# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_a4 _database_code_depnum_ccdc_archive 'CCDC 915950' #TrackingRef '4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H28 Cd2 N4 O16' _chemical_formula_weight 877.32 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M c2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 13.777(4) _cell_length_b 12.017(3) _cell_length_c 18.451(5) _cell_angle_alpha 90.00 _cell_angle_beta 101.020(4) _cell_angle_gamma 90.00 _cell_volume 2998.2(14) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.944 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1744 _exptl_absorpt_coefficient_mu 1.504 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7735 _exptl_absorpt_correction_T_max 0.7948 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9656 _diffrn_reflns_av_R_equivalents 0.0160 _diffrn_reflns_av_sigmaI/netI 0.0198 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 28.16 _reflns_number_total 3643 _reflns_number_gt 3422 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^ > 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^)+(0.0532P)^2^+1.6541P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3643 _refine_ls_number_parameters 238 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0226 _refine_ls_R_factor_gt 0.0210 _refine_ls_wR_factor_ref 0.0836 _refine_ls_wR_factor_gt 0.0825 _refine_ls_goodness_of_fit_ref 1.219 _refine_ls_restrained_S_all 1.219 _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 Cd1 Cd 1.0000 0.465606(13) 0.7500 0.01077(4) Uani 1 2 d S . . Cd2 Cd 0.7500 0.2500 1.0000 0.01178(4) Uani 1 2 d S . . O1 O 0.99575(9) 0.61489(10) 0.83006(7) 0.0157(3) Uani 1 1 d . . . O4 O 0.87274(10) -0.09711(10) 0.70678(7) 0.0167(3) Uani 1 1 d . . . N2 N 0.92446(10) 0.40149(11) 0.83907(8) 0.0107(3) Uani 1 1 d . . . O3 O 0.85420(10) 0.08536(10) 0.63289(7) 0.0158(3) Uani 1 1 d . . . C1 C 0.88151(12) 0.30920(13) 0.86053(9) 0.0101(3) Uani 1 1 d . . . C6 C 0.86698(12) 0.09788(14) 0.70756(9) 0.0123(3) Uani 1 1 d . . . O2 O 0.94532(9) 0.66859(10) 0.93172(7) 0.0157(3) Uani 1 1 d . . . H2 H 0.9197 0.6404 0.9639 0.024 Uiso 1 1 calc R . . N1 N 0.84354(10) 0.32626(12) 0.92220(8) 0.0115(3) Uani 1 1 d . . . C10 C 0.91280(12) 0.48197(14) 0.88899(9) 0.0109(3) Uani 1 1 d . . . C2 C 0.88061(12) 0.20114(14) 0.82238(9) 0.0115(3) Uani 1 1 d . . . C9 C 0.86328(12) 0.43562(14) 0.94039(9) 0.0106(3) Uani 1 1 d . . . C8 C 0.95375(12) 0.59458(14) 0.88255(9) 0.0123(3) Uani 1 1 d . . . C3 C 0.89216(12) 0.10270(14) 0.86194(10) 0.0131(3) Uani 1 1 d . . . H3 H 0.9005 0.1042 0.9131 0.016 Uiso 1 1 calc R . . C4 C 0.89138(12) 0.00084(14) 0.82505(10) 0.0137(3) Uani 1 1 d . . . H4 H 0.9001 -0.0651 0.8519 0.016 Uiso 1 1 calc R . . C5 C 0.87754(12) -0.00234(14) 0.74813(10) 0.0126(3) Uani 1 1 d . . . C7 C 0.86939(12) 0.19892(14) 0.74461(9) 0.0119(3) Uani 1 1 d . . . H7 H 0.8636 0.2652 0.7181 0.014 Uiso 1 1 calc R . . O6 O 0.89715(10) 0.16665(11) 1.06173(8) 0.0185(3) Uani 1 1 d . . . C15 C 0.84780(14) 0.18546(15) 0.59005(10) 0.0180(4) Uani 1 1 d . . . H15A H 0.7920 0.2284 0.5980 0.027 Uiso 1 1 calc R . . H15B H 0.8399 0.1669 0.5386 0.027 Uiso 1 1 calc R . . H15C H 0.9072 0.2281 0.6048 0.027 Uiso 1 1 calc R . . C14 C 0.87079(14) -0.20040(15) 0.74556(11) 0.0188(4) Uani 1 1 d . . . H14A H 0.9312 -0.2088 0.7809 0.028 Uiso 1 1 calc R . . H14B H 0.8640 -0.2609 0.7110 0.028 Uiso 1 1 calc R . . H14C H 0.8159 -0.2005 0.7707 0.028 Uiso 1 1 calc R . . O7 O 0.85872(9) 0.58641(11) 1.02243(7) 0.0160(3) Uani 1 1 d . . . O8 O 0.83472(10) 0.46801(12) 0.68404(8) 0.0209(3) Uani 1 1 d . . . C16 C 0.83580(12) 0.48471(15) 1.00658(10) 0.0125(3) Uani 1 1 d . . . O9 O 0.79345(9) 0.42560(11) 1.04725(7) 0.0157(3) Uani 1 1 d . . . H1W H 0.942(2) 0.223(3) 1.0692(18) 0.048(9) Uiso 1 1 d . . . H3W H 0.825(3) 0.483(3) 0.651(2) 0.074(14) Uiso 1 1 d . . . H2W H 0.897(2) 0.129(3) 1.0959(18) 0.046(9) Uiso 1 1 d . . . H4W H 0.7889(19) 0.488(2) 0.7059(13) 0.018(6) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.01248(8) 0.01094(8) 0.01042(8) 0.000 0.00609(6) 0.000 Cd2 0.01449(8) 0.01146(8) 0.01075(8) 0.00025(5) 0.00585(7) -0.00273(5) O1 0.0219(6) 0.0123(5) 0.0156(6) 0.0009(4) 0.0102(5) -0.0012(5) O4 0.0246(6) 0.0096(5) 0.0164(6) -0.0023(5) 0.0054(5) 0.0003(5) N2 0.0130(6) 0.0103(6) 0.0098(6) 0.0009(5) 0.0046(5) 0.0004(5) O3 0.0247(6) 0.0135(5) 0.0096(5) -0.0010(4) 0.0045(5) -0.0014(5) C1 0.0106(6) 0.0106(7) 0.0095(7) -0.0003(6) 0.0033(5) 0.0005(5) C6 0.0115(7) 0.0138(7) 0.0124(7) -0.0012(6) 0.0039(6) -0.0006(6) O2 0.0231(6) 0.0111(6) 0.0159(6) -0.0019(4) 0.0107(5) -0.0034(5) N1 0.0130(6) 0.0118(6) 0.0104(6) 0.0009(5) 0.0043(5) -0.0008(5) C10 0.0114(7) 0.0112(7) 0.0112(7) 0.0007(6) 0.0052(6) 0.0002(6) C2 0.0103(6) 0.0117(7) 0.0138(7) -0.0028(6) 0.0057(6) -0.0005(5) C9 0.0123(7) 0.0104(7) 0.0100(7) 0.0000(6) 0.0043(6) -0.0005(6) C8 0.0133(7) 0.0108(7) 0.0127(7) 0.0003(6) 0.0026(6) 0.0000(6) C3 0.0145(7) 0.0132(7) 0.0130(7) -0.0007(6) 0.0062(6) -0.0016(6) C4 0.0142(7) 0.0106(7) 0.0173(8) 0.0013(6) 0.0054(6) 0.0008(6) C5 0.0126(7) 0.0106(7) 0.0155(8) -0.0022(6) 0.0052(6) -0.0010(6) C7 0.0128(7) 0.0111(7) 0.0125(7) 0.0001(6) 0.0038(6) -0.0009(6) O6 0.0199(6) 0.0179(6) 0.0174(6) 0.0040(5) 0.0028(5) -0.0023(5) C15 0.0242(9) 0.0177(8) 0.0120(8) 0.0020(6) 0.0028(7) -0.0008(7) C14 0.0236(8) 0.0103(7) 0.0244(9) -0.0021(7) 0.0097(7) -0.0009(6) O7 0.0213(6) 0.0133(6) 0.0156(6) -0.0046(5) 0.0087(5) -0.0025(5) O8 0.0141(6) 0.0341(8) 0.0153(6) 0.0093(5) 0.0046(5) 0.0028(5) C16 0.0121(7) 0.0142(7) 0.0116(7) -0.0006(6) 0.0031(6) -0.0005(6) O9 0.0200(6) 0.0162(6) 0.0129(6) -0.0032(5) 0.0087(5) -0.0042(5) _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 Cd1 N2 2.2431(15) 2_756 ? Cd1 N2 2.2431(15) . ? Cd1 O1 2.3317(13) . ? Cd1 O1 2.3317(13) 2_756 ? Cd1 O8 2.3680(15) . ? Cd1 O8 2.3680(15) 2_756 ? Cd2 N1 2.2952(15) 7_657 ? Cd2 N1 2.2952(15) . ? Cd2 O9 2.3177(14) 7_657 ? Cd2 O9 2.3177(14) . ? Cd2 O6 2.3511(14) . ? Cd2 O6 2.3511(14) 7_657 ? O1 C8 1.244(2) . ? O4 C5 1.365(2) . ? O4 C14 1.435(2) . ? N2 C1 1.351(2) . ? N2 C10 1.366(2) . ? O3 C6 1.364(2) . ? O3 C15 1.433(2) . ? C1 N1 1.356(2) . ? C1 C2 1.476(2) . ? C6 C7 1.391(2) . ? C6 C5 1.411(2) . ? O2 C8 1.291(2) . ? O2 H2 0.8200 . ? N1 C9 1.371(2) . ? C10 C9 1.386(2) . ? C10 C8 1.480(2) . ? C2 C3 1.383(2) . ? C2 C7 1.414(2) . ? C9 C16 1.470(2) . ? C3 C4 1.400(2) . ? C3 H3 0.9300 . ? C4 C5 1.396(3) . ? C4 H4 0.9300 . ? C7 H7 0.9300 . ? O6 H1W 0.91(3) . ? O6 H2W 0.77(3) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? O7 C16 1.282(2) . ? O8 H3W 0.63(4) . ? O8 H4W 0.85(3) . ? C16 O9 1.255(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 N2 Cd1 N2 139.82(7) 2_756 . ? N2 Cd1 O1 143.11(5) 2_756 . ? N2 Cd1 O1 74.26(5) . . ? N2 Cd1 O1 74.26(5) 2_756 2_756 ? N2 Cd1 O1 143.11(5) . 2_756 ? O1 Cd1 O1 79.40(7) . 2_756 ? N2 Cd1 O8 99.37(5) 2_756 . ? N2 Cd1 O8 81.11(5) . . ? O1 Cd1 O8 100.26(5) . . ? O1 Cd1 O8 78.65(5) 2_756 . ? N2 Cd1 O8 81.11(5) 2_756 2_756 ? N2 Cd1 O8 99.37(5) . 2_756 ? O1 Cd1 O8 78.65(5) . 2_756 ? O1 Cd1 O8 100.26(5) 2_756 2_756 ? O8 Cd1 O8 178.60(7) . 2_756 ? N1 Cd2 N1 180.0 7_657 . ? N1 Cd2 O9 74.71(5) 7_657 7_657 ? N1 Cd2 O9 105.29(5) . 7_657 ? N1 Cd2 O9 105.29(5) 7_657 . ? N1 Cd2 O9 74.71(5) . . ? O9 Cd2 O9 180.0 7_657 . ? N1 Cd2 O6 93.56(5) 7_657 . ? N1 Cd2 O6 86.44(5) . . ? O9 Cd2 O6 86.05(5) 7_657 . ? O9 Cd2 O6 93.95(5) . . ? N1 Cd2 O6 86.44(5) 7_657 7_657 ? N1 Cd2 O6 93.56(5) . 7_657 ? O9 Cd2 O6 93.95(5) 7_657 7_657 ? O9 Cd2 O6 86.05(5) . 7_657 ? O6 Cd2 O6 180.0 . 7_657 ? C8 O1 Cd1 114.46(11) . . ? C5 O4 C14 116.51(14) . . ? C1 N2 C10 105.60(14) . . ? C1 N2 Cd1 141.90(11) . . ? C10 N2 Cd1 112.44(11) . . ? C6 O3 C15 116.57(14) . . ? N2 C1 N1 112.49(14) . . ? N2 C1 C2 123.12(15) . . ? N1 C1 C2 124.33(15) . . ? O3 C6 C7 125.40(15) . . ? O3 C6 C5 114.97(15) . . ? C7 C6 C5 119.62(16) . . ? C8 O2 H2 109.5 . . ? C1 N1 C9 105.08(14) . . ? C1 N1 Cd2 144.82(11) . . ? C9 N1 Cd2 109.78(11) . . ? N2 C10 C9 108.27(14) . . ? N2 C10 C8 119.84(15) . . ? C9 C10 C8 131.87(16) . . ? C3 C2 C7 119.91(15) . . ? C3 C2 C1 120.74(16) . . ? C7 C2 C1 119.34(15) . . ? N1 C9 C10 108.55(15) . . ? N1 C9 C16 121.19(15) . . ? C10 C9 C16 130.22(16) . . ? O1 C8 O2 121.99(15) . . ? O1 C8 C10 118.91(15) . . ? O2 C8 C10 119.11(15) . . ? C2 C3 C4 120.13(16) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? C5 C4 C3 120.35(16) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? O4 C5 C4 125.00(16) . . ? O4 C5 C6 115.25(15) . . ? C4 C5 C6 119.75(16) . . ? C6 C7 C2 120.20(15) . . ? C6 C7 H7 119.9 . . ? C2 C7 H7 119.9 . . ? Cd2 O6 H1W 104(2) . . ? Cd2 O6 H2W 120(2) . . ? H1W O6 H2W 115(3) . . ? O3 C15 H15A 109.5 . . ? O3 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? O3 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O4 C14 H14A 109.5 . . ? O4 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O4 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Cd1 O8 H3W 121(4) . . ? Cd1 O8 H4W 119.3(16) . . ? H3W O8 H4W 110(4) . . ? O9 C16 O7 121.71(16) . . ? O9 C16 C9 119.51(16) . . ? O7 C16 C9 118.74(16) . . ? C16 O9 Cd2 113.99(11) . . ? 