H10 120.3 . . ? O5 C5 C4 116.61(18) . . ? O5 C5 C6 123.43(19) . . ? C4 C5 C6 119.8(2) . . ? C14 C14 C11 125.2(3) 7_465 . ? C14 C14 H14 117.4 7_465 . ? C11 C14 H14 117.4 . . ? C12 C11 C10 117.3(2) . . ? C12 C11 C14 119.9(2) . . ? C10 C11 C14 122.8(2) . . ? N1 C13 C12 122.7(2) . . ? N1 C13 H13 118.6 . . ? C12 C13 H13 118.6 . . ? C4 C3 C2 121.9(2) . . ? C4 C3 H3 119.1 . . ? C2 C3 H3 119.1 . . ? _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 1.078 _refine_diff_density_min -0.331 _refine_diff_density_rms 0.066 #===END data_091225 _database_code_depnum_ccdc_archive 'CCDC 787898' #TrackingRef '- Dalton Trans-gy.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C80 H44 Cu2 N8 O19' _chemical_formula_weight 1548.31 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.203(3) _cell_length_b 11.403(3) _cell_length_c 12.953(4) _cell_angle_alpha 91.304(2) _cell_angle_beta 101.586(4) _cell_angle_gamma 91.485(5) _cell_volume 1619.9(7) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4109 _cell_measurement_theta_min 2.1961 _cell_measurement_theta_max 27.4680 _exptl_crystal_description Prism _exptl_crystal_colour Blue _exptl_crystal_size_max 0.2000 _exptl_crystal_size_mid 0.1400 _exptl_crystal_size_min 0.0700 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.587 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 790 _exptl_absorpt_coefficient_mu 0.746 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9316 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 'Rigaku Saturn 70 diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12837 _diffrn_reflns_av_R_equivalents 0.0209 _diffrn_reflns_av_sigmaI/netI 0.0361 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 27.49 _reflns_number_total 7307 _reflns_number_gt 6272 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0658P)^2^+0.7632P] 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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7307 _refine_ls_number_parameters 496 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0532 _refine_ls_R_factor_gt 0.0442 _refine_ls_wR_factor_ref 0.1259 _refine_ls_wR_factor_gt 0.1146 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu -0.10061(2) 0.67854(2) 0.70529(2) 0.03185(11) Uani 1 1 d . . . O1 O 0.06586(14) 0.61833(15) 0.70182(13) 0.0363(4) Uani 1 1 d . . . N1 N -0.15211(17) 0.51748(16) 0.73895(16) 0.0323(4) Uani 1 1 d . . . O2 O 0.11327(15) 0.68560(14) 0.55329(13) 0.0352(4) Uani 1 1 d . . . N4 N -0.06165(17) 0.84189(16) 0.67286(16) 0.0322(4) Uani 1 1 d . . . O3 O 0.09561(16) 0.41726(15) 0.54269(14) 0.0413(4) Uani 1 1 d . . . N3 N -0.26438(17) 0.71413(16) 0.60705(15) 0.0309(4) Uani 1 1 d . . . C5 C -0.16142(19) 0.5044(2) 0.84083(19) 0.0318(5) Uani 1 1 d . . . N2 N -0.09085(17) 0.70364(17) 0.87172(16) 0.0329(4) Uani 1 1 d . . . C31 C 0.13567(19) 0.63308(17) 0.63789(17) 0.0270(4) Uani 1 1 d . . . C30 C 0.25901(19) 0.57908(18) 0.67417(16) 0.0277(4) Uani 1 1 d . . . O4 O 0.1549(2) 0.27799(18) 0.65647(19) 0.0692(7) Uani 1 1 d . . . C4 C -0.1970(2) 0.3963(2) 0.8780(2) 0.0402(6) Uani 1 1 d . . . C6 C -0.13032(19) 0.6037(2) 0.91161(18) 0.0324(5) Uani 1 1 d . . . C25 C 0.2704(2) 0.45698(19) 0.67378(17) 0.0296(4) Uani 1 1 d . . . C13 C 0.0412(2) 0.9037(2) 0.7092(2) 0.0413(6) Uani 1 1 d . . . H13 H 0.1040 0.8690 0.7553 0.050 Uiso 1 1 calc R . . C19 C -0.3583(2) 0.8701(2) 0.4977(2) 0.0373(5) Uani 1 1 d . . . C18 C -0.2612(2) 0.82358(19) 0.56871(17) 0.0297(4) Uani 1 1 d . . . O6 O 0.7978(3) 1.0291(2) 0.9148(3) 0.0830(8) Uani 1 1 d . . . C26 C 0.3803(2) 0.4086(2) 0.7194(2) 