# Electronic Supplementary Material (ESI) for Dalton Transactions # 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_a1 _database_code_depnum_ccdc_archive 'CCDC 895949' #TrackingRef '1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H10 N2 O6 Sr' _chemical_formula_weight 365.84 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' Sr Sr -1.5307 3.2498 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M p2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.085(3) _cell_length_b 6.6736(10) _cell_length_c 12.681(2) _cell_angle_alpha 90.00 _cell_angle_beta 111.524(2) _cell_angle_gamma 90.00 _cell_volume 1266.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 5014 _cell_measurement_theta_min 2.72 _cell_measurement_theta_max 27.86 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.919 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 728 _exptl_absorpt_coefficient_mu 4.289 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4808 _exptl_absorpt_correction_T_max 0.5469 _exptl_absorpt_process_details '(SADABS; Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEXII CCD ' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11482 _diffrn_reflns_av_R_equivalents 0.0480 _diffrn_reflns_av_unetI/netI 0.0427 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.72 _diffrn_reflns_theta_max 27.98 _reflns_number_total 3033 _reflns_number_gt 2524 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0557P)^2^+1.1286P] 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 3033 _refine_ls_number_parameters 200 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0460 _refine_ls_R_factor_gt 0.0351 _refine_ls_wR_factor_ref 0.0924 _refine_ls_wR_factor_gt 0.0852 _refine_ls_goodness_of_fit_ref 0.985 _refine_ls_restrained_S_all 0.985 _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 0.525800(17) 0.56429(3) 0.68184(2) 0.01650(10) Uani 1 1 d . . . O2 O 0.71109(17) 0.5730(3) 0.7598(2) 0.0296(5) Uani 1 1 d . . . H2 H 0.7281 0.6889 0.7602 0.044 Uiso 1 1 calc R . . C2 C 0.35629(18) 0.5603(4) 0.8996(2) 0.0161(5) Uani 1 1 d . . . O3 O 0.39428(14) 0.2882(3) 0.63338(16) 0.0224(4) Uani 1 1 d . . . N3 N 0.28801(16) 0.5315(4) 1.0259(2) 0.0199(5) Uani 1 1 d . . . C1 C 0.34476(19) 0.4390(4) 0.9814(2) 0.0167(5) Uani 1 1 d . . . O5 O 0.57821(15) 0.6314(3) 0.51881(17) 0.0254(5) Uani 1 1 d . . . N2 N 0.30341(17) 0.7254(4) 0.8937(2) 0.0201(5) Uani 1 1 d . . . C15 C 0.38929(18) 0.2530(4) 0.5341(2) 0.0168(5) Uani 1 1 d . . . C5 C 0.1698(2) 1.0081(5) 0.9122(3) 0.0270(6) Uani 1 1 d . . . H5 H 0.1800 1.0083 0.8446 0.032 Uiso 1 1 calc R . . C4 C 0.20643(19) 0.8579(5) 0.9916(2) 0.0220(6) Uani 1 1 d . . . C6 C 0.1180(2) 1.1585(5) 0.9336(3) 0.0296(7) Uani 1 1 d . . . C3 C 0.26473(19) 0.7051(4) 0.9712(2) 0.0197(5) Uani 1 1 d . . . C7 C 0.1909(2) 0.8581(5) 1.0922(3) 0.0315(7) Uani 1 1 d . . . H7 H 0.2150 0.7578 1.1456 0.038 Uiso 1 1 calc R . . C8 C 0.1395(3) 1.0078(6) 1.1125(3) 0.0410(9) Uani 1 1 d . . . H8 H 0.1294 1.0076 1.1802 0.049 Uiso 1 1 calc R . . O7 O 0.47541(13) 0.4309(3) 0.85208(17) 0.0179(4) Uani 1 1 d . . . O6 O 0.40965(14) 0.7131(3) 0.77082(16) 0.0204(4) Uani 1 1 d . . . C9 C 0.1025(2) 1.1583(6) 1.0338(3) 0.0375(8) Uani 1 1 d . . . H9 H 0.0677 1.2580 1.0484 0.045 Uiso 1 1 calc R . . C11 C 0.41739(18) 0.5649(4) 0.8360(2) 0.0155(5) Uani 1 1 d . . . O8 O 0.08564(19) 1.2980(4) 0.8493(2) 0.0453(7) Uani 1 1 d . . . C10 C 0.0332(3) 1.4559(6) 0.8668(4) 0.0519(11) Uani 1 1 d . . . H10A H 0.0663 1.5241 0.9362 0.078 Uiso 1 1 calc R . . H10B H -0.0208 1.4020 0.8713 0.078 Uiso 1 1 calc R . . H10C H 0.0184 1.5486 0.8047 0.078 Uiso 1 1 calc R . . H1W H 0.720(3) 0.549(7) 0.818(4) 0.045(14) Uiso 1 1 d . . . H2W H 0.304(2) 0.816(6) 0.860(3) 0.031(11) 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 Sr1 0.02718(16) 0.00973(14) 0.01712(15) -0.00039(9) 0.01348(11) -0.00091(9) O2 0.0433(14) 0.0268(12) 0.0240(13) -0.0015(10) 0.0187(11) -0.0025(10) C2 0.0195(13) 0.0157(12) 0.0147(12) 0.0005(10) 0.0084(10) 0.0030(10) O3 0.0315(11) 0.0207(10) 0.0179(9) -0.0044(8) 0.0126(8) -0.0044(9) N3 0.0243(12) 0.0207(12) 0.0183(12) 0.0020(10) 0.0120(10) 0.0029(10) C1 0.0210(13) 0.0150(12) 0.0158(13) -0.0015(10) 0.0086(10) 0.0003(10) O5 0.0407(13) 0.0192(10) 0.0225(10) -0.0031(9) 0.0189(9) -0.0080(9) N2 0.0263(13) 0.0167(12) 0.0211(12) 0.0053(10) 0.0132(10) 0.0035(10) C15 0.0206(13) 0.0144(12) 0.0166(12) 0.0004(10) 0.0082(11) 0.0019(10) C5 0.0312(16) 0.0271(15) 0.0259(15) 0.0039(13) 0.0144(13) 0.0077(13) C4 0.0207(14) 0.0221(14) 0.0265(15) -0.0005(12) 0.0124(12) 0.0030(11) C6 0.0290(16) 0.0270(16) 0.0332(17) 0.0006(14) 0.0120(13) 0.0079(13) C3 0.0214(13) 0.0200(13) 0.0214(13) 0.0013(11) 0.0123(11) 0.0021(11) C7 0.0400(19) 0.0327(17) 0.0279(16) 0.0061(14) 0.0195(14) 0.0122(15) C8 0.054(2) 0.046(2) 0.0341(19) 0.0001(17) 0.0293(18) 0.0134(19) O7 0.0245(10) 0.0118(9) 0.0210(10) -0.0015(7) 0.0127(8) 0.0024(7) O6 0.0293(11) 0.0138(9) 0.0220(10) 0.0019(8) 0.0140(8) 0.0025(8) C9 0.0384(19) 0.0339(19) 0.046(2) -0.0031(16) 0.0228(16) 0.0147(15) C11 0.0206(13) 0.0110(11) 0.0163(13) -0.0033(10) 0.0085(10) -0.0036(10) O8 0.0586(17) 0.0344(13) 0.0457(15) 0.0114(12) 0.0225(13) 0.0280(13) C10 0.058(3) 0.034(2) 0.065(3) 0.0101(19) 0.024(2) 0.0258(19) _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 O7 2.4828(18) 2_656 ? Sr1 O5 2.542(2) . ? Sr1 O6 2.544(2) 2_646 ? Sr1 O3 2.677(2) 2_656 ? Sr1 O3 2.701(2) . ? Sr1 O6 2.7013(19) . ? Sr1 O7 2.719(2) . ? Sr1 O2 2.775(3) . ? Sr1 O5 2.803(2) 3_666 ? Sr1 Sr1 3.9831(5) 2_656 ? Sr1 Sr1 3.9831(5) 2_646 ? Sr1 Sr1 4.4592(9) 3_666 ? Sr1 H1W 2.96(5) . ? O2 H2 0.8200 . ? O2 H1W 0.72(5) . ? C2 N2 1.377(3) . ? C2 C1 1.381(4) . ? C2 C11 1.482(4) . ? O3 Sr1 2.677(2) 2_646 ? N3 C3 1.331(4) . ? N3 C1 1.383(4) . ? C1 C15 1.500(4) 4_566 ? O5 C15 1.255(3) 3_666 ? O5 Sr1 2.803(2) 3_666 ? N2 C3 1.350(3) . ? N2 H2W 0.74(4) . ? C15 O5 1.255(3) 3_666 ? C15 C1 1.500(4) 4_565 ? C5 C4 1.389(4) . ? C5 C6 1.394(4) . ? C5 H5 0.9300 . ? C4 C7 1.386(4) . ? C4 C3 1.471(4) . ? C6 O8 1.368(4) . ? C6 C9 1.382(5) . ? C7 C8 1.380(5) . ? C7 H7 0.9300 . ? C8 C9 1.387(5) . ? C8 H8 0.9300 . ? O7 C11 1.254(3) . ? O7 Sr1 2.4828(18) 2_646 ? O6 C11 1.266(3) . ? O6 Sr1 2.544(2) 2_656 ? C9 H9 0.9300 . ? O8 C10 1.417(4) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 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 O7 Sr1 O5 70.70(7) 2_656 . ? O7 Sr1 O6 157.68(6) 2_656 2_646 ? O5 Sr1 O6 97.23(7) . 2_646 ? O7 Sr1 O3 64.68(6) 2_656 2_656 ? O5 Sr1 O3 114.68(7) . 2_656 ? O6 Sr1 O3 106.51(6) 2_646 2_656 ? O7 Sr1 O3 132.62(6) 2_656 . ? O5 Sr1 O3 113.63(6) . . ? O6 Sr1 O3 69.08(6) 2_646 . ? O3 Sr1 O3 131.64(3) 2_656 . ? O7 Sr1 O6 75.37(6) 2_656 . ? O5 Sr1 O6 139.59(7) . . ? O6 Sr1 O6 121.67(5) 2_646 . ? O3 Sr1 O6 67.21(6) 2_656 . ? O3 Sr1 O6 75.04(6) . . ? O7 Sr1 O7 118.33(5) 2_656 . ? O5 Sr1 O7 170.96(6) . . ? O6 Sr1 O7 74.08(6) 2_646 . ? O3 Sr1 O7 71.04(6) 2_656 . ? O3 Sr1 O7 61.35(6) . . ? O6 Sr1 O7 48.35(6) . . ? O7 Sr1 O2 88.87(7) 2_656 . ? O5 Sr1 O2 69.69(7) . . ? O6 Sr1 O2 69.10(7) 2_646 . ? O3 Sr1 O2 64.43(7) 2_656 . ? O3 Sr1 O2 138.11(7) . . ? O6 Sr1 O2 131.33(7) . . ? O7 Sr1 O2 108.54(7) . . ? O7 Sr1 O5 109.74(7) 2_656 3_666 ? O5 Sr1 O5 67.01(8) . 3_666 ? O6 Sr1 O5 80.85(6) 2_646 3_666 ? O3 Sr1 O5 171.81(6) 2_656 3_666 ? O3 Sr1 O5 47.05(6) . 3_666 ? O6 Sr1 O5 106.06(6) . 3_666 ? O7 Sr1 O5 108.40(6) . 3_666 ? O2 Sr1 O5 122.58(7) . 3_666 ? O7 Sr1 Sr1 42.27(5) 2_656 2_656 ? O5 Sr1 Sr1 112.92(5) . 2_656 ? O6 Sr1 Sr1 143.25(4) 2_646 2_656 ? O3 Sr1 Sr1 42.44(4) 2_656 2_656 ? O3 Sr1 Sr1 113.56(4) . 2_656 ? O6 Sr1 Sr1 39.15(4) . 2_656 ? O7 Sr1 Sr1 76.08(4) . 2_656 ? O2 Sr1 Sr1 101.27(5) . 2_656 ? O5 Sr1 Sr1 129.37(5) 3_666 2_656 ? O7 Sr1 Sr1 155.65(5) 2_656 2_646 ? O5 Sr1 Sr1 133.20(5) . 2_646 ? O6 Sr1 Sr1 42.09(4) 2_646 2_646 ? O3 Sr1 Sr1 101.38(4) 2_656 2_646 ? O3 Sr1 Sr1 41.98(4) . 2_646 ? O6 Sr1 Sr1 80.82(4) . 2_646 ? O7 Sr1 Sr1 37.89(4) . 2_646 ? O2 Sr1 Sr1 103.32(5) . 2_646 ? O5 Sr1 Sr1 81.59(4) 3_666 2_646 ? Sr1 Sr1 Sr1 113.806(15) 2_656 2_646 ? O7 Sr1 Sr1 91.36(5) 2_656 3_666 ? O5 Sr1 Sr1 35.35(5) . 3_666 ? O6 Sr1 Sr1 88.38(4) 2_646 3_666 ? O3 Sr1 Sr1 149.33(4) 2_656 3_666 ? O3 Sr1 Sr1 78.48(4) . 3_666 ? O6 Sr1 Sr1 127.44(4) . 3_666 ? O7 Sr1 Sr1 139.59(4) . 3_666 ? O2 Sr1 Sr1 98.08(5) . 3_666 ? O5 Sr1 Sr1 31.66(4) 3_666 3_666 ? Sr1 Sr1 Sr1 128.370(10) 2_656 3_666 ? Sr1 Sr1 Sr1 107.357(11) 2_646 3_666 ? O7 Sr1 H1W 94.3(9) 2_656 . ? O5 Sr1 H1W 83.6(10) . . ? O6 Sr1 H1W 65.1(8) 2_646 . ? O3 Sr1 H1W 56.3(9) 2_656 . ? O3 Sr1 H1W 132.7(9) . . ? O6 Sr1 H1W 120.8(10) . . ? O7 Sr1 H1W 94.7(10) . . ? O2 Sr1 H1W 13.9(10) . . ? O5 Sr1 H1W 131.5(9) 3_666 . ? Sr1 Sr1 H1W 96.9(9) 2_656 . ? Sr1 Sr1 H1W 93.4(9) 2_646 . ? Sr1 Sr1 H1W 110.7(10) 3_666 . ? Sr1 O2 H2 109.5 . . ? Sr1 O2 H1W 98(4) . . ? H2 O2 H1W 105.6 . . ? N2 C2 C1 105.0(2) . . ? N2 C2 C11 118.3(2) . . ? C1 C2 C11 136.0(2) . . ? Sr1 O3 Sr1 95.57(6) 2_646 . ? C3 N3 C1 106.1(2) . . ? C2 C1 N3 109.6(2) . . ? C2 C1 C15 131.4(3) . 4_566 ? N3 C1 C15 118.6(2) . 4_566 ? C15 O5 Sr1 150.48(18) 3_666 . ? C15 O5 Sr1 91.61(16) 3_666 3_666 ? Sr1 O5 Sr1 112.99(8) . 3_666 ? C3 N2 C2 108.7(2) . . ? C3 N2 H2W 127(3) . . ? C2 N2 H2W 123(3) . . ? O5 C15 C1 120.7(2) 3_666 4_565 ? C4 C5 C6 120.2(3) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C7 C4 C5 119.6(3) . . ? C7 C4 C3 120.2(3) . . ? C5 C4 C3 120.0(3) . . ? O8 C6 C9 125.0(3) . . ? O8 C6 C5 114.9(3) . . ? C9 C6 C5 120.1(3) . . ? N3 C3 N2 110.5(2) . . ? N3 C3 C4 126.0(3) . . ? N2 C3 C4 123.5(3) . . ? C8 C7 C4 119.6(3) . . ? C8 C7 H7 120.2 . . ? C4 C7 H7 120.2 . . ? C7 C8 C9 121.3(3) . . ? C7 C8 H8 119.4 . . ? C9 C8 H8 119.4 . . ? C11 O7 Sr1 135.78(17) . 2_646 ? C11 O7 Sr1 93.35(16) . . ? Sr1 O7 Sr1 99.83(7) 2_646 . ? C11 O6 Sr1 129.18(17) . 2_656 ? C11 O6 Sr1 93.92(16) . . ? Sr1 O6 Sr1 98.76(7) 2_656 . ? C6 C9 C8 119.2(3) . . ? C6 C9 H9 120.4 . . ? C8 C9 H9 120.4 . . ? O7 C11 O6 123.5(3) . . ? O7 C11 C2 119.9(2) . . ? O6 C11 C2 116.5(2) . . ? C6 O8 C10 117.5(3) . . ? O8 C10 H10A 109.5 . . ? O8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? O8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 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 O7 Sr1 O3 Sr1 -145.92(7) 2_656 . . 2_646 ? O5 Sr1 O3 Sr1 129.11(7) . . . 2_646 ? O6 Sr1 O3 Sr1 40.27(6) 2_646 . . 2_646 ? O3 Sr1 O3 Sr1 -53.59(10) 2_656 . . 2_646 ? O6 Sr1 O3 Sr1 -92.88(6) . . . 2_646 ? O7 Sr1 O3 Sr1 -42.51(5) . . . 2_646 ? O2 Sr1 O3 Sr1 43.67(11) . . . 2_646 ? O5 Sr1 O3 Sr1 137.35(11) 3_666 . . 2_646 ? Sr1 Sr1 O3 Sr1 -100.00(5) 2_656 . . 2_646 ? Sr1 Sr1 O3 Sr1 132.97(5) 3_666 . . 2_646 ? N2 C2 C1 N3 -1.6(3) . . . . ? C11 C2 C1 N3 167.9(3) . . . . ? N2 C2 C1 C15 -174.2(3) . . . 4_566 ? C11 C2 C1 C15 -4.7(6) . . . 4_566 ? C3 N3 C1 C2 0.6(3) . . . . ? C3 N3 C1 C15 174.4(2) . . . 4_566 ? O7 Sr1 O5 C15 21.7(4) 2_656 . . 3_666 ? O6 Sr1 O5 C15 -139.0(4) 2_646 . . 3_666 ? O3 Sr1 O5 C15 -27.0(4) 2_656 . . 3_666 ? O3 Sr1 O5 C15 150.7(4) . . . 3_666 ? O6 Sr1 O5 C15 56.2(4) . . . 3_666 ? O7 Sr1 O5 C15 -154.8(4) . . . 3_666 ? O2 Sr1 O5 C15 -74.5(4) . . . 3_666 ? O5 Sr1 O5 C15 144.2(5) 3_666 . . 3_666 ? Sr1 Sr1 O5 C15 19.5(4) 2_656 . . 3_666 ? Sr1 Sr1 O5 C15 -163.9(4) 2_646 . . 3_666 ? Sr1 Sr1 O5 C15 144.2(5) 3_666 . . 3_666 ? O7 Sr1 O5 Sr1 -122.50(10) 2_656 . . 3_666 ? O6 Sr1 O5 Sr1 76.83(9) 2_646 . . 3_666 ? O3 Sr1 O5 Sr1 -171.24(7) 2_656 . . 3_666 ? O3 Sr1 O5 Sr1 6.54(11) . . . 3_666 ? O6 Sr1 O5 Sr1 -88.00(11) . . . 3_666 ? O7 Sr1 O5 Sr1 61.0(5) . . . 3_666 ? O2 Sr1 O5 Sr1 141.34(10) . . . 3_666 ? O5 Sr1 O5 Sr1 0.0 3_666 . . 3_666 ? Sr1 Sr1 O5 Sr1 -124.66(6) 2_656 . . 3_666 ? Sr1 Sr1 O5 Sr1 51.94(11) 2_646 . . 3_666 ? C1 C2 N2 C3 1.9(3) . . . . ? C11 C2 N2 C3 -169.8(2) . . . . ? C6 C5 C4 C7 0.2(5) . . . . ? C6 C5 C4 C3 -177.0(3) . . . . ? C4 C5 C6 O8 179.9(3) . . . . ? C4 C5 C6 C9 -0.2(5) . . . . ? C1 N3 C3 N2 0.6(3) . . . . ? C1 N3 C3 C4 -178.5(3) . . . . ? C2 N2 C3 N3 -1.6(3) . . . . ? C2 N2 C3 C4 177.5(3) . . . . ? C7 C4 C3 N3 18.5(5) . . . . ? C5 C4 C3 N3 -164.3(3) . . . . ? C7 C4 C3 N2 -160.5(3) . . . . ? C5 C4 C3 N2 16.7(5) . . . . ? C5 C4 C7 C8 -0.2(5) . . . . ? C3 C4 C7 C8 177.0(3) . . . . ? C4 C7 C8 C9 0.3(6) . . . . ? O7 Sr1 O7 C11 35.36(14) 2_656 . . . ? O5 Sr1 O7 C11 -148.4(4) . . . . ? O6 Sr1 O7 C11 -164.74(16) 2_646 . . . ? O3 Sr1 O7 C11 81.02(15) 2_656 . . . ? O3 Sr1 O7 C11 -90.24(16) . . . . ? O6 Sr1 O7 C11 5.05(14) . . . . ? O2 Sr1 O7 C11 134.40(15) . . . . ? O5 Sr1 O7 C11 -90.35(15) 3_666 . . . ? Sr1 Sr1 O7 C11 36.97(14) 2_656 . . . ? Sr1 Sr1 O7 C11 -137.62(18) 2_646 . . . ? Sr1 Sr1 O7 C11 -97.09(15) 3_666 . . . ? O7 Sr1 O7 Sr1 172.98(9) 2_656 . . 2_646 ? O5 Sr1 O7 Sr1 -10.8(5) . . . 2_646 ? O6 Sr1 O7 Sr1 -27.12(6) 2_646 . . 2_646 ? O3 Sr1 O7 Sr1 -141.36(8) 2_656 . . 2_646 ? O3 Sr1 O7 Sr1 47.38(7) . . . 2_646 ? O6 Sr1 O7 Sr1 142.67(11) . . . 2_646 ? O2 Sr1 O7 Sr1 -87.98(8) . . . 2_646 ? O5 Sr1 O7 Sr1 47.27(8) 3_666 . . 2_646 ? Sr1 Sr1 O7 Sr1 174.59(7) 2_656 . . 2_646 ? Sr1 Sr1 O7 Sr1 40.53(9) 3_666 . . 2_646 ? O7 Sr1 O6 C11 -157.68(17) 2_656 . . . ? O5 Sr1 O6 C11 168.78(15) . . . . ? O6 Sr1 O6 C11 6.53(15) 2_646 . . . ? O3 Sr1 O6 C11 -89.38(16) 2_656 . . . ? O3 Sr1 O6 C11 59.74(16) . . . . ? O7 Sr1 O6 C11 -5.01(14) . . . . ? O2 Sr1 O6 C11 -82.56(17) . . . . ? O5 Sr1 O6 C11 95.57(16) 3_666 . . . ? Sr1 Sr1 O6 C11 -130.64(18) 2_656 . . . ? Sr1 Sr1 O6 C11 17.15(15) 2_646 . . . ? Sr1 Sr1 O6 C11 122.04(15) 3_666 . . . ? O7 Sr1 O6 Sr1 -27.05(6) 2_656 . . 2_656 ? O5 Sr1 O6 Sr1 -60.59(12) . . . 2_656 ? O6 Sr1 O6 Sr1 137.17(9) 2_646 . . 2_656 ? O3 Sr1 O6 Sr1 41.25(6) 2_656 . . 2_656 ? O3 Sr1 O6 Sr1 -169.63(8) . . . 2_656 ? O7 Sr1 O6 Sr1 125.63(10) . . . 2_656 ? O2 Sr1 O6 Sr1 48.07(10) . . . 2_656 ? O5 Sr1 O6 Sr1 -133.79(6) 3_666 . . 2_656 ? Sr1 Sr1 O6 Sr1 147.79(6) 2_646 . . 2_656 ? Sr1 Sr1 O6 Sr1 -107.32(5) 3_666 . . 