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 N2 Cd1 O1 C8 -162.83(11) 2_756 . . . ? N2 Cd1 O1 C8 -1.59(11) . . . . ? O1 Cd1 O1 C8 152.31(14) 2_756 . . . ? O8 Cd1 O1 C8 76.05(12) . . . . ? O8 Cd1 O1 C8 -104.84(12) 2_756 . . . ? N2 Cd1 N2 C1 -18.25(16) 2_756 . . . ? O1 Cd1 N2 C1 179.16(18) . . . . ? O1 Cd1 N2 C1 133.08(16) 2_756 . . . ? O8 Cd1 N2 C1 75.78(18) . . . . ? O8 Cd1 N2 C1 -105.54(17) 2_756 . . . ? N2 Cd1 N2 C10 165.15(11) 2_756 . . . ? O1 Cd1 N2 C10 2.56(10) . . . . ? O1 Cd1 N2 C10 -43.52(14) 2_756 . . . ? O8 Cd1 N2 C10 -100.82(11) . . . . ? O8 Cd1 N2 C10 77.86(11) 2_756 . . . ? C10 N2 C1 N1 -0.52(18) . . . . ? Cd1 N2 C1 N1 -177.25(13) . . . . ? C10 N2 C1 C2 -177.97(15) . . . . ? Cd1 N2 C1 C2 5.3(3) . . . . ? C15 O3 C6 C7 3.3(2) . . . . ? C15 O3 C6 C5 -177.20(15) . . . . ? N2 C1 N1 C9 0.29(18) . . . . ? C2 C1 N1 C9 177.71(15) . . . . ? N2 C1 N1 Cd2 172.53(14) . . . . ? C2 C1 N1 Cd2 -10.1(3) . . . . ? N1 Cd2 N1 C1 -142(100) 7_657 . . . ? O9 Cd2 N1 C1 0.9(2) 7_657 . . . ? O9 Cd2 N1 C1 -179.1(2) . . . . ? O6 Cd2 N1 C1 85.77(19) . . . . ? O6 Cd2 N1 C1 -94.23(19) 7_657 . . . ? N1 Cd2 N1 C9 30(100) 7_657 . . . ? O9 Cd2 N1 C9 172.88(10) 7_657 . . . ? O9 Cd2 N1 C9 -7.12(10) . . . . ? O6 Cd2 N1 C9 -102.20(11) . . . . ? O6 Cd2 N1 C9 77.80(11) 7_657 . . . ? C1 N2 C10 C9 0.52(17) . . . . ? Cd1 N2 C10 C9 178.35(10) . . . . ? C1 N2 C10 C8 178.72(14) . . . . ? Cd1 N2 C10 C8 -3.45(18) . . . . ? N2 C1 C2 C3 141.65(17) . . . . ? N1 C1 C2 C3 -35.5(2) . . . . ? N2 C1 C2 C7 -37.3(2) . . . . ? N1 C1 C2 C7 145.53(16) . . . . ? C1 N1 C9 C10 0.05(17) . . . . ? Cd2 N1 C9 C10 -175.21(10) . . . . ? C1 N1 C9 C16 -177.97(15) . . . . ? Cd2 N1 C9 C16 6.78(18) . . . . ? N2 C10 C9 N1 -0.36(18) . . . . ? C8 C10 C9 N1 -178.27(16) . . . . ? N2 C10 C9 C16 177.41(16) . . . . ? C8 C10 C9 C16 -0.5(3) . . . . ? Cd1 O1 C8 O2 179.97(12) . . . . ? Cd1 O1 C8 C10 0.35(19) . . . . ? N2 C10 C8 O1 2.2(2) . . . . ? C9 C10 C8 O1 179.87(17) . . . . ? N2 C10 C8 O2 -177.47(14) . . . . ? C9 C10 C8 O2 0.2(3) . . . . ? C7 C2 C3 C4 -0.9(2) . . . . ? C1 C2 C3 C4 -179.86(15) . . . . ? C2 C3 C4 C5 -0.9(3) . . . . ? C14 O4 C5 C4 7.3(2) . . . . ? C14 O4 C5 C6 -172.45(15) . . . . ? C3 C4 C5 O4 -178.04(16) . . . . ? C3 C4 C5 C6 1.7(2) . . . . ? O3 C6 C5 O4 -0.4(2) . . . . ? C7 C6 C5 O4 179.09(15) . . . . ? O3 C6 C5 C4 179.77(15) . . . . ? C7 C6 C5 C4 -0.7(2) . . . . ? O3 C6 C7 C2 178.37(15) . . . . ? C5 C6 C7 C2 -1.1(2) . . . . ? C3 C2 C7 C6 1.9(2) . . . . ? C1 C2 C7 C6 -179.10(15) . . . . ? N1 C9 C16 O9 0.0(2) . . . . ? C10 C9 C16 O9 -177.57(17) . . . . ? N1 C9 C16 O7 177.81(15) . . . . ? C10 C9 C16 O7 0.3(3) . . . . ? O7 C16 O9 Cd2 175.35(12) . . . . ? C9 C16 O9 Cd2 -6.87(19) . . . . ? N1 Cd2 O9 C16 -172.30(12) 7_657 . . . ? N1 Cd2 O9 C16 7.70(12) . . . . ? O9 Cd2 O9 C16 -87(100) 7_657 . . . ? O6 Cd2 O9 C16 92.92(12) . . . . ? O6 Cd2 O9 C16 -87.08(12) 7_657 . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O6 H2W O4 0.77(3) 2.17(3) 2.884(2) 154(3) 6_556 O2 H2 O7 0.82 1.62 2.4419(18) 174.6 . O8 H3W O7 0.63(4) 2.63(4) 3.131(2) 138(5) 6_565 O8 H3W O9 0.63(4) 2.17(4) 2.789(2) 166(5) 6_565 O6 H1W O2 0.91(3) 2.03(3) 2.9231(19) 167(3) 5_767 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 28.16 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.617 _refine_diff_density_min -0.775 _refine_diff_density_rms 0.146 data_a5 _database_code_depnum_ccdc_archive 'CCDC 915952' #TrackingRef '5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H18 N4 O6 Zn' _chemical_formula_weight 535.80 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 P2(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 11.949(2) _cell_length_b 16.406(3) _cell_length_c 12.630(2) _cell_angle_alpha 90.00 _cell_angle_beta 117.449(2) _cell_angle_gamma 90.00 _cell_volume 2197.3(7) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _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 1096 _exptl_absorpt_coefficient_mu 1.171 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7996 _exptl_absorpt_correction_T_max 0.8169 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14658 _diffrn_reflns_av_R_equivalents 0.0377 _diffrn_reflns_av_sigmaI/netI 0.0482 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 28.26 _reflns_number_total 5387 _reflns_number_gt 4724 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^ > 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^)+(0.0436P)^2^+1.1555P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5387 _refine_ls_number_parameters 331 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0406 _refine_ls_R_factor_gt 0.0345 _refine_ls_wR_factor_ref 0.0932 _refine_ls_wR_factor_gt 0.0897 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _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 0.844737(14) 0.235971(10) 0.790134(13) 0.01180(4) Uani 1 1 d . . . O5 O 0.82567(10) 0.12756(7) 0.87842(9) 0.0178(2) Uani 1 1 d . . . O6 O 0.89993(10) 0.07265(6) 1.05990(9) 0.0180(2) Uani 1 1 d . . . N3 N 0.66001(11) 0.22769(7) 0.64269(10) 0.0118(2) Uani 1 1 d . . . N5 N 1.00308(11) 0.24861(7) 0.95818(10) 0.0120(2) Uani 1 1 d . . . N2 N 0.87274(11) 0.33749(7) 0.69255(10) 0.0133(2) Uani 1 1 d . . . C18 C 0.65913(13) 0.13333(8) 0.38414(12) 0.0128(3) Uani 1 1 d . . . H18 H 0.6617 0.1835 0.3511 0.015 Uiso 1 1 calc R . . C13 C 0.63644(13) 0.12988(8) 0.48305(11) 0.0120(3) Uani 1 1 d . . . C14 C 0.63882(14) 0.05536(9) 0.53556(12) 0.0154(3) Uani 1 1 d . . . H14 H 0.6302 0.0533 0.6050 0.018 Uiso 1 1 calc R . . C6 C 0.94563(13) 0.22708(8) 0.61645(12) 0.0132(3) Uani 1 1 d . . . C19 C 0.60158(12) 0.20382(8) 0.52747(11) 0.0112(3) Uani 1 1 d . . . C20 C 0.90160(13) 0.12676(9) 0.98654(12) 0.0141(3) Uani 1 1 d . . . N1 N 0.93314(11) 0.17840(7) 0.69699(10) 0.0144(3) Uani 1 1 d . . . C16 C 0.66944(13) -0.01373(8) 0.38287(12) 0.0136(3) Uani 1 1 d . . . C17 C 0.67789(13) 0.06231(9) 0.33501(11) 0.0132(3) Uani 1 1 d . . . C4 C 0.91619(14) 0.36369(9) 0.52597(12) 0.0175(3) Uani 1 1 d . . . C3 C 0.88040(15) 0.44568(10) 0.52558(14) 0.0212(3) Uani 1 1 d . . . H3 H 0.8794 0.4816 0.4683 0.025 Uiso 1 1 calc R . . C1 C 0.84439(13) 0.41580(9) 0.69199(13) 0.0161(3) Uani 1 1 d . . . H1 H 0.8216 0.4343 0.7490 0.019 Uiso 1 1 calc R . . C5 C 0.90975(13) 0.31168(9) 0.61167(11) 0.0131(3) Uani 1 1 d . . . C21 C 0.99832(12) 0.19069(8) 1.03397(11) 0.0119(3) Uani 1 1 d . . . C7 C 0.96821(14) 0.10085(9) 0.70412(13) 0.0193(3) Uani 1 1 d . . . H7 H 0.9583 0.0669 0.7582 0.023 Uiso 1 1 calc R . . C8 C 1.01946(15) 0.06834(10) 0.63338(15) 0.0238(4) Uani 1 1 d . . . H8 H 1.0452 0.0142 0.6422 0.029 Uiso 1 1 calc R . . C15 C 0.65409(14) -0.01673(8) 0.48492(12) 0.0157(3) Uani 1 1 d . . . H15 H 0.6539 -0.0667 0.5197 0.019 Uiso 1 1 calc R . . C10 C 0.99244(14) 0.19903(9) 0.53958(12) 0.0172(3) Uani 1 1 d . . . C2 C 0.84722(14) 0.47191(9) 0.60970(14) 0.0207(3) Uani 1 1 d . . . H2 H 0.8267 0.5263 0.6124 0.025 Uiso 1 1 calc R . . C11 C 1.00000(15) 0.25425(10) 0.45483(13) 0.0221(3) Uani 1 1 d . . . H11 H 1.0319 0.2358 0.4044 0.027 Uiso 1 1 calc R . . C12 C 0.96163(15) 0.33247(10) 0.44706(13) 0.0219(3) Uani 1 1 d . . . H12 H 0.9648 0.3665 0.3896 0.026 Uiso 1 1 calc R . . C9 C 1.03128(15) 0.11692(10) 0.55132(14) 0.0221(3) Uani 1 1 d . . . H9 H 1.0647 0.0960 0.5035 0.026 Uiso 1 1 calc R . . O2 O 0.73524(9) 0.31568(6) 0.84670(8) 0.0154(2) Uani 1 1 d . . . C23 C 0.59404(12) 0.29456(8) 0.64675(11) 0.0117(3) Uani 1 1 d . . . C24 C 0.63475(13) 0.33855(8) 0.76011(11) 0.0129(3) Uani 1 1 d . . . O4 O 0.70127(10) 0.05932(6) 0.23903(9) 0.0178(2) Uani 1 1 d . . . O3 O 0.67853(10) -0.08070(6) 0.32298(9) 0.0167(2) Uani 1 1 d . . . C25 C 0.74231(14) 0.13333(9) 0.20869(13) 0.0189(3) Uani 1 1 d . . . H25A H 0.8166 0.1527 0.2765 0.028 Uiso 1 1 calc R . . H25B H 0.6768 0.1735 0.1854 0.028 Uiso 1 1 calc R . . H25C H 0.7612 0.1236 0.1437 0.028 Uiso 1 1 calc R . . C26 C 0.65452(16) -0.15784(9) 0.36174(13) 0.0214(3) Uani 1 1 d . . . H26A H 0.5714 -0.1577 0.3557 0.032 Uiso 1 1 calc R . . H26B H 0.7156 -0.1672 0.4432 0.032 Uiso 1 1 calc R . . H26C H 0.6604 -0.2004 0.3123 0.032 Uiso 1 1 calc R . . O1 O 0.56630(10) 0.39721(7) 0.76399(9) 0.0175(2) Uani 1 1 d . . . H41 H 0.977(3) 0.0830(18) 1.150(3) 0.070(9) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.01121(8) 0.01517(8) 0.00634(7) 0.00056(5) 0.00175(6) -0.00037(6) O5 0.0161(5) 0.0219(5) 0.0102(4) 0.0013(4) 0.0015(4) -0.0056(4) O6 0.0174(5) 0.0208(5) 0.0133(4) 0.0042(4) 0.0048(4) -0.0055(4) N3 0.0119(5) 0.0141(5) 0.0079(4) -0.0015(4) 0.0032(4) -0.0007(4) N5 0.0121(5) 0.0145(5) 0.0081(5) 0.0011(4) 0.0034(4) -0.0013(4) N2 0.0105(5) 0.0159(5) 0.0105(5) -0.0011(4) 0.0023(4) 0.0006(4) C18 0.0123(6) 0.0139(6) 0.0106(5) 0.0006(4) 0.0039(5) 0.0004(5) C13 0.0114(6) 0.0144(6) 0.0075(5) -0.0016(4) 0.0021(4) 0.0007(5) C14 0.0199(6) 0.0166(6) 0.0099(5) 0.0005(5) 0.0071(5) 0.0021(5) C6 0.0103(6) 0.0163(6) 0.0098(5) -0.0022(5) 0.0019(5) -0.0014(5) C19 0.0115(6) 0.0131(6) 0.0083(5) -0.0005(4) 0.0040(4) -0.0009(5) C20 0.0128(6) 0.0170(6) 0.0124(5) 0.0014(5) 0.0057(5) -0.0006(5) N1 0.0118(5) 0.0166(5) 0.0109(5) -0.0002(4) 0.0020(4) 0.0000(5) C16 0.0132(6) 0.0150(6) 0.0100(5) -0.0015(4) 0.0032(5) 0.0020(5) C17 0.0129(6) 0.0178(6) 0.0079(5) -0.0004(4) 0.0039(4) 0.0003(5) C4 0.0161(6) 0.0223(7) 0.0107(6) 0.0027(5) 0.0031(5) -0.0007(6) C3 0.0193(7) 0.0218(7) 0.0193(6) 0.0097(5) 0.0061(6) 0.0009(6) C1 0.0131(6) 0.0164(6) 0.0174(6) -0.0007(5) 0.0059(5) 0.0006(5) C5 0.0112(6) 0.0165(6) 0.0087(5) -0.0001(4) 0.0021(5) -0.0003(5) C21 0.0113(6) 0.0150(6) 0.0090(5) 0.0017(4) 0.0043(4) 0.0008(5) C7 0.0199(7) 0.0162(6) 0.0191(6) 