0.0391(5) Uani 1 1 d . . . H26 H 0.3869 0.3275 0.7210 0.047 Uiso 1 1 calc R . . O5 O 0.57196(16) 0.67086(19) 0.79819(16) 0.0521(5) Uani 1 1 d . . . C14 C 0.0576(2) 1.0196(2) 0.6799(2) 0.0448(6) Uani 1 1 d . . . H14 H 0.1297 1.0615 0.7075 0.054 Uiso 1 1 calc R . . C29 C 0.3592(2) 0.6509(2) 0.71838(19) 0.0346(5) Uani 1 1 d . . . H29 H 0.3529 0.7321 0.7193 0.042 Uiso 1 1 calc R . . C15 C -0.0330(2) 1.0707(2) 0.6105(2) 0.0431(6) Uani 1 1 d . . . H15 H -0.0223 1.1473 0.5901 0.052 Uiso 1 1 calc R . . C7 C -0.1370(2) 0.5941(3) 1.0180(2) 0.0425(6) Uani 1 1 d . . . C1 C -0.1751(2) 0.4258(2) 0.6723(2) 0.0418(6) Uani 1 1 d . . . H1 H -0.1673 0.4348 0.6028 0.050 Uiso 1 1 calc R . . C32 C 0.1678(2) 0.3746(2) 0.62538(18) 0.0337(5) Uani 1 1 d . . . C17 C -0.1521(2) 0.89294(19) 0.60474(18) 0.0305(5) Uani 1 1 d . . . C16 C -0.1423(2) 1.0075(2) 0.5698(2) 0.0366(5) Uani 1 1 d . . . C27 C 0.4801(2) 0.4808(2) 0.7625(2) 0.0440(6) Uani 1 1 d . . . H27 H 0.5542 0.4487 0.7922 0.053 Uiso 1 1 calc R . . C28 C 0.4682(2) 0.6004(2) 0.7609(2) 0.0381(5) Uani 1 1 d . . . C24 C -0.3658(2) 0.6495(2) 0.5773(2) 0.0395(5) Uani 1 1 d . . . H24 H -0.3694 0.5745 0.6034 0.047 Uiso 1 1 calc R . . C12 C -0.0550(2) 0.7940(2) 0.9369(2) 0.0411(6) Uani 1 1 d . . . H12 H -0.0262 0.8619 0.9103 0.049 Uiso 1 1 calc R . . C34 C 0.6457(2) 0.8409(2) 0.8997(2) 0.0453(6) Uani 1 1 d . . . H34 H 0.6874 0.8606 0.8471 0.054 Uiso 1 1 calc R . . C20 C -0.3442(3) 0.9868(2) 0.4605(2) 0.0459(6) Uani 1 1 d . . . H20 H -0.4071 1.0178 0.4117 0.055 Uiso 1 1 calc R . . C11 C -0.0586(3) 0.7923(3) 1.0440(2) 0.0504(7) Uani 1 1 d . . . H11 H -0.0324 0.8577 1.0876 0.060 Uiso 1 1 calc R . . C10 C -0.1009(3) 0.6935(3) 1.0840(2) 0.0523(7) Uani 1 1 d . . . H10 H -0.1058 0.6919 1.1548 0.063 Uiso 1 1 calc R . . C8 C -0.1757(3) 0.4838(3) 1.0534(2) 0.0544(8) Uani 1 1 d . . . H8 H -0.1817 0.4772 1.1236 0.065 Uiso 1 1 calc R . . C22 C -0.4645(2) 0.7992(2) 0.4674(2) 0.0442(6) Uani 1 1 d . . . H22 H -0.5315 0.8261 0.4204 0.053 Uiso 1 1 calc R . . C3 C -0.2222(2) 0.3012(2) 0.8060(3) 0.0489(7) Uani 1 1 d . . . H3 H -0.2467 0.2287 0.8274 0.059 Uiso 1 1 calc R . . C23 C -0.4676(2) 0.6895(2) 0.5083(2) 0.0460(6) Uani 1 1 d . . . H23 H -0.5376 0.6419 0.4901 0.055 Uiso 1 1 calc R . . C2 C -0.2107(3) 0.3156(2) 0.7040(3) 0.0497(7) Uani 1 1 d . . . H2 H -0.2265 0.2527 0.6558 0.060 Uiso 1 1 calc R . . C33 C 0.5735(2) 0.7398(2) 0.8875(2) 0.0411(6) Uani 1 1 d . . . C21 C -0.2412(3) 1.0517(2) 0.4955(2) 0.0450(6) Uani 1 1 d . . . H21 H -0.2345 1.1269 0.4707 0.054 Uiso 1 1 calc R . . O7 O 0.7561(3) 1.0984(2) 1.0635(3) 0.0949(10) Uani 1 1 d . . . C35 C 0.6578(2) 0.9147(2) 0.9897(2) 0.0484(7) Uani 1 1 d . . . C9 C -0.2034(3) 0.3899(3) 0.9878(3) 0.0531(7) Uani 1 1 d . . . H9 H -0.2270 0.3194 1.0136 0.064 Uiso 1 1 calc R . . C36 C 0.7440(3) 1.0208(3) 0.9882(3) 0.0654(10) Uani 1 1 d . . . O10 O 0.6647(5) 0.0359(4) 0.7120(4) 0.0678(12) Uani 0.50 1 d P . . C39 C 0.5220(3) 0.7814(3) 1.0527(2) 0.0535(7) Uani 1 1 d . . . H39 H 0.4788 0.7609 1.1042 0.064 Uiso 1 1 calc R . . C38 C 0.5938(3) 0.8836(3) 1.0682(2) 0.0506(7) Uani 1 1 d . . . C40 C 0.5113(3) 0.7086(3) 0.9647(2) 0.0497(7) Uani 1 1 d . . . H40 H 0.4632 0.6401 0.9577 0.060 Uiso 1 1 calc R . . O8 O 0.6460(3) 1.0483(2) 1.1935(2) 0.0902(9) Uani 1 1 d . . . O9 O 0.5303(4) 0.9018(3) 1.2314(2) 0.1054(11) Uani 1 1 d . . . C37 C 0.5884(4) 0.9482(3) 1.1732(3) 0.0701(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 Cu1 0.03213(17) 0.02568(15) 0.03754(18) 0.00473(11) 0.00642(12) -0.00161(11) O1 0.0309(8) 0.0400(9) 0.0403(9) 0.0110(7) 