2_656 ? O8 C6 C9 C8 -179.9(4) . . . . ? C5 C6 C9 C8 0.3(6) . . . . ? C7 C8 C9 C6 -0.3(6) . . . . ? Sr1 O7 C11 O6 -117.5(3) 2_646 . . . ? Sr1 O7 C11 O6 -9.7(3) . . . . ? Sr1 O7 C11 C2 65.7(4) 2_646 . . . ? Sr1 O7 C11 C2 173.5(2) . . . . ? Sr1 O6 C11 O7 -94.9(3) 2_656 . . . ? Sr1 O6 C11 O7 9.8(3) . . . . ? Sr1 O6 C11 C2 82.0(3) 2_656 . . . ? Sr1 O6 C11 C2 -173.3(2) . . . . ? N2 C2 C11 O7 169.8(2) . . . . ? C1 C2 C11 O7 1.3(5) . . . . ? N2 C2 C11 O6 -7.3(4) . . . . ? C1 C2 C11 O6 -175.7(3) . . . . ? C9 C6 O8 C10 0.8(6) . . . . ? C5 C6 O8 C10 -179.3(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 O2 H1W N3 0.72(5) 2.10(5) 2.800(4) 166(5) 3_667 N2 H2W O2 0.74(4) 2.24(4) 2.982(3) 173(4) 2_656 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.98 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.522 _refine_diff_density_min -0.714 _refine_diff_density_rms 0.115 data_a2 _database_code_depnum_ccdc_archive 'CCDC 895950' #TrackingRef '2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H18 N4 O10 Sr' _chemical_formula_weight 610.04 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' Sr Sr -1.5307 3.2498 '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' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 16.7894(12) _cell_length_b 16.7894(12) _cell_length_c 17.349(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4890.4(9) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 1689 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 20.42 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.657 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2464 _exptl_absorpt_coefficient_mu 2.272 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6593 _exptl_absorpt_correction_T_max 0.7125 _exptl_absorpt_process_details '(SADABS; Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEXII CCD ' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14668 _diffrn_reflns_av_R_equivalents 0.0843 _diffrn_reflns_av_unetI/netI 0.0680 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 27.49 _reflns_number_total 2803 _reflns_number_gt 1882 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0512P)^2^+7.9464P] 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 2803 _refine_ls_number_parameters 179 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0861 _refine_ls_R_factor_gt 0.0468 _refine_ls_wR_factor_ref 0.1217 _refine_ls_wR_factor_gt 0.1074 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.8551(3) 0.6148(3) 1.0069(3) 0.0435(12) Uani 1 1 d . . . H1 H 0.9079 0.6256 1.0192 0.052 Uiso 1 1 calc R . . C2 C 0.8068(3) 0.6739(3) 0.9772(3) 0.0388(11) Uani 1 1 d . . . C3 C 0.7274(2) 0.6584(2) 0.9595(2) 0.0311(10) Uani 1 1 d . . . H3 H 0.6950 0.6988 0.9405 0.037 Uiso 1 1 calc R . . C4 C 0.6969(2) 0.5822(2) 0.9705(2) 0.0280(9) Uani 1 1 d . . . C5 C 0.7455(3) 0.5227(3) 0.9995(3) 0.0341(10) Uani 1 1 d . . . H5 H 0.7254 0.4716 1.0065 0.041 Uiso 1 1 calc R . . C7 C 0.6147(2) 0.5650(2) 0.9474(2) 0.0253(8) Uani 1 1 d . . . C8 C 0.5125(2) 0.4996(2) 0.8995(2) 0.0253(9) Uani 1 1 d . . . C9 C 0.8034(4) 0.8034(4) 0.9231(5) 0.087(2) Uani 1 1 d . . . H9A H 0.7542 0.8174 0.9479 0.131 Uiso 1 1 calc R . . H9B H 0.7925 0.7828 0.8726 0.131 Uiso 1 1 calc R . . H9C H 0.8365 0.8498 0.9190 0.131 Uiso 1 1 calc R . . C10 C 0.4911(2) 0.5769(2) 0.9156(2) 0.0255(9) Uani 1 1 d . . . C11 C 0.4682(2) 0.4303(2) 0.8670(2) 0.0258(8) Uani 1 1 d . . . C12 C 0.4154(2) 0.6199(2) 0.9031(2) 0.0306(9) Uani 1 1 d . . . C13 C 0.8240(3) 0.5392(3) 1.0180(3) 0.0405(11) Uani 1 1 d . . . H13 H 0.8561 0.4991 1.0381 0.049 Uiso 1 1 calc R . . N1 N 0.55543(18) 0.61734(18) 0.94668(19) 0.0249(7) Uani 1 1 d . . . N2 N 0.59023(18) 0.49343(18) 0.92072(19) 0.0260(7) Uani 1 1 d . . . H2 H 0.6190 0.4511 0.9177 0.031 Uiso 1 1 calc R . . O1 O 0.8425(2) 0.7455(2) 0.9666(2) 0.0638(11) Uani 1 1 d . . . O2 O 0.50493(16) 0.36619(16) 0.86543(17) 0.0324(7) Uani 1 1 d . . . O3 O 0.39806(17) 0.44209(16) 0.84394(18) 0.0357(7) Uani 1 1 d . . . O4 O 0.40740(17) 0.68834(17) 0.92628(19) 0.0415(8) Uani 1 1 d . . . O5 O 0.35773(18) 0.58377(17) 0.8676(2) 0.0423(8) Uani 1 1 d . . . H5A H 0.3707 0.5376 0.8588 0.064 Uiso 1 1 calc R . . Sr1 Sr 0.5000 0.7500 1.02105(3) 0.02397(16) Uani 1 2 d S . . 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 0.027(2) 0.054(3) 0.050(3) -0.012(2) -0.005(2) -0.002(2) C2 0.034(2) 0.039(3) 0.043(3) -0.011(2) 0.002(2) -0.009(2) C3 0.029(2) 0.031(2) 0.033(2) -0.0046(18) 0.0006(17) 0.0019(18) C4 0.027(2) 0.026(2) 0.030(2) -0.0060(17) 0.0019(17) 0.0039(17) C5 0.032(2) 0.033(2) 0.038(2) -0.006(2) -0.0038(18) 0.0009(18) C7 0.026(2) 0.025(2) 0.025(2) -0.0024(16) 0.0001(16) -0.0021(16) C8 0.024(2) 0.026(2) 0.026(2) -0.0005(15) 0.0034(16) 0.0002(16) C9 0.090(5) 0.063(4) 0.108(6) 0.022(4) -0.006(4) -0.019(4) C10 0.027(2) 0.024(2) 0.026(2) -0.0016(16) 0.0010(16) 0.0004(17) C11 0.029(2) 0.022(2) 0.026(2) -0.0010(16) 0.0017(17) -0.0029(16) C12 0.029(2) 0.029(2) 0.035(2) 0.0024(18) -0.0034(18) 0.0002(18) C13 0.034(3) 0.040(3) 0.047(3) -0.007(2) -0.009(2) 0.014(2) N1 0.0220(17) 0.0200(17) 0.0325(19) -0.0025(14) -0.0006(14) -0.0014(13) N2 0.0215(17) 0.0221(17) 0.034(2) -0.0027(14) -0.0009(14) 0.0042(13) O1 0.058(2) 0.049(2) 0.084(3) 0.002(2) -0.002(2) -0.0245(19) O2 0.0294(15) 0.0227(14) 0.0451(19) -0.0071(13) -0.0005(13) -0.0006(11) O3 0.0304(16) 0.0271(16) 0.0495(19) -0.0040(13) -0.0103(14) -0.0005(12) O4 0.0335(17) 0.0303(17) 0.061(2) -0.0136(15) -0.0127(15) 0.0084(13) O5 0.0336(17) 0.0330(17) 0.060(2) -0.0142(16) -0.0139(15) 0.0051(13) Sr1 0.0218(3) 0.0216(3) 0.0285(3) 0.000 0.000 0.0012(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.381(6) . ? C1 C13 1.386(6) . ? C1 H1 0.9300 . ? C2 O1 1.357(5) . ? C2 C3 1.391(6) . ? C3 C4 1.391(5) . ? C3 H3 0.9300 . ? C4 C5 1.385(5) . ? C4 C7 1.466(5) . ? C5 C13 1.384(6) . ? C5 H5 0.9300 . ? C7 N1 1.327(5) . ? C7 N2 1.352(5) . ? C8 N2 1.360(5) . ? C8 C10 1.375(5) . ? C8 C11 1.491(5) . ? C9 O1 1.395(7) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 N1 1.385(5) . ? C10 C12 1.478(6) . ? C11 O2 1.241(4) . ? C11 O3 1.259(5) . ? C12 O4 1.224(5) . ? C12 O5 1.298(5) . ? C13 H13 0.9300 . ? N1 Sr1 2.737(3) . ? N2 H2 0.8600 . ? O2 Sr1 2.548(3) 7_544 ? O2 Sr1 2.773(3) 9_667 ? O4 Sr1 2.488(3) . ? O5 H5A 0.8200 . ? Sr1 O4 2.488(3) 6_564 ? Sr1 O2 2.548(3) 8_454 ? Sr1 O2 2.548(3) 3 ? Sr1 N1 2.737(3) 6_564 ? Sr1 O2 2.773(3) 14_557 ? Sr1 O2 2.773(3) 9_667 ? Sr1 C12 3.312(4) 6_564 ? Sr1 Sr1 3.6070(12) 15_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 C13 119.3(4) . . ? C2 C1 H1 120.4 . . ? C13 C1 H1 120.4 . . ? O1 C2 C1 115.4(4) . . ? O1 C2 C3 124.0(4) . . ? C1 C2 C3 120.6(4) . . ? C4 C3 C2 119.7(4) . . ? C4 C3 H3 120.2 . . ? C2 C3 H3 120.2 . . ? C5 C4 C3 119.7(4) . . ? C5 C4 C7 120.8(4) . . ? C3 C4 C7 119.4(4) . . ? C13 C5 C4 120.1(4) . . ? C13 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? N1 C7 N2 111.0(3) . . ? N1 C7 C4 125.3(3) . . ? N2 C7 C4 123.7(3) . . ? N2 C8 C10 105.5(3) . . ? N2 C8 C11 121.4(3) . . ? C10 C8 C11 133.1(4) . . ? O1 C9 H9A 109.5 . . ? O1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? O1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 N1 109.8(3) . . ? C8 C10 C12 131.0(4) . . ? N1 C10 C12 119.2(3) . . ? O2 C11 O3 126.4(4) . . ? O2 C11 C8 115.9(3) . . ? O3 C11 C8 117.6(3) . . ? O4 C12 O5 120.9(4) . . ? O4 C12 C10 120.3(4) . . ? O5 C12 C10 118.8(4) . . ? C5 C13 C1 120.6(4) . . ? C5 C13 H13 119.7 . . ? C1 C13 H13 119.7 . . ? C7 N1 C10 105.3(3) . . ? C7 N1 Sr1 142.1(3) . . ? C10 N1 Sr1 108.5(2) . . ? C7 N2 C8 108.4(3) . . ? C7 N2 H2 125.8 . . ? C8 N2 H2 125.8 . . ? C2 O1 C9 118.9(4) . . ? C11 O2 Sr1 131.5(3) . 7_544 ? C11 O2 Sr1 125.4(2) . 9_667 ? Sr1 O2 Sr1 85.23(8) 7_544 9_667 ? C12 O4 Sr1 122.6(3) . . ? C12 O5 H5A 109.5 . . ? O4 Sr1 O4 97.29(16) . 6_564 ? O4 Sr1 O2 152.79(9) . 8_454 ? O4 Sr1 O2 87.69(10) 6_564 8_454 ? O4 Sr1 O2 87.69(10) . 3 ? O4 Sr1 O2 152.79(9) 6_564 3 ? O2 Sr1 O2 100.03(13) 8_454 3 ? O4 Sr1 N1 64.05(9) . . ? O4 Sr1 N1 79.32(10) 6_564 . ? O2 Sr1 N1 90.93(9) 8_454 . ? O2 Sr1 N1 126.13(9) 3 . ? O4 Sr1 N1 79.32(10) . 6_564 ? O4 Sr1 N1 64.05(9) 6_564 6_564 ? O2 Sr1 N1 126.13(9) 8_454 6_564 ? O2 Sr1 N1 90.93(9) 3 6_564 ? N1 Sr1 N1 123.75(14) . 6_564 ? O4 Sr1 O2 141.31(9) . 14_557 ? O4 Sr1 O2 99.08(9) 6_564 14_557 ? O2 Sr1 O2 62.85(5) 8_454 14_557 ? O2 Sr1 O2 62.85(5) 3 14_557 ? N1 Sr1 O2 153.77(9) . 14_557 ? N1 Sr1 O2 76.85(9) 6_564 14_557 ? O4 Sr1 O2 99.08(9) . 9_667 ? O4 Sr1 O2 141.31(9) 6_564 9_667 ? O2 Sr1 O2 62.85(5) 8_454 9_667 ? O2 Sr1 O2 62.85(5) 3 9_667 ? N1 Sr1 O2 76.85(9) . 9_667 ? N1 Sr1 O2 153.77(9) 6_564 9_667 ? O2 Sr1 O2 89.50(11) 14_557 9_667 ? O4 Sr1 C12 97.72(11) . 6_564 ? O4 Sr1 C12 18.14(9) 6_564 6_564 ? O2 Sr1 C12 95.16(10) 8_454 6_564 ? O2 Sr1 C12 134.73(9) 3 6_564 ? N1 Sr1 C12 95.71(10) . 6_564 ? N1 Sr1 C12 47.02(10) 6_564 6_564 ? O2 Sr1 C12 87.82(9) 14_557 6_564 ? O2 Sr1 C12 156.22(9) 9_667 6_564 ? O4 Sr1 Sr1 131.35(8) . 15_567 ? O4 Sr1 Sr1 131.35(8) 6_564 15_567 ? O2 Sr1 Sr1 50.02(7) 8_454 15_567 ? O2 Sr1 Sr1 50.02(7) 3 15_567 ? N1 Sr1 Sr1 118.12(7) . 15_567 ? N1 Sr1 Sr1 118.12(7) 6_564 15_567 ? O2 Sr1 Sr1 44.75(6) 14_557 15_567 ? O2 Sr1 Sr1 44.75(6) 9_667 15_567 ? C12 Sr1 Sr1 128.14(7) 6_564 15_567 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.772 _refine_diff_density_min -0.428 _refine_diff_density_rms 0.088 data_p _database_code_depnum_ccdc_archive 'CCDC 895951' #TrackingRef '3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H38 Cd3 N8 O22' _chemical_formula_sum 'C48 H38 Cd3 N8 O22' _chemical_formula_weight 1416.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-p 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.145(3) _cell_length_b 10.039(3) _cell_length_c 14.935(4) _cell_angle_alpha 70.431(3) _cell_angle_beta 72.443(4) _cell_angle_gamma 73.837(3) _cell_volume 1207.5(6) _cell_formula_units_Z 1 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 850 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 20.03 _exptl_crystal_description strip _exptl_crystal_colour colorless _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.947 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 702 _exptl_absorpt_coefficient_mu 1.407 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6463 _exptl_absorpt_correction_T_max 0.7662 _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 6067 _diffrn_reflns_av_R_equivalents 0.0689 _diffrn_reflns_av_unetI/netI 0.0950 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 24.99 _reflns_number_total 4171 _reflns_number_gt 2876 _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. ; _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^)+(0.0588P)^2^] 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 4171 _refine_ls_number_parameters 370 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0705 _refine_ls_R_factor_gt 0.0487 _refine_ls_wR_factor_ref 0.1197 _refine_ls_wR_factor_gt 0.1109 _refine_ls_goodness_of_fit_ref 0.916 _refine_ls_restrained_S_all 0.916 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.8076(8) 0.6635(7) 0.6556(5) 0.0274(15) Uani 1 1 d . . . C2 C 0.7278(8) 0.6934(6) 0.7512(5) 0.0288(16) Uani 1 1 d . . . C3 C 0.7293(9) 0.6108(7) 0.8448(5) 0.0333(17) Uani 1 1 d . . . C4 C 0.8131(10) 0.4658(7) 0.8904(6) 0.042(2) Uani 1 1 d . . . C5 C 0.5739(8) 0.8197(7) 0.8457(5) 0.0316(17) Uani 1 1 d . . . C6 C 0.4608(8) 0.9360(7) 0.8865(5) 0.0308(16) Uani 1 1 d . . . C7 C 0.3210(8) 0.9079(8) 0.9512(5) 0.0362(17) Uani 1 1 d . . . H7A H 0.2970 0.8169 0.9702 0.043 Uiso 1 1 calc R . . C8 C 0.2180(9) 1.0183(8) 0.9870(6) 0.0441(19) Uani 1 1 d . . . H8 H 0.1225 1.0018 1.0291 0.053 Uiso 1 1 calc R . . C9 C 0.2540(9) 1.1502(9) 0.9618(6) 0.043(2) Uani 1 1 d . . . H9 H 0.1833 1.2228 0.9870 0.052 Uiso 1 1 calc R . . C10 C 0.3938(9) 1.1777(7) 0.8995(5) 0.0330(17) Uani 1 1 d . . . C11 C 0.4981(8) 1.0698(7) 0.8605(5) 0.0297(16) Uani 1 1 d . . . H11 H 0.5924 1.0878 0.8173 0.036 Uiso 1 1 calc R . . C12 C 0.5629(10) 1.3459(8) 0.8117(6) 0.055(2) Uani 1 1 d . . . H12A H 0.6528 1.2860 0.8356 0.082 Uiso 1 1 calc R . . H12B H 0.5655 1.4454 0.7997 0.082 Uiso 1 1 calc R . . H12C H 0.5639 1.3284 0.7521 0.082 Uiso 1 1 calc R . . C13 C 1.2785(8) 0.4717(7) 0.5859(5) 0.0325(17) Uani 1 1 d . . . C14 C 1.2509(7) 0.6226(6) 0.5289(5) 0.0228(14) Uani 1 1 d . A . C15 C 1.3118(7) 0.7377(6) 0.5217(5) 0.0237(15) Uani 1 1 d . . . C16 C 1.4204(8) 0.7495(7) 0.5731(5) 0.0296(16) Uani 1 1 d . A . C17 C 1.1549(7) 0.8097(6) 0.4250(5) 0.0255(15) Uani 1 1 d . . . C18 C 1.0668(7) 0.9039(6) 0.3515(4) 0.0224(14) Uani 1 1 d . A . C19 C 1.0284(8) 0.8474(7) 0.2914(5) 0.0304(16) Uani 1 1 d . . . H19 H 1.0538 0.7484 0.2992 0.036 Uiso 1 1 calc R A . C20 C 0.9528(8) 0.9368(8) 0.2198(5) 0.0372(18) Uani 1 1 d . A . H20 H 0.9275 0.8975 0.1796 0.045 Uiso 1 1 calc R . . C21 C 0.9139(8) 1.0835(7) 0.2065(5) 0.0338(17) Uani 1 1 d . . . H21 H 0.8639 1.1430 0.1572 0.041 Uiso 1 1 calc R A . C22 C 0.9495(8) 1.1413(7) 0.2669(5) 0.0275(15) Uani 1 1 d . A . C23 C 1.0253(7) 1.0504(7) 0.3403(5) 0.0273(15) Uani 1 1 d . . . H23 H 1.0478 1.0890 0.3820 0.033 Uiso 1 1 calc R A . C24 C 0.8456(10) 1.3819(8) 0.1846(6) 0.056(2) Uani 1 1 d . A . H24A H 0.9148 1.3758 0.1227 0.084 Uiso 1 1 calc R . . H24B H 0.8250 1.4787 0.1894 0.084 Uiso 1 1 calc R . . H24C H 0.7491 1.3562 0.1899 0.084 Uiso 1 1 calc R . . N1 N 0.6298(6) 0.8257(5) 0.7525(4) 0.0259(13) Uani 1 1 d . . . N2 N 0.6297(7) 0.6934(6) 0.9027(4) 0.0371(15) Uani 1 1 d . . . H2 H 0.6067 0.6682 0.9655 0.045 Uiso 1 1 calc R . . N3 N 1.1502(6) 0.6694(5) 0.4673(4) 0.0248(12) Uani 1 1 d . A . N4 N 1.2528(6) 0.8558(5) 0.4551(4) 0.0237(12) Uani 1 1 d . . . O1 O 0.8885(6) 0.5357(4) 0.6570(3) 0.0352(12) Uani 1 1 d . A . O2 O 0.7959(5) 0.7602(4) 0.5791(3) 0.0300(11) Uani 1 1 d . . . O3 O 0.9144(7) 0.3937(5) 0.8309(4) 0.0511(15) Uani 1 1 d . . . H3 H 0.9017 0.4323 0.7752 0.077 Uiso 1 1 calc R . . O4 O 0.7892(8) 0.4192(5) 0.9776(4) 0.0660(19) Uani 1 1 d . . . O5 O 0.4241(7) 1.3128(5) 0.8828(4) 0.0480(14) Uani 1 1 d . . . O6 O 1.2092(6) 0.3841(4) 0.5812(3) 0.0363(12) Uani 1 1 d . A . O7 O 1.3790(6) 0.4296(5) 0.6401(4) 0.0452(14) Uani 1 1 d . A 1 H7 H 1.4162 0.4981 0.6350 0.068 Uiso 1 1 calc R A 1 O8 O 1.4785(6) 0.6395(5) 0.6329(4) 0.0403(13) Uani 1 1 d . . . O9 O 1.4476(5) 0.8749(4) 