0.0004(5) 0.0066(5) 0.0004(6) C8 0.0228(7) 0.0172(7) 0.0298(8) -0.0056(6) 0.0108(6) 0.0021(6) C15 0.0211(7) 0.0134(6) 0.0118(5) 0.0016(5) 0.0068(5) 0.0024(5) C10 0.0145(6) 0.0217(7) 0.0137(6) -0.0063(5) 0.0049(5) -0.0041(6) C2 0.0166(7) 0.0157(6) 0.0266(7) 0.0065(6) 0.0074(6) 0.0040(6) C11 0.0224(7) 0.0326(8) 0.0136(6) -0.0061(5) 0.0104(5) -0.0058(6) C12 0.0239(7) 0.0298(8) 0.0119(6) 0.0013(5) 0.0081(5) -0.0051(6) C9 0.0191(7) 0.0253(7) 0.0223(7) -0.0105(6) 0.0099(5) -0.0008(6) O2 0.0154(4) 0.0208(5) 0.0078(4) -0.0024(3) 0.0034(3) -0.0002(4) C23 0.0114(6) 0.0142(6) 0.0098(5) -0.0012(4) 0.0050(4) -0.0001(5) C24 0.0144(6) 0.0156(6) 0.0101(5) -0.0024(4) 0.0067(5) -0.0034(5) O4 0.0275(5) 0.0166(5) 0.0156(4) -0.0009(3) 0.0153(4) -0.0004(4) O3 0.0251(5) 0.0134(4) 0.0127(4) -0.0019(3) 0.0097(4) 0.0017(4) C25 0.0203(6) 0.0227(7) 0.0166(6) 0.0014(5) 0.0110(5) -0.0015(6) C26 0.0348(8) 0.0134(6) 0.0155(6) -0.0011(5) 0.0113(6) 0.0002(6) O1 0.0172(5) 0.0230(5) 0.0107(4) -0.0050(4) 0.0049(4) 0.0029(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N5 2.1037(11) . ? Zn1 N1 2.1302(13) . ? Zn1 N3 2.1375(11) . ? Zn1 O5 2.1664(11) . ? Zn1 N2 2.1875(13) . ? Zn1 O2 2.1896(11) . ? O5 C20 1.2433(16) . ? O6 C20 1.2899(18) . ? O6 H41 1.10(3) . ? N3 C19 1.3498(17) . ? N3 C23 1.3656(18) . ? N5 C19 1.3456(17) 4_666 ? N5 C21 1.3685(18) . ? N2 C1 1.3280(19) . ? N2 C5 1.3544(19) . ? C18 C17 1.386(2) . ? C18 C13 1.396(2) . ? C18 H18 0.9300 . ? C13 C14 1.385(2) . ? C13 C19 1.4749(19) . ? C14 C15 1.396(2) . ? C14 H14 0.9300 . ? C6 N1 1.3546(19) . ? C6 C10 1.403(2) . ? C6 C5 1.446(2) . ? C19 N5 1.3456(17) 4_565 ? C20 C21 1.4685(19) . ? N1 C7 1.330(2) . ? C16 O3 1.3664(17) . ? C16 C15 1.384(2) . ? C16 C17 1.410(2) . ? C17 O4 1.3646(18) . ? C4 C5 1.408(2) . ? C4 C3 1.411(2) . ? C4 C12 1.432(2) . ? C3 C2 1.364(2) . ? C3 H3 0.9300 . ? C1 C2 1.400(2) . ? C1 H1 0.9300 . ? C21 C23 1.3762(17) 4_666 ? C7 C8 1.401(2) . ? C7 H7 0.9300 . ? C8 C9 1.365(3) . ? C8 H8 0.9300 . ? C15 H15 0.9300 . ? C10 C9 1.410(2) . ? C10 C11 1.437(2) . ? C2 H2 0.9300 . ? C11 C12 1.351(2) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C9 H9 0.9300 . ? O2 C24 1.2523(16) . ? C23 C21 1.3762(17) 4_565 ? C23 C24 1.4715(18) . ? C24 O1 1.2785(18) . ? O4 C25 1.4266(18) . ? O3 C26 1.4328(18) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Zn1 N1 99.00(5) . . ? N5 Zn1 N3 166.55(5) . . ? N1 Zn1 N3 93.82(5) . . ? N5 Zn1 O5 79.67(4) . . ? N1 Zn1 O5 96.71(5) . . ? N3 Zn1 O5 94.87(4) . . ? N5 Zn1 N2 101.15(5) . . ? N1 Zn1 N2 77.46(5) . . ? N3 Zn1 N2 85.54(4) . . ? O5 Zn1 N2 174.16(5) . . ? N5 Zn1 O2 90.39(4) . . ? N1 Zn1 O2 165.48(4) . . ? N3 Zn1 O2 77.87(4) . . ? O5 Zn1 O2 95.85(4) . . ? N2 Zn1 O2 89.93(4) . . ? C20 O5 Zn1 112.17(9) . . ? C20 O6 H41 110.9(16) . . ? C19 N3 C23 104.65(11) . . ? C19 N3 Zn1 140.44(10) . . ? C23 N3 Zn1 107.36(8) . . ? C19 N5 C21 104.70(11) 4_666 . ? C19 N5 Zn1 145.45(10) 4_666 . ? C21 N5 Zn1 109.22(9) . . ? C1 N2 C5 118.01(13) . . ? C1 N2 Zn1 129.40(11) . . ? C5 N2 Zn1 112.02(9) . . ? C17 C18 C13 120.31(13) . . ? C17 C18 H18 119.8 . . ? C13 C18 H18 119.8 . . ? C14 C13 C18 119.64(13) . . ? C14 C13 C19 119.40(13) . . ? C18 C13 C19 120.83(12) . . ? C13 C14 C15 120.45(14) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? N1 C6 C10 122.92(13) . . ? N1 C6 C5 117.66(13) . . ? C10 C6 C5 119.42(13) . . ? N5 C19 N3 113.31(12) 4_565 . ? N5 C19 C13 123.05(11) 4_565 . ? N3 C19 C13 123.53(11) . . ? O5 C20 O6 123.44(13) . . ? O5 C20 C21 118.63(13) . . ? O6 C20 C21 117.93(12) . . ? C7 N1 C6 118.34(14) . . ? C7 N1 Zn1 127.45(11) . . ? C6 N1 Zn1 114.06(10) . . ? O3 C16 C15 124.44(13) . . ? O3 C16 C17 115.75(13) . . ? C15 C16 C17 119.81(13) . . ? O4 C17 C18 124.72(13) . . ? O4 C17 C16 115.69(12) . . ? C18 C17 C16 119.57(13) . . ? C5 C4 C3 117.17(14) . . ? C5 C4 C12 119.41(14) . . ? C3 C4 C12 123.39(14) . . ? C2 C3 C4 119.64(14) . . ? C2 C3 H3 120.2 . . ? C4 C3 H3 120.2 . . ? N2 C1 C2 123.13(15) . . ? N2 C1 H1 118.4 . . ? C2 C1 H1 118.4 . . ? N2 C5 C4 122.88(13) . . ? N2 C5 C6 117.53(13) . . ? C4 C5 C6 119.58(14) . . ? N5 C21 C23 108.61(12) . 4_666 ? N5 C21 C20 119.29(11) . . ? C23 C21 C20 132.08(13) 4_666 . ? N1 C7 C8 122.55(15) . . ? N1 C7 H7 118.7 . . ? C8 C7 H7 118.7 . . ? C9 C8 C7 119.38(15) . . ? C9 C8 H8 120.3 . . ? C7 C8 H8 120.3 . . ? C16 C15 C14 119.87(13) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C6 C10 C9 117.22(14) . . ? C6 C10 C11 119.40(14) . . ? C9 C10 C11 123.37(15) . . ? C3 C2 C1 119.08(14) . . ? C3 C2 H2 120.5 . . ? C1 C2 H2 120.5 . . ? C12 C11 C10 121.15(15) . . ? C12 C11 H11 119.4 . . ? C10 C11 H11 119.4 . . ? C11 C12 C4 120.95(15) . . ? C11 C12 H12 119.5 . . ? C4 C12 H12 119.5 . . ? C8 C9 C10 119.56(15) . . ? C8 C9 H9 120.2 . . ? C10 C9 H9 120.2 . . ? C24 O2 Zn1 111.76(9) . . ? N3 C23 C21 108.73(12) . 4_565 ? N3 C23 C24 119.53(11) . . ? C21 C23 C24 131.69(13) 4_565 . ? O2 C24 O1 124.40(12) . . ? O2 C24 C23 117.17(13) . . ? O1 C24 C23 118.43(11) . . ? C17 O4 C25 116.40(11) . . ? C16 O3 C26 116.20(12) . . ? O4 C25 H25A 109.5 . . ? O4 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? O4 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? O3 C26 H26A 109.5 . . ? O3 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? O3 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N5 Zn1 O5 C20 8.52(11) . . . . ? N1 Zn1 O5 C20 106.50(11) . . . . ? N3 Zn1 O5 C20 -159.07(11) . . . . ? N2 Zn1 O5 C20 107.1(4) . . . . ? O2 Zn1 O5 C20 -80.81(11) . . . . ? N5 Zn1 N3 C19 -166.81(17) . . . . ? N1 Zn1 N3 C19 -4.42(15) . . . . ? O5 Zn1 N3 C19 -101.49(15) . . . . ? N2 Zn1 N3 C19 72.67(15) . . . . ? O2 Zn1 N3 C19 163.55(16) . . . . ? N5 Zn1 N3 C23 50.6(2) . . . . ? N1 Zn1 N3 C23 -147.03(10) . . . . ? O5 Zn1 N3 C23 115.90(10) . . . . ? N2 Zn1 N3 C23 -69.94(10) . . . . ? O2 Zn1 N3 C23 20.95(9) . . . . ? N1 Zn1 N5 C19 87.92(19) . . . 4_666 ? N3 Zn1 N5 C19 -109.9(2) . . . 4_666 ? O5 Zn1 N5 C19 -176.83(19) . . . 4_666 ? N2 Zn1 N5 C19 9.05(19) . . . 4_666 ? O2 Zn1 N5 C19 -80.96(19) . . . 4_666 ? N1 Zn1 N5 C21 -103.52(10) . . . . ? N3 Zn1 N5 C21 58.7(2) . . . . ? O5 Zn1 N5 C21 -8.28(9) . . . . ? N2 Zn1 N5 C21 177.60(9) . . . . ? O2 Zn1 N5 C21 87.60(10) . . . . ? N5 Zn1 N2 C1 -82.11(12) . . . . ? N1 Zn1 N2 C1 -178.97(12) . . . . ? N3 Zn1 N2 C1 86.11(12) . . . . ? O5 Zn1 N2 C1 -179.6(3) . . . . ? O2 Zn1 N2 C1 8.27(12) . . . . ? N5 Zn1 N2 C5 106.92(9) . . . . ? N1 Zn1 N2 C5 10.05(9) . . . . ? N3 Zn1 N2 C5 -84.87(9) . . . . ? O5 Zn1 N2 C5 9.4(4) . . . . ? O2 Zn1 N2 C5 -162.70(9) . . . . ? C17 C18 C13 C14 3.1(2) . . . . ? C17 C18 C13 C19 -172.75(12) . . . . ? C18 C13 C14 C15 -4.9(2) . . . . ? C19 C13 C14 C15 171.00(13) . . . . ? C23 N3 C19 N5 0.20(17) . . . 4_565 ? Zn1 N3 C19 N5 -143.00(12) . . . 4_565 ? C23 N3 C19 C13 -175.93(13) . . . . ? Zn1 N3 C19 C13 40.9(2) . . . . ? C14 C13 C19 N5 -120.85(15) . . . 4_565 ? C18 C13 C19 N5 55.0(2) . . . 4_565 ? C14 C13 C19 N3 54.9(2) . . . . ? C18 C13 C19 N3 -129.21(15) . . . . ? Zn1 O5 C20 O6 172.94(12) . . . . ? Zn1 O5 C20 C21 -6.88(17) . . . . ? C10 C6 N1 C7 0.8(2) . . . . ? C5 C6 N1 C7 -178.63(12) . . . . ? C10 C6 N1 Zn1 -174.97(10) . . . . ? C5 C6 N1 Zn1 5.64(15) . . . . ? N5 Zn1 N1 C7 76.88(12) . . . . ? N3 Zn1 N1 C7 -99.03(12) . . . . ? O5 Zn1 N1 C7 -3.67(12) . . . . ? N2 Zn1 N1 C7 176.40(12) . . . . ? O2 Zn1 N1 C7 -153.38(15) . . . . ? N5 Zn1 N1 C6 -107.86(9) . . . . ? N3 Zn1 N1 C6 76.23(10) . . . . ? O5 Zn1 N1 C6 171.59(9) . . . . ? N2 Zn1 N1 C6 -8.34(9) . . . . ? O2 Zn1 N1 C6 21.9(2) . . . . ? C13 C18 C17 O4 -179.66(12) . . . . ? C13 C18 C17 C16 2.3(2) . . . . ? O3 C16 C17 O4 -3.59(18) . . . . ? C15 C16 C17 O4 175.83(12) . . . . ? O3 C16 C17 C18 174.65(12) . . . . ? C15 C16 C17 C18 -5.9(2) . . . . ? C5 C4 C3 C2 2.9(2) . . . . ? C12 C4 C3 C2 -175.03(14) . . . . ? C5 N2 C1 C2 2.1(2) . . . . ? Zn1 N2 C1 C2 -168.46(11) . . . . ? C1 N2 C5 C4 -1.64(19) . . . . ? Zn1 N2 C5 C4 170.47(10) . . . . ? C1 N2 C5 C6 177.38(12) . . . . ? Zn1 N2 C5 C6 -10.51(14) . . . . ? C3 C4 C5 N2 -0.8(2) . . . . ? C12 C4 C5 N2 177.23(13) . . . . ? C3 C4 C5 C6 -179.83(13) . . . . ? C12 C4 C5 C6 -1.8(2) . . . . ? N1 C6 C5 N2 3.58(18) . . . . ? C10 C6 C5 N2 -175.83(12) . . . . ? N1 C6 C5 C4 -177.37(12) . . . . ? C10 C6 C5 C4 3.22(19) . . . . ? C19 N5 C21 C23 0.19(16) 4_666 . . 4_666 ? Zn1 N5 C21 C23 -173.13(10) . . . 4_666 ? C19 N5 C21 C20 -178.82(13) 4_666 . . . ? Zn1 N5 C21 C20 7.86(16) . . . . ? O5 C20 C21 N5 -0.7(2) . . . . ? O6 C20 C21 N5 179.52(13) . . . . ? O5 C20 C21 C23 -179.39(15) . . . 4_666 ? O6 C20 C21 C23 0.8(2) . . . 4_666 ? C6 N1 C7 C8 1.2(2) . . . . ? Zn1 N1 C7 C8 176.32(11) . . . . ? N1 C7 C8 C9 -1.8(2) . . . . ? O3 C16 C15 C14 -176.46(13) . . . . ? C17 C16 C15 C14 4.2(2) . . . . ? C13 C14 C15 C16 1.3(2) . . . . ? N1 C6 C10 C9 -2.1(2) . . . . ? C5 C6 C10 C9 177.29(12) . . . . ? N1 C6 C10 C11 178.60(13) . . . . ? C5 C6 C10 C11 -2.0(2) . . . . ? C4 C3 C2 C1 -2.6(2) . . . . ? N2 C1 C2 C3 0.1(2) . . . . ? C6 C10 C11 C12 -0.7(2) . . . . ? C9 C10 C11 C12 -179.95(14) . . . . ? C10 C11 C12 C4 2.2(2) . . . . ? C5 C4 C12 C11 -0.9(2) . . . . ? C3 C4 C12 C11 176.99(15) . . . . ? C7 C8 C9 C10 0.4(2) . . . . ? C6 C10 C9 C8 1.5(2) . . . . ? C11 C10 C9 C8 -179.26(14) . . . . ? N5 Zn1 O2 C24 166.62(10) . . . . ? N1 Zn1 O2 C24 36.0(2) . . . . ? N3 Zn1 O2 C24 -19.99(10) . . . . ? O5 Zn1 O2 C24 -113.73(10) . . . . ? N2 Zn1 O2 C24 65.47(10) . . . . ? C19 N3 C23 C21 -0.31(16) . . . 