0.0110(7) 0.0057(7) N1 0.0308(10) 0.0284(9) 0.0390(11) 0.0027(8) 0.0099(8) -0.0010(7) O2 0.0401(9) 0.0311(8) 0.0319(8) 0.0063(6) 0.0011(7) -0.0030(7) N4 0.0291(9) 0.0274(9) 0.0393(11) 0.0021(8) 0.0052(8) -0.0015(7) O3 0.0433(10) 0.0333(9) 0.0400(10) 0.0047(7) -0.0084(7) -0.0062(7) N3 0.0306(9) 0.0296(9) 0.0333(10) 0.0009(7) 0.0083(8) -0.0021(7) C5 0.0233(10) 0.0329(11) 0.0400(12) 0.0118(9) 0.0066(9) 0.0047(8) N2 0.0295(9) 0.0335(10) 0.0357(10) 0.0030(8) 0.0063(8) 0.0031(8) C31 0.0293(10) 0.0194(9) 0.0303(11) -0.0024(8) 0.0018(8) -0.0053(8) C30 0.0288(10) 0.0280(10) 0.0259(10) -0.0010(8) 0.0052(8) -0.0038(8) O4 0.0766(15) 0.0388(11) 0.0737(15) 0.0232(10) -0.0280(12) -0.0252(10) C4 0.0277(11) 0.0390(13) 0.0546(16) 0.0175(11) 0.0075(10) 0.0029(10) C6 0.0238(10) 0.0388(12) 0.0358(12) 0.0089(9) 0.0075(9) 0.0061(9) C25 0.0303(11) 0.0298(11) 0.0274(11) -0.0022(8) 0.0030(8) -0.0014(9) C13 0.0339(12) 0.0351(13) 0.0520(15) 0.0012(11) 0.0021(11) -0.0032(10) C19 0.0377(12) 0.0354(12) 0.0381(13) 0.0007(10) 0.0059(10) 0.0038(10) C18 0.0307(11) 0.0292(11) 0.0295(11) -0.0011(8) 0.0070(9) 0.0012(9) O6 0.0721(17) 0.0540(14) 0.115(2) 0.0124(15) 0.0031(16) -0.0219(13) C26 0.0371(13) 0.0326(12) 0.0446(14) -0.0002(10) 0.0005(10) 0.0052(10) O5 0.0284(9) 0.0645(13) 0.0603(12) -0.0227(10) 0.0058(8) -0.0139(8) C14 0.0386(13) 0.0349(13) 0.0584(17) -0.0005(11) 0.0058(12) -0.0112(11) C29 0.0319(11) 0.0315(11) 0.0391(13) -0.0065(9) 0.0061(9) -0.0064(9) C15 0.0460(14) 0.0284(12) 0.0555(16) 0.0047(11) 0.0122(12) -0.0056(10) C7 0.0321(12) 0.0611(17) 0.0350(13) 0.0109(11) 0.0069(10) 0.0078(11) C1 0.0442(14) 0.0321(12) 0.0505(15) -0.0030(10) 0.0135(12) -0.0018(10) C32 0.0375(12) 0.0286(11) 0.0335(12) 0.0002(9) 0.0040(9) -0.0023(9) C17 0.0328(11) 0.0272(11) 0.0322(11) 0.0010(8) 0.0084(9) 0.0013(9) C16 0.0403(13) 0.0284(11) 0.0417(13) 0.0026(9) 0.0100(10) 0.0002(9) C27 0.0277(12) 0.0473(15) 0.0528(16) -0.0027(12) -0.0020(11) 0.0052(10) C28 0.0256(11) 0.0464(14) 0.0403(13) -0.0109(10) 0.0040(9) -0.0075(10) C24 0.0379(13) 0.0358(12) 0.0450(14) 0.0007(10) 0.0100(11) -0.0065(10) C12 0.0398(13) 0.0385(13) 0.0441(14) -0.0039(10) 0.0070(11) 0.0037(10) C34 0.0289(12) 0.0414(14) 0.0597(17) 0.0014(12) -0.0044(11) -0.0035(10) C20 0.0499(15) 0.0377(13) 0.0462(15) 0.0080(11) -0.0016(12) 0.0085(12) C11 0.0476(15) 0.0581(17) 0.0417(15) -0.0123(13) 0.0010(12) 0.0081(13) C10 0.0470(15) 0.077(2) 0.0323(14) -0.0001(13) 0.0049(11) 0.0099(14) C8 0.0485(16) 0.076(2) 0.0418(15) 0.0252(15) 0.0126(12) 0.0034(15) C22 0.0348(13) 0.0472(15) 0.0457(15) -0.0015(11) -0.0036(11) 0.0028(11) C3 0.0376(13) 0.0303(12) 0.079(2) 0.0155(13) 0.0105(13) -0.0007(10) C23 0.0355(13) 0.0471(15) 0.0520(16) -0.0037(12) 0.0027(11) -0.0096(11) C2 0.0467(15) 0.0310(13) 0.071(2) -0.0011(12) 0.0104(14) -0.0020(11) C33 0.0256(11) 0.0416(13) 0.0501(15) -0.0056(11) -0.0057(10) -0.0021(10) C21 0.0513(15) 0.0302(12) 0.0523(16) 0.0111(11) 0.0060(12) 0.0037(11) O7 0.0884(19) 0.0495(14) 0.125(3) -0.0237(15) -0.0252(17) -0.0172(13) C35 0.0342(13) 0.0330(13) 0.0655(19) -0.0017(12) -0.0193(12) 0.0015(10) C9 0.0421(15) 0.0601(18) 0.0598(18) 0.0317(15) 0.0132(13) 0.0020(13) C36 0.0473(17) 0.0360(15) 0.097(3) 0.0046(16) -0.0214(18) -0.0052(13) O10 0.097(4) 0.061(3) 0.050(3) 0.002(2) 0.026(2) -0.005(3) C39 0.0539(17) 0.0561(17) 0.0458(16) -0.0026(13) -0.0005(13) -0.0009(14) C38 0.0473(15) 0.0436(15) 0.0498(16) -0.0049(12) -0.0166(13) 0.0082(12) C40 0.0464(15) 0.0437(15) 0.0543(17) -0.0041(12) 0.0012(12) -0.0113(12) O8 0.096(2) 0.0626(16) 0.090(2) -0.0356(14) -0.0298(16) 