0.5547(3) 0.0341(12) Uani 1 1 d . . . O10 O 0.9167(6) 1.2855(5) 0.2612(4) 0.0442(14) Uani 1 1 d . . . O11 O 0.3834(6) 1.1064(5) 0.6606(4) 0.0545(15) Uani 1 1 d . . . H11A H 0.3119 1.1505 0.6295 0.082 Uiso 1 1 d R . . H11B H 0.3847 1.1577 0.6954 0.082 Uiso 1 1 d R . . Cd1 Cd 1.0000 0.5000 0.5000 0.0274(2) Uani 1 2 d S . . Cd2 Cd 0.61304(6) 0.96547(5) 0.59629(4) 0.02578(17) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.027(4) 0.025(4) 0.037(4) -0.011(3) -0.012(3) -0.007(3) C2 0.036(4) 0.020(3) 0.038(4) -0.010(3) -0.014(3) -0.009(3) C3 0.046(5) 0.024(3) 0.032(4) -0.010(3) -0.012(3) -0.006(3) C4 0.069(6) 0.023(4) 0.044(5) -0.011(4) -0.026(4) -0.006(4) C5 0.038(5) 0.020(3) 0.038(5) -0.005(3) -0.018(4) -0.003(3) C6 0.033(4) 0.028(4) 0.033(4) -0.011(3) -0.013(3) -0.001(3) C7 0.034(5) 0.037(4) 0.037(4) -0.007(3) -0.008(3) -0.012(3) C8 0.028(4) 0.055(5) 0.046(5) -0.018(4) -0.001(4) -0.007(4) C9 0.031(5) 0.054(5) 0.051(5) -0.032(4) -0.011(4) 0.007(4) C10 0.038(5) 0.028(4) 0.039(4) -0.016(3) -0.018(4) 0.004(3) C11 0.029(4) 0.029(4) 0.031(4) -0.012(3) -0.006(3) -0.003(3) C12 0.060(6) 0.031(4) 0.077(6) -0.007(4) -0.030(5) -0.011(4) C13 0.027(4) 0.026(4) 0.049(5) -0.013(3) -0.010(3) -0.007(3) C14 0.019(4) 0.019(3) 0.034(4) -0.008(3) -0.008(3) -0.004(3) C15 0.020(4) 0.019(3) 0.035(4) -0.008(3) -0.011(3) -0.004(3) C16 0.030(4) 0.027(4) 0.041(4) -0.011(3) -0.017(3) -0.009(3) C17 0.021(4) 0.021(3) 0.040(4) -0.014(3) -0.008(3) -0.004(3) C18 0.016(3) 0.020(3) 0.029(4) -0.004(3) -0.007(3) -0.003(3) C19 0.035(4) 0.027(4) 0.034(4) -0.010(3) -0.012(3) -0.009(3) C20 0.038(5) 0.042(4) 0.044(5) -0.016(4) -0.020(4) -0.009(3) C21 0.038(5) 0.032(4) 0.034(4) -0.008(3) -0.017(3) -0.002(3) C22 0.020(4) 0.027(3) 0.031(4) -0.006(3) -0.005(3) -0.002(3) C23 0.021(4) 0.028(4) 0.038(4) -0.017(3) -0.011(3) 0.000(3) C24 0.068(7) 0.028(4) 0.070(6) 0.000(4) -0.037(5) 0.002(4) N1 0.035(3) 0.017(3) 0.028(3) -0.004(2) -0.012(3) -0.005(2) N2 0.056(4) 0.025(3) 0.028(3) -0.006(3) -0.011(3) -0.006(3) N3 0.024(3) 0.018(3) 0.036(3) -0.007(2) -0.009(3) -0.009(2) N4 0.024(3) 0.015(3) 0.034(3) -0.005(2) -0.013(2) -0.001(2) O1 0.042(3) 0.020(2) 0.047(3) -0.014(2) -0.017(2) 0.002(2) O2 0.034(3) 0.025(2) 0.033(3) -0.011(2) -0.010(2) -0.003(2) O3 0.074(4) 0.025(3) 0.058(4) -0.016(3) -0.036(3) 0.012(3) O4 0.118(6) 0.031(3) 0.049(4) -0.003(3) -0.041(4) 0.000(3) O5 0.052(4) 0.023(3) 0.074(4) -0.018(3) -0.021(3) -0.001(2) O6 0.040(3) 0.018(2) 0.060(3) -0.008(2) -0.024(3) -0.010(2) O7 0.045(3) 0.023(2) 0.075(4) -0.002(2) -0.040(3) -0.004(2) O8 0.041(3) 0.028(3) 0.057(3) 0.005(2) -0.033(3) -0.012(2) O9 0.040(3) 0.024(2) 0.050(3) -0.007(2) -0.027(2) -0.010(2) O10 0.054(4) 0.026(3) 0.057(3) -0.013(2) -0.031(3) 0.008(2) O11 0.044(4) 0.037(3) 0.071(4) -0.014(3) -0.014(3) 0.011(3) Cd1 0.0278(4) 0.0241(4) 0.0374(4) -0.0078(3) -0.0112(3) -0.0126(3) Cd2 0.0268(3) 0.0169(2) 0.0378(3) -0.0050(2) -0.0147(2) -0.00587(19) _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 O2 1.238(7) . ? C1 O1 1.287(7) . ? C1 C2 1.482(9) . ? C2 C3 1.367(9) . ? C2 N1 1.383(8) . ? C3 N2 1.360(9) . ? C3 C4 1.484(9) . ? C4 O4 1.200(9) . ? C4 O3 1.316(9) . ? C5 N1 1.317(8) . ? C5 N2 1.332(8) . ? C5 C6 1.492(9) . ? C6 C11 1.377(9) . ? C6 C7 1.386(10) . ? C7 C8 1.383(10) . ? C7 H7A 0.9300 . ? C8 C9 1.355(10) . ? C8 H8 0.9300 . ? C9 C10 1.373(10) . ? C9 H9 0.9300 . ? C10 O5 1.385(8) . ? C10 C11 1.391(9) . ? C11 H11 0.9300 . ? C12 O5 1.426(10) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 O6 1.249(7) . ? C13 O7 1.298(8) . ? C13 C14 1.461(8) . ? C14 C15 1.377(8) . ? C14 N3 1.377(7) . ? C15 N4 1.365(7) . ? C15 C16 1.476(8) . ? C16 O8 1.264(8) . ? C16 O9 1.274(7) . ? C17 N3 1.343(7) . ? C17 N4 1.354(8) . ? C17 C18 1.471(8) . ? C18 C19 1.376(8) . ? C18 C23 1.377(8) . ? C19 C20 1.373(9) . ? C19 H19 0.9300 . ? C20 C21 1.375(9) . ? C20 H20 0.9300 . ? C21 C22 1.375(9) . ? C21 H21 0.9300 . ? C22 O10 1.372(7) . ? C22 C23 1.397(9) . ? C23 H23 0.9300 . ? C24 O10 1.424(8) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? N1 Cd2 2.311(5) . ? N2 H2 0.8600 . ? N3 Cd1 2.314(5) . ? N4 Cd2 2.246(5) 2_776 ? O1 Cd1 2.363(5) . ? O2 Cd2 2.299(4) . ? O3 H3 0.8200 . ? O6 Cd1 2.387(4) . ? O7 H7 0.8200 . ? O9 Cd2 2.283(4) 1_655 ? O9 Cd2 2.408(4) 2_776 ? O11 Cd2 2.318(5) . ? O11 H11A 0.8501 . ? O11 H11B 0.8500 . ? Cd1 N3 2.314(5) 2_766 ? Cd1 O1 2.363(5) 2_766 ? Cd1 O6 2.387(4) 2_766 ? Cd2 N4 2.246(5) 2_776 ? Cd2 O9 2.283(4) 1_455 ? Cd2 O9 2.408(4) 2_776 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 C1 O1 123.0(6) . . ? O2 C1 C2 119.9(6) . . ? O1 C1 C2 117.1(6) . . ? C3 C2 N1 109.6(6) . . ? C3 C2 C1 131.7(6) . . ? N1 C2 C1 118.7(6) . . ? N2 C3 C2 105.3(6) . . ? N2 C3 C4 119.4(6) . . ? C2 C3 C4 135.3(7) . . ? O4 C4 O3 122.7(7) . . ? O4 C4 C3 120.5(7) . . ? O3 C4 C3 116.8(7) . . ? N1 C5 N2 111.6(6) . . ? N1 C5 C6 126.2(6) . . ? N2 C5 C6 122.1(6) . . ? C11 C6 C7 120.7(6) . . ? C11 C6 C5 119.4(6) . . ? C7 C6 C5 119.9(6) . . ? C8 C7 C6 118.5(7) . . ? C8 C7 H7A 120.7 . . ? C6 C7 H7A 120.7 . . ? C9 C8 C7 121.1(7) . . ? C9 C8 H8 119.5 . . ? C7 C8 H8 119.5 . . ? C8 C9 C10 120.6(7) . . ? C8 C9 H9 119.7 . . ? C10 C9 H9 119.7 . . ? C9 C10 O5 116.4(6) . . ? C9 C10 C11 119.6(7) . . ? O5 C10 C11 124.0(7) . . ? C6 C11 C10 119.5(7) . . ? C6 C11 H11 120.3 . . ? C10 C11 H11 120.3 . . ? 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 . . ? O6 C13 O7 120.5(6) . . ? O6 C13 C14 120.8(6) . . ? O7 C13 C14 118.7(6) . . ? C15 C14 N3 108.2(5) . . ? C15 C14 C13 131.6(6) . . ? N3 C14 C13 120.2(5) . . ? N4 C15 C14 109.0(5) . . ? N4 C15 C16 120.0(5) . . ? C14 C15 C16 131.1(6) . . ? O8 C16 O9 123.7(6) . . ? O8 C16 C15 120.1(6) . . ? O9 C16 C15 116.2(5) . . ? N3 C17 N4 113.1(5) . . ? N3 C17 C18 124.1(5) . . ? N4 C17 C18 122.8(5) . . ? C19 C18 C23 119.2(6) . . ? C19 C18 C17 120.4(5) . . ? C23 C18 C17 120.4(6) . . ? C20 C19 C18 120.1(6) . . ? C20 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? C19 C20 C21 121.2(6) . . ? C19 C20 H20 119.4 . . ? C21 C20 H20 119.4 . . ? C20 C21 C22 119.3(6) . . ? C20 C21 H21 120.3 . . ? C22 C21 H21 120.3 . . ? O10 C22 C21 124.9(6) . . ? O10 C22 C23 115.5(6) . . ? C21 C22 C23 119.5(6) . . ? C18 C23 C22 120.6(6) . . ? C18 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? O10 C24 H24A 109.5 . . ? O10 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? O10 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C5 N1 C2 105.0(5) . . ? C5 N1 Cd2 143.7(4) . . ? C2 N1 Cd2 111.1(4) . . ? C5 N2 C3 108.4(6) . . ? C5 N2 H2 125.8 . . ? C3 N2 H2 125.8 . . ? C17 N3 C14 105.0(5) . . ? C17 N3 Cd1 142.4(4) . . ? C14 N3 Cd1 110.6(4) . . ? C17 N4 C15 104.8(5) . . ? C17 N4 Cd2 139.2(4) . 2_776 ? C15 N4 Cd2 113.4(4) . 2_776 ? C1 O1 Cd1 113.6(4) . . ? C1 O2 Cd2 115.7(4) . . ? C4 O3 H3 109.5 . . ? C10 O5 C12 116.4(6) . . ? C13 O6 Cd1 112.5(4) . . ? C13 O7 H7 109.5 . . ? C16 O9 Cd2 134.6(4) . 1_655 ? C16 O9 Cd2 112.9(4) . 2_776 ? Cd2 O9 Cd2 108.39(17) 1_655 2_776 ? C22 O10 C24 117.0(5) . . ? Cd2 O11 H11A 122.7 . . ? Cd2 O11 H11B 120.3 . . ? H11A O11 H11B 107.7 . . ? N3 Cd1 N3 180.000(1) 2_766 . ? N3 Cd1 O1 91.22(17) 2_766 . ? N3 Cd1 O1 88.78(17) . . ? N3 Cd1 O1 88.78(17) 2_766 2_766 ? N3 Cd1 O1 91.22(17) . 2_766 ? O1 Cd1 O1 180.000(1) . 2_766 ? N3 Cd1 O6 72.98(16) 2_766 2_766 ? N3 Cd1 O6 107.02(16) . 2_766 ? O1 Cd1 O6 102.37(16) . 2_766 ? O1 Cd1 O6 77.63(16) 2_766 2_766 ? N3 Cd1 O6 107.02(16) 2_766 . ? N3 Cd1 O6 72.98(16) . . ? O1 Cd1 O6 77.63(16) . . ? O1 Cd1 O6 102.37(16) 2_766 . ? O6 Cd1 O6 180.000(1) 2_766 . ? N4 Cd2 O9 142.97(17) 2_776 1_455 ? N4 Cd2 O2 106.02(17) 2_776 . ? O9 Cd2 O2 87.16(16) 1_455 . ? N4 Cd2 N1 111.86(18) 2_776 . ? O9 Cd2 N1 105.00(17) 1_455 . ? O2 Cd2 N1 73.79(17) . . ? N4 Cd2 O11 93.15(19) 2_776 . ? O9 Cd2 O11 83.51(19) 1_455 . ? O2 Cd2 O11 158.17(18) . . ? N1 Cd2 O11 89.61(19) . . ? N4 Cd2 O9 71.43(16) 2_776 2_776 ? O9 Cd2 O9 71.61(17) 1_455 2_776 ? O2 Cd2 O9 114.12(16) . 2_776 ? N1 Cd2 O9 170.76(18) . 2_776 ? O11 Cd2 O9 81.50(18) . 2_776 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 C1 C2 C3 -175.3(7) . . . . ? O1 C1 C2 C3 4.0(11) . . . . ? O2 C1 C2 N1 5.9(9) . . . . ? O1 C1 C2 N1 -174.9(6) . . . . ? N1 C2 C3 N2 0.9(8) . . . . ? C1 C2 C3 N2 -178.0(7) . . . . ? N1 C2 C3 C4 -177.2(8) . . . . ? C1 C2 C3 C4 3.9(14) . . . . ? N2 C3 C4 O4 2.7(12) . . . . ? C2 C3 C4 O4 -179.4(8) . . . . ? N2 C3 C4 O3 -176.4(7) . . . . ? C2 C3 C4 O3 1.5(13) . . . . ? N1 C5 C6 C11 -57.7(10) . . . . ? N2 C5 C6 C11 122.9(7) . . . . ? N1 C5 C6 C7 123.4(8) . . . . ? N2 C5 C6 C7 -55.9(9) . . . . ? C11 C6 C7 C8 1.8(10) . . . . ? C5 C6 C7 C8 -179.4(6) . . . . ? C6 C7 C8 C9 -1.8(11) . . . . ? C7 C8 C9 C10 0.3(12) . . . . ? C8 C9 C10 O5 -176.2(6) . . . . ? C8 C9 C10 C11 1.1(11) . . . . ? C7 C6 C11 C10 -0.3(10) . . . . ? C5 C6 C11 C10 -179.1(6) . . . . ? C9 C10 C11 C6 -1.2(10) . . . . ? O5 C10 C11 C6 175.9(6) . . . . ? O6 C13 C14 C15 180.0(7) . . . . ? O7 C13 C14 C15 -1.4(11) . . . . ? O6 C13 C14 N3 -1.5(10) . . . . ? O7 C13 C14 N3 177.1(6) . . . . ? N3 C14 C15 N4 -1.0(7) . . . . ? C13 C14 C15 N4 177.6(7) . . . . ? N3 C14 C15 C16 177.8(7) . . . . ? C13 C14 C15 C16 -3.5(12) . . . . ? N4 C15 C16 O8 -178.1(6) . . . . ? C14 C15 C16 O8 3.1(12) . . . . ? N4 C15 C16 O9 3.1(10) . . . . ? C14 C15 C16 O9 -175.7(7) . . . . ? N3 C17 C18 C19 -28.0(10) . . . . ? N4 C17 C18 C19 150.2(6) . . . . ? N3 C17 C18 C23 153.7(6) . . . . ? N4 C17 C18 C23 -28.2(10) . . . . ? C23 C18 C19 C20 1.5(10) . . . . ? C17 C18 C19 C20 -176.9(7) . . . . ? C18 C19 C20 C21 0.0(11) . . . . ? C19 C20 C21 C22 -0.9(12) . . . . ? C20 C21 C22 O10 -179.9(7) . . . . ? C20 C21 C22 C23 0.3(11) . . . . ? C19 C18 C23 C22 -2.0(10) . . . . ? C17 C18 C23 C22 176.3(6) . . . . ? O10 C22 C23 C18 -178.7(6) . . . . ? C21 C22 C23 C18 1.1(10) . . . . ? N2 C5 N1 C2 0.0(8) . . . . ? C6 C5 N1 C2 -179.4(6) . . . . ? N2 C5 N1 Cd2 174.6(5) . . . . ? C6 C5 N1 Cd2 -4.8(12) . . . . ? C3 C2 N1 C5 -0.5(7) . . . . ? C1 C2 N1 C5 178.5(6) . . . . ? C3 C2 N1 Cd2 -177.1(5) . . . . ? C1 C2 N1 Cd2 1.9(7) . . . . ? N1 C5 N2 C3 0.6(8) . . . . ? C6 C5 N2 C3 -180.0(6) . . . . ? C2 C3 N2 C5 -0.9(8) . . . . ? C4 C3 N2 C5 177.5(6) . . . . ? N4 C17 N3 C14 0.4(7) . . . . ? C18 C17 N3 C14 178.7(6) . . . . ? N4 C17 N3 Cd1 160.8(5) . . . . ? C18 C17 N3 Cd1 -20.9(11) . . . . ? C15 C14 N3 C17 0.4(7) . . . . ? C13 C14 N3 C17 -178.4(6) . . . . ? C15 C14 N3 Cd1 -167.0(4) . . . . ? C13 C14 N3 Cd1 14.2(7) . . . . ? N3 C17 N4 C15 -1.0(7) . . . . ? C18 C17 N4 C15 -179.4(6) . . . . ? N3 C17 N4 Cd2 158.1(5) . . . 2_776 ? C18 C17 N4 Cd2 -20.2(10) . . . 2_776 ? C14 C15 N4 C17 1.2(7) . . . . ? C16 C15 N4 C17 -177.8(6) . . . . ? C14 C15 N4 Cd2 -164.1(4) . . . 2_776 ? C16 C15 N4 Cd2 16.9(7) . . . 2_776 ? O2 C1 O1 Cd1 -3.3(8) . . . . ? C2 C1 O1 Cd1 177.5(4) . . . . ? O1 C1 O2 Cd2 170.3(5) . . . . ? C2 C1 O2 Cd2 -10.5(7) . . . . ? C9 C10 O5 C12 -174.8(6) . . . . ? C11 C10 O5 C12 8.0(10) . . . . ? O7 C13 O6 Cd1 169.5(5) . . . . ? C14 C13 O6 Cd1 -11.9(8) . . . . ? O8 C16 O9 Cd2 7.4(11) . . . 1_655 ? C15 C16 O9 Cd2 -173.9(4) . . . 1_655 ? O8 C16 O9 Cd2 161.3(6) . . . 2_776 ? C15 C16 O9 Cd2 -20.0(7) . . . 2_776 ? C21 C22 O10 C24 -2.4(11) . . . . ? C23 C22 O10 C24 177.4(6) . . . . ? C17 N3 Cd1 N3 60(100) . . . 2_766 ? C14 N3 Cd1 N3 -141(100) . . . 2_766 ? C17 N3 Cd1 O1 -96.3(7) . . . . ? C14 N3 Cd1 O1 63.5(4) . . . . ? C17 N3 Cd1 O1 83.7(7) . . . 2_766 ? C14 N3 Cd1 O1 -116.5(4) . . . 2_766 ? C17 N3 Cd1 O6 6.3(7) . . . 2_766 ? C14 N3 Cd1 O6 166.0(4) . . . 2_766 ? C17 N3 Cd1 O6 -173.7(7) . . . . ? C14 N3 Cd1 O6 -14.0(4) . . . . ? C1 O1 Cd1 N3 -115.3(4) . . . 2_766 ? C1 O1 Cd1 N3 64.7(4) . . . . ? C1 O1 Cd1 O1 15(100) . . . 2_766 ? C1 O1 Cd1 O6 -42.5(4) . . . 2_766 ? C1 O1 Cd1 O6 137.5(4) . . . . ? C13 O6 Cd1 N3 -165.9(5) . . . 2_766 ? C13 O6 Cd1 N3 14.1(5) . . . . ? C13 O6 Cd1 O1 -78.5(5) . . . . ? C13 O6 Cd1 O1 101.5(5) . . . 2_766 ? C13 O6 Cd1 O6 19(100) . . . 2_766 ? C1 O2 Cd2 N4 117.1(4) . . . 2_776 ? C1 O2 Cd2 O9 -98.1(4) . . . 1_455 ? C1 O2 Cd2 N1 8.5(4) . . . . ? C1 O2 Cd2 O11 -33.4(7) . . . . ? C1 O2 Cd2 O9 -166.4(4) . . . 2_776 ? C5 N1 Cd2 N4 79.5(8) . . . 2_776 ? C2 N1 Cd2 N4 -106.1(4) . . . 2_776 ? C5 N1 Cd2 O9 -96.9(7) . . . 1_455 ? C2 N1 Cd2 O9 77.5(4) . . . 1_455 ? C5 N1 Cd2 O2 -179.4(8) . . . . ? C2 N1 Cd2 O2 -4.9(4) . . . . ? C5 N1 Cd2 O11 -13.7(8) . . . . ? C2 N1 Cd2 O11 160.7(4) . . . . ? C5 N1 Cd2 O9 -29.7(15) . . . 2_776 ? C2 N1 Cd2 O9 144.7(9) . . . 