4_565 ? Zn1 N3 C23 C21 156.13(10) . . . 4_565 ? C19 N3 C23 C24 -178.17(13) . . . . ? Zn1 N3 C23 C24 -21.74(16) . . . . ? Zn1 O2 C24 O1 -165.44(12) . . . . ? Zn1 O2 C24 C23 14.38(16) . . . . ? N3 C23 C24 O2 5.3(2) . . . . ? C21 C23 C24 O2 -171.99(15) 4_565 . . . ? N3 C23 C24 O1 -174.87(13) . . . . ? C21 C23 C24 O1 7.8(2) 4_565 . . . ? C18 C17 O4 C25 17.60(19) . . . . ? C16 C17 O4 C25 -164.26(12) . . . . ? C15 C16 O3 C26 8.08(19) . . . . ? C17 C16 O3 C26 -172.53(12) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O6 H41 O1 1.10(3) 1.37(3) 2.4733(14) 174(3) 4_666 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 28.26 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.610 _refine_diff_density_min -1.307 _refine_diff_density_rms 0.081 data_a3 _database_code_depnum_ccdc_archive 'CCDC 915953' #TrackingRef '3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H22 N4 O12 Sr' _chemical_formula_weight 670.10 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' 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' Sr Sr -1.5307 3.2498 '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 Tetragonal _symmetry_space_group_name_H-M I4(1)/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y+3/4, x+1/4, z+1/4' '-x+1/2, -y, z+1/2' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-y+5/4, x+3/4, z+3/4' '-x+1, -y+1/2, z+1' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'y-3/4, -x-1/4, -z-1/4' 'x-1/2, y, -z-1/2' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'y-1/4, -x+1/4, -z+1/4' 'x, y+1/2, -z' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 16.820(5) _cell_length_b 16.820(5) _cell_length_c 18.022(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5099(3) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.746 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2720 _exptl_absorpt_coefficient_mu 2.194 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4740 _exptl_absorpt_correction_T_max 0.6681 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12157 _diffrn_reflns_av_R_equivalents 0.1342 _diffrn_reflns_av_sigmaI/netI 0.0967 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 25.01 _reflns_number_total 2244 _reflns_number_gt 1368 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+171.2025P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2244 _refine_ls_number_parameters 223 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1443 _refine_ls_R_factor_gt 0.0763 _refine_ls_wR_factor_ref 0.1995 _refine_ls_wR_factor_gt 0.1590 _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_restrained_S_all 1.106 _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 Sr1 Sr 1.0000 0.7500 0.97497(7) 0.0254(4) Uani 1 2 d S . . N1 N 0.6345(5) 0.8042(4) 0.7977(4) 0.0259(19) Uani 1 1 d . . . N2 N 0.7560(5) 0.8408(5) 0.8286(4) 0.0269(19) Uani 1 1 d . . . H2 H 0.7973 0.8702 0.8345 0.032 Uiso 1 1 calc R . . O1 O 0.8836(4) 0.7554(4) 0.8829(4) 0.0337(17) Uani 1 1 d . . . O2 O 0.8070(4) 0.6476(4) 0.9007(4) 0.0383(19) Uani 1 1 d . . . O3 O 0.6680(4) 0.6067(4) 0.8727(5) 0.044(2) Uani 1 1 d . . . H3 H 0.7128 0.6208 0.8848 0.066 Uiso 1 1 calc R . . O4 O 0.5659(4) 0.6556(4) 0.8109(4) 0.0400(19) Uani 1 1 d . . . O6 O 0.6200(5) 1.1806(5) 0.7291(5) 0.051(2) Uani 1 1 d . . . C61 C 0.6634(12) 1.2353(11) 0.7188(13) 0.051(6) Uani 0.611(12) 1 d P A 1 H61A H 0.6326 1.2823 0.7093 0.076 Uiso 0.611(12) 1 calc PR A 1 H61B H 0.6968 1.2243 0.6769 0.076 Uiso 0.611(12) 1 calc PR A 1 H61C H 0.6958 1.2435 0.7620 0.076 Uiso 0.611(12) 1 calc PR A 1 C62 C 0.5707(18) 1.2231(18) 0.741(2) 0.051(9) Uani 0.389(12) 1 d P A 2 H62A H 0.5821 1.2734 0.7185 0.076 Uiso 0.389(12) 1 calc PR A 2 H62B H 0.5659 1.2299 0.7939 0.076 Uiso 0.389(12) 1 calc PR A 2 H62C H 0.5218 1.2025 0.7217 0.076 Uiso 0.389(12) 1 calc PR A 2 C1 C 0.8183(5) 0.7183(6) 0.8796(6) 0.026(2) Uani 1 1 d . . . C2 C 0.7499(6) 0.7625(6) 0.8461(5) 0.023(2) Uani 1 1 d . . . C3 C 0.6754(6) 0.7406(6) 0.8283(6) 0.027(2) Uani 1 1 d . . . C4 C 0.6332(6) 0.6635(6) 0.8368(6) 0.032(2) Uani 1 1 d . . . C5 C 0.6852(6) 0.8644(6) 0.8003(5) 0.028(2) Uani 1 1 d . . . C6 C 0.6677(6) 0.9467(6) 0.7781(6) 0.032(3) Uani 1 1 d . . . C7 C 0.5918(7) 0.9758(6) 0.7850(6) 0.038(3) Uani 1 1 d . A . H7 H 0.5508 0.9427 0.8007 0.046 Uiso 1 1 calc R . . C8 C 0.5763(7) 1.0557(7) 0.7684(8) 0.049(3) Uani 1 1 d . . . H8 H 0.5250 1.0757 0.7735 0.058 Uiso 0.389(12) 1 calc PR A 2 O81 O 0.4993(7) 1.0887(7) 0.7787(8) 0.049(4) Uani 0.611(12) 1 d P A 1 C81 C 0.4422(11) 1.0477(11) 0.8203(12) 0.049(6) Uani 0.611(12) 1 d P A 1 H81A H 0.3938 1.0779 0.8214 0.073 Uiso 0.611(12) 1 calc PR A 1 H81B H 0.4613 1.0404 0.8700 0.073 Uiso 0.611(12) 1 calc PR A 1 H81C H 0.4324 0.9968 0.7980 0.073 Uiso 0.611(12) 1 calc PR A 1 C9 C 0.6370(7) 1.1046(7) 0.7445(8) 0.051(3) Uani 1 1 d . A . C10 C 0.7119(8) 1.0728(7) 0.7355(8) 0.054(4) Uani 1 1 d . . . H10 H 0.7523 1.1045 0.7165 0.065 Uiso 0.611(12) 1 calc PR A 1 O101 O 0.7784(13) 1.1187(12) 0.7064(13) 0.054(7) Uani 0.389(12) 1 d P A 2 C101 C 0.852(2) 1.0872(19) 0.686(2) 0.054(9) Uani 0.389(12) 1 d P A 2 H10A H 0.8861 1.1291 0.6686 0.081 Uiso 0.389(12) 1 calc PR A 2 H10B H 0.8453 1.0482 0.6481 0.081 Uiso 0.389(12) 1 calc PR A 2 H10C H 0.8765 1.0627 0.7290 0.081 Uiso 0.389(12) 1 calc PR A 2 C11 C 0.7281(6) 0.9961(7) 0.7538(6) 0.037(3) Uani 1 1 d . A . H11 H 0.7797 0.9768 0.7499 0.044 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 Sr1 0.0254(8) 0.0252(8) 0.0255(6) 0.000 0.000 0.0005(6) N1 0.030(5) 0.020(4) 0.028(5) 0.003(4) -0.004(4) -0.001(4) N2 0.023(4) 0.027(5) 0.031(5) -0.001(4) -0.004(4) 0.005(4) O1 0.016(3) 0.037(4) 0.048(5) -0.002(4) -0.007(3) 0.000(3) O2 0.036(4) 0.032(4) 0.047(5) 0.013(4) -0.007(4) 0.003(3) O3 0.034(4) 0.036(4) 0.061(5) 0.018(4) -0.011(4) -0.001(3) O4 0.033(4) 0.036(4) 0.051(5) 0.014(4) -0.014(4) -0.015(3) O6 0.043(5) 0.034(5) 0.075(6) 0.003(5) -0.008(5) 0.014(4) C61 0.043(12) 0.034(12) 0.075(16) 0.003(11) -0.008(11) 0.014(10) C62 0.043(19) 0.034(17) 0.07(2) 0.003(16) -0.008(17) 0.014(15) C1 0.026(5) 0.027(5) 0.025(5) 0.004(5) -0.003(5) 0.005(4) C2 0.024(5) 0.027(6) 0.019(5) 0.001(4) 0.001(4) -0.001(4) C3 0.022(5) 0.028(6) 0.030(6) 0.003(4) -0.002(4) -0.002(4) C4 0.027(6) 0.032(6) 0.035(6) 0.005(5) -0.001(5) 0.005(5) C5 0.029(6) 0.032(6) 0.025(5) -0.007(5) 0.001(5) 0.000(5) C6 0.030(6) 0.032(6) 0.034(6) 0.001(5) -0.005(5) -0.003(5) C7 0.037(7) 0.031(6) 0.047(7) 0.001(5) -0.007(5) 0.001(5) C8 0.038(7) 0.035(7) 0.074(9) 0.000(6) -0.009(6) 0.017(5) O81 0.038(8) 0.035(7) 0.074(10) 0.000(7) -0.009(7) 0.017(6) C81 0.038(11) 0.035(11) 0.074(15) 0.000(10) -0.009(11) 0.017(9) C9 0.043(8) 0.034(7) 0.075(9) 0.003(6) -0.008(7) 0.014(6) C10 0.056(9) 0.038(7) 0.068(9) 0.007(7) -0.004(7) -0.010(6) O101 0.056(15) 0.038(13) 0.068(16) 0.007(11) -0.004(12) -0.010(10) C101 0.06(2) 0.038(19) 0.07(2) 0.007(17) -0.004(18) -0.010(16) C11 0.033(6) 0.035(6) 0.042(6) 0.006(5) -0.007(6) -0.003(5) _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 Sr1 O4 2.480(7) 8_454 ? Sr1 O4 2.480(7) 2_655 ? Sr1 O1 2.568(7) . ? Sr1 O1 2.568(7) 7_664 ? Sr1 O1 2.760(7) 16_757 ? Sr1 O1 2.760(7) 10_677 ? Sr1 N1 2.769(8) 2_655 ? Sr1 N1 2.769(8) 8_454 ? Sr1 C4 3.347(10) 2_655 ? Sr1 C4 3.347(10) 8_454 ? Sr1 Sr1 3.603(3) 10_677 ? N1 C5 1.324(12) . ? N1 C3 1.386(12) . ? N1 Sr1 2.769(8) 6_544 ? N2 C5 1.355(12) . ? N2 C2 1.359(12) . ? N2 H2 0.8600 . ? O1 C1 1.265(11) . ? O1 Sr1 2.760(7) 10_677 ? O2 C1 1.263(11) . ? O3 C4 1.293(12) . ? O3 H3 0.8200 . ? O4 C4 1.232(12) . ? O4 Sr1 2.480(7) 6_544 ? O6 C62 1.12(3) . ? O6 C61 1.19(2) . ? O6 C9 1.340(13) . ? C61 H61A 0.9600 . ? C61 H61B 0.9600 . ? C61 H61C 0.9600 . ? C62 H62A 0.9600 . ? C62 H62B 0.9600 . ? C62 H62C 0.9600 . ? C1 C2 1.497(13) . ? C2 C3 1.346(13) . ? C3 C4 1.487(14) . ? C4 Sr1 3.347(10) 6_544 ? C5 C6 1.470(14) . ? C6 C7 1.373(14) . ? C6 C11 1.383(14) . ? C7 C8 1.400(15) . ? C7 H7 0.9300 . ? C8 C9 1.381(17) . ? C8 O81 1.421(16) . ? C8 H8 0.9300 . ? O81 C81 1.40(2) . ? C81 H81A 0.9600 . ? C81 H81B 0.9600 . ? C81 H81C 0.9600 . ? C9 C10 1.378(17) . ? C10 C11 1.358(16) . ? C10 O101 1.46(2) . ? C10 H10 0.9300 . ? O101 C101 1.40(4) . ? C101 H10A 0.9600 . ? C101 H10B 0.9600 . ? C101 H10C 0.9600 . ? C11 H11 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 O4 Sr1 O4 102.7(4) 8_454 2_655 ? O4 Sr1 O1 86.1(2) 8_454 . ? O4 Sr1 O1 151.2(2) 2_655 . ? O4 Sr1 O1 151.2(2) 8_454 7_664 ? O4 Sr1 O1 86.1(2) 2_655 7_664 ? O1 Sr1 O1 99.5(3) . 7_664 ? O4 Sr1 O1 95.9(2) 8_454 16_757 ? O4 Sr1 O1 141.1(2) 2_655 16_757 ? O1 Sr1 O1 62.93(11) . 16_757 ? O1 Sr1 O1 62.93(11) 7_664 16_757 ? O4 Sr1 O1 141.1(2) 8_454 10_677 ? O4 Sr1 O1 95.9(2) 2_655 10_677 ? O1 Sr1 O1 62.93(11) . 10_677 ? O1 Sr1 O1 62.93(11) 7_664 10_677 ? O1 Sr1 O1 90.5(3) 16_757 10_677 ? O4 Sr1 N1 81.9(2) 8_454 2_655 ? O4 Sr1 N1 63.3(2) 2_655 2_655 ? O1 Sr1 N1 91.5(2) . 2_655 ? O1 Sr1 N1 125.9(2) 7_664 2_655 ? O1 Sr1 N1 154.4(2) 16_757 2_655 ? O1 Sr1 N1 76.4(2) 10_677 2_655 ? O4 Sr1 N1 63.3(2) 8_454 8_454 ? O4 Sr1 N1 81.9(2) 2_655 8_454 ? O1 Sr1 N1 125.9(2) . 8_454 ? O1 Sr1 N1 91.5(2) 7_664 8_454 ? O1 Sr1 N1 76.4(2) 16_757 8_454 ? O1 Sr1 N1 154.4(2) 10_677 8_454 ? N1 Sr1 N1 123.5(3) 2_655 8_454 ? O4 Sr1 C4 101.6(3) 8_454 2_655 ? O4 Sr1 C4 17.5(2) 2_655 2_655 ? O1 Sr1 C4 134.2(2) . 