0.0113(14) O9 0.162(3) 0.096(2) 0.0546(17) -0.0182(15) 0.0154(19) -0.005(2) C37 0.080(2) 0.060(2) 0.055(2) -0.0112(16) -0.0230(18) 0.0172(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N4 1.9759(19) . ? Cu1 N1 1.9947(19) . ? Cu1 O1 2.0124(16) . ? Cu1 N3 2.068(2) . ? Cu1 N2 2.149(2) . ? O1 C31 1.259(3) . ? N1 C1 1.326(3) . ? N1 C5 1.356(3) . ? O2 C31 1.245(3) . ? N4 C13 1.331(3) . ? N4 C17 1.356(3) . ? O3 C32 1.317(3) . ? N3 C24 1.323(3) . ? N3 C18 1.356(3) . ? C5 C4 1.411(3) . ? C5 C6 1.430(3) . ? N2 C12 1.319(3) . ? N2 C6 1.362(3) . ? C31 C30 1.518(3) . ? C30 C29 1.390(3) . ? C30 C25 1.402(3) . ? O4 C32 1.197(3) . ? C4 C3 1.399(4) . ? C4 C9 1.441(4) . ? C6 C7 1.402(3) . ? C25 C26 1.388(3) . ? C25 C32 1.491(3) . ? C13 C14 1.401(4) . ? C13 H13 0.9300 . ? C19 C18 1.401(3) . ? C19 C22 1.404(4) . ? C19 C20 1.441(4) . ? C18 C17 1.428(3) . ? O6 C36 1.229(5) . ? C26 C27 1.386(4) . ? C26 H26 0.9300 . ? O5 C33 1.381(3) . ? O5 C28 1.392(3) . ? C14 C15 1.365(4) . ? C14 H14 0.9300 . ? C29 C28 1.381(3) . ? C29 H29 0.9300 . ? C15 C16 1.405(4) . ? C15 H15 0.9300 . ? C7 C10 1.404(4) . ? C7 C8 1.435(4) . ? C1 C2 1.404(4) . ? C1 H1 0.9300 . ? C17 C16 1.401(3) . ? C16 C21 1.424(4) . ? C27 C28 1.375(4) . ? C27 H27 0.9300 . ? C24 C23 1.394(4) . ? C24 H24 0.9300 . ? C12 C11 1.397(4) . ? C12 H12 0.9300 . ? C34 C33 1.378(4) . ? C34 C35 1.404(4) . ? C34 H34 0.9300 . ? C20 C21 1.348(4) . ? C20 H20 0.9300 . ? C11 C10 1.363(4) . ? C11 H11 0.9300 . ? C10 H10 0.9300 . ? C8 C9 1.342(5) . ? C8 H8 0.9300 . ? C22 C23 1.372(4) . ? C22 H22 0.9300 . ? C3 C2 1.366(4) . ? C3 H3 0.9300 . ? C23 H23 0.9300 . ? C2 H2 0.9300 . ? C33 C40 1.377(4) . ? C21 H21 0.9300 . ? O7 C36 1.286(5) . ? C35 C38 1.404(5) . ? C35 C36 1.531(4) . ? C9 H9 0.9300 . ? C39 C40 1.377(4) . ? C39 C38 1.387(4) . ? C39 H39 0.9300 . ? C38 C37 1.544(5) . ? C40 H40 0.9300 . ? O8 C37 1.292(5) . ? O9 C37 1.212(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Cu1 N1 175.77(8) . . ? N4 Cu1 O1 95.37(7) . . ? N1 Cu1 O1 88.86(7) . . ? N4 Cu1 N3 81.72(8) . . ? N1 Cu1 N3 95.10(8) . . ? O1 Cu1 N3 141.47(7) . . ? N4 Cu1 N2 98.15(8) . . ? N1 Cu1 N2 80.76(8) . . ? O1 Cu1 N2 101.66(7) . . ? N3 Cu1 N2 116.82(7) . . ? C31 O1 Cu1 131.85(15) . . ? C1 N1 C5 119.4(2) . . ? C1 N1 Cu1 126.14(17) . . ? C5 N1 Cu1 114.47(15) . . ? C13 N4 C17 118.6(2) . . ? C13 N4 Cu1 127.41(17) . . ? C17 N4 Cu1 113.99(15) . . ? C24 N3 C18 117.9(2) . . ? C24 N3 Cu1 131.24(17) . . ? C18 N3 Cu1 110.87(14) . . ? N1 C5 C4 121.9(2) . . ? N1 C5 C6 117.8(2) . . ? C4 C5 C6 120.2(2) . . ? C12 N2 C6 118.3(2) . . ? C12 N2 Cu1 132.21(17) . . ? C6 N2 Cu1 109.53(15) . . ? O2 C31 O1 127.2(2) . . ? O2 C31 C30 120.17(19) . . ? O1 C31 C30 112.67(18) . . ? C29 C30 C25 119.4(2) . . ? C29 C30 C31 119.48(19) . . ? C25 C30 C31 120.73(18) . . ? C3 C4 C5 117.7(2) . . ? C3 C4 C9 124.0(2) . . ? C5 C4 C9 118.2(3) . . ? N2 C6 C7 122.7(2) . . ? N2 C6 C5 117.2(2) . . ? C7 C6 C5 120.0(2) . . ? C26 C25 C30 120.0(2) . . ? C26 C25 C32 117.5(2) . . ? C30 C25 C32 122.4(2) . . ? N4 C13 C14 121.9(2) . . ? N4 C13 H13 119.1 . . ? C14 C13 H13 119.1 . . ? C18 C19 C22 117.3(2) . . ? C18 C19 C20 118.8(2) . . ? C22 C19 C20 123.9(2) . . ? N3 C18 C19 123.4(2) . . ? N3 C18 C17 116.8(2) . . ? C19 C18 C17 119.8(2) . . ? C27 C26 C25 120.2(2) . . ? C27 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? C33 O5 C28 117.40(19) . . ? C15 C14 C13 119.6(2) . . ? C15 C14 H14 120.2 . . ? C13 C14 H14 120.2 . . ? C28 C29 C30 119.3(2) . . ? C28 C29 H29 120.4 . . ? C30 C29 H29 120.4 . . ? C14 C15 C16 120.0(2) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C6 