2_776 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3 O1 0.82 1.74 2.556(7) 170.8 . O7 H7 O8 0.82 1.66 2.476(6) 174.9 . N2 H2 O5 0.86 2.26 3.073(8) 156.8 2_677 O11 H11A O6 0.85 2.23 2.859(6) 131.3 1_465 O11 H11B O7 0.85 2.56 3.146(7) 126.6 1_465 _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 2.559 _refine_diff_density_min -1.256 _refine_diff_density_rms 0.157 data_a3 _database_code_depnum_ccdc_archive 'CCDC 895952' #TrackingRef '4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H16 Cu N4 O5' _chemical_formula_sum 'C24 H16 Cu N4 O5' _chemical_formula_weight 503.95 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c n ' _symmetry_space_group_name_Hall '-P 2n 2ab ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 16.9360(4) _cell_length_b 12.3483(8) _cell_length_c 20.2453(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4233.9(3) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 6171 _cell_measurement_theta_min 3.087 _cell_measurement_theta_max 28.446 _exptl_crystal_description block _exptl_crystal_colour Blue _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.581 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2056 _exptl_absorpt_coefficient_mu 1.078 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7380 _exptl_absorpt_correction_T_max 0.8998 _exptl_absorpt_process_details '(SADABS; Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20355 _diffrn_reflns_av_R_equivalents 0.0686 _diffrn_reflns_av_unetI/netI 0.0574 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 24.99 _reflns_number_total 3730 _reflns_number_gt 3091 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0566P)^2^+1.7731P] 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 3730 _refine_ls_number_parameters 309 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0461 _refine_ls_R_factor_gt 0.0376 _refine_ls_wR_factor_ref 0.1056 _refine_ls_wR_factor_gt 0.0987 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _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 Cu1 Cu 0.250115(15) 1.03593(2) 0.285260(13) 0.01486(13) Uani 1 1 d . . . N3 N 0.24541(10) 0.87474(17) 0.27200(9) 0.0144(4) Uani 1 1 d . . . N2 N 0.17773(11) 1.04300(15) 0.36387(9) 0.0164(4) Uani 1 1 d . . . O3 O 0.32646(11) 1.02865(13) 0.21023(8) 0.0224(4) Uani 1 1 d . . . N1 N 0.33381(11) 0.99884(17) 0.37100(9) 0.0168(4) Uani 1 1 d . . . O4 O -0.04211(10) 0.77658(17) 0.40178(9) 0.0352(5) Uani 1 1 d . . . C19 C 0.22198(14) 0.78133(18) 0.29916(11) 0.0145(5) Uani 1 1 d . . . C18 C 0.08699(14) 0.78152(19) 0.34885(12) 0.0201(5) Uani 1 1 d . . . H18 H 0.0655 0.7952 0.3074 0.024 Uiso 1 1 calc R . . O2 O 0.39126(10) 0.91107(14) 0.14734(8) 0.0271(4) Uani 1 1 d . . . C13 C 0.16832(14) 0.77219(18) 0.35659(11) 0.0168(5) Uani 1 1 d . . . C12 C 0.10296(14) 1.0731(2) 0.36051(12) 0.0218(5) Uani 1 1 d . . . H12 H 0.0814 1.0881 0.3193 0.026 Uiso 1 1 calc R . . C17 C 0.03851(14) 0.7702(2) 0.40331(12) 0.0235(6) Uani 1 1 d . . . C14 C 0.20017(15) 0.75272(19) 0.41798(11) 0.0185(5) Uani 1 1 d . . . H14 H 0.2545 0.7463 0.4231 0.022 Uiso 1 1 calc R . . C4 C 0.32298(14) 0.95731(19) 0.48732(12) 0.0190(5) Uani 1 1 d . . . C15 C 0.15072(15) 0.7427(2) 0.47227(11) 0.0225(5) Uani 1 1 d . . . H15 H 0.1721 0.7302 0.5139 0.027 Uiso 1 1 calc R . . C6 C 0.27461(16) 0.9577(2) 0.54510(12) 0.0221(6) Uani 1 1 d . . . H6 H 0.2953 0.9334 0.5850 0.027 Uiso 1 1 calc R . . C8 C 0.16449(14) 1.02495(19) 0.48169(12) 0.0190(5) Uani 1 1 d . . . C16 C 0.07104(15) 0.7510(2) 0.46487(11) 0.0236(6) Uani 1 1 d . . . H16 H 0.0383 0.7437 0.5015 0.028 Uiso 1 1 calc R . . C9 C 0.20906(13) 1.01985(18) 0.42351(11) 0.0154(5) Uani 1 1 d . . . C21 C 0.34187(14) 0.9339(2) 0.19155(11) 0.0190(5) Uani 1 1 d . . . C1 C 0.40894(14) 0.9719(2) 0.37380(12) 0.0247(6) Uani 1 1 d . . . H1 H 0.4392 0.9784 0.3357 0.030 Uiso 1 1 calc R . . C20 C 0.29933(13) 0.84613(19) 0.22517(10) 0.0160(5) Uani 1 1 d . . . C11 C 0.05532(15) 1.0834(2) 0.41597(12) 0.0275(6) Uani 1 1 d . . . H11 H 0.0031 1.1058 0.4119 0.033 Uiso 1 1 calc R . . C7 C 0.19949(15) 0.9928(2) 0.54268(11) 0.0231(6) Uani 1 1 d . . . H7 H 0.1700 0.9962 0.5813 0.028 Uiso 1 1 calc R . . C10 C 0.08641(15) 1.0602(2) 0.47649(13) 0.0261(6) Uani 1 1 d . . . H10 H 0.0556 1.0678 0.5142 0.031 Uiso 1 1 calc R . . C3 C 0.40225(14) 0.9271(2) 0.48780(12) 0.0264(6) Uani 1 1 d . . . H3 H 0.4256 0.9024 0.5266 0.032 Uiso 1 1 calc R . . C5 C 0.29099(13) 0.99071(19) 0.42676(11) 0.0153(5) Uani 1 1 d . . . C2 C 0.44546(15) 0.9339(2) 0.43112(12) 0.0284(6) Uani 1 1 d . . . H2 H 0.4983 0.9137 0.4307 0.034 Uiso 1 1 calc R . . C22 C -0.07980(17) 0.7876(3) 0.33899(15) 0.0426(8) Uani 1 1 d . . . H22A H -0.0637 0.8545 0.3189 0.064 Uiso 1 1 calc R . . H22B H -0.1361 0.7877 0.3449 0.064 Uiso 1 1 calc R . . H22C H -0.0649 0.7282 0.3111 0.064 Uiso 1 1 calc R . . N4 N 0.25763(11) 0.69502(17) 0.27221(10) 0.0149(4) Uani 1 1 d . . . O5 O 0.40338(11) 0.70988(14) 0.14200(9) 0.0292(5) Uani 1 1 d . . . H5 H 0.4006 0.7759 0.1455 0.044 Uiso 1 1 calc R . . C23 C 0.30695(14) 0.73589(19) 0.22513(10) 0.0162(5) Uani 1 1 d . . . C24 C 0.35954(14) 0.6644(2) 0.18757(11) 0.0196(5) Uani 1 1 d . . . O6 O 0.36168(11) 0.56727(15) 0.19814(8) 0.0256(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0214(2) 0.0098(2) 0.0134(2) 0.00056(10) 0.00324(10) 0.00072(10) N3 0.0206(11) 0.0099(11) 0.0125(9) -0.0002(8) 0.0034(7) -0.0013(7) N2 0.0183(10) 0.0145(11) 0.0163(10) -0.0009(8) -0.0013(8) 0.0025(8) O3 0.0305(10) 0.0159(10) 0.0208(9) 0.0015(7) 0.0086(7) -0.0015(7) N1 0.0179(10) 0.0155(11) 0.0171(10) 0.0010(9) 0.0019(8) 0.0017(8) O4 0.0209(10) 0.0615(15) 0.0231(9) -0.0003(9) 0.0063(7) -0.0014(8) C19 0.0173(11) 0.0124(12) 0.0138(10) 0.0004(9) -0.0014(9) 0.0003(9) C18 0.0241(13) 0.0203(14) 0.0159(11) 0.0003(10) 0.0025(10) -0.0007(10) O2 0.0343(10) 0.0220(10) 0.0249(9) 0.0024(8) 0.0173(8) 0.0014(8) C13 0.0244(13) 0.0099(12) 0.0160(11) -0.0014(9) 0.0042(9) -0.0017(9) C12 0.0218(13) 0.0219(14) 0.0216(12) 0.0022(11) -0.0016(10) 0.0052(10) C17 0.0234(14) 0.0252(14) 0.0218(12) -0.0027(11) 0.0067(10) -0.0014(10) C14 0.0244(13) 0.0124(12) 0.0188(12) -0.0012(10) 0.0026(9) 0.0010(9) C4 0.0229(13) 0.0148(13) 0.0192(12) 0.0007(10) -0.0020(10) -0.0007(9) C15 0.0359(15) 0.0176(13) 0.0140(11) 0.0016(10) 0.0023(10) 0.0000(10) C6 0.0283(14) 0.0239(15) 0.0140(12) 0.0003(10) -0.0035(10) -0.0020(10) C8 0.0234(13) 0.0146(13) 0.0190(12) -0.0022(10) 0.0036(10) -0.0001(9) C16 0.0303(15) 0.0235(15) 0.0171(12) 0.0004(11) 0.0100(10) -0.0036(10) C9 0.0189(12) 0.0105(12) 0.0167(12) 0.0003(9) 0.0010(9) -0.0002(9) C21 0.0233(13) 0.0165(13) 0.0171(11) 0.0015(10) 0.0026(10) 0.0007(10) C1 0.0199(13) 0.0290(15) 0.0253(13) -0.0012(11) 0.0048(10) 0.0018(10) C20 0.0180(12) 0.0170(13) 0.0129(10) -0.0003(9) 0.0019(9) 0.0022(9) C11 0.0191(13) 0.0329(17) 0.0304(13) 0.0025(12) 0.0046(10) 0.0087(11) C7 0.0302(15) 0.0254(14) 0.0138(12) -0.0022(11) 0.0041(10) -0.0016(11) C10 0.0256(14) 0.0279(14) 0.0248(13) 0.0008(12) 0.0093(10) 0.0041(11) C3 0.0239(14) 0.0296(15) 0.0257(13) 0.0025(12) -0.0064(10) 0.0033(11) C5 0.0165(12) 0.0112(12) 0.0183(12) -0.0003(9) -0.0005(9) -0.0003(9) C2 0.0167(12) 0.0368(16) 0.0318(14) 0.0026(13) -0.0005(10) 0.0081(11) C22 0.0236(15) 0.070(3) 0.0347(16) -0.0027(15) -0.0021(12) 0.0026(14) N4 0.0210(11) 0.0109(11) 0.0128(9) 0.0000(8) 0.0021(7) 0.0003(7) O5 0.0369(11) 0.0203(10) 0.0304(10) 0.0012(8) 0.0188(8) 0.0065(8) C23 0.0207(12) 0.0152(12) 0.0126(10) 0.0009(9) 0.0011(9) 0.0000(10) C24 0.0254(13) 0.0198(15) 0.0136(11) -0.0003(10) 0.0020(9) 0.0043(10) O6 0.0393(11) 0.0154(10) 0.0220(9) -0.0010(8) 0.0055(8) 0.0069(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N4 1.986(2) 8_665 ? Cu1 O3 1.9967(16) . ? Cu1 N3 2.010(2) . ? Cu1 N2 2.0108(19) . ? Cu1 N1 2.2874(19) . ? N3 C19 1.338(3) . ? N3 C20 1.363(3) . ? N2 C12 1.322(3) . ? N2 C9 1.350(3) . ? O3 C21 1.257(3) . ? N1 C1 1.317(3) . ? N1 C5 1.345(3) . ? O4 C17 1.368(3) . ? O4 C22 1.429(3) . ? C19 N4 1.341(3) . ? C19 C13 1.480(3) . ? C18 C17 1.382(3) . ? C18 C13 1.391(3) . ? C18 H18 0.9300 . ? O2 C21 1.257(3) . ? C13 C14 1.376(3) . ? C12 C11 1.388(3) . ? C12 H12 0.9300 . ? C17 C16 1.383(3) . ? C14 C15 1.387(3) . ? C14 H14 0.9300 . ? C4 C3 1.393(3) . ? C4 C5 1.402(3) . ? C4 C6 1.428(3) . ? C15 C16 1.362(4) . ? C15 H15 0.9300 . ? C6 C7 1.345(4) . ? C6 H6 0.9300 . ? C8 C10 1.396(4) . ? C8 C9 1.400(3) . ? C8 C7 1.426(3) . ? C16 H16 0.9300 . ? C9 C5 1.435(3) . ? C21 C20 1.469(3) . ? C1 C2 1.396(4) . ? C1 H1 0.9300 . ? C20 C23 1.367(4) . ? C11 C10 1.364(4) . ? C11 H11 0.9300 . ? C7 H7 0.9300 . ? C10 H10 0.9300 . ? C3 C2 1.363(4) . ? C3 H3 0.9300 . ? C2 H2 0.9300 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? N4 C23 1.364(3) . ? N4 Cu1 1.986(2) 8_655 ? O5 C24 1.311(3) . ? O5 H5 0.8200 . ? C23 C24 1.467(3) . ? C24 O6 1.219(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Cu1 O3 89.21(7) 8_665 . ? N4 Cu1 N3 163.51(9) 8_665 . ? O3 Cu1 N3 83.08(7) . . ? N4 Cu1 N2 91.26(8) 8_665 . ? O3 Cu1 N2 177.20(7) . . ? N3 Cu1 N2 97.15(7) . . ? N4 Cu1 N1 109.87(8) 8_665 . ? O3 Cu1 N1 99.61(7) . . ? N3 Cu1 N1 85.85(8) . . ? N2 Cu1 N1 77.64(7) . . ? C19 N3 C20 105.1(2) . . ? C19 N3 Cu1 144.14(16) . . ? C20 N3 Cu1 108.85(15) . . ? C12 N2 C9 118.8(2) . . ? C12 N2 Cu1 123.75(16) . . ? C9 N2 Cu1 117.34(15) . . ? C21 O3 Cu1 113.91(15) . . ? C1 N1 C5 117.8(2) . . ? C1 N1 Cu1 133.02(16) . . ? C5 N1 Cu1 108.52(14) . . ? C17 O4 C22 118.1(2) . . ? N3 C19 N4 112.6(2) . . ? N3 C19 C13 124.8(2) . . ? N4 C19 C13 122.4(2) . . ? C17 C18 C13 119.3(2) . . ? C17 C18 H18 120.3 . . ? C13 C18 H18 120.3 . . ? C14 C13 C18 120.3(2) . . ? C14 C13 C19 118.8(2) . . ? C18 C13 C19 120.9(2) . . ? N2 C12 C11 122.7(2) . . ? N2 C12 H12 118.6 . . ? C11 C12 H12 118.6 . . ? O4 C17 C18 124.7(2) . . ? O4 C17 C16 115.3(2) . . ? C18 C17 C16 120.0(2) . . ? C13 C14 C15 119.6(2) . . ? C13 C14 H14 120.2 . . ? C15 C14 H14 120.2 . . ? C3 C4 C5 117.2(2) . . ? C3 C4 C6 123.2(2) . . ? C5 C4 C6 119.6(2) . . ? C16 C15 C14 120.3(2) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C7 C6 C4 120.9(2) . . ? C7 C6 H6 119.5 . . ? C4 C6 H6 119.5 . . ? C10 C8 C9 117.5(2) . . ? C10 C8 C7 123.1(2) . . ? C9 C8 C7 119.5(2) . . ? C15 C16 C17 120.5(2) . . ? C15 C16 H16 119.8 . . ? C17 C16 H16 119.8 . . ? N2 C9 C8 122.1(2) . . ? N2 C9 C5 118.3(2) . . ? C8 C9 C5 119.6(2) . . ? O3 C21 O2 124.1(2) . . ? O3 C21 C20 116.5(2) . . ? O2 C21 C20 119.4(2) . . ? N1 C1 C2 123.3(2) . . ? N1 C1 H1 118.4 . . ? C2 C1 H1 118.4 . . ? N3 C20 C23 108.8(2) . . ? N3 C20 C21 117.4(2) . . ? C23 C20 C21 133.5(2) . . ? C10 C11 C12 118.9(2) . . ? C10 C11 H11 120.6 . . ? C12 C11 H11 120.6 . . ? C6 C7 C8 121.0(2) . . ? C6 C7 H7 119.5 . . ? C8 C7 H7 119.5 . . ? C11 C10 C8 119.9(2) . . ? C11 C10 H10 120.0 . . ? C8 C10 H10 120.0 . . ? C2 C3 C4 119.6(2) . . ? C2 C3 H3 120.2 . . ? C4 C3 H3 120.2 . . ? N1 C5 C4 123.2(2) . . ? N1 C5 C9 117.65(19) . . ? C4 C5 C9 119.2(2) . . ? C3 C2 C1 118.9(2) . . ? C3 C2 H2 120.6 . . ? C1 C2 H2 120.6 . . ? O4 C22 H22A 109.5 . . ? O4 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? O4 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C19 N4 C23 105.4(2) . . ? C19 N4 Cu1 134.61(16) . 8_655 ? C23 N4 Cu1 119.94(17) . 8_655 ? C24 O5 H5 109.5 . . ? N4 C23 C20 108.1(2) . . ? N4 C23 C24 120.8(2) . . ? C20 C23 C24 131.1(2) . . ? O6 C24 O5 121.9(2) . . ? O6 C24 C23 121.3(2) . . ? O5 C24 C23 116.8(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 Cu1 N3 C19 -131.6(3) 8_665 . . . ? O3 Cu1 N3 C19 165.7(3) . . . . ? N2 Cu1 N3 C19 -11.5(3) . . . . ? N1 Cu1 N3 C19 65.5(3) . . . . ? N4 Cu1 N3 C20 67.8(3) 8_665 . . . ? O3 Cu1 N3 C20 5.12(15) . . . . ? N2 Cu1 N3 C20 -172.08(15) . . . . ? N1 Cu1 N3 C20 -95.11(15) . . . . ? N4 Cu1 N2 C12 64.3(2) 8_665 . . . ? O3 Cu1 N2 C12 163.9(14) . . . . ? N3 Cu1 N2 C12 -101.5(2) . . . . ? N1 Cu1 N2 C12 174.3(2) . . . . ? N4 Cu1 N2 C9 -112.81(17) 8_665 . . . ? O3 Cu1 N2 C9 -13.1(16) . . . . ? N3 Cu1 N2 C9 81.40(17) . . . . ? N1 Cu1 N2 C9 -2.74(16) . . . . ? N4 Cu1 O3 C21 -169.84(17) 8_665 . . . ? N3 Cu1 O3 C21 -4.45(17) . . . . ? N2 Cu1 O3 C21 90.4(15) . . . . ? N1 Cu1 O3 C21 80.13(17) . . . . ? N4 Cu1 N1 C1 -97.3(2) 8_665 . . . ? O3 Cu1 N1 C1 -4.7(2) . . . . ? N3 Cu1 N1 C1 77.6(2) . . . . ? N2 Cu1 N1 C1 175.8(2) . . . . ? N4 Cu1 N1 C5 92.68(16) 8_665 . . . ? O3 Cu1 N1 C5 -174.66(16) . . . . ? N3 Cu1 N1 C5 -92.42(16) . . . . ? N2 Cu1 N1 C5 5.85(15) . . . . ? C20 N3 C19 N4 -0.2(3) . . . . ? Cu1 N3 C19 N4 -161.23(19) . . . . ? C20 N3 C19 C13 174.5(2) . . . . ? Cu1 N3 C19 C13 13.5(4) . . . . ? C17 C18 C13 C14 -0.5(4) . . . . ? C17 C18 C13 C19 178.6(2) . . . . ? N3 C19 C13 C14 -100.5(3) . . . . ? N4 C19 C13 C14 73.8(3) . . . . ? N3 C19 C13 C18 80.4(3) . . . . ? N4 C19 C13 C18 -105.3(3) . . . . ? C9 N2 C12 C11 0.9(4) . . . . ? Cu1 N2 C12 C11 -176.2(2) . . . . ? C22 O4 C17 C18 4.9(4) . . . . ? C22 O4 C17 C16 -175.1(3) . . . . ? C13 C18 C17 O4 -179.3(2) . . . . ? C13 C18 C17 C16 0.7(4) . . . . ? C18 C13 C14 C15 -0.2(4) . . . . ? C19 C13 C14 C15 -179.3(2) . . . . ? C13 C14 C15 C16 0.6(4) . . . . ? C3 C4 C6 C7 176.6(2) . . . . ? C5 C4 C6 C7 -2.1(4) . . . . ? C14 C15 C16 C17 -0.4(4) . . . . ? O4 C17 C16 C15 179.7(2) . . . . ? C18 C17 C16 C15 -0.2(4) . . . . ? C12 N2 C9 C8 1.1(3) . . . . ? Cu1 N2 C9 C8 178.37(17) . . . . ? C12 N2 C9 C5 -178.0(2) . . . . ? Cu1 N2 C9 C5 -0.7(3) . . . . ? C10 C8 C9 N2 -3.0(4) . . . . ? C7 C8 C9 N2 176.0(2) . . . . ? C10 C8 C9 C5 176.1(2) . . . . ? C7 C8 C9 C5 -4.9(3) . . . . ? Cu1 O3 C21 O2 -176.37(19) . . . . ? Cu1 O3 C21 C20 2.7(3) . . . . ? C5 N1 C1 C2 1.1(4) . . . . ? Cu1 N1 C1 C2 -168.2(2) . . . . ? C19 N3 C20 C23 0.2(2) . . . . ? Cu1 N3 C20 C23 168.55(15) . . . . ? C19 N3 C20 C21 -173.7(2) . . . . ? Cu1 N3 C20 C21 -5.3(2) . . . . ? O3 C21 C20 N3 1.9(3) . . . . ? O2 C21 C20 N3 -178.9(2) . . . . ? O3 C21 C20 C23 -170.0(2) . . . . ? O2 C21 C20 C23 9.1(4) . . . . ? N2 C12 C11 C10 -0.9(4) . . . . ? C4 C6 C7 C8 3.6(4) . . . . ? C10 C8 C7 C6 178.9(2) . . . . ? C9 C8 C7 C6 0.0(4) . . . . ? C12 C11 C10 C8 -1.1(4) . . . . ? C9 C8 C10 C11 2.9(4) . . . . ? C7 C8 C10 C11 -176.0(3) . . . . ? C5 C4 C3 C2 1.9(4) . . . . ? C6 C4 C3 C2 -176.8(3) . . . . ? C1 N1 C5 C4 1.4(4) . . . . ? Cu1 N1 C5 C4 173.10(18) . . . . ? C1 N1 C5 C9 -179.8(2) . . . . ? Cu1 N1 C5 C9 -8.1(2) . . . . ? C3 C4 C5 N1 -2.8(4) . . . . ? C6 C4 C5 N1 175.9(2) . . . . ? C3 C4 C5 C9 178.4(2) . . . . ? C6 C4 C5 C9 -2.9(3) . . . . ? N2 C9 C5 N1 6.6(3) . . . . ? C8 C9 C5 N1 -172.5(2) . . . . ? N2 C9 C5 C4 -174.5(2) . . . . ? C8 C9 C5 C4 6.4(3) . . . . ? C4 C3 C2 C1 0.3(4) . . . . ? N1 C1 C2 C3 -1.9(4) . . . . ? N3 C19 N4 C23 0.2(3) . . . . ? C13 C19 N4 C23 -174.7(2) . . . . ? N3 C19 N4 Cu1 -177.78(15) . . . 8_655 ? C13 C19 N4 Cu1 7.3(4) . . . 8_655 ? C19 N4 C23 C20 -0.1(2) . . . . ? Cu1 N4 C23 C20 178.26(15) 8_655 . . . ? C19 N4 C23 C24 176.5(2) . . . . ? Cu1 N4 C23 C24 -5.2(3) 8_655 . . . ? N3 C20 C23 N4 -0.1(2) . . . . ? C21 C20 C23 N4 172.4(2) . . . . ? N3 C20 C23 C24 -176.2(2) . . . . ? C21 C20 C23 C24 -3.7(4) . . . . ? N4 C23 C24 O6 -1.4(4) . . . . ? C20 C23 C24 O6 174.3(2) . . . . ? N4 C23 C24 O5 178.1(2) . . . . ? C20 C23 C24 O5 -6.2(4) . . . . ? 