2_655 ? O1 Sr1 C4 94.7(2) 7_664 2_655 ? O1 Sr1 C4 156.0(2) 16_757 2_655 ? O1 Sr1 C4 86.3(2) 10_677 2_655 ? N1 Sr1 C4 46.5(2) 2_655 2_655 ? N1 Sr1 C4 96.8(2) 8_454 2_655 ? O4 Sr1 C4 17.5(2) 8_454 8_454 ? O4 Sr1 C4 101.6(3) 2_655 8_454 ? O1 Sr1 C4 94.7(2) . 8_454 ? O1 Sr1 C4 134.2(2) 7_664 8_454 ? O1 Sr1 C4 86.3(2) 16_757 8_454 ? O1 Sr1 C4 156.0(2) 10_677 8_454 ? N1 Sr1 C4 96.8(2) 2_655 8_454 ? N1 Sr1 C4 46.5(2) 8_454 8_454 ? C4 Sr1 C4 105.9(4) 2_655 8_454 ? O4 Sr1 Sr1 128.66(19) 8_454 10_677 ? O4 Sr1 Sr1 128.66(19) 2_655 10_677 ? O1 Sr1 Sr1 49.74(16) . 10_677 ? O1 Sr1 Sr1 49.74(16) 7_664 10_677 ? O1 Sr1 Sr1 45.23(14) 16_757 10_677 ? O1 Sr1 Sr1 45.23(14) 10_677 10_677 ? N1 Sr1 Sr1 118.24(17) 2_655 10_677 ? N1 Sr1 Sr1 118.24(17) 8_454 10_677 ? C4 Sr1 Sr1 127.04(18) 2_655 10_677 ? C4 Sr1 Sr1 127.04(18) 8_454 10_677 ? C5 N1 C3 104.9(8) . . ? C5 N1 Sr1 142.6(7) . 6_544 ? C3 N1 Sr1 109.8(6) . 6_544 ? C5 N2 C2 107.8(8) . . ? C5 N2 H2 126.1 . . ? C2 N2 H2 126.1 . . ? C1 O1 Sr1 132.4(6) . . ? C1 O1 Sr1 124.6(6) . 10_677 ? Sr1 O1 Sr1 85.03(19) . 10_677 ? C4 O3 H3 109.5 . . ? C4 O4 Sr1 125.4(6) . 6_544 ? C62 O6 C61 90(2) . . ? C62 O6 C9 137(2) . . ? C61 O6 C9 129.7(13) . . ? O6 C61 H61A 109.5 . . ? O6 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? O6 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? O6 C62 H62A 109.5 . . ? O6 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? O6 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? O2 C1 O1 125.5(9) . . ? O2 C1 C2 118.3(8) . . ? O1 C1 C2 116.1(8) . . ? C3 C2 N2 106.2(9) . . ? C3 C2 C1 132.6(9) . . ? N2 C2 C1 121.2(8) . . ? C2 C3 N1 110.2(8) . . ? C2 C3 C4 131.2(9) . . ? N1 C3 C4 118.6(8) . . ? O4 C4 O3 121.7(10) . . ? O4 C4 C3 119.5(9) . . ? O3 C4 C3 118.8(9) . . ? O4 C4 Sr1 37.2(5) . 6_544 ? O3 C4 Sr1 157.6(7) . 6_544 ? C3 C4 Sr1 83.0(6) . 6_544 ? N1 C5 N2 110.8(9) . . ? N1 C5 C6 125.5(9) . . ? N2 C5 C6 123.7(9) . . ? C7 C6 C11 119.8(10) . . ? C7 C6 C5 119.8(10) . . ? C11 C6 C5 120.3(10) . . ? C6 C7 C8 119.7(11) . . ? C6 C7 H7 120.1 . . ? C8 C7 H7 120.1 . . ? C9 C8 C7 120.0(10) . . ? C9 C8 O81 118.8(11) . . ? C7 C8 O81 121.1(12) . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? O81 C8 H8 2.6 . . ? C81 O81 C8 120.1(13) . . ? O81 C81 H81A 109.5 . . ? O81 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? O81 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? O6 C9 C10 122.8(12) . . ? O6 C9 C8 118.4(11) . . ? C10 C9 C8 118.8(11) . . ? C11 C10 C9 121.5(12) . . ? C11 C10 O101 115.9(14) . . ? C9 C10 O101 122.5(14) . . ? C11 C10 H10 119.2 . . ? C9 C10 H10 119.2 . . ? O101 C10 H10 3.3 . . ? C101 O101 C10 125(2) . . ? O101 C101 H10A 109.5 . . ? O101 C101 H10B 109.5 . . ? H10A C101 H10B 109.5 . . ? O101 C101 H10C 109.5 . . ? H10A C101 H10C 109.5 . . ? H10B C101 H10C 109.5 . . ? C10 C11 C6 120.0(12) . . ? C10 C11 H11 120.0 . . ? C6 C11 H11 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 Sr1 O1 C1 -17.7(8) 8_454 . . . ? O4 Sr1 O1 C1 -127.1(8) 2_655 . . . ? O1 Sr1 O1 C1 133.8(9) 7_664 . . . ? O1 Sr1 O1 C1 80.9(9) 16_757 . . . ? O1 Sr1 O1 C1 -173.3(10) 10_677 . . . ? N1 Sr1 O1 C1 -99.5(8) 2_655 . . . ? N1 Sr1 O1 C1 35.0(9) 8_454 . . . ? C4 Sr1 O1 C1 -120.1(8) 2_655 . . . ? C4 Sr1 O1 C1 -2.5(9) 8_454 . . . ? Sr1 Sr1 O1 C1 133.8(9) 10_677 . . . ? O4 Sr1 O1 Sr1 -151.5(2) 8_454 . . 10_677 ? O4 Sr1 O1 Sr1 99.2(5) 2_655 . . 10_677 ? O1 Sr1 O1 Sr1 0.0 7_664 . . 10_677 ? O1 Sr1 O1 Sr1 -52.88(17) 16_757 . . 10_677 ? O1 Sr1 O1 Sr1 52.88(17) 10_677 . . 10_677 ? N1 Sr1 O1 Sr1 126.8(2) 2_655 . . 10_677 ? N1 Sr1 O1 Sr1 -98.8(3) 8_454 . . 10_677 ? C4 Sr1 O1 Sr1 106.1(3) 2_655 . . 10_677 ? C4 Sr1 O1 Sr1 -136.3(2) 8_454 . . 10_677 ? Sr1 O1 C1 O2 -32.7(15) . . . . ? Sr1 O1 C1 O2 86.4(12) 10_677 . . . ? Sr1 O1 C1 C2 148.8(6) . . . . ? Sr1 O1 C1 C2 -92.1(9) 10_677 . . . ? C5 N2 C2 C3 -0.3(11) . . . . ? C5 N2 C2 C1 -179.3(8) . . . . ? O2 C1 C2 C3 -4.8(17) . . . . ? O1 C1 C2 C3 173.7(10) . . . . ? O2 C1 C2 N2 173.8(9) . . . . ? O1 C1 C2 N2 -7.6(14) . . . . ? N2 C2 C3 N1 1.6(11) . . . . ? C1 C2 C3 N1 -179.6(10) . . . . ? N2 C2 C3 C4 -177.8(10) . . . . ? C1 C2 C3 C4 1.0(19) . . . . ? C5 N1 C3 C2 -2.2(11) . . . . ? Sr1 N1 C3 C2 163.6(7) 6_544 . . . ? C5 N1 C3 C4 177.2(9) . . . . ? Sr1 N1 C3 C4 -16.9(11) 6_544 . . . ? Sr1 O4 C4 O3 -170.0(7) 6_544 . . . ? Sr1 O4 C4 C3 11.3(14) 6_544 . . . ? C2 C3 C4 O4 -174.4(11) . . . . ? N1 C3 C4 O4 6.3(15) . . . . ? C2 C3 C4 O3 6.9(17) . . . . ? N1 C3 C4 O3 -172.4(9) . . . . ? C2 C3 C4 Sr1 -167.5(11) . . . 6_544 ? N1 C3 C4 Sr1 13.2(8) . . . 6_544 ? C3 N1 C5 N2 2.0(11) . . . . ? Sr1 N1 C5 N2 -155.8(8) 6_544 . . . ? C3 N1 C5 C6 -176.3(10) . . . . ? Sr1 N1 C5 C6 25.9(17) 6_544 . . . ? C2 N2 C5 N1 -1.1(11) . . . . ? C2 N2 C5 C6 177.2(9) . . . . ? N1 C5 C6 C7 30.2(16) . . . . ? N2 C5 C6 C7 -147.9(10) . . . . ? N1 C5 C6 C11 -153.2(11) . . . . ? N2 C5 C6 C11 28.8(16) . . . . ? C11 C6 C7 C8 -0.9(17) . . . . ? C5 C6 C7 C8 175.8(11) . . . . ? C6 C7 C8 C9 0.6(19) . . . . ? C6 C7 C8 O81 -176.7(12) . . . . ? C9 C8 O81 C81 -163.5(15) . . . . ? C7 C8 O81 C81 14(2) . . . . ? C62 O6 C9 C10 -165(3) . . . . ? C61 O6 C9 C10 -14(3) . . . . ? C62 O6 C9 C8 17(3) . . . . ? C61 O6 C9 C8 167.4(18) . . . . ? C7 C8 C9 O6 -180.0(12) . . . . ? O81 C8 C9 O6 -3(2) . . . . ? C7 C8 C9 C10 2(2) . . . . ? O81 C8 C9 C10 179.0(13) . . . . ? O6 C9 C10 C11 177.8(12) . . . . ? C8 C9 C10 C11 -4(2) . . . . ? O6 C9 C10 O101 -2(2) . . . . ? C8 C9 C10 O101 176.4(15) . . . . ? C11 C10 O101 C101 10(3) . . . . ? C9 C10 O101 C101 -171(2) . . . . ? C9 C10 C11 C6 4(2) . . . . ? O101 C10 C11 C6 -176.5(14) . . . . ? C7 C6 C11 C10 -1.2(18) . . . . ? C5 C6 C11 C10 -177.9(11) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.011 _refine_diff_density_min -2.391 _refine_diff_density_rms 0.141 data_a _database_code_depnum_ccdc_archive 'CCDC 915954' #TrackingRef '1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H26 Mn3 N4 O16, 2(H2 O)' _chemical_formula_sum 'C24 H30 Mn3 N4 O18' _chemical_formula_weight 827.34 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 trigonal _symmetry_space_group_name_H-M 'R -3' _symmetry_space_group_name_Hall '-R 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 25.1437(13) _cell_length_b 25.1437(13) _cell_length_c 14.5663(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 7975.1(10) _cell_formula_units_Z 9 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 2876 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 25.08 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.550 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3789 _exptl_absorpt_coefficient_mu 1.131 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7207 _exptl_absorpt_correction_T_max 0.7425 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEXII CCD area-detector' _diffrn_measurement_method '\f and \w' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13659 _diffrn_reflns_av_R_equivalents 0.0787 _diffrn_reflns_av_sigmaI/netI 0.0754 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 25.01 _reflns_number_total 3128 _reflns_number_gt 2034 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2008)' _computing_cell_refinement 'SAINT (Bruker, 2008)' _computing_data_reduction 'SAINT (Bruker, 2008)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'DIAMOND (Brandenburg & Berndt, 1999)' _computing_publication_material 'SHELXL97 (Sheldrick, 2008)' _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. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.000 0.000 219.2 28.0 2 0.333 0.667 0.167 81.0 0.7 3 0.667 0.333 0.333 221.2 29.0 4 0.000 0.000 0.500 79.9 0.7 5 0.333 0.667 0.667 221.2 28.9 6 0.667 0.333 0.833 81.0 0.8 _platon_squeeze_details ; ? ; _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^)+(0.1498P)^2^+6.3731P] 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 3128 _refine_ls_number_parameters 218 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1137 _refine_ls_R_factor_gt 0.0808 _refine_ls_wR_factor_ref 0.2531 _refine_ls_wR_factor_gt 0.2299 _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_restrained_S_all 1.100 _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 Mn1 Mn 0.8333 0.6667 0.1667 0.0648(7) Uani 1 2 d S . . Mn2 Mn 0.92276(4) 0.60176(5) -0.18663(7) 0.0253(4) Uani 1 1 d . . . C1 C 0.8788(3) 0.6254(4) -0.0096(5) 0.0377(18) Uani 1 1 d . . . C2 C 0.8252(3) 0.6066(3) -0.0713(5) 0.0328(17) Uani 1 1 d . . . C3 C 0.7678(3) 0.5999(4) -0.0625(5) 0.0345(17) Uani 1 1 d . . . C4 C 0.7335(4) 0.6075(4) 0.0153(5) 0.0398(19) Uani 1 1 d . . . C5 C 0.7772(3) 0.5742(3) -0.1994(5) 0.0334(17) Uani 1 1 d . . . C6 C 0.7616(3) 0.5512(4) -0.2953(5) 0.0340(17) Uani 1 1 d . . . C7 C 0.7043(4) 0.5016(4) -0.3139(5) 0.045(2) Uani 1 1 d . . . H7 H 0.6752 0.4833 -0.2677 0.054 Uiso 1 1 calc R . . C8 C 0.6912(4) 0.4798(4) -0.4040(6) 0.057(2) Uani 1 1 d . . . C9 C 0.7334(4) 0.5070(4) -0.4734(6) 0.055(2) Uani 1 1 d . . . H9 H 0.7237 0.4926 -0.5334 0.066 Uiso 1 1 calc R . . C10 C 0.7894(4) 0.5550(4) -0.4530(5) 0.051(2) Uani 1 1 d . . . H10 H 0.8182 0.5731 -0.4997 0.062 Uiso 1 1 calc R . . C11 C 0.8054(4) 0.5783(4) -0.3646(5) 0.044(2) Uani 1 1 d . . . H11 H 0.8443 0.6112 -0.3519 0.053 Uiso 1 1 calc R . . C12 C 0.5998(5) 0.3861(5) -0.3617(8) 0.085(3) Uani 1 1 d . . . H12A H 0.6249 0.3707 -0.3368 0.127 Uiso 1 1 calc R . . H12B H 0.5639 0.3530 -0.3896 0.127 Uiso 1 1 calc R . . H12C H 0.5877 0.4038 -0.3134 