C7 C10 117.1(3) . . ? C6 C7 C8 118.7(3) . . ? C10 C7 C8 124.2(3) . . ? N1 C1 C2 121.7(3) . . ? N1 C1 H1 119.1 . . ? C2 C1 H1 119.1 . . ? O4 C32 O3 123.4(2) . . ? O4 C32 C25 123.3(2) . . ? O3 C32 C25 113.23(19) . . ? N4 C17 C16 123.2(2) . . ? N4 C17 C18 116.56(19) . . ? C16 C17 C18 120.2(2) . . ? C17 C16 C15 116.7(2) . . ? C17 C16 C21 118.8(2) . . ? C15 C16 C21 124.5(2) . . ? C28 C27 C26 119.2(2) . . ? C28 C27 H27 120.4 . . ? C26 C27 H27 120.4 . . ? C27 C28 C29 121.9(2) . . ? C27 C28 O5 117.9(2) . . ? C29 C28 O5 120.1(2) . . ? N3 C24 C23 122.6(2) . . ? N3 C24 H24 118.7 . . ? C23 C24 H24 118.7 . . ? N2 C12 C11 122.8(3) . . ? N2 C12 H12 118.6 . . ? C11 C12 H12 118.6 . . ? C33 C34 C35 121.6(3) . . ? C33 C34 H34 119.2 . . ? C35 C34 H34 119.2 . . ? C21 C20 C19 120.9(2) . . ? C21 C20 H20 119.6 . . ? C19 C20 H20 119.6 . . ? C10 C11 C12 119.2(3) . . ? C10 C11 H11 120.4 . . ? C12 C11 H11 120.4 . . ? C11 C10 C7 119.8(3) . . ? C11 C10 H10 120.1 . . ? C7 C10 H10 120.1 . . ? C9 C8 C7 121.7(3) . . ? C9 C8 H8 119.2 . . ? C7 C8 H8 119.2 . . ? C23 C22 C19 118.8(2) . . ? C23 C22 H22 120.6 . . ? C19 C22 H22 120.6 . . ? C2 C3 C4 119.6(2) . . ? C2 C3 H3 120.2 . . ? C4 C3 H3 120.2 . . ? C22 C23 C24 120.0(2) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C3 C2 C1 119.7(3) . . ? C3 C2 H2 120.1 . . ? C1 C2 H2 120.1 . . ? C40 C33 C34 120.1(3) . . ? C40 C33 O5 122.8(2) . . ? C34 C33 O5 117.0(3) . . ? C20 C21 C16 121.5(2) . . ? C20 C21 H21 119.3 . . ? C16 C21 H21 119.3 . . ? C38 C35 C34 118.4(2) . . ? C38 C35 C36 128.5(3) . . ? C34 C35 C36 113.1(3) . . ? C8 C9 C4 121.2(3) . . ? C8 C9 H9 119.4 . . ? C4 C9 H9 119.4 . . ? O6 C36 O7 122.6(3) . . ? O6 C36 C35 118.8(3) . . ? O7 C36 C35 118.6(4) . . ? C40 C39 C38 123.3(3) . . ? C40 C39 H39 118.3 . . ? C38 C39 H39 118.3 . . ? C39 C38 C35 118.1(3) . . ? C39 C38 C37 112.3(3) . . ? C35 C38 C37 129.6(3) . . ? C39 C40 C33 118.4(3) . . ? C39 C40 H40 120.8 . . ? C33 C40 H40 120.8 . . ? O9 C37 O8 124.1(4) . . ? O9 C37 C38 118.0(3) . . ? O8 C37 C38 118.0(4) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.478 _refine_diff_density_min -0.474 _refine_diff_density_rms 0.098 #===END #===END data_10030103 _database_code_depnum_ccdc_archive 'CCDC 787899' #TrackingRef '- Dalton Trans-gy.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H68 N4 O19 Zn2' _chemical_formula_weight 1255.94 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' 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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7725(9) _cell_length_b 11.5217(10) _cell_length_c 12.8609(13) _cell_angle_alpha 99.200(4) _cell_angle_beta 99.788(5) _cell_angle_gamma 91.110(5) _cell_volume 1407.0(2) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3189 _cell_measurement_theta_min 3.1993 _cell_measurement_theta_max 27.4797 _exptl_crystal_description Prism _exptl_crystal_colour White _exptl_crystal_size_max 0.2000 _exptl_crystal_size_mid 0.2000 _exptl_crystal_size_min 0.1500 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.482 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 656 _exptl_absorpt_coefficient_mu 0.933 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5434 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 'Rigaku Mercury 70 diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8692 _diffrn_reflns_av_R_equivalents 0.0353 _diffrn_reflns_av_sigmaI/netI 0.0543 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.43 _diffrn_reflns_theta_max 24.51 _reflns_number_total 4511 _reflns_number_gt 3682 