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 O5 H5 O2 0.82 1.68 2.495(2) 175.8 . _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.486 _refine_diff_density_min -0.460 _refine_diff_density_rms 0.104 data_a4 _database_code_depnum_ccdc_archive 'CCDC 895953' #TrackingRef '5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H32 Cd2 N8 O10' _chemical_formula_sum 'C48 H32 Cd2 N8 O10' _chemical_formula_weight 1105.62 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 Orthorhombic _symmetry_space_group_name_H-M 'P b c a ' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 19.014(2) _cell_length_b 21.245(2) _cell_length_c 25.136(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 10153.5(19) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 6071 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 20.24 _exptl_crystal_description strip-shaped _exptl_crystal_colour colorless _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 1.447 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4416 _exptl_absorpt_coefficient_mu 0.899 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7149 _exptl_absorpt_correction_T_max 0.8406 _exptl_absorpt_process_details '(SADABS; Bruker, 2008)' _exptl_special_details ; ? ; 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 _platon_squeeze_void_content 1 -0.019 0.000 0.000 543 132 ' ' 2 -0.020 0.000 0.500 543 132 ' ' 3 -0.019 0.500 0.000 543 132 ' ' 4 -0.015 0.500 0.500 543 132 ' ' _platon_squeeze_details ; Spek, A. L. (2009). Acta Cryst. D65, 148 C155. ; _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 48939 _diffrn_reflns_av_R_equivalents 0.0700 _diffrn_reflns_av_unetI/netI 0.0588 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8922 _reflns_number_gt 5178 _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. ; _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^)+(0.1206P)^2^] 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 8922 _refine_ls_number_parameters 591 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1107 _refine_ls_R_factor_gt 0.0676 _refine_ls_wR_factor_ref 0.2096 _refine_ls_wR_factor_gt 0.1894 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _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 C1 C 0.4536(5) 0.6137(4) 0.3470(4) 0.069(2) Uani 1 1 d . . . C2 C 0.4860(3) 0.6761(4) 0.3368(3) 0.0521(19) Uani 1 1 d . . . C3 C 0.5151(4) 0.7218(3) 0.3705(3) 0.0480(17) Uani 1 1 d . . . C4 C 0.5272(4) 0.7216(4) 0.4279(3) 0.058(2) Uani 1 1 d . . . C5 C 0.5198(4) 0.7561(4) 0.2896(3) 0.0500(18) Uani 1 1 d . . . C6 C 0.5348(4) 0.7958(4) 0.2450(3) 0.057(2) Uani 1 1 d . . . C7 C 0.5592(4) 0.7705(4) 0.1964(3) 0.062(2) Uani 1 1 d . . . H7 H 0.5647 0.7271 0.1935 0.074 Uiso 1 1 calc R . . C8 C 0.5749(5) 0.8075(5) 0.1534(4) 0.078(3) Uani 1 1 d . . . C9 C 0.5662(6) 0.8714(5) 0.1576(4) 0.092(3) Uani 1 1 d . . . H9 H 0.5773 0.8970 0.1288 0.111 Uiso 1 1 calc R . . C10 C 0.5419(6) 0.8977(5) 0.2029(5) 0.095(3) Uani 1 1 d . . . H10 H 0.5359 0.9411 0.2046 0.114 Uiso 1 1 calc R . . C11 C 0.5257(5) 0.8609(4) 0.2474(4) 0.073(2) Uani 1 1 d . . . H11 H 0.5088 0.8796 0.2783 0.088 Uiso 1 1 calc R . . C12 C 0.6113(8) 0.8110(7) 0.0644(4) 0.150(6) Uani 1 1 d . . . H12A H 0.6543 0.8340 0.0687 0.225 Uiso 1 1 calc R . . H12B H 0.5735 0.8399 0.0577 0.225 Uiso 1 1 calc R . . H12C H 0.6157 0.7826 0.0348 0.225 Uiso 1 1 calc R . . C13 C 0.7578(5) 0.8367(4) 0.3834(4) 0.070(3) Uani 1 1 d . . . C14 C 0.7430(5) 0.8472(4) 0.4381(5) 0.078(3) Uani 1 1 d . . . C15 C 0.6650(7) 0.8669(6) 0.5062(5) 0.114(4) Uani 1 1 d . . . H15 H 0.6185 0.8717 0.5170 0.136 Uiso 1 1 calc R . . C16 C 0.7161(9) 0.8710(7) 0.5441(5) 0.132(5) Uani 1 1 d . . . H16 H 0.7057 0.8805 0.5794 0.158 Uiso 1 1 calc R . . C17 C 0.7843(9) 0.8603(7) 0.5273(7) 0.133(5) Uani 1 1 d . . . H17 H 0.8203 0.8615 0.5523 0.160 Uiso 1 1 calc R . . C18 C 0.8007(6) 0.8480(5) 0.4755(6) 0.106(4) Uani 1 1 d . . . C19 C 0.8710(7) 0.8401(6) 0.4538(7) 0.122(5) Uani 1 1 d . . . H19 H 0.9097 0.8428 0.4764 0.146 Uiso 1 1 calc R . . C20 C 0.8810(6) 0.8293(6) 0.4029(7) 0.109(4) Uani 1 1 d . . . H20 H 0.9269 0.8232 0.3911 0.131 Uiso 1 1 calc R . . C21 C 0.8262(5) 0.8263(4) 0.3649(6) 0.088(3) Uani 1 1 d . . . C22 C 0.8369(6) 0.8194(5) 0.3115(6) 0.098(4) Uani 1 1 d . . . H22 H 0.8826 0.8166 0.2986 0.117 Uiso 1 1 calc R . . C23 C 0.7829(6) 0.8166(4) 0.2774(5) 0.091(3) Uani 1 1 d . . . H23 H 0.7905 0.8100 0.2413 0.110 Uiso 1 1 calc R . . C24 C 0.7147(5) 0.8239(4) 0.2975(5) 0.083(3) Uani 1 1 d . . . H24 H 0.6770 0.8226 0.2739 0.099 Uiso 1 1 calc R . . C25 C 0.5684(4) 0.5639(4) 0.1640(4) 0.068(2) Uani 1 1 d . . . C26 C 0.5073(4) 0.5199(4) 0.1618(3) 0.0548(19) Uani 1 1 d . . . C27 C 0.5024(4) 0.9651(4) 0.3684(3) 0.061(2) Uani 1 1 d . . . C28 C 0.4550(5) 0.9288(5) 0.4026(4) 0.082(3) Uani 1 1 d . . . C29 C 0.4019(4) 0.4890(4) 0.1721(3) 0.058(2) Uani 1 1 d . . . C30 C 0.3261(4) 0.4872(4) 0.1890(4) 0.076 Uani 1 1 d . . . C31 C 0.3087(4) 0.4910(4) 0.2412(4) 0.076 Uani 1 1 d . . . H31 H 0.3443 0.4940 0.2664 0.091 Uiso 1 1 calc R . . C32 C 0.2366(4) 0.4907(4) 0.2588(4) 0.076 Uani 1 1 d . . . H32 H 0.2241 0.4922 0.2946 0.091 Uiso 1 1 calc R . . C33 C 0.1886(5) 0.4881(4) 0.2195(4) 0.076 Uani 1 1 d . . . H33 H 0.1414 0.4859 0.2290 0.091 Uiso 1 1 calc R . . C34 C 0.2044(4) 0.4885(4) 0.1677(4) 0.076 Uani 1 1 d . . . C35 C 0.2757(4) 0.4864(4) 0.1509(4) 0.076 Uani 1 1 d . . . H35 H 0.2873 0.4846 0.1150 0.091 Uiso 1 1 calc R . . C36 C 0.0885(4) 0.4966(4) 0.1298(4) 0.076 Uani 1 1 d . . . H36A H 0.0789 0.5396 0.1394 0.114 Uiso 1 1 calc R . . H36B H 0.0703 0.4691 0.1568 0.114 Uiso 1 1 calc R . . H36C H 0.0664 0.4872 0.0964 0.114 Uiso 1 1 calc R . . C37 C 0.3010(4) 0.6599(4) 0.1709(4) 0.069(2) Uani 1 1 d . . . C38 C 0.3494(5) 0.6661(4) 0.1273(4) 0.067(2) Uani 1 1 d . . . C39 C 0.4632(6) 0.6712(4) 0.0972(4) 0.081(3) Uani 1 1 d . . . H39 H 0.5111 0.6712 0.1048 0.097 Uiso 1 1 calc R . . C40 C 0.4435(8) 0.6757(5) 0.0446(4) 0.100(4) Uani 1 1 d . . . H40 H 0.4768 0.6798 0.0176 0.120 Uiso 1 1 calc R . . C41 C 0.3728(9) 0.6739(6) 0.0335(5) 0.119(4) Uani 1 1 d . . . H41 H 0.3571 0.6755 -0.0015 0.143 Uiso 1 1 calc R . . C42 C 0.3239(6) 0.6696(5) 0.0761(5) 0.097(3) Uani 1 1 d . . . C43 C 0.2490(8) 0.6690(7) 0.0690(7) 0.139(6) Uani 1 1 d . . . H43 H 0.2311 0.6712 0.0347 0.167 Uiso 1 1 calc R . . C44 C 0.2042(6) 0.6656(6) 0.1092(7) 0.122(5) Uani 1 1 d . . . H44 H 0.1561 0.6658 0.1025 0.147 Uiso 1 1 calc R . . C45 C 0.2284(5) 0.6617(4) 0.1618(6) 0.094(4) Uani 1 1 d . . . C46 C 0.1844(6) 0.6560(6) 0.2058(8) 0.119(5) Uani 1 1 d . . . H46 H 0.1362 0.6519 0.2006 0.142 Uiso 1 1 calc R . . C47 C 0.2102(7) 0.6561(5) 0.2559(7) 0.113(5) Uani 1 1 d . . . H47 H 0.1805 0.6596 0.2852 0.136 Uiso 1 1 calc R . . C48 C 0.2843(6) 0.6508(5) 0.2624(5) 0.096(3) Uani 1 1 d . . . H48 H 0.3028 0.6441 0.2962 0.115 Uiso 1 1 calc R . . N1 N 0.4891(3) 0.6986(3) 0.2856(2) 0.0508(15) Uani 1 1 d . . . N2 N 0.5362(3) 0.7712(3) 0.3395(3) 0.0506(15) Uani 1 1 d . . . N3 N 0.7015(4) 0.8329(3) 0.3498(3) 0.0653(18) Uani 1 1 d . . . N4 N 0.6770(4) 0.8567(3) 0.4549(3) 0.074(2) Uani 1 1 d . . . N5 N 0.3282(4) 0.6554(3) 0.2204(3) 0.069(2) Uani 1 1 d . . . N6 N 0.4189(3) 0.6668(3) 0.1377(3) 0.0576(16) Uani 1 1 d . . . N7 N 0.4465(3) 0.5335(3) 0.1869(3) 0.0533(15) Uani 1 1 d . . . N8 N 0.5697(3) 0.9459(3) 0.3613(3) 0.0573(16) Uani 1 1 d . . . O1 O 0.4317(3) 0.5824(3) 0.3100(3) 0.0798(18) Uani 1 1 d . . . O2 O 0.4493(4) 0.5973(3) 0.3958(3) 0.0856(19) Uani 1 1 d . . . O3 O 0.5041(3) 0.6744(3) 0.4554(2) 0.0812(18) Uani 1 1 d . . . H3 H 0.4846 0.6492 0.4355 0.122 Uiso 1 1 calc R . . O4 O 0.5577(3) 0.7660(3) 0.4491(2) 0.0662(14) Uani 1 1 d . . . O5 O 0.5972(4) 0.7771(4) 0.1101(3) 0.107(3) Uani 1 1 d . . . O6 O 0.4774(4) 0.8799(3) 0.4234(3) 0.096(2) Uani 1 1 d . . . O7 O 0.3926(3) 0.9512(4) 0.4108(4) 0.128(3) Uani 1 1 d . . . H7A H 0.3878 0.9841 0.3941 0.193 Uiso 1 1 calc R . . O8 O 0.6237(3) 0.5508(3) 0.1388(3) 0.090(2) Uani 1 1 d . . . O9 O 0.5633(3) 0.6112(3) 0.1934(3) 0.0729(16) Uani 1 1 d . . . O10 O 0.1600(3) 0.4881(2) 0.1254(3) 0.076 Uani 1 1 d . . . Cd1 Cd 0.59070(3) 0.84771(3) 0.38939(2) 0.0578(2) Uani 1 1 d . . . Cd2 Cd 0.44685(3) 0.63074(3) 0.22489(2) 0.0569(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.064(6) 0.068(6) 0.074(7) 0.002(5) 0.010(5) -0.007(4) C2 0.029(4) 0.066(5) 0.062(5) 0.003(4) 0.003(3) 0.003(3) C3 0.044(4) 0.057(5) 0.043(4) 0.001(3) 0.004(3) 0.003(3) C4 0.055(5) 0.065(6) 0.054(5) 0.000(4) 0.009(4) 0.011(4) C5 0.042(4) 0.067(5) 0.041(4) 0.004(4) 0.000(3) 0.004(4) C6 0.054(5) 0.070(5) 0.048(5) 0.009(4) -0.009(4) -0.013(4) C7 0.062(5) 0.077(6) 0.046(5) 0.003(4) -0.012(4) -0.015(4) C8 0.073(6) 0.103(8) 0.058(6) 0.010(6) -0.005(5) -0.025(5) C9 0.118(9) 0.097(8) 0.062(7) 0.015(6) -0.018(6) -0.042(7) C10 0.122(9) 0.073(7) 0.090(8) 0.015(6) -0.028(7) -0.018(6) C11 0.081(6) 0.081(7) 0.058(5) 0.010(5) -0.019(5) -0.008(5) C12 0.200(15) 0.195(15) 0.055(7) 0.016(8) 0.008(8) -0.050(12) C13 0.051(5) 0.046(5) 0.115(8) 0.001(5) -0.003(5) 0.004(4) C14 0.045(5) 0.081(6) 0.107(8) 0.004(6) -0.017(5) 0.000(4) C15 0.103(9) 0.150(11) 0.087(9) 0.000(7) -0.008(7) -0.027(8) C16 0.126(12) 0.185(14) 0.084(9) -0.012(8) -0.030(9) -0.018(10) C17 0.123(13) 0.156(13) 0.120(12) -0.005(9) -0.064(10) 0.001(10) C18 0.083(9) 0.107(9) 0.129(11) 0.009(7) -0.046(8) 0.001(6) C19 0.075(9) 0.117(10) 0.173(14) -0.004(10) -0.048(10) -0.002(7) C20 0.052(6) 0.106(9) 0.170(13) 0.022(9) -0.008(8) 0.014(6) C21 0.053(6) 0.068(6) 0.143(10) 0.005(6) 0.005(7) 0.005(5) C22 0.067(7) 0.072(7) 0.154(12) -0.018(7) 0.021(8) 0.013(5) C23 0.085(8) 0.068(6) 0.121(9) -0.017(6) 0.041(7) -0.002(5) C24 0.074(7) 0.071(6) 0.103(8) -0.009(5) 0.005(6) -0.001(5) C25 0.039(5) 0.069(6) 0.096(7) -0.017(5) 0.000(4) 0.003(4) C26 0.042(4) 0.061(5) 0.062(5) -0.005(4) -0.003(4) 0.001(4) C27 0.050(5) 0.063(5) 0.071(5) 0.002(4) 0.007(4) 0.001(4) C28 0.070(6) 0.073(6) 0.104(8) 0.020(6) 0.027(5) 0.008(5) C29 0.046(4) 0.062(5) 0.066(5) -0.005(4) 0.004(4) -0.002(4) C30 0.045 0.056 0.127 -0.021(5) 0.013(5) -0.004(4) C31 0.045 0.056 0.127 -0.021(5) 0.017(5) -0.008(4) C32 0.045 0.056 0.127 -0.012(5) 0.013(5) -0.005(4) C33 0.045 0.056 0.127 -0.008(5) 0.009(5) 0.003(4) C34 0.045 0.056 0.127 -0.009(5) -0.020(5) -0.004(4) C35 0.045 0.056 0.127 -0.021(5) -0.009(5) 0.001(4) C36 0.045 0.056 0.127 0.001(5) -0.009(5) -0.002(4) C37 0.047(5) 0.049(5) 0.112(8) 0.000(5) -0.009(5) 0.006(4) C38 0.061(6) 0.054(5) 0.086(7) -0.008(4) -0.012(5) 0.004(4) C39 0.085(7) 0.077(6) 0.080(7) 0.004(5) 0.016(6) 0.003(5) C40 0.139(11) 0.098(8) 0.063(7) -0.002(5) 0.001(7) 0.025(8) C41 0.172(14) 0.105(9) 0.080(9) -0.017(7) -0.040(10) 0.025(9) C42 0.098(9) 0.090(7) 0.101(9) -0.007(6) -0.044(8) 0.022(6) C43 0.105(11) 0.146(12) 0.167(15) -0.033(11) -0.065(11) 0.014(10) C44 0.056(7) 0.108(9) 0.203(17) -0.019(10) -0.053(9) 0.011(7) C45 0.048(6) 0.053(5) 0.183(12) 0.001(6) -0.021(8) -0.004(4) C46 0.041(6) 0.089(8) 0.226(18) 0.000(10) 0.006(9) 0.003(5) C47 0.072(8) 0.083(8) 0.185(14) -0.003(9) 0.063(9) -0.008(6) C48 0.068(7) 0.093(7) 0.127(9) 0.022(6) 0.028(6) 0.026(6) N1 0.047(4) 0.053(4) 0.053(4) 0.009(3) 0.000(3) -0.003(3) N2 0.042(3) 0.049(4) 0.061(4) 0.006(3) 0.001(3) -0.004(3) N3 0.058(4) 0.053(4) 0.085(6) -0.002(3) 0.006(4) 0.002(3) N4 0.059(5) 0.074(5) 0.087(6) 0.004(4) -0.016(4) 0.004(4) N5 0.047(4) 0.068(5) 0.093(6) 0.014(4) 0.016(4) -0.001(3) N6 0.050(4) 0.059(4) 0.063(4) -0.003(3) 0.003(3) -0.001(3) N7 0.039(3) 0.053(4) 0.068(4) 0.000(3) 0.004(3) -0.005(3) N8 0.042(4) 0.051(4) 0.079(5) 0.003(3) 0.001(3) 0.007(3) O1 0.093(5) 0.068(4) 0.078(4) 0.007(3) -0.005(3) -0.033(3) O2 0.108(5) 0.079(4) 0.070(4) 0.021(3) 0.009(4) -0.016(4) O3 0.106(5) 0.079(4) 0.058(4) 0.018(3) 0.000(3) -0.007(4) O4 0.072(4) 0.071(4) 0.055(3) 0.004(3) -0.006(3) -0.001(3) O5 0.136(7) 0.133(7) 0.052(4) -0.001(4) 0.015(4) -0.038(5) O6 0.090(5) 0.077(5) 0.121(6) 0.037(4) 0.046(4) 0.017(4) O7 0.069(4) 0.118(6) 0.198(8) 0.088(6) 0.064(5) 0.035(4) O8 0.052(4) 0.095(5) 0.121(5) -0.032(4) 0.024(4) -0.020(3) O9 0.044(3) 0.076(4) 0.098(5) -0.021(3) -0.008(3) -0.008(3) O10 0.045 0.056 0.127 -0.001(3) -0.006(3) -0.001(3) Cd1 0.0489(4) 0.0578(4) 0.0668(4) 0.0048(3) -0.0031(3) 0.0015(3) Cd2 0.0457(3) 0.0616(4) 0.0634(4) -0.0059(3) -0.0018(3) -0.0040(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.217(10) . ? C1 O2 1.277(10) . ? C1 C2 1.483(11) . ? C2 N1 1.375(9) . ? C2 C3 1.404(10) . ? C3 N2 1.369(9) . ? C3 C4 1.461(10) . ? C4 O4 1.228(9) . ? C4 O3 1.295(9) . ? C5 N2 1.331(9) . ? C5 N1 1.357(9) . ? C5 C6 1.432(10) . ? C6 C11 1.394(11) . ? C6 C7 1.413(11) . ? C7 C8 1.370(11) . ? C7 H7 0.9300 . ? C8 O5 1.334(12) . ? C8 C9 1.372(14) . ? C9 C10 1.351(15) . ? C9 H9 0.9300 . ? C10 C11 1.399(14) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 O5 1.383(12) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 N3 1.365(11) . ? C13 C21 1.399(13) . ? C13 C14 1.420(13) . ? C14 N4 1.339(12) . ? C14 C18 1.445(14) . ? C15 N4 1.328(13) . ? C15 C16 1.365(17) . ? C15 H15 0.9300 . ? C16 C17 1.382(19) . ? C16 H16 0.9300 . ? C17 C18 1.364(18) . ? C17 H17 0.9300 . ? C18 C19 1.454(18) . ? C19 C20 1.315(17) . ? C19 H19 0.9300 . ? C20 C21 1.414(16) . ? C20 H20 0.9300 . ? C21 C22 1.366(15) . ? C22 C23 1.340(14) . ? C22 H22 0.9300 . ? C23 C24 1.400(13) . ? C23 H23 0.9300 . ? C24 N3 1.352(11) . ? C24 H24 0.9300 . ? C25 O9 1.252(10) . ? C25 O8 1.260(9) . ? C25 C26 1.492(10) . ? C26 N7 1.349(9) . ? C26 C27 1.402(11) 3_645 ? C27 N8 1.356(9) . ? C27 C26 1.402(11) 3_655 ? C27 C28 1.464(11) . ? C28 O6 1.239(10) . ? C28 O7 1.295(10) . ? C29 N7 1.322(9) . ? C29 N8 1.356(9) 3_645 ? C29 C30 1.502(11) . ? C30 C35 1.355(12) . ? C30 C31 1.358(13) . ? C31 C32 1.440(11) . ? C31 H31 0.9300 . ? C32 C33 1.346(12) . ? C32 H32 0.9300 . ? C33 C34 1.337(12) . ? C33 H33 0.9300 . ? C34 O10 1.357(10) . ? C34 C35 1.420(11) . ? C35 H35 0.9300 . ? C36 O10 1.376(9) . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 N5 1.351(11) . ? C37 C45 1.401(12) . ? C37 C38 1.437(13) . ? C38 N6 1.347(10) . ? C38 C42 1.376(13) . ? C39 N6 1.325(11) . ? C39 C40 1.378(14) . ? C39 H39 0.9300 . ? C40 C41 1.374(17) . ? C40 H40 0.9300 . ? C41 C42 1.421(17) . ? C41 H41 0.9300 . ? C42 C43 1.436(17) . ? C43 C44 1.323(19) . ? C43 H43 0.9300 . ? C44 C45 1.400(17) . ? C44 H44 0.9300 . ? C45 C46 1.392(17) . ? C46 C47 1.353(18) . ? C46 H46 0.9300 . ? C47 C48 1.423(16) . ? C47 H47 0.9300 . ? C48 N5 1.350(12) . ? C48 H48 0.9300 . ? N1 Cd2 2.248(6) . ? N2 Cd1 2.300(6) . ? N3 Cd1 2.351(7) . ? N4 Cd1 2.332(7) . ? N5 Cd2 2.318(7) . ? N6 Cd2 2.381(7) . ? N7 Cd2 2.276(6) . ? N8 C29 1.356(9) 3_655 ? N8 Cd1 2.237(6) . ? O1 Cd2 2.391(6) . ? O3 H3 0.8200 . ? O4 Cd1 2.379(5) . ? O6 Cd1 2.416(6) . ? O7 H7A 0.8200 . ? O9 Cd2 2.387(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 O2 124.2(8) . . ? O1 C1 C2 119.9(8) . . ? O2 C1 C2 115.8(8) . . ? N1 C2 C3 107.9(6) . . ? N1 C2 C1 119.4(7) . . ? C3 C2 C1 132.6(8) . . ? N2 C3 C2 107.5(6) . . ? N2 C3 C4 121.3(7) . . ? C2 C3 C4 131.1(7) . . ? O4 C4 O3 121.6(8) . . ? O4 C4 C3 120.0(7) . . ? O3 C4 C3 118.3(8) . . ? N2 C5 N1 112.8(6) . . ? N2 C5 C6 123.3(7) . . ? N1 C5 C6 123.9(7) . . ? C11 C6 C7 117.1(8) . . ? C11 C6 C5 121.8(8) . . ? C7 C6 C5 121.1(8) . . ? C8 C7 C6 122.4(9) . . ? C8 C7 H7 118.8 . . ? C6 C7 H7 118.8 . . ? O5 C8 C7 115.8(10) . . ? O5 C8 C9 125.4(9) . . ? C7 C8 C9 118.7(10) . . ? C10 C9 C8 121.1(10) . . ? C10 C9 H9 119.5 . . ? C8 C9 H9 119.5 . . ? C9 C10 C11 121.2(10) . . ? C9 C10 H10 119.4 . . ? C11 C10 H10 119.4 . . ? C6 C11 C10 119.5(10) . . ? C6 C11 H11 120.2 . . ? C10 C11 H11 120.2 . . ? 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 . . ? N3 C13 C21 121.0(10) . . ? N3 C13 C14 117.0(8) . . ? C21 C13 C14 122.0(10) . . ? N4 C14 C13 120.9(8) . . ? N4 C14 C18 120.2(11) . . ? C13 C14 C18 118.9(10) . . ? N4 C15 C16 124.5(13) . . ? N4 C15 H15 117.8 . . ? C16 C15 H15 117.8 . . ? C15 C16 C17 116.4(13) . . ? C15 C16 H16 121.8 . . ? C17 C16 H16 121.8 . . ? C18 C17 C16 122.5(12) . . ? C18 C17 H17 118.7 . . ? C16 C17 H17 118.7 . . ? C17 C18 C14 116.8(13) . . ? C17 C18 C19 126.2(13) . . ? C14 C18 C19 116.9(13) . . ? C20 C19 C18 121.2(13) . . ? C20 C19 H19 119.4 . . ? C18 C19 H19 119.4 . . ? C19 C20 C21 123.9(12) . . ? C19 C20 H20 118.0 . . ? C21 C20 H20 118.0 . . ? C22 C21 C13 118.8(11) . . ? C22 C21 C20 123.9(11) . . ? C13 C21 C20 117.1(12) . . ? C23 C22 C21 121.4(11) . . ? C23 C22 H22 119.3 . . ? C21 C22 H22 119.3 . . ? C22 C23 C24 118.3(11) . . ? C22 C23 H23 120.9 . . ? C24 C23 H23 120.9 . . ? N3 C24 C23 122.6(10) . . ? N3 C24 H24 118.7 . . ? C23 C24 H24 118.7 . . ? O9 C25 O8 122.6(8) . . ? O9 C25 C26 117.7(7) . . ? O8 C25 C26 119.6(8) . . ? N7 C26 C27 108.6(6) . 3_645 ? N7 C26 C25 121.1(7) . . ? C27 C26 C25 130.0(7) 3_645 . ? N8 C27 C26 107.6(7) . 3_655 ? N8 C27 C28 120.0(7) . . ? C26 C27 C28 132.4(8) 3_655 . ? O6 C28 O7 123.8(8) . . ? O6 C28 C27 118.5(8) . . ? O7 C28 C27 117.7(8) . . ? N7 C29 N8 113.7(6) . 3_645 ? N7 C29 C30 123.7(7) . . ? N8 C29 C30 122.6(7) 3_645 . ? C35 C30 C31 120.7(8) . . ? C35 C30 C29 118.7(9) . . ? C31 C30 C29 120.4(9) . . ? C30 C31 C32 122.0(9) . . ? C30 C31 H31 119.0 . . ? C32 C31 H31 119.0 . . ? C33 C32 C31 114.8(9) . . ? C33 C32 H32 122.6 . . ? C31 C32 H32 122.6 . . ? C34 C33 C32 124.3(9) . . ? C34 C33 H33 117.8 . . ? C32 C33 H33 117.8 . . ? C33 C34 O10 128.6(8) . . ? C33 C34 C35 120.2(9) . . ? O10 C34 C35 111.2(9) . . ? C30 C35 C34 117.8(10) . . ? C30 C35 H35 121.1 . . ? C34 C35 H35 121.1 . . ? O10 C36 H36A 109.5 . . ? O10 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? O10 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N5 C37 C45 122.0(10) . . ? N5 C37 C38 117.6(7) . . ? C45 C37 C38 120.3(11) . . ? N6 C38 C42 121.8(10) . . ? N6 C38 C37 118.7(8) . . ? C42 C38 C37 119.4(10) . . ? N6 C39 C40 124.8(10) . . ? N6 C39 H39 117.6 . . ? C40 C39 H39 117.6 . . ? C41 C40 C39 117.2(11) . . ? C41 C40 H40 121.4 . . ? C39 C40 H40 121.4 . . ? C40 C41 C42 119.3(11) . . ? C40 C41 H41 120.3 . . ? C42 C41 H41 120.3 . . ? C38 C42 C41 118.5(10) . . ? C38 C42 C43 117.7(13) . . ? C41 C42 C43 123.8(13) . . ? C44 C43 C42 123.0(14) . . ? C44 C43 H43 118.5 . . ? C42 C43 H43 118.5 . . ? C43 C44 C45 120.8(12) . . ? C43 C44 H44 119.6 . . ? C45 C44 H44 119.6 . . ? C46 C45 C44 123.9(12) . . ? C46 C45 C37 117.4(12) . . ? C44 C45 C37 118.7(12) . . ? C47 C46 C45 121.5(11) . . ? C47 C46 H46 119.2 . . ? C45 C46 H46 119.2 . . ? C46 C47 C48 117.7(12) . . ? C46 C47 H47 121.1 . . ? C48 C47 H47 121.1 . . ? N5 C48 C47 121.1(12) . . ? N5 C48 H48 119.4 . . ? C47 C48 H48 119.4 . . ? C5 N1 C2 105.2(6) . . ? C5 N1 Cd2 141.4(5) . . ? C2 N1 Cd2 113.3(5) . . ? C5 N2 C3 106.5(6) . . ? C5 N2 Cd1 142.2(5) . . ? C3 N2 Cd1 111.3(5) . . ? C24 N3 C13 117.6(8) . . ? C24 N3 Cd1 126.7(6) . . ? C13 N3 Cd1 115.6(6) . . ? C15 N4 C14 119.5(9) . . ? C15 N4 Cd1 125.2(7) . . ? C14 N4 Cd1 115.1(7) . . ? C48 N5 C37 119.3(8) . . ? C48 N5 Cd2 123.1(7) . . ? C37 N5 Cd2 115.7(5) . . ? C39 N6 C38 118.3(8) . . ? C39 N6 Cd2 126.0(6) . . ? C38 N6 Cd2 113.2(6) . . ? C29 N7 C26 105.4(6) . . ? C29 N7 Cd2 140.2(5) . . ? C26 N7 Cd2 112.8(5) . . ? C29 N8 C27 104.7(6) 3_655 . ? C29 N8 Cd1 139.0(5) 3_655 . ? C27 N8 Cd1 114.0(5) . . ? C1 O1 Cd2 114.0(6) . . ? C4 O3 H3 109.5 . . ? C4 O4 Cd1 114.3(5) . . ? C8 O5 C12 119.2(11) . . ? C28 O6 Cd1 113.3(6) . . ? C28 O7 H7A 109.5 . . ? C25 O9 Cd2 114.0(5) . . ? C34 O10 C36 123.3(8) . . ? N8 Cd1 N2 114.0(2) . . ? N8 Cd1 N4 105.8(2) . . ? N2 Cd1 N4 139.4(2) . . ? N8 Cd1 N3 98.7(2) . . ? N2 Cd1 N3 94.5(2) . . ? N4 Cd1 N3 71.3(3) . . ? N8 Cd1 O4 146.3(2) . . ? N2 Cd1 O4 73.1(2) . . ? N4 Cd1 O4 78.5(2) . . ? N3 Cd1 O4 113.9(2) . . ? N8 Cd1 O6 71.9(2) . . ? N2 Cd1 O6 89.5(2) . . ? N4 Cd1 O6 110.8(3) . . ? N3 Cd1 O6 170.6(2) . . ? O4 Cd1 O6 75.4(2) . . ? N1 Cd2 N7 150.3(2) . . ? N1 Cd2 N5 103.6(2) . . ? N7 Cd2 N5 100.5(2) . . ? N1 Cd2 N6 119.8(2) . . ? N7 Cd2 N6 84.6(2) . . ? N5 Cd2 N6 70.4(2) . . ? N1 Cd2 O9 90.3(2) . . ? N7 Cd2 O9 72.9(2) . . ? N5 Cd2 O9 157.7(3) . . ? N6 Cd2 O9 87.6(2) . . ? N1 Cd2 O1 73.2(2) . . ? N7 Cd2 O1 89.1(2) . . ? N5 Cd2 O1 91.4(2) . . ? N6 Cd2 O1 159.2(2) . . ? O9 Cd2 O1 109.5(2) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.685 _refine_diff_density_min -2.879 _refine_diff_density_rms 0.113 data_a5 _database_code_depnum_ccdc_archive 'CCDC 903675' #TrackingRef '6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H32 Cd2 N8 O10' _chemical_formula_sum 'C44 H32 Cd2 N8 O10' _chemical_formula_weight 1057.58 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 'P 21' _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.3619(6) _cell_length_b 22.6503(15) _cell_length_c 9.6061(6) _cell_angle_alpha 90.00 _cell_angle_beta 94.8710(10) _cell_angle_gamma 90.00 _cell_volume 2029.6(2) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 850 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 20.03 _exptl_crystal_description strip-shaped _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.731 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1056 _exptl_absorpt_coefficient_mu 1.120 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7299 _exptl_absorpt_correction_T_max 0.8962 _exptl_absorpt_process_details '(SADABS; Bruker, 2008)' _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10798 _diffrn_reflns_av_R_equivalents 0.0193 _diffrn_reflns_av_unetI/netI 0.0328 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6013 _reflns_number_gt 5849 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0212P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.005(13) _refine_ls_number_reflns 6013 _refine_ls_number_parameters 588 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0197 _refine_ls_R_factor_gt 0.0188 _refine_ls_wR_factor_ref 0.0443 _refine_ls_wR_factor_gt 0.0439 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.031 _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 -0.05208(2) 0.564014(8) 0.80158(2) 0.01455(5) Uani 1 1 d . . . Cd2 Cd 0.29630(2) 0.785458(9) 1.17441(2) 0.01617(6) Uani 1 1 d . . . O3 O 0.1850(2) 0.52944(10) 0.8334(2) 0.0205(5) Uani 1 1 d . . . N3 N -0.0063(3) 0.57504(12) 0.5633(2) 0.0185(6) Uani 1 1 d . . . C5 C -0.0542(3) 0.73101(13) 0.9591(3) 0.0160(6) Uani 1 1 d . . . N5 N 0.2606(3) 0.77015(11) 1.4084(3) 0.0172(6) Uani 1 1 d . . . O2 O 0.4636(2) 0.70731(9) 1.1904(2) 0.0232(5) Uani 1 1 d . . . C4 C 0.2678(3) 0.56003(15) 0.9135(3) 0.0165(6) Uani 1 1 d . . . C6 C 0.0706(3) 0.69100(13) 0.9782(3) 0.0153(6) Uani 1 1 d . . . C11 C 0.0314(4) 0.58684(16) 0.2832(4) 0.0305(9) Uani 1 1 d . . . H11 H 0.0448 0.5912 0.1890 0.037 Uiso 1 1 calc R . . O1 O 0.5135(2) 0.61938(10) 1.1074(2) 0.0256(5) Uani 1 1 d . . . C13 C -0.1160(4) 0.59253(14) 0.4737(3) 0.0200(7) Uani 1 1 d . . . N6 N 0.4707(3) 0.84044(12) 1.3134(3) 0.0201(6) Uani 1 1 d . . . N2 N 0.0799(3) 0.63727(11) 0.9193(2) 0.0137(5) Uani 1 1 d . . . C1 C 0.2846(3) 0.66061(13) 1.0453(3) 0.0139(6) Uani 1 1 d . . . C3 C 0.4290(3) 0.66329(14) 1.1186(3) 0.0193(7) Uani 1 1 d . . . N4 N -0.2579(3) 0.59833(12) 0.6720(3) 0.0207(6) Uani 1 1 d . . . N1 N 0.1910(3) 0.70685(11) 1.0556(3) 0.0149(6) Uani 1 1 d . . . C9 C 0.1435(4) 0.56808(17) 0.3769(3) 0.0270(7) Uani 1 1 d . . . H9 H 0.2327 0.5593 0.3464 0.032 Uiso 1 1 calc R . . C17 C 0.3479(3) 0.79985(12) 1.5029(3) 0.0170(7) Uani 1 1 d . . . C12 C -0.0987(4) 0.59871(16) 0.3313(3) 0.0264(8) Uani 1 1 d . . . H12 H -0.1752 0.6108 0.2699 0.032 Uiso 1 1 calc R . . C18 C 0.3472(3) 0.78923(17) 1.6445(3) 0.0232(7) Uani 1 1 d . . . H18 H 0.4106 0.8090 1.7081 0.028 Uiso 1 1 calc R . . C20 C 0.1598(4) 0.71919(15) 1.5946(4) 0.0268(8) Uani 1 1 d . . . H20 H 0.0937 0.6920 1.6228 0.032 Uiso 1 1 calc R . . C15 C -0.2561(4) 0.60410(14) 0.5326(3) 0.0214(7) Uani 1 1 d . . . C16 C -0.3806(4) 0.60766(16) 0.7301(4) 0.0279(8) Uani 1 1 d . . . H16 H -0.3818 0.6026 0.8260 0.033 Uiso 1 1 calc R . . C2 C 0.2159(3) 0.61769(13) 0.9615(3) 0.0147(6) Uani 1 1 d . . . C7 C -0.1943(4) 0.71042(14) 0.9590(3) 0.0220(7) Uani 1 1 d . . . H7 H -0.2125 0.6704 0.9708 0.026 Uiso 1 1 calc R . . C19 C 0.2500(4) 0.74839(16) 1.6905(4) 0.0261(8) Uani 1 1 d . . . H19 H 0.2466 0.7411 1.7854 0.031 Uiso 1 1 calc R . . C8 C -0.0285(3) 0.79080(15) 0.9426(3) 0.0173(6) Uani 1 1 d . . . H8 H 0.0653 0.8042 0.9407 0.021 Uiso 1 1 calc R . . C10 C 0.1197(3) 0.56274(16) 0.5154(3) 0.0243(7) Uani 1 1 d . . . H10 H 0.1945 0.5500 0.5782 0.029 Uiso 1 1 calc R . . O10 O -0.1819(2) 0.56575(10) 1.0100(2) 0.0204(4) Uani 1 1 d . . . O9 O -0.3012(2) 0.50942(10) 1.1502(2) 0.0226(5) Uani 1 1 d . . . H9A H -0.3753 0.5283 1.1330 0.034 Uiso 1 1 d R . . O5 O 0.3754(2) 0.82402(9) 0.9662(2) 0.0185(5) Uani 1 1 d . . . O4 O -0.1029(2) 0.88869(9) 0.9153(2) 0.0242(5) Uani 1 1 d . . . O8 O 0.3935(2) 0.90734(10) 0.8460(2) 0.0225(5) Uani 1 1 d . . . H8A H 0.3634 0.9413 0.8484 0.034 Uiso 1 1 calc R . . O7 O 0.3948(2) 0.54396(9) 0.9559(2) 0.0215(5) Uani 1 1 d . . . N8 N -0.1330(3) 0.47136(11) 0.8381(3) 0.0160(5) Uani 1 1 d . . . N10 N 0.1953(3) 0.87648(11) 1.1426(2) 0.0154(5) Uani 1 1 d . . . C24 C -0.2321(3) 0.51716(14) 1.0401(3) 0.0173(7) Uani 1 1 d . . . C28 C 0.3444(3) 0.87719(14) 0.9445(3) 0.0175(7) Uani 1 1 d . . . C22 C -0.1414(3) 0.83116(14) 0.9287(3) 0.0189(7) Uani 1 1 d . . . C21 C -0.2824(4) 0.81079(15) 0.9263(3) 0.0232(7) Uani 1 1 d . . . H21 H -0.3590 0.8370 0.9150 0.028 Uiso 1 1 calc R . . C25 C -0.1260(3) 0.41666(13) 0.7847(3) 0.0157(6) Uani 1 1 d . . . C23 C -0.2116(3) 0.46554(14) 0.9512(3) 0.0164(6) Uani 1 1 d . . . C27 C 0.2495(3) 0.90718(14) 1.0370(3) 0.0149(6) Uani 1 1 d . . . C40 C -0.0564(3) 0.40061(14) 0.6589(3) 0.0178(7) Uani 1 1 d . . . C37 C 0.4446(3) 0.84526(14) 1.4479(3) 0.0186(7) Uani 1 1 d . . . C41 C 0.0349(3) 0.35201(15) 0.6654(3) 0.0218(7) Uani 1 1 d . . . H41 H 0.0556 0.3321 0.7494 0.026 Uiso 1 1 calc R . . C38 C -0.3063(4) 0.75058(16) 0.9412(4) 0.0255(8) Uani 1 1 d . . . H38 H -0.4000 0.7368 0.9391 0.031 Uiso 1 1 calc R . . C36 C 0.1692(4) 0.73110(14) 1.4551(3) 0.0226(7) Uani 1 1 d . . . H36 H 0.1087 0.7108 1.3899 0.027 Uiso 1 1 calc R . . C29 C 0.5576(4) 0.88004(16) 1.2608(3) 0.0265(8) Uani 1 1 d . . . H29 H 0.5768 0.8762 1.1678 0.032 Uiso 1 1 calc R . . C35 C -0.3777(4) 0.62018(17) 0.4498(4) 0.0330(9) Uani 1 1 d . . . H35 H -0.3753 0.6233 0.3534 0.040 Uiso 1 1 calc R . . C42 C -0.0896(4) 0.42969(15) 0.5332(3) 0.0244(7) Uani 1 1 d . . . H42 H -0.1515 0.4619 0.5287 0.029 Uiso 1 1 calc R . . C32 C 0.5027(4) 0.89008(16) 1.5314(4) 0.0321(9) Uani 1 1 d . . . H32 H 0.4822 0.8930 1.6242 0.038 Uiso 1 1 calc R . . C30 C 0.6198(4) 0.92603(17) 1.3370(4) 0.0320(9) Uani 1 1 d . . . H30 H 0.6786 0.9531 1.2969 0.038 Uiso 1 1 calc R . . C31 C 0.5916(5) 0.93046(18) 1.4755(4) 0.0398(10) Uani 1 1 d . . . H31 H 0.6327 0.9607 1.5308 0.048 Uiso 1 1 calc R . . C33 C -0.2144(4) 0.93152(16) 0.8996(4) 0.0332(9) Uani 1 1 d . . . H33A H -0.2669 0.9314 0.9813 0.050 Uiso 1 1 calc R . . H33B H -0.2780 0.9222 0.8190 0.050 Uiso 1 1 calc R . . H33C H -0.1736 0.9699 0.8882 0.050 Uiso 1 1 calc R . . C39 C -0.5026(4) 0.63161(18) 0.5110(4) 0.0369(9) Uani 1 1 d . . . H39 H -0.5843 0.6440 0.4570 0.044 Uiso 1 1 calc R . . C34 C -0.5051(4) 0.62443(17) 0.6540(4) 0.0331(9) Uani 1 1 d . . . H34 H -0.5888 0.6308 0.6974 0.040 Uiso 1 1 calc R . . O11 O 0.1847(3) 0.28535(15) 0.5513(2) 0.0403(6) Uani 1 1 d U . . C44 C 0.0947(4) 0.33352(16) 0.5459(4) 0.0294(8) Uani 1 1 d . A . C47 C -0.0293(4) 0.41020(17) 0.4142(3) 0.0326(9) Uani 1 1 d . A . H47 H -0.0501 0.4297 0.3298 0.039 Uiso 1 1 calc R . . C43 C 0.0613(4) 0.36204(17) 0.4204(4) 0.0350(9) Uani 1 1 d . . . H43 H 0.0999 0.3488 0.3400 0.042 Uiso 1 1 calc R A . C45 C 0.2261(7) 0.2559(3) 0.6825(7) 0.0354(17) Uani 0.569(8) 1 d PU A 1 H45A H 0.2889 0.2236 0.6665 0.053 Uiso 0.569(8) 1 calc PR A 1 H45B H 0.1421 0.2413 0.7218 0.053 Uiso 0.569(8) 1 calc PR A 1 H45C H 0.2747 0.2834 0.7462 0.053 Uiso 0.569(8) 1 calc PR A 1 C45' C 0.2392(10) 0.2699(4) 0.4215(10) 0.045(3) Uani 0.431(8) 1 d P A 2 H45D H 0.3006 0.2361 0.4348 0.067 Uiso 0.431(8) 1 calc PR A 2 H45E H 0.2927 0.3024 0.3886 0.067 Uiso 0.431(8) 1 calc PR A 2 H45F H 0.1608 0.2608 0.3539 0.067 Uiso 0.431(8) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.01731(11) 0.01241(11) 0.01389(10) 0.00054(9) 0.00112(8) -0.00141(9) Cd2 0.02155(12) 0.01247(11) 0.01424(10) -0.00115(9) 0.00008(8) 0.00007(9) O3 0.0233(12) 0.0177(12) 0.0202(11) -0.0069(9) -0.0003(9) 0.0024(9) N3 0.0209(14) 0.0165(16) 0.0181(13) -0.0001(11) 0.0021(10) -0.0021(11) C5 0.0181(16) 0.0144(16) 0.0154(15) -0.0024(12) 0.0012(12) 0.0020(12) N5 0.0174(14) 0.0167(15) 0.0177(13) 0.0003(10) 0.0016(11) 0.0007(10) O2 0.0225(12) 0.0174(12) 0.0279(12) -0.0059(10) -0.0085(10) 