0.127 Uiso 1 1 calc R . . N1 N 0.8313(2) 0.5899(3) -0.1588(4) 0.0273(13) Uani 1 1 d . . . N2 N 0.7371(2) 0.5792(3) -0.1440(3) 0.0288(13) Uani 1 1 d . . . O1 O 0.9232(2) 0.6217(3) -0.0423(3) 0.0403(13) Uani 1 1 d . . . O2 O 0.8813(3) 0.6453(3) 0.0694(4) 0.0613(18) Uani 1 1 d . . . O3 O 0.7532(3) 0.6160(3) 0.0953(4) 0.064(2) Uani 1 1 d . . . O4 O 0.6820(2) 0.6018(2) -0.0038(3) 0.0362(12) Uani 1 1 d . . . O5 O 0.6331(3) 0.4306(4) -0.4274(5) 0.084 Uani 1 1 d . . . O6 O 0.9475(3) 0.6949(3) -0.2374(4) 0.0562(16) Uani 1 1 d . . . H6A H 0.9849 0.7133 -0.2206 0.084 Uiso 1 1 d R . . H6B H 0.9433 0.6805 -0.2914 0.084 Uiso 1 1 d R . . O7 O 1.0245(3) 0.6477(3) -0.1695(4) 0.0655(19) Uani 1 1 d . . . H7A H 1.0457 0.6458 -0.2135 0.098 Uiso 1 1 d R . . H7B H 1.0296 0.6285 -0.1255 0.098 Uiso 1 1 d R . . O8 O 0.8087(4) 0.5806(5) 0.2403(6) 0.115(3) Uani 1 1 d . . . H8A H 0.8348 0.5744 0.2706 0.173 Uiso 1 1 d R . . H8B H 0.7714 0.5516 0.2535 0.173 Uiso 1 1 d R . . O1W O 0.9044(4) 0.5752(5) 0.3166(6) 0.125(4) Uani 1 1 d . . . H1A H 0.9379 0.6003 0.2893 0.188 Uiso 1 1 d R . . H1B H 0.9136 0.5528 0.3511 0.188 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0515(13) 0.124(2) 0.0364(11) -0.0322(11) -0.0145(9) 0.0574(13) Mn2 0.0268(6) 0.0285(6) 0.0238(6) -0.0023(4) 0.0022(4) 0.0162(5) C1 0.037(4) 0.055(5) 0.028(4) -0.009(3) -0.006(3) 0.028(4) C2 0.034(4) 0.048(4) 0.026(4) -0.008(3) -0.004(3) 0.028(4) C3 0.033(4) 0.053(5) 0.025(4) -0.009(3) -0.003(3) 0.027(4) C4 0.038(4) 0.058(5) 0.029(4) -0.013(4) -0.003(3) 0.028(4) C5 0.037(4) 0.046(4) 0.028(4) -0.008(3) -0.005(3) 0.029(4) C6 0.039(4) 0.052(5) 0.027(4) -0.010(3) -0.007(3) 0.035(4) C7 0.044(5) 0.058(5) 0.036(4) -0.013(4) -0.004(4) 0.028(4) C8 0.055(6) 0.062(6) 0.046(5) -0.016(4) -0.012(4) 0.025(5) C9 0.060(6) 0.067(6) 0.038(5) -0.019(4) -0.007(4) 0.031(5) C10 0.054(5) 0.072(6) 0.032(4) -0.009(4) 0.001(4) 0.033(5) C11 0.045(5) 0.059(5) 0.033(4) -0.005(4) -0.008(4) 0.030(4) C12 0.073(7) 0.072(8) 0.087(8) -0.023(7) -0.017(6) 0.020(6) N1 0.029(3) 0.032(3) 0.025(3) -0.004(2) -0.002(2) 0.018(3) N2 0.022(3) 0.042(4) 0.021(3) -0.006(2) -0.002(2) 0.015(3) O1 0.035(3) 0.072(4) 0.028(3) -0.015(3) -0.005(2) 0.037(3) O2 0.044(3) 0.110(5) 0.041(3) -0.033(3) -0.013(3) 0.047(4) O3 0.041(3) 0.120(6) 0.039(4) -0.029(4) -0.011(3) 0.045(4) O4 0.030(3) 0.062(3) 0.030(3) -0.012(2) -0.005(2) 0.033(3) O5 0.071 0.090 0.063 -0.024 -0.017 0.019 O6 0.059(4) 0.051(4) 0.067(4) 0.015(3) 0.019(3) 0.034(3) O7 0.040(3) 0.105(5) 0.046(4) -0.024(4) -0.006(3) 0.032(4) O8 0.104(7) 0.136(8) 0.106(7) 0.019(6) -0.010(6) 0.060(6) O1W 0.096(7) 0.133(8) 0.115(9) -0.009(6) -0.006(6) 0.033(6) _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 Mn1 O3 2.049(6) 13_665 ? Mn1 O3 2.049(6) . ? Mn1 O2 2.096(5) . ? Mn1 O2 2.096(5) 13_665 ? Mn1 O8 2.209(9) . ? Mn1 O8 2.209(9) 13_665 ? Mn2 O1 2.161(5) . ? Mn2 O4 2.168(5) 17_554 ? Mn2 N1 2.204(5) . ? Mn2 N2 2.221(5) 17_554 ? Mn2 O6 2.227(5) . ? Mn2 O7 2.233(6) . ? C1 O2 1.244(8) . ? C1 O1 1.258(8) . ? C1 C2 1.486(9) . ? C2 C3 1.372(10) . ? C2 N1 1.374(8) . ? C3 N2 1.370(8) . ? C3 C4 1.494(10) . ? C4 O3 1.242(8) . ? C4 O4 1.260(9) . ? C5 N2 1.345(8) . ? C5 N1 1.348(8) . ? C5 C6 1.487(9) . ? C6 C7 1.380(11) . ? C6 C11 1.395(11) . ? C7 C8 1.396(11) . ? C7 H7 0.9300 . ? C8 C9 1.376(12) . ? C8 O5 1.405(11) . ? C9 C10 1.352(12) . ? C9 H9 0.9300 . ? C10 C11 1.387(11) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 O5 1.390(13) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? N2 Mn2 2.221(5) 18_544 ? O4 Mn2 2.168(5) 18_544 ? O6 H6A 0.8499 . ? O6 H6B 0.8500 . ? O7 H7A 0.8503 . ? O7 H7B 0.8500 . ? O8 H8A 0.8669 . ? O8 H8B 0.8736 . ? O1W H1A 0.8571 . ? O1W H1B 0.8672 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Mn1 O3 179.997(1) 13_665 . ? O3 Mn1 O2 89.4(2) 13_665 . ? O3 Mn1 O2 90.6(2) . . ? O3 Mn1 O2 90.6(2) 13_665 13_665 ? O3 Mn1 O2 89.4(2) . 13_665 ? O2 Mn1 O2 180.0(3) . 13_665 ? O3 Mn1 O8 94.0(3) 13_665 . ? O3 Mn1 O8 86.0(3) . . ? O2 Mn1 O8 89.6(3) . . ? O2 Mn1 O8 90.4(3) 13_665 . ? O3 Mn1 O8 86.0(3) 13_665 13_665 ? O3 Mn1 O8 94.0(3) . 13_665 ? O2 Mn1 O8 90.4(3) . 13_665 ? O2 Mn1 O8 89.6(3) 13_665 13_665 ? O8 Mn1 O8 179.997(1) . 13_665 ? O1 Mn2 O4 172.50(19) . 17_554 ? O1 Mn2 N1 74.67(18) . . ? O4 Mn2 N1 112.7(2) 17_554 . ? O1 Mn2 N2 104.3(2) . 17_554 ? O4 Mn2 N2 75.36(18) 17_554 17_554 ? N1 Mn2 N2 107.3(2) . 17_554 ? O1 Mn2 O6 96.5(2) . . ? O4 Mn2 O6 83.0(2) 17_554 . ? N1 Mn2 O6 85.8(2) . . ? N2 Mn2 O6 157.7(2) 17_554 . ? O1 Mn2 O7 84.3(2) . . ? O4 Mn2 O7 88.3(2) 17_554 . ? N1 Mn2 O7 153.8(2) . . ? N2 Mn2 O7 92.7(2) 17_554 . ? O6 Mn2 O7 81.2(2) . . ? O2 C1 O1 120.8(6) . . ? O2 C1 C2 122.9(6) . . ? O1 C1 C2 116.3(6) . . ? C3 C2 N1 108.6(6) . . ? C3 C2 C1 135.4(6) . . ? N1 C2 C1 115.9(6) . . ? N2 C3 C2 109.0(6) . . ? N2 C3 C4 117.0(6) . . ? C2 C3 C4 134.0(6) . . ? O3 C4 O4 121.7(7) . . ? O3 C4 C3 121.8(7) . . ? O4 C4 C3 116.4(6) . . ? N2 C5 N1 113.7(6) . . ? N2 C5 C6 122.4(6) . . ? N1 C5 C6 123.9(6) . . ? C7 C6 C11 120.7(7) . . ? C7 C6 C5 119.3(7) . . ? C11 C6 C5 120.0(7) . . ? C6 C7 C8 118.3(8) . . ? C6 C7 H7 120.8 . . ? C8 C7 H7 120.8 . . ? C9 C8 C7 121.6(8) . . ? C9 C8 O5 117.6(8) . . ? C7 C8 O5 120.7(9) . . ? C10 C9 C8 118.8(8) . . ? C10 C9 H9 120.6 . . ? C8 C9 H9 120.6 . . ? C9 C10 C11 122.3(8) . . ? C9 C10 H10 118.9 . . ? C11 C10 H10 118.9 . . ? C10 C11 C6 118.3(8) . . ? C10 C11 H11 120.8 . . ? C6 C11 H11 120.8 . . ? O5 C12 H12A 109.5 . . ? O5 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? O5 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C5 N1 C2 104.3(5) . . ? C5 N1 Mn2 142.2(5) . . ? C2 N1 Mn2 113.4(4) . . ? C5 N2 C3 104.4(5) . . ? C5 N2 Mn2 142.1(4) . 18_544 ? C3 N2 Mn2 110.8(4) . 18_544 ? C1 O1 Mn2 119.0(4) . . ? C1 O2 Mn1 144.0(5) . . ? C4 O3 Mn1 140.0(6) . . ? C4 O4 Mn2 117.8(4) . 18_544 ? C12 O5 C8 119.0(8) . . ? Mn2 O6 H6A 97.4 . . ? Mn2 O6 H6B 87.2 . . ? H6A O6 H6B 111.6 . . ? Mn2 O7 H7A 118.2 . . ? Mn2 O7 H7B 104.5 . . ? H7A O7 H7B 105.0 . . ? Mn1 O8 H8A 123.7 . . ? Mn1 O8 H8B 125.6 . . ? H8A O8 H8B 109.4 . . ? H1A O1W H1B 105.3 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O6 H6A O7 0.85 2.43 2.903(9) 115.8 . O6 H6A O2 0.85 2.56 3.310(8) 147.5 9_664 O6 H6B O4 0.85 2.34 2.912(7) 125.4 17_554 O7 H7A O1W 0.85 2.23 3.044(11) 160.2 5_654 O7 H7B O4 0.85 2.29 2.805(7) 118.8 12_655 O8 H8A O1W 0.87 1.87 2.716(13) 166.4 . _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.652 _refine_diff_density_min -1.875 _refine_diff_density_rms 0.137 data_a6 _database_code_depnum_ccdc_archive 'CCDC 915955' #TrackingRef '81.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H0 N12 O60 Zn9' _chemical_formula_weight 2581.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M p-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.9799(8) _cell_length_b 14.9811(5) _cell_length_c 14.9811(5) _cell_angle_alpha 110.7850(10) _cell_angle_beta 108.123(2) _cell_angle_gamma 108.1230(10) _cell_volume 2454.29(18) _cell_formula_units_Z 1 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.746 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1266 _exptl_absorpt_coefficient_mu 2.272 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3963 _exptl_absorpt_correction_T_max 0.5489 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13325 _diffrn_reflns_av_R_equivalents 0.1039 _diffrn_reflns_av_sigmaI/netI 0.2307 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 25.99 _reflns_number_total 9172 _reflns_number_gt 4359 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^ > 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^)+(0.1564P)^2^+2.3475P] 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 9172 _refine_ls_number_parameters 686 _refine_ls_number_restraints 1872 _refine_ls_R_factor_all 0.2140 _refine_ls_R_factor_gt 0.1162 _refine_ls_wR_factor_ref 0.3458 _refine_ls_wR_factor_gt 0.3007 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.014 _refine_ls_shift/su_max 0.182 _refine_ls_shift/su_mean 0.006 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2090(13) -0.0486(11) 0.8768(12) 0.033(2) Uani 1 1 d U . . C2 C 0.2680(13) 0.0603(11) 0.9225(12) 0.032(2) Uani 1 1 d U . . C3 C 0.0875(13) 0.0168(12) 0.8665(12) 0.035(2) Uani 1 1 d U . . C4 C -0.0174(13) 0.0234(12) 0.8408(12) 0.037(2) Uani 1 1 d U . . C7 C 0.2375(13) -0.1381(11) 0.8573(12) 0.033(2) Uani 1 1 d U . . C8 C 0.3924(13) 0.1413(12) 0.9758(12) 0.035(2) Uani 1 1 d U . . C12 C 0.1554(13) 0.4258(12) 0.8623(12) 0.034(2) Uani 1 1 d U . . C13 C 0.1694(13) 0.3765(12) 0.9260(12) 0.033(2) Uani 1 1 d U . . C14 C 0.0834(13) 0.4733(12) 0.8333(12) 0.034(2) Uani 1 1 d U . . C15 C 0.1162(13) 0.3550(12) 0.9940(12) 0.036(2) Uani 1 1 d U . . C16 C 0.2776(13) 0.3674(12) 0.8517(12) 0.0337(19) Uani 1 1 d U . . C17 C 0.3595(13) 0.3409(12) 0.8151(12) 0.035(2) Uani 1 1 d U . . C18 C 0.4616(13) 0.3580(12) 0.8879(13) 0.038(2) Uani 1 1 d U . . H18 H 0.4811 0.3866 0.9610 0.046 Uiso 1 1 calc R . . C19 C 0.3251(14) 0.2929(12) 0.7059(13) 0.040(2) Uani 1 1 d U . . H19 H 0.2565 0.2815 0.6562 0.048 Uiso 1 1 calc R . . C20 C -0.2080(13) -0.3615(12) 0.5604(12) 0.035(2) Uani 1 1 d U . . C21 C -0.2530(14) -0.3343(13) 0.6401(13) 0.043(3) Uani 1 1 d U . . C22 C 0.2568(13) 0.4250(12) 0.5475(12) 0.035(2) Uani 1 1 d U . . C23 C 0.3794(13) 0.4978(12) 0.6407(12) 0.036(2) Uani 1 1 d U . . C24 C 0.0698(13) 0.3482(12) 