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0634P)^2^+1.6287P] 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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4511 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0623 _refine_ls_R_factor_gt 0.0483 _refine_ls_wR_factor_ref 0.1337 _refine_ls_wR_factor_gt 0.1240 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.79996(5) 0.07830(4) 0.49905(3) 0.02689(17) Uani 1 1 d . . . O1 O 0.9020(3) 0.2128(2) 0.4700(2) 0.0299(6) Uani 1 1 d . . . O2 O 1.0610(3) 0.3062(3) 0.4062(2) 0.0469(8) Uani 1 1 d . . . O3 O 1.0522(4) -0.1334(3) 0.2774(3) 0.0482(9) Uani 1 1 d . . . O7 O 0.6731(3) 0.0284(3) 0.3598(2) 0.0374(7) Uani 1 1 d . . . O8 O 0.6461(3) -0.1409(3) 0.4171(2) 0.0377(7) Uani 1 1 d . . . O9 O 0.9196(3) -0.0160(3) 0.5871(2) 0.0354(7) Uani 1 1 d . . . O6 O 0.6509(3) 0.1198(3) 0.5826(2) 0.0418(8) Uani 1 1 d . . . O4 O 0.7354(3) 0.2522(3) 0.0416(2) 0.0427(8) Uani 1 1 d . . . O5 O 0.6947(3) 0.3116(3) 0.6507(2) 0.0472(8) Uani 1 1 d . . . C11 C 0.8415(4) 0.0662(4) 0.0662(3) 0.0316(9) Uani 1 1 d . . . H11 H 0.8173 0.0349 -0.0060 0.038 Uiso 1 1 calc R . . C12 C 0.9151(4) 0.0024(4) 0.1375(3) 0.0311(9) Uani 1 1 d . . . H12 H 0.9388 -0.0734 0.1122 0.037 Uiso 1 1 calc R . . C13 C 0.9553(4) 0.0476(4) 0.2459(3) 0.0253(9) Uani 1 1 d . . . C8 C 0.9211(4) 0.1622(3) 0.2836(3) 0.0231(8) Uani 1 1 d . . . C9 C 0.8453(4) 0.2260(4) 0.2125(3) 0.0286(9) Uani 1 1 d . . . H9 H 0.8215 0.3019 0.2371 0.034 Uiso 1 1 calc R . . C10 C 0.8047(4) 0.1781(4) 0.1056(3) 0.0284(9) Uani 1 1 d . . . C15 C 0.9682(4) 0.2296(4) 0.3961(3) 0.0274(9) Uani 1 1 d . . . C14 C 1.0344(4) -0.0303(4) 0.3166(3) 0.0290(9) Uani 1 1 d . . . C4 C 0.3472(4) -0.2018(4) 0.0547(3) 0.0296(9) Uani 1 1 d . . . C5 C 0.3144(4) -0.2307(4) 0.1479(3) 0.0300(9) Uani 1 1 d . . . H5 H 0.2360 -0.2787 0.1453 0.036 Uiso 1 1 calc R . . C6 C 0.3988(4) -0.1879(3) 0.2459(3) 0.0245(9) Uani 1 1 d . . . C1 C 0.5167(4) -0.1160(3) 0.2491(3) 0.0241(8) Uani 1 1 d . . . C2 C 0.5481(4) -0.0879(4) 0.1539(3) 0.0308(9) Uani 1 1 d . . . H2 H 0.6264 -0.0399 0.1557 0.037 Uiso 1 1 calc R . . C3 C 0.4638(4) -0.1309(4) 0.0563(3) 0.0331(10) Uani 1 1 d . . . H3 H 0.4853 -0.1123 -0.0069 0.040 Uiso 1 1 calc R . . C7 C 0.6176(4) -0.0750(4) 0.3505(3) 0.0275(9) Uani 1 1 d . . . C16 C 0.6524(4) 0.2118(4) 0.6541(3) 0.0315(10) Uani 1 1 d . . . N1 N 0.0085(4) 0.3521(3) -0.3273(3) 0.0466(10) Uani 1 1 d . . . H1A H -0.0388 0.3570 -0.3928 0.056 Uiso 1 1 calc R . . H1B H -0.0239 0.2869 -0.3074 0.056 Uiso 1 1 calc R . . N2 N 0.4311(4) 0.1791(4) 0.3952(3) 0.0505(11) Uani 1 1 d . . . H2A H 0.5122 0.1511 0.3805 0.061 Uiso 1 1 calc R . . H2B H 0.4105 0.1475 0.4507 0.061 Uiso 1 1 calc R . . C26 C 0.2406(5) 0.3359(5) -0.2236(4) 0.0514(13) Uani 1 1 d . . . H26A H 0.2120 0.2655 -0.1988 0.062 Uiso 1 1 calc R . . H26B H 0.3385 0.3317 -0.2280 0.062 Uiso 1 1 calc R . . C24 C 0.3122(5) 0.4511(5) -0.0363(4) 0.0479(12) Uani 1 1 d . . . H24A H 0.4061 0.4371 -0.0487 0.057 Uiso 1 1 calc R . . H24B H 0.3126 0.5315 0.0005 0.057 Uiso 1 1 calc R . . C17 C 0.4467(7) 0.3092(5) 0.4257(4) 0.0658(16) Uani 1 1 d . . . H17A H 0.5240 0.3299 0.4845 0.079 Uiso 1 1 calc R . . H17B H 0.3631 0.3387 0.4498 0.079 Uiso 1 1 calc R . . C22 C 0.3897(5) 0.3910(5) 0.1414(4) 0.0471(12) Uani 1 1 d . . . H22A H 0.4772 0.3640 0.1228 0.056 Uiso 1 1 calc R . . H22B H 0.4022 0.4751 0.1667 0.056 Uiso 1 1 calc R . . C23 C 0.2795(5) 0.3709(4) 0.0391(4) 0.0437(12) Uani 1 1 d . . . H23A H 0.2779 0.2895 0.0045 0.052 Uiso 1 1 calc R . . H23B H 0.1884 0.3865 0.0571 0.052 Uiso 1 1 calc R . . C19 C 0.3605(5) 0.3319(4) 0.2338(3) 0.0388(11) Uani 1 1 d . . . H19 H 0.2722 0.3597 0.2524 0.047 Uiso 1 1 calc R . . C20 C 0.3467(5) 0.1982(4) 0.2066(4) 0.0463(12) Uani 1 1 d . . . H20A H 0.2708 0.1753 0.1471 0.056 Uiso 1 1 calc R . . H20B H 0.4314 0.1688 0.1845 0.056 Uiso 1 1 calc R . . C18 C 0.4720(6) 0.3666(5) 0.3317(4) 0.0578(15) Uani 1 1 d . . . H18A H 0.4758 0.4515 0.3527 0.069 Uiso 1 1 calc R . . H18B H 0.5614 0.3444 0.3137 0.069 Uiso 1 1 calc R . . C28 C -0.0182(5) 0.4542(4) -0.2527(4) 0.0470(12) Uani 1 1 d . . . H28A H -0.1164 0.4538 -0.2486 0.056 Uiso 1 1 calc R . . H28B H 0.0054 0.5253 -0.2786 0.056 Uiso 1 1 calc R . . C29 C 0.0652(5) 0.4546(5) -0.1430(4) 0.0439(11) Uani 1 1 d . . . H29A H 0.0312 0.3900 -0.1129 0.053 Uiso 1 1 calc R . . H29B H 0.0517 0.5274 -0.0971 0.053 Uiso 1 1 calc R . . C25 C 0.2193(5) 0.4431(4) -0.1445(3) 0.0408(11) Uani 1 1 d . . . H25 H 0.2481 0.5108 -0.1744 0.049 Uiso 1 1 calc R . . C21 C 0.3201(5) 0.1428(4) 0.3006(4) 0.0468(12) Uani 1 1 d . . . H21A H 0.2311 0.1662 0.3187 0.056 Uiso 1 1 calc R . . H21B H 0.3158 0.0578 0.2810 0.056 Uiso 1 1 calc R . . C27 C 0.1575(5) 0.3405(5) -0.3334(4) 0.0545(14) Uani 1 1 d . . . H27A H 0.1914 0.4070 -0.3611 0.065 Uiso 1 1 calc R . . H27B H 0.1693 0.2693 -0.3820 0.065 Uiso 1 1 calc R . . O10 O 0.7968(8) 0.4694(5) 0.5069(4) 0.0504(19) 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 Zn1 0.0303(3) 0.0322(3) 0.0172(3) 0.00634(19) -0.00073(18) -0.0009(2) O1 0.0411(16) 0.0306(17) 0.0171(14) 0.0029(12) 0.0045(12) -0.0054(13) O2 0.058(2) 0.050(2) 0.0279(17) 0.0030(15) 0.0001(14) -0.0274(17) O3 0.060(2) 0.0303(19) 0.046(2) 0.0036(15) -0.0109(16) 0.0103(16) O7 0.0425(17) 0.045(2) 0.0215(15) 0.0034(13) 0.0006(12) -0.0141(15) O8 0.0387(17) 0.053(2) 0.0210(15) 0.0119(14) -0.0008(12) 0.0068(14) O9 0.0439(17) 0.0402(18) 0.0213(15) 0.0094(13) -0.0012(12) 0.0064(14) O6 0.0351(16) 0.061(2) 0.0256(16) -0.0062(16) 0.0087(12) -0.0061(15) O4 0.067(2) 0.0297(17) 0.0211(15) 0.0037(13) -0.0190(14) -0.0004(15) O5 0.054(2) 0.052(2) 0.0384(19) 0.0160(16) 0.0073(15) -0.0176(17) C11 0.042(2) 0.032(3) 0.017(2) 0.0007(17) -0.0008(17) -0.0006(19) C12 0.034(2) 0.033(2) 0.026(2) 0.0025(18) 0.0055(17) 0.0018(19) C13 0.025(2) 0.030(2) 0.021(2) 0.0082(17) 0.0002(15) -0.0021(17) C8 0.0261(19) 0.025(2) 0.0166(19) 0.0029(16) 0.0021(15) -0.0078(17) C9 0.035(2) 0.028(2) 0.022(2) 0.0062(17) 0.0008(16) 0.0031(18) C10 0.035(2) 0.030(2) 0.019(2) 0.0091(17) -0.0014(16) -0.0012(18) C15 0.032(2) 0.031(2) 0.019(2) 0.0082(17) 0.0010(16) -0.0046(19) C14 0.028(2) 0.030(3) 0.028(2) 0.0075(19) 0.0032(17) -0.0031(18) C4 0.041(2) 0.027(2) 0.016(2) 0.0014(17) -0.0058(16) 0.0039(19) C5 0.031(2) 0.030(2) 0.026(2) 0.0038(18) -0.0012(17) -0.0010(18) C6 0.028(2) 0.026(2) 0.0185(19) 0.0032(16) 0.0017(15) 0.0015(17) C1 0.030(2) 0.026(2) 0.0165(19) 0.0054(16) 0.0018(15) 0.0042(17) C2 0.035(2) 0.035(3) 0.022(2) 0.0072(18) 0.0037(17) 0.0014(19) C3 0.047(3) 0.035(3) 0.018(2) 0.0086(18) 0.0035(17) 0.002(2) C7 0.025(2) 0.040(3) 0.018(2) 0.0030(18) 0.0059(15) 0.0017(19) C16 0.023(2) 0.049(3) 0.021(2) 0.008(2) -0.0022(16) -0.004(2) N1 0.058(3) 0.042(2) 0.032(2) 0.0029(18) -0.0129(18) 0.003(2) N2 0.063(3) 0.063(3) 0.035(2) 0.027(2) 0.0138(19) 0.011(2) C26 0.048(3) 0.062(4) 0.041(3) 0.002(2) 0.001(2) 0.017(3) C24 0.050(3) 0.056(3) 0.036(3) 0.017(2) -0.007(2) -0.007(2) C17 0.093(4) 0.074(4) 0.027(3) 0.015(3) -0.005(3) -0.002(3) C22 0.058(3) 0.051(3) 0.033(3) 0.021(2) -0.003(2) -0.002(2) C23 0.044(3) 0.051(3) 0.036(3) 0.014(2) -0.002(2) 0.002(2) C19 0.046(3) 0.044(3) 