0.0009(9) C4 0.0214(15) 0.0143(15) 0.0148(14) 0.0021(14) 0.0069(11) 0.0014(14) C6 0.0176(16) 0.0131(15) 0.0153(15) 0.0005(12) 0.0023(12) 0.0006(12) C11 0.044(2) 0.031(2) 0.0182(17) -0.0053(15) 0.0102(16) -0.0085(17) O1 0.0212(12) 0.0177(12) 0.0367(13) -0.0053(10) -0.0054(10) 0.0088(10) C13 0.0289(18) 0.0138(16) 0.0172(15) -0.0010(13) 0.0003(13) -0.0048(13) N6 0.0215(14) 0.0209(14) 0.0182(13) 0.0006(11) 0.0031(11) 0.0002(11) N2 0.0155(13) 0.0134(13) 0.0126(12) -0.0003(10) 0.0032(10) 0.0023(10) C1 0.0166(16) 0.0133(15) 0.0125(14) 0.0026(12) 0.0042(12) 0.0048(12) C3 0.0193(17) 0.0205(17) 0.0179(16) 0.0038(14) 0.0002(13) 0.0003(13) N4 0.0197(14) 0.0220(15) 0.0201(14) 0.0020(11) 0.0006(11) -0.0014(11) N1 0.0164(14) 0.0138(14) 0.0144(13) -0.0008(10) 0.0009(10) 0.0008(10) C9 0.0306(18) 0.0280(18) 0.0238(16) -0.0032(17) 0.0108(13) -0.0006(17) C17 0.0196(16) 0.0122(17) 0.0199(15) -0.0015(12) 0.0047(12) 0.0016(12) C12 0.033(2) 0.026(2) 0.0184(17) 0.0023(15) -0.0060(15) -0.0030(16) C18 0.0286(17) 0.0236(17) 0.0172(14) -0.0044(16) 0.0016(12) -0.0016(17) C20 0.032(2) 0.0207(18) 0.0290(19) 0.0051(15) 0.0100(15) -0.0029(15) C15 0.0255(18) 0.0181(17) 0.0202(16) 0.0018(13) -0.0011(13) -0.0027(14) C16 0.0259(19) 0.032(2) 0.0266(18) 0.0040(16) 0.0055(15) 0.0005(15) C2 0.0147(15) 0.0165(16) 0.0131(14) 0.0011(12) 0.0017(11) 0.0005(12) C7 0.0229(18) 0.0143(17) 0.0291(18) -0.0001(14) 0.0042(14) 0.0004(13) C19 0.037(2) 0.024(2) 0.0185(17) 0.0014(15) 0.0089(15) -0.0007(16) C8 0.0173(15) 0.0170(16) 0.0176(14) -0.0022(14) 0.0019(11) -0.0002(14) C10 0.0242(16) 0.0241(17) 0.0246(15) -0.0012(16) 0.0014(12) -0.0007(16) O10 0.0277(11) 0.0130(11) 0.0212(10) -0.0001(10) 0.0063(8) -0.0016(11) O9 0.0306(13) 0.0175(12) 0.0214(11) 0.0015(10) 0.0118(9) 0.0040(10) O5 0.0226(12) 0.0160(12) 0.0172(11) -0.0010(9) 0.0041(9) 0.0038(9) O4 0.0275(13) 0.0127(11) 0.0318(13) 0.0010(10) -0.0012(10) 0.0028(10) O8 0.0306(13) 0.0149(11) 0.0237(12) -0.0032(9) 0.0130(10) 0.0032(9) O7 0.0185(12) 0.0181(12) 0.0273(12) -0.0042(9) -0.0003(9) 0.0050(9) N8 0.0197(14) 0.0142(13) 0.0148(13) 0.0008(11) 0.0060(10) -0.0017(11) N10 0.0207(14) 0.0116(13) 0.0144(13) -0.0020(11) 0.0036(10) 0.0002(10) C24 0.0185(16) 0.0164(17) 0.0169(15) 0.0021(13) 0.0021(12) 0.0033(13) C28 0.0167(16) 0.0181(17) 0.0181(15) -0.0018(13) 0.0030(12) 0.0012(12) C22 0.0263(18) 0.0150(16) 0.0152(15) -0.0011(13) 0.0003(13) 0.0009(13) C21 0.0212(17) 0.0233(18) 0.0257(17) 0.0019(14) 0.0052(14) 0.0102(14) C25 0.0167(16) 0.0144(16) 0.0164(15) 0.0002(12) 0.0044(12) -0.0023(12) C23 0.0171(16) 0.0186(17) 0.0135(15) -0.0012(13) 0.0016(12) 0.0019(13) C27 0.0134(16) 0.0183(16) 0.0129(15) 0.0008(12) 0.0009(12) 0.0000(12) C40 0.0197(16) 0.0163(17) 0.0182(16) -0.0012(13) 0.0068(13) -0.0062(13) C37 0.0199(16) 0.0177(16) 0.0185(15) 0.0008(13) 0.0029(12) 0.0004(13) C41 0.0224(17) 0.0233(18) 0.0201(16) -0.0001(14) 0.0050(13) 0.0011(14) C38 0.0186(18) 0.0244(19) 0.034(2) -0.0005(16) 0.0040(14) -0.0005(14) C36 0.0243(18) 0.0169(17) 0.0265(18) -0.0014(14) 0.0010(14) -0.0053(14) C29 0.0286(19) 0.034(2) 0.0174(16) 0.0018(15) 0.0062(14) -0.0099(16) C35 0.029(2) 0.045(2) 0.0235(19) 0.0073(17) -0.0071(15) -0.0024(18) C42 0.034(2) 0.0167(17) 0.0228(17) 0.0007(14) 0.0025(14) -0.0055(14) C32 0.043(2) 0.033(2) 0.0208(17) -0.0063(16) 0.0090(16) -0.0165(18) C30 0.038(2) 0.029(2) 0.030(2) 0.0008(16) 0.0092(16) -0.0174(17) C31 0.058(3) 0.030(2) 0.033(2) -0.0119(17) 0.0077(19) -0.023(2) C33 0.038(2) 0.0202(19) 0.041(2) 0.0010(17) 0.0006(17) 0.0103(16) C39 0.0216(19) 0.047(2) 0.040(2) 0.0121(19) -0.0070(16) 0.0018(17) C34 0.0217(18) 0.037(2) 0.041(2) 0.0111(18) 0.0046(16) 0.0037(16) O11 0.0437(15) 0.0447(15) 0.0339(12) -0.0101(14) 0.0118(11) 0.0158(15) C44 0.0266(18) 0.0255(19) 0.037(2) -0.0092(16) 0.0094(15) -0.0022(14) C47 0.051(2) 0.035(2) 0.0125(16) 0.0010(15) 0.0075(16) -0.0097(18) C43 0.042(2) 0.041(2) 0.0249(19) -0.0105(17) 0.0160(16) -0.0069(18) C45 0.029(4) 0.027(4) 0.049(3) -0.008(3) 0.000(3) 0.015(3) C45' 0.038(6) 0.052(7) 0.045(6) -0.020(5) 0.011(4) 0.010(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 Cd1 N8 2.268(2) . ? Cd1 N2 2.306(3) . ? Cd1 N4 2.337(3) . ? Cd1 O3 2.349(2) . ? Cd1 N3 2.378(2) . ? Cd1 O10 2.4285(19) . ? Cd2 N10 2.278(2) . ? Cd2 N1 2.292(3) . ? Cd2 N5 2.326(2) . ? Cd2 O5 2.359(2) . ? Cd2 O2 2.360(2) . ? Cd2 N6 2.373(3) . ? O3 C4 1.253(4) . ? N3 C10 1.331(4) . ? N3 C13 1.343(4) . ? C5 C8 1.387(5) . ? C5 C7 1.391(5) . ? C5 C6 1.478(4) . ? N5 C36 1.334(4) . ? N5 C17 1.349(4) . ? O2 C3 1.240(4) . ? C4 O7 1.276(4) . ? C4 C2 1.481(4) . ? C6 N1 1.345(4) . ? C6 N2 1.348(4) . ? C11 C12 1.365(5) . ? C11 C9 1.390(5) . ? C11 H11 0.9300 . ? O1 C3 1.281(4) . ? C13 C12 1.397(5) . ? C13 C15 1.495(5) . ? N6 C29 1.339(4) . ? N6 C37 1.340(4) . ? N2 C2 1.377(4) . ? C1 N1 1.374(4) . ? C1 C2 1.385(4) . ? C1 C3 1.472(4) . ? N4 C16 1.335(4) . ? N4 C15 1.346(4) . ? C9 C10 1.373(4) . ? C9 H9 0.9300 . ? C17 C18 1.382(4) . ? C17 C37 1.496(4) . ? C12 H12 0.9300 . ? C18 C19 1.395(5) . ? C18 H18 0.9300 . ? C20 C19 1.366(5) . ? C20 C36 1.377(5) . ? C20 H20 0.9300 . ? C15 C35 1.382(5) . ? C16 C34 1.376(5) . ? C16 H16 0.9300 . ? C7 C38 1.388(5) . ? C7 H7 0.9300 . ? C19 H19 0.9300 . ? C8 C22 1.396(4) . ? C8 H8 0.9300 . ? C10 H10 0.9300 . ? O10 C24 1.241(4) . ? O9 C24 1.298(4) . ? O9 H9A 0.8200 . ? O5 C28 1.252(4) . ? O4 C22 1.361(4) . ? O4 C33 1.424(4) . ? O8 C28 1.283(4) . ? O8 H8A 0.8200 . ? N8 C25 1.345(4) . ? N8 C23 1.370(4) . ? N10 C25 1.347(4) 2_557 ? N10 C27 1.364(4) . ? C24 C23 1.470(4) . ? C28 C27 1.474(4) . ? C22 C21 1.397(5) . ? C21 C38 1.391(5) . ? C21 H21 0.9300 . ? C25 N10 1.347(4) 2_547 ? C25 C40 1.466(4) . ? C23 C27 1.376(5) 2_547 ? C27 C23 1.376(4) 2_557 ? C40 C42 1.387(4) . ? C40 C41 1.392(5) . ? C37 C32 1.377(5) . ? C41 C44 1.384(5) . ? C41 H41 0.9300 . ? C38 H38 0.9300 . ? C36 H36 0.9300 . ? C29 C30 1.374(5) . ? C29 H29 0.9300 . ? C35 C39 1.377(5) . ? C35 H35 0.9300 . ? C42 C47 1.389(5) . ? C42 H42 0.9300 . ? C32 C31 1.376(5) . ? C32 H32 0.9300 . ? C30 C31 1.381(5) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C39 C34 1.385(5) . ? C39 H39 0.9300 . ? C34 H34 0.9300 . ? O11 C44 1.377(5) . ? O11 C45' 1.430(9) . ? O11 C45 1.450(7) . ? C44 C43 1.380(5) . ? C47 C43 1.380(6) . ? C47 H47 0.9300 . ? C43 H43 0.9300 . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C45' H45D 0.9600 . ? C45' H45E 0.9600 . ? C45' H45F 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 N8 Cd1 N2 139.62(9) . . ? N8 Cd1 N4 96.83(9) . . ? N2 Cd1 N4 113.89(9) . . ? N8 Cd1 O3 89.76(9) . . ? N2 Cd1 O3 73.45(8) . . ? N4 Cd1 O3 155.19(8) . . ? N8 Cd1 N3 109.63(9) . . ? N2 Cd1 N3 105.27(9) . . ? N4 Cd1 N3 70.13(9) . . ? O3 Cd1 N3 85.11(8) . . ? N8 Cd1 O10 71.97(8) . . ? N2 Cd1 O10 82.47(8) . . ? N4 Cd1 O10 89.20(8) . . ? O3 Cd1 O10 115.55(7) . . ? N3 Cd1 O10 159.33(8) . . ? N10 Cd2 N1 118.70(9) . . ? N10 Cd2 N5 99.92(9) . . ? N1 Cd2 N5 105.92(9) . . ? N10 Cd2 O5 73.01(8) . . ? N1 Cd2 O5 91.04(8) . . ? N5 Cd2 O5 162.89(8) . . ? N10 Cd2 O2 162.42(8) . . ? N1 Cd2 O2 72.82(8) . . ? N5 Cd2 O2 88.53(8) . . ? O5 Cd2 O2 94.51(8) . . ? N10 Cd2 N6 81.86(9) . . ? N1 Cd2 N6 159.11(9) . . ? N5 Cd2 N6 71.51(9) . . ? O5 Cd2 N6 91.85(8) . . ? O2 Cd2 N6 86.33(8) . . ? C4 O3 Cd1 115.09(19) . . ? C10 N3 C13 119.5(3) . . ? C10 N3 Cd1 123.2(2) . . ? C13 N3 Cd1 117.2(2) . . ? C8 C5 C7 120.0(3) . . ? C8 C5 C6 118.0(3) . . ? C7 C5 C6 122.0(3) . . ? C36 N5 C17 118.2(3) . . ? C36 N5 Cd2 124.9(2) . . ? C17 N5 Cd2 116.60(19) . . ? C3 O2 Cd2 115.3(2) . . ? O3 C4 O7 123.3(3) . . ? O3 C4 C2 118.4(3) . . ? O7 C4 C2 118.3(3) . . ? N1 C6 N2 113.1(3) . . ? N1 C6 C5 121.4(3) . . ? N2 C6 C5 125.4(3) . . ? C12 C11 C9 119.2(3) . . ? C12 C11 H11 120.4 . . ? C9 C11 H11 120.4 . . ? N3 C13 C12 120.7(3) . . ? N3 C13 C15 117.2(3) . . ? C12 C13 C15 122.1(3) . . ? C29 N6 C37 118.4(3) . . ? C29 N6 Cd2 123.4(2) . . ? C37 N6 Cd2 114.4(2) . . ? C6 N2 C2 104.9(2) . . ? C6 N2 Cd1 143.6(2) . . ? C2 N2 Cd1 110.86(19) . . ? N1 C1 C2 108.1(3) . . ? N1 C1 C3 120.0(3) . . ? C2 C1 C3 132.0(3) . . ? O2 C3 O1 122.5(3) . . ? O2 C3 C1 119.0(3) . . ? O1 C3 C1 118.5(3) . . ? C16 N4 C15 119.0(3) . . ? C16 N4 Cd1 122.0(2) . . ? C15 N4 Cd1 118.8(2) . . ? C6 N1 C1 105.4(3) . . ? C6 N1 Cd2 141.9(2) . . ? C1 N1 Cd2 112.2(2) . . ? C10 C9 C11 118.6(3) . . ? C10 C9 H9 120.7 . . ? C11 C9 H9 120.7 . . ? N5 C17 C18 121.5(3) . . ? N5 C17 C37 117.1(3) . . ? C18 C17 C37 121.4(3) . . ? C11 C12 C13 119.5(3) . . ? C11 C12 H12 120.3 . . ? C13 C12 H12 120.3 . . ? C17 C18 C19 119.0(3) . . ? C17 C18 H18 120.5 . . ? C19 C18 H18 120.5 . . ? C19 C20 C36 118.3(3) . . ? C19 C20 H20 120.9 . . ? C36 C20 H20 120.9 . . ? N4 C15 C35 121.3(3) . . ? N4 C15 C13 116.4(3) . . ? C35 C15 C13 122.3(3) . . ? N4 C16 C34 122.8(3) . . ? N4 C16 H16 118.6 . . ? C34 C16 H16 118.6 . . ? N2 C2 C1 108.5(3) . . ? N2 C2 C4 120.8(3) . . ? C1 C2 C4 130.7(3) . . ? C38 C7 C5 118.8(3) . . ? C38 C7 H7 120.6 . . ? C5 C7 H7 120.6 . . ? C20 C19 C18 119.3(3) . . ? C20 C19 H19 120.3 . . ? C18 C19 H19 120.3 . . ? C5 C8 C22 120.8(3) . . ? C5 C8 H8 119.6 . . ? C22 C8 H8 119.6 . . ? N3 C10 C9 122.5(3) . . ? N3 C10 H10 118.7 . . ? C9 C10 H10 118.7 . . ? C24 O10 Cd1 113.84(19) . . ? C24 O9 H9A 103.7 . . ? C28 O5 Cd2 114.36(19) . . ? C22 O4 C33 117.7(3) . . ? C28 O8 H8A 109.5 . . ? C25 N8 C23 105.1(2) . . ? C25 N8 Cd1 140.0(2) . . ? C23 N8 Cd1 114.88(19) . . ? C25 N10 C27 105.5(2) 2_557 . ? C25 N10 Cd2 139.01(19) 2_557 . ? C27 N10 Cd2 112.61(19) . . ? O10 C24 O9 122.4(3) . . ? O10 C24 C23 119.9(3) . . ? O9 C24 C23 117.7(3) . . ? O5 C28 O8 122.8(3) . . ? O5 C28 C27 119.1(3) . . ? O8 C28 C27 118.1(3) . . ? O4 C22 C8 115.6(3) . . ? O4 C22 C21 124.9(3) . . ? C8 C22 C21 119.5(3) . . ? C38 C21 C22 118.8(3) . . ? C38 C21 H21 120.6 . . ? C22 C21 H21 120.6 . . ? N8 C25 N10 112.6(2) . 2_547 ? N8 C25 C40 125.6(3) . . ? N10 C25 C40 121.8(3) 2_547 . ? N8 C23 C27 108.5(3) . 2_547 ? N8 C23 C24 119.3(3) . . ? C27 C23 C24 132.0(3) 2_547 . ? N10 C27 C23 108.3(3) . 2_557 ? N10 C27 C28 119.7(3) . . ? C23 C27 C28 131.7(3) 2_557 . ? C42 C40 C41 120.4(3) . . ? C42 C40 C25 121.1(3) . . ? C41 C40 C25 118.2(3) . . ? N6 C37 C32 121.7(3) . . ? N6 C37 C17 116.7(3) . . ? C32 C37 C17 121.5(3) . . ? C44 C41 C40 119.5(3) . . ? C44 C41 H41 120.3 . . ? C40 C41 H41 120.3 . . ? C7 C38 C21 122.0(3) . . ? C7 C38 H38 119.0 . . ? C21 C38 H38 119.0 . . ? N5 C36 C20 123.6(3) . . ? N5 C36 H36 118.2 . . ? C20 C36 H36 118.2 . . ? N6 C29 C30 123.4(3) . . ? N6 C29 H29 118.3 . . ? C30 C29 H29 118.3 . . ? C39 C35 C15 119.4(3) . . ? C39 C35 H35 120.3 . . ? C15 C35 H35 120.3 . . ? C40 C42 C47 119.2(3) . . ? C40 C42 H42 120.4 . . ? C47 C42 H42 120.4 . . ? C31 C32 C37 119.0(3) . . ? C31 C32 H32 120.5 . . ? C37 C32 H32 120.5 . . ? C29 C30 C31 117.5(3) . . ? C29 C30 H30 121.3 . . ? C31 C30 H30 121.3 . . ? C32 C31 C30 119.9(3) . . ? C32 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? O4 C33 H33A 109.5 . . ? O4 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? O4 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C35 C39 C34 119.2(3) . . ? C35 C39 H39 120.4 . . ? C34 C39 H39 120.4 . . ? C16 C34 C39 118.3(3) . . ? C16 C34 H34 120.8 . . ? C39 C34 H34 120.8 . . ? C44 O11 C45' 115.1(5) . . ? C44 O11 C45 121.0(3) . . ? C45' O11 C45 123.8(5) . . ? O11 C44 C43 119.8(3) . . ? O11 C44 C41 119.9(3) . . ? C43 C44 C41 120.4(3) . . ? C43 C47 C42 120.4(3) . . ? C43 C47 H47 119.8 . . ? C42 C47 H47 119.8 . . ? C44 C43 C47 120.1(3) . . ? C44 C43 H43 120.0 . . ? C47 C43 H43 120.0 . . ? O11 C45 H45A 109.5 . . ? O11 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? O11 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? O11 C45' H45D 109.5 . . ? O11 C45' H45E 109.5 . . ? H45D C45' H45E 109.5 . . ? O11 C45' H45F 109.5 . . ? H45D C45' H45F 109.5 . . ? H45E C45' H45F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N8 Cd1 O3 C4 -132.8(2) . . . . ? N2 Cd1 O3 C4 9.9(2) . . . . ? N4 Cd1 O3 C4 121.2(2) . . . . ? N3 Cd1 O3 C4 117.4(2) . . . . ? O10 Cd1 O3 C4 -63.0(2) . . . . ? N8 Cd1 N3 C10 -89.5(3) . . . . ? N2 Cd1 N3 C10 69.9(3) . . . . ? N4 Cd1 N3 C10 -179.8(3) . . . . ? O3 Cd1 N3 C10 -1.5(3) . . . . ? O10 Cd1 N3 C10 179.7(2) . . . . ? N8 Cd1 N3 C13 88.0(2) . . . . ? N2 Cd1 N3 C13 -112.6(2) . . . . ? N4 Cd1 N3 C13 -2.3(2) . . . . ? O3 Cd1 N3 C13 176.0(2) . . . . ? O10 Cd1 N3 C13 -2.8(4) . . . . ? N10 Cd2 N5 C36 110.0(2) . . . . ? N1 Cd2 N5 C36 -13.9(3) . . . . ? O5 Cd2 N5 C36 173.9(2) . . . . ? O2 Cd2 N5 C36 -85.5(2) . . . . ? N6 Cd2 N5 C36 -172.2(3) . . . . ? N10 Cd2 N5 C17 -75.7(2) . . . . ? N1 Cd2 N5 C17 160.4(2) . . . . ? O5 Cd2 N5 C17 -11.8(4) . . . . ? O2 Cd2 N5 C17 88.8(2) . . . . ? N6 Cd2 N5 C17 2.2(2) . . . . ? N10 Cd2 O2 C3 -126.1(3) . . . . ? N1 Cd2 O2 C3 7.4(2) . . . . ? N5 Cd2 O2 C3 114.6(2) . . . . ? O5 Cd2 O2 C3 -82.2(2) . . . . ? N6 Cd2 O2 C3 -173.8(2) . . . . ? Cd1 O3 C4 O7 171.1(2) . . . . ? Cd1 O3 C4 C2 -8.8(3) . . . . ? C8 C5 C6 N1 38.7(4) . . . . ? C7 C5 C6 N1 -140.5(3) . . . . ? C8 C5 C6 N2 -139.0(3) . . . . ? C7 C5 C6 N2 41.8(4) . . . . ? C10 N3 C13 C12 -0.9(5) . . . . ? Cd1 N3 C13 C12 -178.5(2) . . . . ? C10 N3 C13 C15 178.3(3) . . . . ? Cd1 N3 C13 C15 0.7(4) . . . . ? N10 Cd2 N6 C29 -67.2(3) . . . . ? N1 Cd2 N6 C29 103.2(3) . . . . ? N5 Cd2 N6 C29 -170.6(3) . . . . ? O5 Cd2 N6 C29 5.4(3) . . . . ? O2 Cd2 N6 C29 99.8(3) . . . . ? N10 Cd2 N6 C37 90.4(2) . . . . ? N1 Cd2 N6 C37 -99.2(3) . . . . ? N5 Cd2 N6 C37 -13.0(2) . . . . ? O5 Cd2 N6 C37 163.0(2) . . . . ? O2 Cd2 N6 C37 -102.6(2) . . . . ? N1 C6 N2 C2 -0.4(3) . . . . ? C5 C6 N2 C2 177.6(3) . . . . ? N1 C6 N2 Cd1 168.8(2) . . . . ? C5 C6 N2 Cd1 -13.3(5) . . . . ? N8 Cd1 N2 C6 -108.7(3) . . . . ? N4 Cd1 N2 C6 27.5(4) . . . . ? O3 Cd1 N2 C6 -177.8(3) . . . . ? N3 Cd1 N2 C6 102.2(3) . . . . ? O10 Cd1 N2 C6 -58.3(3) . . . . ? N8 Cd1 N2 C2 60.1(2) . . . . ? N4 Cd1 N2 C2 -163.74(18) . . . . ? O3 Cd1 N2 C2 -9.05(18) . . . . ? N3 Cd1 N2 C2 -89.08(19) . . . . ? O10 Cd1 N2 C2 110.49(19) . . . . ? Cd2 O2 C3 O1 174.1(2) . . . . ? Cd2 O2 C3 C1 -7.0(4) . . . . ? N1 C1 C3 O2 0.9(4) . . . . ? C2 C1 C3 O2 -178.6(3) . . . . ? N1 C1 C3 O1 179.7(3) . . . . ? C2 C1 C3 O1 0.2(5) . . . . ? N8 Cd1 N4 C16 69.8(3) . . . . ? N2 Cd1 N4 C16 -83.4(3) . . . . ? O3 Cd1 N4 C16 174.2(2) . . . . ? N3 Cd1 N4 C16 178.2(3) . . . . ? O10 Cd1 N4 C16 -2.0(3) . . . . ? N8 Cd1 N4 C15 -104.6(2) . . . . ? N2 Cd1 N4 C15 102.3(2) . . . . ? O3 Cd1 N4 C15 -0.2(4) . . . . ? N3 Cd1 N4 C15 3.9(2) . . . . ? O10 Cd1 N4 C15 -176.3(2) . . . . ? N2 C6 N1 C1 0.5(3) . . . . ? C5 C6 N1 C1 -177.5(3) . . . . ? N2 C6 N1 Cd2 171.7(2) . . . . ? C5 C6 N1 Cd2 -6.3(5) . . . . ? C2 C1 N1 C6 -0.4(3) . . . . ? C3 C1 N1 C6 -180.0(3) . . . . ? C2 C1 N1 Cd2 -174.54(19) . . . . ? C3 C1 N1 Cd2 5.9(3) . . . . ? N10 Cd2 N1 C6 -11.8(4) . . . . ? N5 Cd2 N1 C6 99.3(3) . . . . ? O5 Cd2 N1 C6 -82.9(3) . . . . ? O2 Cd2 N1 C6 -177.3(3) . . . . ? N6 Cd2 N1 C6 179.1(3) . . . . ? N10 Cd2 N1 C1 159.06(18) . . . . ? N5 Cd2 N1 C1 -89.8(2) . . . . ? O5 Cd2 N1 C1 87.9(2) . . . . ? O2 Cd2 N1 C1 -6.48(19) . . . . ? N6 Cd2 N1 C1 -10.0(4) . . . . ? C12 C11 C9 C10 -0.7(5) . . . . ? C36 N5 C17 C18 2.1(4) . . . . ? Cd2 N5 C17 C18 -172.7(2) . . . . ? C36 N5 C17 C37 -177.4(3) . . . . ? Cd2 N5 C17 C37 7.9(3) . . . . ? C9 C11 C12 C13 0.8(5) . . . . ? N3 C13 C12 C11 0.0(5) . . . . ? C15 C13 C12 C11 -179.2(3) . . . . ? N5 C17 C18 C19 -2.5(5) . . . . ? C37 C17 C18 C19 176.9(3) . . . . ? C16 N4 C15 C35 0.9(5) . . . . ? Cd1 N4 C15 C35 175.4(3) . . . . ? C16 N4 C15 C13 -179.4(3) . . . . ? Cd1 N4 C15 C13 -4.9(4) . . . . ? N3 C13 C15 N4 2.7(4) . . . . ? C12 C13 C15 N4 -178.1(3) . . . . ? N3 C13 C15 C35 -177.6(3) . . . . ? C12 C13 C15 C35 1.6(5) . . . . ? C15 N4 C16 C34 -1.7(5) . . . . ? Cd1 N4 C16 C34 -176.0(3) . . . . ? C6 N2 C2 C1 0.1(3) . . . . ? Cd1 N2 C2 C1 -173.00(19) . . . . ? C6 N2 C2 C4 -178.2(3) . . . . ? Cd1 N2 C2 C4 8.7(3) . . . . ? N1 C1 C2 N2 0.2(3) . . . . ? C3 C1 C2 N2 179.7(3) . . . . ? N1 C1 C2 C4 178.3(3) . . . . ? C3 C1 C2 C4 -2.2(6) . . . . ? O3 C4 C2 N2 0.0(4) . . . . ? O7 C4 C2 N2 -179.9(3) . . . . ? O3 C4 C2 C1 -177.9(3) . . . . ? O7 C4 C2 C1 2.2(5) . . . . ? C8 C5 C7 C38 0.5(5) . . . . ? C6 C5 C7 C38 179.7(3) . . . . ? C36 C20 C19 C18 0.4(5) . . . . ? C17 C18 C19 C20 1.2(5) . . . . ? C7 C5 C8 C22 1.4(4) . . . . ? C6 C5 C8 C22 -177.9(3) . . . . ? C13 N3 C10 C9 1.0(5) . . . . ? Cd1 N3 C10 C9 178.5(3) . . . . ? C11 C9 C10 N3 -0.3(6) . . . . ? N8 Cd1 O10 C24 -0.34(19) . . . . ? N2 Cd1 O10 C24 -148.7(2) . . . . ? N4 Cd1 O10 C24 97.1(2) . . . . ? O3 Cd1 O10 C24 -81.1(2) . . . . ? N3 Cd1 O10 C24 97.6(3) . . . . ? N10 Cd2 O5 C28 9.2(2) . . . . ? N1 Cd2 O5 C28 129.0(2) . . . . ? N5 Cd2 O5 C28 -58.5(4) . . . . ? O2 Cd2 O5 C28 -158.2(2) . . . . ? N6 Cd2 O5 C28 -71.7(2) . . . . ? N2 Cd1 N8 C25 -122.7(3) . . . . ? N4 Cd1 N8 C25 96.9(3) . . . . ? O3 Cd1 N8 C25 -59.1(3) . . . . ? N3 Cd1 N8 C25 25.6(3) . . . . ? O10 Cd1 N8 C25 -176.2(3) . . . . ? N2 Cd1 N8 C23 54.8(3) . . . . ? N4 Cd1 N8 C23 -85.6(2) . . . . ? O3 Cd1 N8 C23 118.4(2) . . . . ? N3 Cd1 N8 C23 -156.9(2) . . . . ? O10 Cd1 N8 C23 1.34(19) . . . . ? N1 Cd2 N10 C25 112.0(3) . . . 2_557 ? N5 Cd2 N10 C25 -2.4(3) . . . 2_557 ? O5 Cd2 N10 C25 -166.4(3) . . . 2_557 ? O2 Cd2 N10 C25 -120.2(3) . . . 2_557 ? N6 Cd2 N10 C25 -71.9(3) . . . 2_557 ? N1 Cd2 N10 C27 -90.9(2) . . . . ? N5 Cd2 N10 C27 154.7(2) . . . . ? O5 Cd2 N10 C27 -9.27(19) . . . . ? O2 Cd2 N10 C27 36.9(4) . . . . ? N6 Cd2 N10 C27 85.2(2) . . . . ? Cd1 O10 C24 O9 178.0(2) . . . . ? Cd1 O10 C24 C23 -0.7(3) . . . . ? Cd2 O5 C28 O8 171.3(2) . . . . ? Cd2 O5 C28 C27 -7.6(3) . . . . ? C33 O4 C22 C8 179.5(3) . . . . ? C33 O4 C22 C21 1.0(4) . . . . ? C5 C8 C22 O4 179.1(3) . . . . ? C5 C8 C22 C21 -2.4(4) . . . . ? O4 C22 C21 C38 179.9(3) . . . . ? C8 C22 C21 C38 1.5(5) . . . . ? C23 N8 C25 N10 -0.1(3) . . . 2_547 ? Cd1 N8 C25 N10 177.5(2) . . . 2_547 ? C23 N8 C25 C40 177.9(3) . . . . ? Cd1 N8 C25 C40 -4.5(5) . . . . ? C25 N8 C23 C27 0.2(3) . . . 2_547 ? Cd1 N8 C23 C27 -178.2(2) . . . 2_547 ? C25 N8 C23 C24 176.1(3) . . . . ? Cd1 N8 C23 C24 -2.3(3) . . . . ? O10 C24 C23 N8 2.0(4) . . . . ? O9 C24 C23 N8 -176.7(3) . . . . ? O10 C24 C23 C27 176.8(3) . . . 2_547 ? O9 C24 C23 C27 -1.9(5) . . . 2_547 ? C25 N10 C27 C23 0.1(3) 2_557 . . 2_557 ? Cd2 N10 C27 C23 -164.6(2) . . . 2_557 ? C25 N10 C27 C28 174.1(3) 2_557 . . . ? Cd2 N10 C27 C28 9.4(3) . . . . ? O5 C28 C27 N10 -1.1(4) . . . . ? O8 C28 C27 N10 179.9(3) . . . . ? O5 C28 C27 C23 171.2(3) . . . 2_557 ? O8 C28 C27 C23 -7.7(5) . . . 2_557 ? N8 C25 C40 C42 -52.8(5) . . . . ? N10 C25 C40 C42 125.1(3) 2_547 . . . ? N8 C25 C40 C41 132.7(3) . . . . ? N10 C25 C40 C41 -49.5(4) 2_547 . . . ? C29 N6 C37 C32 1.1(5) . . . . ? Cd2 N6 C37 C32 -157.7(3) . . . . ? C29 N6 C37 C17 -179.5(3) . . . . ? Cd2 N6 C37 C17 21.7(3) . . . . ? N5 C17 C37 N6 -20.4(4) . . . . ? C18 C17 C37 N6 160.2(3) . . . . ? N5 C17 C37 C32 159.0(3) . . . . ? C18 C17 C37 C32 -20.4(5) . . . . ? C42 C40 C41 C44 1.2(5) . . . . ? C25 C40 C41 C44 175.8(3) . . . . ? C5 C7 C38 C21 -1.4(5) . . . . ? C22 C21 C38 C7 0.4(5) . . . . ? C17 N5 C36 C20 -0.4(5) . . . . ? Cd2 N5 C36 C20 173.8(3) . . . . ? C19 C20 C36 N5 -0.8(5) . . . . ? C37 N6 C29 C30 -1.1(5) . . . . ? Cd2 N6 C29 C30 155.7(3) . . . . ? N4 C15 C35 C39 1.2(5) . . . . ? C13 C15 C35 C39 -178.4(3) . . . . ? C41 C40 C42 C47 -0.8(5) . . . . ? C25 C40 C42 C47 -175.2(3) . . . . ? N6 C37 C32 C31 -1.0(6) . . . . ? C17 C37 C32 C31 179.7(3) . . . . ? N6 C29 C30 C31 0.9(6) . . . . ? C37 C32 C31 C30 0.8(7) . . . . ? C29 C30 C31 C32 -0.8(7) . . . . ? C15 C35 C39 C34 -2.6(6) . . . . ? N4 C16 C34 C39 0.3(6) . . . . ? C35 C39 C34 C16 1.8(6) . . . . ? C45' O11 C44 C43 1.4(6) . . . . ? C45 O11 C44 C43 177.6(4) . . . . ? C45' O11 C44 C41 179.4(5) . . . . ? C45 O11 C44 C41 -4.3(6) . . . . ? C40 C41 C44 O11 -179.8(3) . . . . ? C40 C41 C44 C43 -1.7(5) . . . . ? C40 C42 C47 C43 0.8(5) . . . . ? O11 C44 C43 C47 179.7(3) . . . . ? C41 C44 C43 C47 1.7(6) . . . . ? C42 C47 C43 C44 -1.2(6) . . . . ? 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 O9 H9A O1 0.82 2.31 3.043(3) 148.5 1_455 O9 H9A O7 0.82 2.65 3.361(3) 145.7 1_455 O8 H8A O9 0.82 1.65 2.470(3) 178.8 2_557 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.473 _refine_diff_density_min -0.384 _refine_diff_density_rms 0.052 data_a6 _database_code_depnum_ccdc_archive 'CCDC 903676' #TrackingRef '7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H10 Co N2 O7' _chemical_formula_weight 353.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M p-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.0394(14) _cell_length_b 8.8500(15) _cell_length_c 9.4594(16) _cell_angle_alpha 90.930(2) _cell_angle_beta 97.192(2) _cell_angle_gamma 102.019(2) _cell_volume 652.47(19) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2741 _cell_measurement_theta_min 2.355 _cell_measurement_theta_max 27.862 _exptl_crystal_description block _exptl_crystal_colour Pink _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.798 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 358 _exptl_absorpt_coefficient_mu 1.355 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7733 _exptl_absorpt_correction_T_max 0.8124 _exptl_absorpt_process_details '(SADABS; Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8956 _diffrn_reflns_av_R_equivalents 0.0342 _diffrn_reflns_av_unetI/netI 0.0416 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 28.25 _reflns_number_total 3201 _reflns_number_gt 2571 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0499P)^2^+0.7256P] 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 3201 _refine_ls_number_parameters 209 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0512 _refine_ls_R_factor_gt 0.0376 _refine_ls_wR_factor_ref 0.1025 _refine_ls_wR_factor_gt 0.0957 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.5000 0.0000 0.5000 0.01277(13) Uani 1 2 d S . . Co2 Co 1.0000 0.0000 0.0000 0.01507(13) Uani 1 2 d S . . O1 O 1.1679(2) 0.3411(2) 0.71182(19) 0.0195(4) Uani 1 1 d . . . O3 O 0.3325(2) -0.2654(2) 0.13008(19) 0.0165(4) Uani 1 1 d . . . O2 O 0.3515(2) -0.1673(2) 0.35161(19) 0.0175(4) Uani 1 1 d . . . N1 N 0.8298(3) 0.0291(2) 0.1509(2) 0.0134(4) Uani 1 1 d . . . C11 C 0.4130(3) -0.1781(3) 0.2373(3) 0.0139(5) Uani 1 1 d . . . C3 C 1.0354(3) 0.3206(3) 0.2728(3) 0.0169(5) Uani 1 1 d . . . H3 H 1.0060 0.3135 0.1743 0.020 Uiso 1 1 calc R . . C9 C 0.6795(3) -0.0748(3) 0.1123(3) 0.0131(5) Uani 1 1 d . . . C10 C 0.5844(3) -0.0862(3) 0.2248(2) 0.0123(5) Uani 1 1 d . . . C5 C 0.9997(3) 0.2174(3) 0.5045(3) 0.0142(5) Uani 1 1 d . . . H5 H 0.9460 0.1429 0.5617 0.017 Uiso 1 1 calc R . . C6 C 1.1276(3) 0.3414(3) 0.5659(3) 0.0150(5) Uani 1 1 d . . . C8 C 0.8195(3) 0.0802(3) 0.2849(3) 0.0130(5) Uani 1 1 d . . . C4 C 0.9534(3) 0.2063(3) 0.3573(3) 0.0139(5) Uani 1 1 d . . . C1 C 1.2072(3) 0.4556(3) 0.4828(3) 0.0180(5) Uani 1 1 d . . . H1 H 1.2907 0.5387 0.5245 0.022 Uiso 1 1 calc R . . C7 C 1.3000(4) 0.4648(3) 0.7788(3) 0.0245(6) Uani 1 1 d . . . H7A H 1.4059 0.4622 0.7429 0.037 Uiso 1 1 calc R . . H7B H 1.3138 0.4533 0.8801 0.037 Uiso 1 1 calc R . . H7C H 1.2687 0.5619 0.7583 0.037 Uiso 1 1 calc R . . C2 C 1.1592(3) 0.4431(3) 0.3356(3) 0.0190(5) Uani 1 1 d . . . H2 H 1.2116 0.5186 0.2788 0.023 Uiso 1 1 calc R . . O5 O 0.7556(2) -0.1114(2) -0.11427(18) 0.0161(4) Uani 1 1 d . . . O4 O 0.5019(2) -0.2426(2) -0.0712(2) 0.0189(4) Uani 1 1 d . . . O7 O 0.9850(2) 0.2104(2) -0.0862(2) 0.0203(4) Uani 1 1 d . . . H7 H 0.8840 0.2140 -0.1083 0.030 Uiso 1 1 calc R . . O6 O 0.6094(3) -0.1695(2) 0.60211(19) 0.0217(4) Uani 1 1 d . . . H6 H 0.6434 -0.1417 0.6857 0.033 Uiso 1 1 calc R . . N2 N 0.6723(3) 0.0119(2) 0.3344(2) 0.0126(4) Uani 1 1 d . . . C12 C 0.6446(3) -0.1467(3) -0.0318(3) 0.0141(5) Uani 1 1 d . . . H19 H 0.440(5) -0.256(5) 0.008(4) 0.050(12) 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 Co1 0.0132(2) 0.0159(2) 0.0094(2) -0.00160(17) 0.00318(18) 0.00269(18) Co2 0.0147(2) 0.0186(3) 0.0120(2) -0.00100(18) 0.00403(19) 0.00244(19) O1 0.0214(9) 0.0195(10) 0.0133(9) -0.0027(7) -0.0026(7) -0.0020(8) O3 0.0157(9) 0.0179(9) 0.0140(9) -0.0039(7) 0.0026(7) -0.0012(7) O2 0.0156(9) 0.0216(9) 0.0142(9) -0.0023(7) 0.0051(7) -0.0001(7) N1 0.0137(10) 0.0163(10) 0.0102(9) -0.0005(8) 0.0044(8) 0.0016(8) C11 0.0145(11) 0.0144(12) 0.0131(11) 0.0013(9) 0.0026(10) 0.0032(9) C3 0.0197(12) 0.0174(12) 0.0135(12) -0.0007(9) 0.0034(10) 0.0034(10) C9 0.0152(11) 0.0145(12) 0.0092(11) -0.0015(9) 0.0012(9) 0.0026(9) C10 0.0145(11) 0.0138(12) 0.0091(11) -0.0002(9) 0.0031(9) 0.0032(9) C5 0.0152(12) 0.0144(12) 0.0142(11) 0.0002(9) 0.0052(10) 0.0040(9) C6 0.0149(12) 0.0168(12) 0.0138(12) -0.0033(9) 0.0009(10) 0.0051(10) C8 0.0134(11) 0.0157(12) 0.0109(11) -0.0001(9) 0.0030(9) 0.0047(9) C4 0.0136(11) 0.0131(12) 0.0154(12) -0.0020(9) 0.0040(10) 0.0031(9) C1 0.0178(12) 0.0145(12) 0.0204(13) -0.0018(10) 0.0022(10) 0.0012(10) C7 0.0245(14) 0.0208(14) 0.0232(14) -0.0055(11) -0.0051(12) -0.0008(11) C2 0.0212(13) 0.0159(13) 0.0199(13) 0.0023(10) 0.0070(11) 0.0012(10) O5 0.0172(9) 0.0201(9) 0.0102(8) -0.0027(7) 0.0032(7) 0.0016(7) O4 0.0200(9) 0.0203(10) 0.0138(9) -0.0057(7) 0.0040(8) -0.0022(8) O7 0.0171(9) 0.0248(10) 0.0196(9) 0.0032(8) 0.0036(8) 0.0052(8) O6 0.0287(11) 0.0288(11) 0.0109(9) -0.0011(8) 0.0019(8) 0.0140(9) N2 0.0127(10) 0.0146(10) 0.0102(9) -0.0011(8) 0.0023(8) 0.0021(8) C12 0.0183(12) 0.0147(12) 0.0101(11) -0.0001(9) 0.0023(10) 0.0055(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O6 2.0838(19) . ? Co1 O6 2.0838(19) 2_656 ? Co1 O2 2.0891(18) . ? Co1 O2 2.0891(18) 2_656 ? Co1 N2 2.207(2) . ? Co1 N2 2.207(2) 2_656 ? Co2 O7 2.0648(19) . ? Co2 O7 2.0648(19) 2_755 ? Co2 N1 2.145(2) 2_755 ? Co2 N1 2.145(2) . ? Co2 O5 2.1510(18) . ? Co2 O5 2.1510(18) 2_755 ? O1 C6 1.378(3) . ? O1 C7 1.432(3) . ? O3 C11 1.283(3) . ? O2 C11 1.254(3) . ? N1 C8 1.357(3) . ? N1 C9 1.362(3) . ? C11 C10 1.467(3) . ? C3 C2 1.379(4) . ? C3 C4 1.405(3) . ? C9 C10 1.380(3) . ? C9 C12 1.464(3) . ? C10 N2 1.364(3) . ? C5 C4 1.392(3) . ? C5 C6 1.400(4) . ? C6 C1 1.390(4) . ? C8 N2 1.355(3) . ? C8 C4 1.471(3) . ? C1 C2 1.393(4) . ? O5 C12 1.253(3) . ? O4 C12 1.285(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Co1 O6 180.0 . 2_656 ? O6 Co1 O2 89.99(8) . . ? O6 Co1 O2 90.01(8) 2_656 . ? O6 Co1 O2 90.01(8) . 2_656 ? O6 Co1 O2 89.99(8) 2_656 2_656 ? O2 Co1 O2 180.0 . 2_656 ? O6 Co1 N2 90.91(8) . . ? O6 Co1 N2 89.09(8) 2_656 . ? O2 Co1 N2 79.81(7) . . ? O2 Co1 N2 100.19(7) 2_656 . ? O6 Co1 N2 89.09(8) . 2_656 ? O6 Co1 N2 90.91(8) 2_656 2_656 ? O2 Co1 N2 100.19(7) . 2_656 ? O2 Co1 N2 79.81(7) 2_656 2_656 ? N2 Co1 N2 180.000(1) . 2_656 ? O7 Co2 O7 180.00(10) . 2_755 ? O7 Co2 N1 88.17(8) . 2_755 ? O7 Co2 N1 91.83(8) 2_755 2_755 ? O7 Co2 N1 91.83(8) . . ? O7 Co2 N1 88.17(8) 2_755 . ? N1 Co2 N1 180.00(9) 2_755 . ? O7 Co2 O5 92.28(7) . . ? O7 Co2 O5 87.72(7) 2_755 . ? N1 Co2 O5 101.36(7) 2_755 . ? N1 Co2 O5 78.64(7) . . ? O7 Co2 O5 87.72(7) . 2_755 ? O7 Co2 O5 92.28(7) 2_755 2_755 ? N1 Co2 O5 78.64(7) 2_755 2_755 ? N1 Co2 O5 101.36(7) . 2_755 ? O5 Co2 O5 180.00(11) . 2_755 ? C6 O1 C7 117.4(2) . . ? C11 O2 Co1 114.71(16) . . ? C8 N1 C9 104.8(2) . . ? C8 N1 Co2 145.18(17) . . ? C9 N1 Co2 107.41(15) . . ? O2 C11 O3 123.1(2) . . ? O2 C11 C10 118.7(2) . . ? O3 C11 C10 118.3(2) . . ? C2 C3 C4 120.2(2) . . ? N1 C9 C10 108.5(2) . . ? N1 C9 C12 119.0(2) . . ? C10 C9 C12 132.4(2) . . ? N2 C10 C9 109.2(2) . . ? N2 C10 C11 120.3(2) . . ? C9 C10 C11 130.4(2) . . ? C4 C5 C6 119.5(2) . . ? O1 C6 C1 123.2(2) . . ? O1 C6 C5 115.6(2) . . ? C1 C6 C5 121.2(2) . . ? N2 C8 N1 113.1(2) . . ? N2 C8 C4 126.3(2) . . ? N1 C8 C4 120.4(2) . . ? C5 C4 C3 119.4(2) . . ? C5 C4 C8 122.8(2) . . ? C3 C4 C8 117.8(2) . . ? C6 C1 C2 118.6(2) . . ? C3 C2 C1 121.1(2) . . ? C12 O5 Co2 111.46(15) . . ? C8 N2 C10 104.33(19) . . ? C8 N2 Co1 149.10(17) . . ? C10 N2 Co1 106.20(15) . . ? O5 C12 O4 121.7(2) . . ? O5 C12 C9 118.4(2) . . ? O4 C12 C9 119.9(2) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 28.25 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.747 _refine_diff_density_min -0.636 _refine_diff_density_rms 0.092