0.4829(12) 0.035(2) Uani 1 1 d U . . C25 C -0.0403(14) 0.3157(13) 0.4759(12) 0.038(2) Uani 1 1 d U . . C26 C -0.0720(14) 0.3881(14) 0.5291(13) 0.043(2) Uani 1 1 d U . . H26 H -0.0214 0.4621 0.5712 0.051 Uiso 1 1 calc R . . C27 C -0.1197(14) 0.2051(13) 0.4140(13) 0.043(3) Uani 1 1 d U . . H27 H -0.1001 0.1550 0.3778 0.052 Uiso 1 1 calc R . . C28 C 0.5006(15) 0.2870(13) 0.7472(14) 0.047(2) Uani 1 1 d U . . H28 H 0.5508 0.2715 0.7239 0.057 Uiso 1 1 calc R . . C29 C 0.5339(15) 0.3334(12) 0.8536(14) 0.044(3) Uani 1 1 d U . . H29 H 0.6047 0.3484 0.9028 0.053 Uiso 1 1 calc R . . C31 C 0.2658(16) 0.1603(14) 0.4873(14) 0.055(4) Uani 1 1 d U . . H31A H 0.2344 0.2076 0.4809 0.082 Uiso 1 1 calc R . . H31B H 0.2221 0.1120 0.5047 0.082 Uiso 1 1 calc R . . H31C H 0.2629 0.1188 0.4199 0.082 Uiso 1 1 calc R . . C32 C 0.3994(15) 0.2619(13) 0.6729(14) 0.047(2) Uani 1 1 d U . . C36 C -0.1012(14) -0.0275(13) 0.8593(13) 0.043(2) Uani 1 1 d U . . H36 H -0.0930 -0.0700 0.8908 0.051 Uiso 1 1 calc R . . C37 C -0.0319(14) 0.0888(12) 0.7901(13) 0.043(2) Uani 1 1 d U . . H37 H 0.0236 0.1236 0.7751 0.051 Uiso 1 1 calc R . . C43 C -0.2799(19) -0.0180(18) 0.3231(19) 0.086(3) Uani 1 1 d U . . H43A H -0.2353 -0.0124 0.3901 0.129 Uiso 1 1 calc R . . H43B H -0.2351 -0.0100 0.2864 0.129 Uiso 1 1 calc R . . H43C H -0.3469 -0.0877 0.2780 0.129 Uiso 1 1 calc R . . C44 C -0.2567(16) 0.2430(14) 0.4579(14) 0.052(3) Uani 1 1 d U . . H44 H -0.3301 0.2191 0.4503 0.062 Uiso 1 1 calc R . . C45 C -0.2288(15) 0.1697(14) 0.4066(14) 0.051(3) Uani 1 1 d U . . C46 C -0.1852(14) 0.3456(14) 0.5175(13) 0.046(2) Uani 1 1 d U . . H46 H -0.2076 0.3930 0.5535 0.055 Uiso 1 1 calc R . . C52 C -0.1016(17) 0.1761(16) 0.6636(16) 0.066(2) Uani 1 1 d U . . H52A H -0.1298 0.1114 0.5970 0.100 Uiso 1 1 calc R . . H52B H -0.0215 0.2030 0.7077 0.100 Uiso 1 1 calc R . . H52C H -0.1127 0.2300 0.6479 0.100 Uiso 1 1 calc R . . C56 C -0.1999(15) -0.0162(13) 0.8313(14) 0.048(3) Uani 1 1 d U . . H56 H -0.2560 -0.0491 0.8468 0.058 Uiso 1 1 calc R . . C58 C -0.1347(14) 0.0970(13) 0.7648(13) 0.044(2) Uani 1 1 d U . . C59 C -0.2150(16) 0.0413(14) 0.7825(14) 0.052(3) Uani 1 1 d U . . H59 H -0.2843 0.0425 0.7599 0.062 Uiso 1 1 calc R . . N1 N 0.0946(9) -0.0778(8) 0.8409(9) 0.025(3) Uani 1 1 d . . . N2 N 0.1944(9) 0.1031(8) 0.9179(10) 0.029(3) Uani 1 1 d . . . N3 N 0.2240(10) 0.4177(9) 0.8141(9) 0.028(3) Uani 1 1 d . . . N4 N 0.2466(10) 0.3406(9) 0.9167(9) 0.027(3) Uani 1 1 d . . . N5 N -0.0895(9) -0.3147(8) 0.6018(8) 0.025(3) Uani 1 1 d . . . N6 N 0.1711(10) 0.4165(9) 0.5776(8) 0.028(3) Uani 1 1 d . . . O1 O 0.3379(9) -0.1232(8) 0.8872(9) 0.045(2) Uani 1 1 d U . . O2 O 0.1537(8) -0.2335(7) 0.8024(8) 0.030(2) Uani 1 1 d U . . O3 O 0.4640(9) 0.1089(8) 0.9647(9) 0.044(2) Uani 1 1 d U . . O4 O 0.4153(9) 0.2402(8) 1.0163(8) 0.037(2) Uani 1 1 d U . . O6 O 0.1494(9) 0.3029(8) 1.0356(8) 0.0333(18) Uani 1 1 d U . . O7 O 0.0479(10) 0.3867(9) 1.0104(9) 0.045(2) Uani 1 1 d U . . O8 O 0.0997(9) 0.5165(8) 0.7742(8) 0.0383(19) Uani 1 1 d U . . O9 O 0.0008(10) 0.4661(9) 0.8547(9) 0.046(2) Uani 1 1 d U . . O10 O -0.1761(8) -0.2751(8) 0.7406(7) 0.033(2) Uani 1 1 d U . . O11 O -0.3554(9) -0.3554(9) 0.6097(8) 0.047(3) Uani 1 1 d U . . O12 O 0.3883(10) 0.5368(8) 0.7342(8) 0.039(2) Uani 1 1 d U . . O13 O 0.3717(14) 0.2177(13) 0.5640(13) 0.098(3) Uani 1 1 d U . . O14 O 0.4481(12) 0.0318(10) 1.1185(11) 0.075(4) Uani 1 1 d U . . H14B H 0.5043 0.0403 1.1734 0.112 Uiso 1 1 d R . . O15 O -0.1718(11) 0.3784(11) 0.9086(11) 0.072(4) Uani 1 1 d U . . H15B H -0.1980 0.3584 0.9463 0.108 Uiso 1 1 d R . . O16 O -0.0559(11) -0.4007(9) 0.7589(11) 0.070(3) Uani 1 1 d U . . H16B H -0.0718 -0.4177 0.6937 0.105 Uiso 1 1 d R . . H16A H -0.0236 -0.4360 0.7758 0.105 Uiso 1 1 d R . . O17 O 0.0314(11) -0.2066(10) 0.9385(10) 0.067(3) Uani 1 1 d U . . H17A H -0.0060 -0.2132 0.9729 0.101 Uiso 1 1 d R . . H17B H 0.0648 -0.1399 0.9575 0.101 Uiso 1 1 d R . . O18 O -0.4196(11) -0.5905(10) 0.5295(10) 0.071(4) Uani 1 1 d U . . H18A H -0.3714 -0.5914 0.5800 0.107 Uiso 1 1 d R . . H18B H -0.4191 -0.6257 0.4711 0.107 Uiso 1 1 d R . . O19 O 0.3173(11) 0.2621(10) 1.1632(10) 0.062(3) Uani 1 1 d U . . H19A H 0.3751 0.3247 1.1970 0.092 Uiso 1 1 d R . . H19B H 0.2620 0.2738 1.1658 0.092 Uiso 1 1 d R . . O20 O 0.4074(11) 0.4404(9) 1.1433(10) 0.071(4) Uani 1 1 d U . . H20B H 0.4798 0.4678 1.1730 0.106 Uiso 1 1 d R . . H20A H 0.3880 0.4690 1.1058 0.106 Uiso 1 1 d R . . O21 O -0.3101(12) 0.0582(12) 0.3431(12) 0.086(3) Uani 1 1 d U . . O23 O 0.4634(11) 0.5115(10) 0.6237(10) 0.066(3) Uani 1 1 d U . . O24 O 0.3420(12) 0.6585(10) 0.8971(10) 0.079(4) Uani 1 1 d U . . H24B H 0.3290 0.6878 0.9489 0.118 Uiso 1 1 d R . . H24A H 0.4134 0.6927 0.9194 0.118 Uiso 1 1 d R . . O25 O 0.2389(12) 0.6443(10) 0.7040(10) 0.065(3) Uani 1 1 d U . . H25B H 0.1862 0.6524 0.7168 0.098 Uiso 1 1 d R . . H25A H 0.2092 0.6079 0.6354 0.098 Uiso 1 1 d R . . O27 O -0.1542(11) 0.1553(10) 0.7130(11) 0.066(2) Uani 1 1 d U . . Zn1 Zn 0.27755(13) 0.27056(11) 1.01438(11) 0.0213(4) Uani 1 1 d . . . Zn2 Zn 0.23635(13) 0.51391(11) 0.74328(11) 0.0212(4) Uani 1 1 d . . . Zn3 Zn -0.00694(13) -0.24362(11) 0.77059(11) 0.0220(4) Uani 1 1 d . . . Zn4 Zn 0.5000 0.0000 1.0000 0.0433(8) Uani 1 2 d S . . Zn5 Zn -0.5000 -0.5000 0.5000 0.0423(8) Uani 1 2 d S . . Zn6 Zn 0.0000 0.5000 1.0000 0.0415(7) Uani 1 2 d S . . O1W O 0.5147(14) 0.2399(12) 0.2584(13) 0.104(5) Uani 1 1 d U A 1 H1B H 0.5044 0.2875 0.2447 0.156 Uiso 1 1 d R A 1 O2W O 0.7249(14) 0.4816(12) 0.7390(13) 0.101(4) Uani 1 1 d U . . H2A H 0.7797 0.5411 0.7941 0.151 Uiso 1 1 d R . . H2B H 0.6662 0.4906 0.7200 0.151 Uiso 1 1 d R . . O3W O 0.2380(13) 0.7558(11) 1.0159(11) 0.078(3) Uani 1 1 d U . . H3B H 0.2164 0.7408 0.9504 0.116 Uiso 1 1 d R . . H3A H 0.1877 0.7654 1.0324 0.116 Uiso 1 1 d R . . O4W O 0.444(4) 0.912(4) 0.216(6) 0.55(5) Uani 1 1 d . . . H4B H 0.4898 0.9245 0.1912 0.818 Uiso 1 1 d R . . H4A H 0.4805 0.9546 0.2847 0.818 Uiso 1 1 d R . . O5W O 0.7489(16) 0.3157(15) 0.7095(15) 0.132(5) Uani 1 1 d U . . H5B H 0.7202 0.2471 0.6782 0.198 Uiso 1 1 d R . . O5 O 0.4640(15) 0.2092(14) 0.3919(15) 0.121(4) Uani 1 1 d U . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.033(3) 0.038(3) 0.042(3) 0.023(3) 0.021(3) 0.025(3) C2 0.034(3) 0.038(3) 0.044(3) 0.028(3) 0.022(3) 0.028(3) C3 0.034(3) 0.041(3) 0.042(3) 0.022(2) 0.021(3) 0.027(3) C4 0.035(3) 0.042(3) 0.043(3) 0.021(3) 0.020(3) 0.027(3) C7 0.032(4) 0.038(3) 0.043(4) 0.023(3) 0.021(3) 0.026(3) C8 0.036(3) 0.039(3) 0.047(3) 0.027(2) 0.023(3) 0.026(3) C12 0.035(3) 0.045(3) 0.043(3) 0.029(2) 0.026(2) 0.028(2) C13 0.035(3) 0.043(3) 0.042(3) 0.029(2) 0.024(3) 0.027(3) C14 0.036(3) 0.047(3) 0.043(3) 0.031(2) 0.027(2) 0.027(2) C15 0.035(3) 0.045(3) 0.042(3) 0.024(3) 0.023(3) 0.027(3) C16 0.035(3) 0.041(2) 0.045(3) 0.026(2) 0.026(2) 0.029(2) C17 0.036(3) 0.042(3) 0.046(3) 0.026(2) 0.028(2) 0.028(2) C18 0.039(3) 0.041(3) 0.050(3) 0.028(3) 0.026(3) 0.024(3) C19 0.039(3) 0.045(3) 0.048(3) 0.025(3) 0.028(3) 0.025(3) C20 0.032(4) 0.043(4) 0.039(4) 0.019(3) 0.023(3) 0.023(3) C21 0.038(4) 0.045(4) 0.044(4) 0.018(3) 0.019(3) 0.023(3) C22 0.038(3) 0.044(3) 0.044(3) 0.025(3) 0.029(3) 0.028(3) C23 0.038(3) 0.043(3) 0.046(3) 0.025(3) 0.028(3) 0.028(3) C24 0.037(3) 0.046(3) 0.044(3) 0.031(2) 0.028(3) 0.025(3) C25 0.039(3) 0.052(3) 0.042(3) 0.032(3) 0.027(3) 0.024(3) C26 0.038(3) 0.054(3) 0.047(3) 0.030(3) 0.026(3) 0.024(3) C27 0.042(3) 0.053(3) 0.046(3) 0.033(3) 0.024(3) 0.021(3) C28 0.042(3) 0.047(3) 0.056(3) 0.021(3) 0.028(3) 0.025(3) C29 0.040(3) 0.045(3) 0.054(3) 0.024(3) 0.024(3) 0.026(3) C31 0.056(5) 0.052(5) 0.054(5) 0.021(4) 0.033(4) 0.024(5) C32 0.043(3) 0.047(3) 0.052(3) 0.018(3) 0.030(3) 0.023(3) C36 0.037(3) 0.046(3) 0.045(3) 0.018(3) 0.018(3) 0.026(3) C37 0.037(3) 0.047(3) 0.047(3) 0.021(2) 0.018(3) 0.027(3) C43 0.059(5) 0.077(5) 0.079(5) 0.031(4) 0.018(4) 0.007(4) C44 0.043(4) 0.060(4) 0.052(3) 0.033(3) 0.023(3) 0.018(3) C45 0.045(4) 0.057(4) 0.052(4) 0.032(3) 0.022(3) 0.020(3) C46 0.041(3) 0.057(3) 0.049(3) 0.029(3) 0.025(3) 0.026(3) C52 0.055(3) 0.068(3) 0.062(3) 0.029(3) 0.016(3) 0.029(3) C56 0.038(3) 0.051(3) 0.048(3) 0.015(3) 0.019(3) 0.025(3) C58 0.038(3) 0.049(3) 0.047(3) 0.021(3) 0.017(3) 0.029(3) C59 0.041(3) 0.052(3) 0.051(3) 0.015(3) 0.015(3) 0.027(3) N1 0.022(6) 0.024(5) 0.036(6) 0.018(5) 0.014(5) 0.015(5) N2 0.008(5) 0.027(6) 0.054(8) 0.028(6) 0.013(5) 0.006(5) N3 0.038(7) 0.048(7) 0.033(6) 0.030(6) 0.029(6) 0.034(6) N4 0.029(7) 0.033(6) 0.043(7) 0.027(6) 0.024(6) 0.025(6) N5 0.018(6) 0.025(5) 0.020(5) 0.005(5) 0.008(5) 0.005(5) N6 0.023(6) 0.035(6) 0.022(6) 0.009(5) 0.009(5) 0.015(5) O1 0.034(4) 0.036(4) 0.066(4) 0.023(3) 0.021(4) 0.023(3) O2 0.027(4) 0.028(3) 0.045(4) 0.021(3) 0.018(3) 0.021(3) O3 0.033(4) 0.036(4) 0.068(4) 0.028(3) 0.020(4) 0.024(3) O4 0.033(4) 0.037(4) 0.056(4) 0.032(3) 0.022(3) 0.022(3) O6 0.044(4) 0.049(3) 0.044(3) 0.037(3) 0.034(3) 0.036(3) O7 0.052(4) 0.067(4) 0.051(4) 0.041(3) 0.036(3) 0.042(3) O8 0.053(4) 0.061(4) 0.042(3) 0.039(3) 0.034(3) 0.045(3) O9 0.054(4) 0.070(4) 0.047(3) 0.040(3) 0.035(3) 0.044(3) O10 0.029(4) 0.038(4) 0.030(4) 0.010(3) 0.018(3) 0.016(3) O11 0.032(5) 0.051(5) 0.036(5) -0.002(4) 0.023(4) 0.014(4) O12 0.052(4) 0.052(4) 0.045(4) 0.033(3) 0.038(3) 0.037(3) O13 0.081(5) 0.089(5) 0.082(5) 0.015(4) 0.036(4) 0.029(5) O14 