0.027(2) 0.013(2) 0.0013(19) 0.004(2) C20 0.058(3) 0.052(3) 0.030(3) 0.014(2) 0.006(2) 0.005(2) C18 0.079(4) 0.058(4) 0.032(3) 0.017(2) -0.010(2) -0.014(3) C28 0.042(3) 0.045(3) 0.048(3) 0.005(2) -0.006(2) 0.007(2) C29 0.048(3) 0.046(3) 0.034(3) -0.002(2) 0.002(2) 0.007(2) C25 0.045(3) 0.044(3) 0.030(2) 0.009(2) -0.0048(19) -0.003(2) C21 0.048(3) 0.046(3) 0.053(3) 0.021(2) 0.013(2) 0.003(2) C27 0.062(3) 0.064(4) 0.034(3) 0.000(2) 0.005(2) 0.014(3) O10 0.116(6) 0.010(3) 0.020(3) 0.003(2) -0.003(3) -0.009(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O1 1.946(3) . ? Zn1 O9 1.956(3) . ? Zn1 O6 1.975(3) . ? Zn1 O7 1.991(3) . ? O1 C15 1.274(4) . ? O2 C15 1.228(5) . ? O3 C14 1.241(5) . ? O7 C7 1.279(5) . ? O8 C7 1.234(5) . ? O9 C14 1.269(5) 2_756 ? O6 C16 1.287(5) . ? O4 C10 1.387(5) . ? O4 C4 1.391(5) 2_655 ? O5 C16 1.223(5) . ? C11 C12 1.382(6) . ? C11 C10 1.385(6) . ? C12 C13 1.394(5) . ? C13 C8 1.400(6) . ? C13 C14 1.509(5) . ? C8 C9 1.389(5) . ? C8 C15 1.519(5) . ? C9 C10 1.384(5) . ? C14 O9 1.269(5) 2_756 ? C4 C5 1.380(6) . ? C4 C3 1.384(6) . ? C4 O4 1.391(5) 2_655 ? C5 C6 1.394(5) . ? C6 C1 1.398(5) . ? C6 C16 1.518(5) 2_656 ? C1 C2 1.395(5) . ? C1 C7 1.498(5) . ? C2 C3 1.390(6) . ? C16 C6 1.518(5) 2_656 ? N1 C28 1.452(6) . ? N1 C27 1.480(6) . ? N2 C21 1.484(6) . ? N2 C17 1.487(7) . ? C26 C25 1.511(7) . ? C26 C27 1.514(7) . ? C24 C23 1.509(6) . ? C24 C25 1.515(6) . ? C17 C18 1.521(7) . ? C22 C19 1.524(6) . ? C22 C23 1.535(6) . ? C19 C18 1.512(6) . ? C19 C20 1.523(7) . ? C20 C21 1.510(6) . ? C28 C29 1.504(6) . ? C29 C25 1.518(6) . ? 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 O9 111.87(12) . . ? O1 Zn1 O6 114.47(13) . . ? O9 Zn1 O6 103.18(13) . . ? O1 Zn1 O7 101.56(11) . . ? O9 Zn1 O7 129.56(13) . . ? O6 Zn1 O7 95.52(12) . . ? C15 O1 Zn1 134.2(3) . . ? C7 O7 Zn1 113.0(2) . . ? C14 O9 Zn1 117.1(3) 2_756 . ? C16 O6 Zn1 125.5(3) . . ? C10 O4 C4 118.3(3) . 2_655 ? C12 C11 C10 118.1(4) . . ? C11 C12 C13 122.4(4) . . ? C12 C13 C8 118.7(3) . . ? C12 C13 C14 117.9(4) . . ? C8 C13 C14 123.4(3) . . ? C9 C8 C13 119.0(3) . . ? C9 C8 C15 114.9(3) . . ? C13 C8 C15 125.9(3) . . ? C10 C9 C8 120.9(4) . . ? C9 C10 C11 120.8(4) . . ? C9 C10 O4 115.6(4) . . ? C11 C10 O4 123.4(3) . . ? O2 C15 O1 124.3(4) . . ? O2 C15 C8 115.9(3) . . ? O1 C15 C8 119.4(3) . . ? O3 C14 O9 124.4(4) . 2_756 ? O3 C14 C13 118.8(4) . . ? O9 C14 C13 116.8(4) 2_756 . ? C5 C4 C3 121.0(4) . . ? C5 C4 O4 118.0(4) . 2_655 ? C3 C4 O4 120.8(4) . 2_655 ? C4 C5 C6 120.1(4) . . ? C5 C6 C1 119.6(3) . . ? C5 C6 C16 117.1(3) . 2_656 ? C1 C6 C16 123.0(3) . 2_656 ? C2 C1 C6 119.4(4) . . ? C2 C1 C7 118.3(4) . . ? C6 C1 C7 122.2(3) . . ? C3 C2 C1 120.8(4) . . ? C4 C3 C2 119.1(4) . . ? O8 C7 O7 124.0(4) . . ? O8 C7 C1 120.4(4) . . ? O7 C7 C1 115.6(3) . . ? O5 C16 O6 127.1(4) . . ? O5 C16 C6 119.0(4) . 2_656 ? O6 C16 C6 113.9(4) . 2_656 ? C28 N1 C27 113.4(4) . . ? C21 N2 C17 111.7(4) . . ? C25 C26 C27 111.1(4) . . ? C23 C24 C25 119.0(4) . . ? N2 C17 C18 111.0(4) . . ? C19 C22 C23 116.9(4) . . ? C24 C23 C22 109.9(4) . . ? C18 C19 C20 108.8(4) . . ? C18 C19 C22 111.2(4) . . ? C20 C19 C22 113.6(4) . . ? C21 C20 C19 112.0(4) . . ? C19 C18 C17 112.8(4) . . ? N1 C28 C29 111.3(4) . . ? C28 C29 C25 112.5(4) . . ? C26 C25 C24 113.7(4) . . ? C26 C25 C29 109.6(4) . . ? C24 C25 C29 115.9(4) . . ? N2 C21 C20 111.3(4) . . ? N1 C27 C26 110.1(4) . . ? _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 24.51 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 0.813 _refine_diff_density_min -0.472 _refine_diff_density_rms 0.076