0.052(6) 0.068(6) 0.072(6) 0.016(5) 0.032(5) 0.010(5) O15 0.047(6) 0.086(6) 0.078(6) 0.047(5) 0.013(5) 0.036(5) O16 0.054(6) 0.053(5) 0.084(6) 0.038(5) 0.012(5) 0.021(5) O17 0.056(6) 0.066(6) 0.054(5) 0.026(5) 0.029(5) 0.002(5) O18 0.068(7) 0.085(7) 0.056(6) 0.012(6) 0.037(6) 0.051(6) O19 0.054(6) 0.079(6) 0.059(5) 0.037(5) 0.026(5) 0.038(5) O20 0.056(6) 0.052(5) 0.069(6) 0.020(5) 0.001(5) 0.027(5) O21 0.059(5) 0.077(5) 0.079(5) 0.031(4) 0.018(4) 0.007(4) O23 0.055(5) 0.075(5) 0.063(5) 0.016(4) 0.040(4) 0.034(4) O24 0.065(6) 0.073(6) 0.064(6) -0.002(5) 0.042(5) 0.027(5) O25 0.080(6) 0.067(5) 0.059(6) 0.026(5) 0.038(5) 0.048(5) O27 0.055(3) 0.068(3) 0.062(3) 0.029(3) 0.016(3) 0.029(3) Zn1 0.0211(8) 0.0203(7) 0.0188(7) 0.0082(6) 0.0057(6) 0.0113(6) Zn2 0.0287(9) 0.0208(7) 0.0197(7) 0.0099(6) 0.0135(7) 0.0162(7) Zn3 0.0240(9) 0.0208(7) 0.0179(7) 0.0094(6) 0.0089(6) 0.0085(7) Zn4 0.0227(13) 0.0303(12) 0.089(2) 0.0376(14) 0.0257(14) 0.0179(11) Zn5 0.0158(12) 0.0440(14) 0.0261(13) -0.0134(11) 0.0103(10) 0.0045(11) Zn6 0.0499(17) 0.092(2) 0.0402(14) 0.0515(15) 0.0374(13) 0.0606(17) O1W 0.094(7) 0.085(6) 0.094(7) 0.046(5) 0.011(6) 0.030(6) O2W 0.079(5) 0.087(5) 0.083(5) 0.018(4) 0.030(5) 0.018(5) O3W 0.081(5) 0.083(5) 0.057(5) 0.023(4) 0.033(4) 0.039(4) O4W 0.48(6) 0.64(8) 1.42(16) 0.91(11) 0.75(10) 0.52(7) O5W 0.096(6) 0.116(6) 0.097(6) 0.019(6) 0.023(6) 0.018(6) O5 0.089(6) 0.103(5) 0.097(6) 0.015(5) 0.022(5) 0.026(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.352(19) . ? C1 N1 1.379(18) . ? C1 C7 1.472(18) . ? C2 N2 1.369(17) . ? C2 C8 1.51(2) . ? C3 N2 1.369(18) . ? C3 N1 1.374(17) . ? C3 C4 1.44(2) . ? C4 C36 1.35(2) . ? C4 C37 1.46(2) . ? C7 O1 1.250(17) . ? C7 O2 1.271(16) . ? C8 O3 1.270(17) . ? C8 O4 1.269(16) . ? C12 N3 1.377(17) . ? C12 C13 1.40(2) . ? C12 C14 1.451(19) . ? C13 N4 1.370(17) . ? C13 C15 1.50(2) . ? C14 O9 1.275(18) . ? C14 O8 1.301(17) . ? C15 O7 1.242(17) . ? C15 O6 1.266(17) . ? C16 N4 1.315(18) . ? C16 N3 1.354(17) . ? C16 C17 1.51(2) . ? C17 C18 1.38(2) . ? C17 C19 1.37(2) . ? C18 C29 1.36(2) . ? C19 C32 1.41(2) . ? C20 C22 1.34(2) 2_556 ? C20 N5 1.396(18) . ? C20 C21 1.51(2) . ? C21 O11 1.252(19) . ? C21 O10 1.290(18) . ? C22 C20 1.34(2) 2_556 ? C22 N6 1.392(18) . ? C22 C23 1.53(2) . ? C23 O23 1.248(18) . ? C23 O12 1.260(17) . ? C24 N5 1.338(17) 2_556 ? C24 N6 1.373(18) . ? C24 C25 1.42(2) . ? C25 C26 1.38(2) . ? C25 C27 1.40(2) . ? C26 C46 1.44(2) . ? C27 C45 1.40(2) . ? C28 C32 1.33(2) . ? C28 C29 1.34(2) . ? C31 O13 1.30(2) . ? C32 O13 1.39(2) . ? C36 C56 1.40(2) . ? C37 C58 1.42(2) . ? C43 O21 1.31(3) . ? C44 C46 1.29(2) . ? C44 C45 1.34(2) . ? C45 O21 1.42(2) . ? C52 O27 1.24(2) . ? C56 C59 1.34(2) . ? C58 C59 1.34(2) . ? C58 O27 1.39(2) . ? N1 Zn3 2.077(10) . ? N2 Zn1 2.074(11) . ? N3 Zn2 2.069(11) . ? N4 Zn1 2.099(11) . ? N5 C24 1.338(17) 2_556 ? N5 Zn3 2.090(10) . ? N6 Zn2 2.077(11) . ? O1 Zn4 2.050(10) . ? O2 Zn3 2.090(9) . ? O3 Zn4 2.037(10) . ? O4 Zn1 2.107(10) . ? O6 Zn1 2.081(10) . ? O7 Zn6 2.046(10) . ? O8 Zn2 2.109(10) . ? O9 Zn6 2.056(10) . ? O10 Zn3 2.124(10) . ? O11 Zn5 2.040(10) . ? O12 Zn2 2.100(11) . ? O14 Zn4 2.079(14) . ? O15 Zn6 2.103(13) . ? O16 Zn3 2.160(11) . ? O17 Zn3 2.215(12) . ? O18 Zn5 2.088(13) . ? O19 Zn1 2.184(12) . ? O20 Zn1 2.226(11) . ? O23 Zn5 2.036(13) 1_665 ? O24 Zn2 2.129(12) . ? O25 Zn2 2.224(12) . ? Zn4 O3 2.037(10) 2_657 ? Zn4 O1 2.050(11) 2_657 ? Zn4 O14 2.079(14) 2_657 ? Zn5 O11 2.040(10) 2_446 ? Zn5 O23 2.036(13) 1_445 ? Zn5 O23 2.036(13) 2_556 ? Zn5 O18 2.088(13) 2_446 ? Zn6 O7 2.046(10) 2_567 ? Zn6 O9 2.056(10) 2_567 ? Zn6 O15 2.103(13) 2_567 ? 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 C2 C1 N1 108.2(12) . . ? C2 C1 C7 135.9(14) . . ? N1 C1 C7 115.9(13) . . ? C1 C2 N2 109.8(13) . . ? C1 C2 C8 134.8(13) . . ? N2 C2 C8 115.4(12) . . ? N2 C3 N1 110.0(12) . . ? N2 C3 C4 125.2(13) . . ? N1 C3 C4 124.8(14) . . ? C36 C4 C3 124.3(14) . . ? C36 C4 C37 119.5(15) . . ? C3 C4 C37 116.2(15) . . ? O1 C7 O2 120.6(12) . . ? O1 C7 C1 122.7(14) . . ? O2 C7 C1 116.5(13) . . ? O3 C8 O4 123.7(14) . . ? O3 C8 C2 119.9(13) . . ? O4 C8 C2 115.7(13) . . ? N3 C12 C13 107.3(12) . . ? N3 C12 C14 117.5(12) . . ? C13 C12 C14 135.1(14) . . ? N4 C13 C12 107.9(13) . . ? N4 C13 C15 118.6(12) . . ? C12 C13 C15 133.6(13) . . ? O9 C14 O8 119.8(13) . . ? O9 C14 C12 123.3(13) . . ? O8 C14 C12 116.6(13) . . ? O7 C15 O6 122.6(14) . . ? O7 C15 C13 123.9(13) . . ? O6 C15 C13 113.5(12) . . ? N4 C16 N3 113.4(13) . . ? N4 C16 C17 125.0(13) . . ? N3 C16 C17 121.4(13) . . ? C18 C17 C19 121.3(15) . . ? C18 C17 C16 121.1(14) . . ? C19 C17 C16 117.5(14) . . ? C29 C18 C17 120.3(15) . . ? C17 C19 C32 116.4(15) . . ? C22 C20 N5 108.2(13) 2_556 . ? C22 C20 C21 134.3(15) 2_556 . ? N5 C20 C21 117.4(13) . . ? O11 C21 O10 122.6(15) . . ? O11 C21 C20 121.7(15) . . ? O10 C21 C20 115.0(14) . . ? C20 C22 N6 108.7(13) 2_556 . ? C20 C22 C23 135.7(14) 2_556 . ? N6 C22 C23 115.5(12) . . ? O23 C23 O12 123.2(15) . . ? O23 C23 C22 121.4(14) . . ? O12 C23 C22 115.2(14) . . ? N5 C24 N6 110.4(13) 2_556 . ? N5 C24 C25 124.7(14) 2_556 . ? N6 C24 C25 124.9(13) . . ? C26 C25 C27 118.5(15) . . ? C26 C25 C24 122.9(15) . . ? C27 C25 C24 118.5(15) . . ? C25 C26 C46 118.0(16) . . ? C25 C27 C45 120.2(16) . . ? C32 C28 C29 123.4(17) . . ? C18 C29 C28 118.4(16) . . ? C28 C32 O13 120.7(17) . . ? C28 C32 C19 119.8(16) . . ? O13 C32 C19 119.0(17) . . ? C4 C36 C56 120.0(16) . . ? C58 C37 C4 117.1(16) . . ? C46 C44 C45 122.5(19) . . ? C44 C45 C27 119.3(17) . . ? C44 C45 O21 120.1(17) . . ? C27 C45 O21 120.5(17) . . ? C44 C46 C26 121.5(17) . . ? C59 C56 C36 120.9(19) . . ? C59 C58 O27 120.9(15) . . ? C59 C58 C37 119.7(16) . . ? O27 C58 C37 119.1(17) . . ? C56 C59 C58 122.7(17) . . ? C1 N1 C3 106.2(11) . . ? C1 N1 Zn3 112.4(8) . . ? C3 N1 Zn3 141.3(10) . . ? C3 N2 C2 105.8(11) . . ? C3 N2 Zn1 139.6(10) . . ? C2 N2 Zn1 112.9(9) . . ? C16 N3 C12 105.1(11) . . ? C16 N3 Zn2 141.9(10) . . ? C12 N3 Zn2 110.8(8) . . ? C16 N4 C13 106.2(11) . . ? C16 N4 Zn1 143.2(10) . . ? C13 N4 Zn1 110.5(9) . . ? C24 N5 C20 106.9(12) 2_556 . ? C24 N5 Zn3 140.8(10) 2_556 . ? C20 N5 Zn3 110.9(9) . . ? C24 N6 C22 105.8(11) . . ? C24 N6 Zn2 141.8(10) . . ? C22 N6 Zn2 112.3(9) . . ? C7 O1 Zn4 138.0(10) . . ? C7 O2 Zn3 115.7(8) . . ? C8 O3 Zn4 129.6(10) . . ? C8 O4 Zn1 115.9(10) . . ? C15 O6 Zn1 117.9(9) . . ? C15 O7 Zn6 138.1(11) . . ? C14 O8 Zn2 113.5(9) . . ? C14 O9 Zn6 128.9(10) . . ? C21 O10 Zn3 115.4(9) . . ? C21 O11 Zn5 129.1(10) . . ? C23 O12 Zn2 116.7(10) . . ? C31 O13 C32 121.7(18) . . ? C43 O21 C45 122.1(17) . . ? C23 O23 Zn5 138.5(12) . 1_665 ? C52 O27 C58 121.5(16) . . ? N2 Zn1 O6 103.0(4) . . ? N2 Zn1 N4 109.6(4) . . ? O6 Zn1 N4 79.0(4) . . ? N2 Zn1 O4 78.5(4) . . ? O6 Zn1 O4 171.4(4) . . ? N4 Zn1 O4 108.6(4) . . ? N2 Zn1 O19 92.4(5) . . ? O6 Zn1 O19 86.0(4) . . ? N4 Zn1 O19 155.6(5) . . ? O4 Zn1 O19 85.4(4) . . ? N2 Zn1 O20 162.7(4) . . ? O6 Zn1 O20 89.8(5) . . ? N4 Zn1 O20 83.9(5) . . ? O4 Zn1 O20 87.1(5) . . ? O19 Zn1 O20 76.8(5) . . ? N3 Zn2 N6 109.2(4) . . ? N3 Zn2 O12 102.5(4) . . ? N6 Zn2 O12 79.5(4) . . ? N3 Zn2 O8 79.6(4) . . ? N6 Zn2 O8 108.5(4) . . ? O12 Zn2 O8 170.7(4) . . ? N3 Zn2 O24 92.0(5) . . ? N6 Zn2 O24 156.2(5) . . ? O12 Zn2 O24 85.6(5) . . ? O8 Zn2 O24 85.3(5) . . ? N3 Zn2 O25 163.2(4) . . ? N6 Zn2 O25 84.7(4) . . ? O12 Zn2 O25 88.9(4) . . ? O8 Zn2 O25 87.2(4) . . ? O24 Zn2 O25 76.5(5) . . ? N1 Zn3 O2 78.8(4) . . ? N1 Zn3 N5 109.7(4) . . ? O2 Zn3 N5 102.0(4) . . ? N1 Zn3 O10 108.8(4) . . ? O2 Zn3 O10 171.4(4) . . ? N5 Zn3 O10 79.6(4) . . ? N1 Zn3 O16 156.0(5) . . ? O2 Zn3 O16 85.8(4) . . ? N5 Zn3 O16 91.4(5) . . ? O10 Zn3 O16 85.7(4) . . ? N1 Zn3 O17 84.8(4) . . ? O2 Zn3 O17 89.9(5) . . ? N5 Zn3 O17 162.7(4) . . ? O10 Zn3 O17 86.8(4) . . ? O16 Zn3 O17 76.7(5) . . ? O3 Zn4 O3 180.000(5) . 2_657 ? O3 Zn4 O1 88.3(4) . 2_657 ? O3 Zn4 O1 91.7(4) 2_657 2_657 ? O3 Zn4 O1 91.7(4) . . ? O3 Zn4 O1 88.3(4) 2_657 . ? O1 Zn4 O1 180.000(1) 2_657 . ? O3 Zn4 O14 88.2(5) . 2_657 ? O3 Zn4 O14 91.8(5) 2_657 2_657 ? O1 Zn4 O14 90.0(5) 2_657 2_657 ? O1 Zn4 O14 90.0(5) . 2_657 ? O3 Zn4 O14 91.8(5) . . ? O3 Zn4 O14 88.2(5) 2_657 . ? O1 Zn4 O14 90.0(5) 2_657 . ? O1 Zn4 O14 90.0(5) . . ? O14 Zn4 O14 180.0(4) 2_657 . ? O11 Zn5 O11 180.0(7) . 2_446 ? O11 Zn5 O23 87.4(5) . 1_445 ? O11 Zn5 O23 92.6(5) 2_446 1_445 ? O11 Zn5 O23 92.6(5) . 2_556 ? O11 Zn5 O23 87.4(5) 2_446 2_556 ? O23 Zn5 O23 180.000(1) 1_445 2_556 ? O11 Zn5 O18 93.3(5) . . ? O11 Zn5 O18 86.7(5) 2_446 . ? O23 Zn5 O18 89.7(5) 1_445 . ? O23 Zn5 O18 90.3(5) 2_556 . ? O11 Zn5 O18 86.7(5) . 2_446 ? O11 Zn5 O18 93.3(5) 2_446 2_446 ? O23 Zn5 O18 90.3(5) 1_445 2_446 ? O23 Zn5 O18 89.7(5) 2_556 2_446 ? O18 Zn5 O18 180.000(2) . 2_446 ? O7 Zn6 O7 180.000(7) . 2_567 ? O7 Zn6 O9 87.4(4) . 2_567 ? O7 Zn6 O9 92.6(4) 2_567 2_567 ? O7 Zn6 O9 92.6(4) . . ? O7 Zn6 O9 87.4(4) 2_567 . ? O9 Zn6 O9 180.000(3) 2_567 . ? O7 Zn6 O15 89.2(5) . . ? O7 Zn6 O15 90.8(5) 2_567 . ? O9 Zn6 O15 93.0(5) 2_567 . ? O9 Zn6 O15 86.9(5) . . ? O7 Zn6 O15 90.8(5) . 2_567 ? O7 Zn6 O15 89.2(5) 2_567 2_567 ? O9 Zn6 O15 87.0(5) 2_567 2_567 ? O9 Zn6 O15 93.0(5) . 2_567 ? O15 Zn6 O15 180.000(1) . 2_567 ? _diffrn_measured_fraction_theta_max 0.953 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.953 _refine_diff_density_max 1.417 _refine_diff_density_min -1.460 _refine_diff_density_rms 0.223