# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # 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_201107b _database_code_depnum_ccdc_archive 'CCDC 855100' #TrackingRef '18.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C11 H12 Mn N2 O8' _chemical_formula_weight 355.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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 8.9885(3) _cell_length_b 18.7361(6) _cell_length_c 7.8637(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.878(3) _cell_angle_gamma 90.00 _cell_volume 1308.46(8) _cell_formula_units_Z 4 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 3205 _cell_measurement_theta_min 3.1545 _cell_measurement_theta_max 29.1579 _exptl_crystal_description prismatic _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.803 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 724 _exptl_absorpt_coefficient_mu 1.056 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8166 _exptl_absorpt_correction_T_max 0.8409 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(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 'Xcalibur, Eos, Gemini' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5788 _diffrn_reflns_av_R_equivalents 0.0240 _diffrn_reflns_av_sigmaI/netI 0.0346 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.16 _diffrn_reflns_theta_max 26.37 _reflns_number_total 2670 _reflns_number_gt 2329 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0316P)^2^+0.4743P] 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 2670 _refine_ls_number_parameters 220 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0382 _refine_ls_R_factor_gt 0.0314 _refine_ls_wR_factor_ref 0.0766 _refine_ls_wR_factor_gt 0.0727 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.079 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.58625(4) 0.373459(16) 0.29313(4) 0.01870(11) Uani 1 1 d D . . O1 O 0.7235(2) 0.05000(8) 0.30592(18) 0.0328(4) Uani 1 1 d . . . O2 O 0.66732(18) 0.07500(8) 0.02872(17) 0.0269(4) Uani 1 1 d . . . O3 O 0.50193(16) 0.31659(8) 0.05326(17) 0.0232(3) Uani 1 1 d . . . O4 O 0.48887(16) 0.20700(8) -0.05756(17) 0.0226(3) Uani 1 1 d . . . O5 O 1.3356(2) 0.39678(9) 0.8088(2) 0.0382(4) Uani 1 1 d . . . H5 H 1.3832 0.3682 0.8751 0.057 Uiso 1 1 calc R . . O6 O 0.6698(3) 0.45615(9) 0.1431(2) 0.0455(5) Uani 1 1 d D . . O7 O 0.3570(2) 0.41744(10) 0.2816(2) 0.0349(4) Uani 1 1 d D . . O8 O 1.0519(3) 0.42520(12) 0.0328(3) 0.0679(7) Uani 1 1 d D . . N1 N 0.76276(18) 0.28820(9) 0.26480(19) 0.0178(4) Uani 1 1 d . . . N2 N 0.86370(19) 0.18479(9) 0.35222(19) 0.0183(4) Uani 1 1 d . . . H2 H 0.9219 0.1541 0.4105 0.022 Uiso 1 1 calc R . . C1 C 1.0990(2) 0.25446(11) 0.5967(3) 0.0221(4) Uani 1 1 d . . . H1 H 1.0909 0.2050 0.6001 0.026 Uiso 1 1 calc R . . C2 C 1.2129(2) 0.28795(12) 0.7050(3) 0.0231(5) Uani 1 1 d . . . H2A H 1.2811 0.2612 0.7802 0.028 Uiso 1 1 calc R . . C3 C 1.2256(2) 0.36150(12) 0.7014(3) 0.0236(5) Uani 1 1 d . . . C4 C 1.1254(3) 0.40151(12) 0.5852(3) 0.0280(5) Uani 1 1 d . . . H4 H 1.1349 0.4509 0.5810 0.034 Uiso 1 1 calc R . . C5 C 1.0122(2) 0.36708(12) 0.4767(3) 0.0237(5) Uani 1 1 d . . . H5A H 0.9460 0.3936 0.3987 0.028 Uiso 1 1 calc R . . C6 C 0.9957(2) 0.29323(11) 0.4822(2) 0.0175(4) Uani 1 1 d . . . C7 C 0.8743(2) 0.25685(11) 0.3693(2) 0.0172(4) Uani 1 1 d . . . C8 C 0.7074(2) 0.09275(11) 0.1824(2) 0.0200(4) Uani 1 1 d . . . C9 C 0.7445(2) 0.16901(11) 0.2264(2) 0.0172(4) Uani 1 1 d . . . C10 C 0.6832(2) 0.23380(10) 0.1729(2) 0.0162(4) Uani 1 1 d . . . C11 C 0.5480(2) 0.25253(11) 0.0470(2) 0.0174(4) Uani 1 1 d . . . H6A H 0.684(3) 0.4512(10) 0.0399(15) 0.026 Uiso 1 1 d D . . H6B H 0.658(3) 0.5005(5) 0.157(2) 0.026 Uiso 1 1 d D . . H8B H 1.1419(12) 0.4266(13) 0.076(3) 0.026 Uiso 1 1 d D . . H8A H 0.998(2) 0.4556(11) 0.071(3) 0.026 Uiso 1 1 d D . . H7B H 0.339(4) 0.4613(19) 0.264(4) 0.061(10) Uiso 1 1 d . . . H7A H 0.324(4) 0.407(2) 0.375(3) 0.078(12) Uiso 1 1 d 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 Mn1 0.02565(19) 0.01466(17) 0.01465(17) -0.00054(11) -0.00052(12) 0.00136(13) O1 0.0586(11) 0.0193(8) 0.0184(7) 0.0033(6) -0.0008(7) -0.0061(8) O2 0.0442(9) 0.0177(8) 0.0162(7) -0.0015(6) -0.0037(6) -0.0017(7) O3 0.0282(8) 0.0183(8) 0.0201(7) -0.0035(6) -0.0061(6) 0.0063(7) O4 0.0220(7) 0.0215(8) 0.0221(7) -0.0073(6) -0.0039(6) 0.0017(6) O5 0.0385(10) 0.0238(9) 0.0427(10) -0.0008(7) -0.0240(8) -0.0036(8) O6 0.0938(16) 0.0211(9) 0.0256(9) -0.0011(7) 0.0220(10) -0.0098(10) O7 0.0393(10) 0.0258(10) 0.0406(10) 0.0070(8) 0.0094(8) 0.0110(8) O8 0.0619(15) 0.0396(13) 0.0890(17) -0.0131(11) -0.0304(13) -0.0018(12) N1 0.0185(8) 0.0178(9) 0.0163(8) -0.0011(6) 0.0006(7) 0.0001(7) N2 0.0209(9) 0.0168(9) 0.0153(8) 0.0015(6) -0.0028(7) 0.0014(7) C1 0.0244(11) 0.0170(10) 0.0234(10) -0.0018(8) -0.0007(8) 0.0028(9) C2 0.0207(10) 0.0240(12) 0.0218(10) 0.0019(8) -0.0053(8) 0.0002(9) C3 0.0199(11) 0.0254(12) 0.0230(11) -0.0020(8) -0.0042(9) -0.0023(9) C4 0.0305(12) 0.0177(11) 0.0326(12) 0.0004(9) -0.0052(10) -0.0006(10) C5 0.0209(11) 0.0248(12) 0.0225(11) 0.0026(8) -0.0059(9) 0.0023(9) C6 0.0161(9) 0.0198(10) 0.0159(9) -0.0021(8) 0.0008(7) -0.0006(9) C7 0.0187(10) 0.0182(10) 0.0143(9) -0.0032(7) 0.0015(8) 0.0011(8) C8 0.0229(10) 0.0177(10) 0.0189(10) 0.0022(8) 0.0014(8) 0.0011(9) C9 0.0184(10) 0.0193(11) 0.0134(9) -0.0003(7) 0.0004(7) -0.0015(9) C10 0.0183(10) 0.0170(10) 0.0130(9) -0.0021(7) 0.0012(7) -0.0011(8) C11 0.0184(10) 0.0200(10) 0.0138(9) -0.0008(8) 0.0025(8) 0.0006(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 Mn1 O2 2.1164(14) 4_566 ? Mn1 O6 2.1516(17) . ? Mn1 O4 2.1759(14) 4_566 ? Mn1 O3 2.1969(13) . ? Mn1 O7 2.2081(18) . ? Mn1 N1 2.2865(17) . ? O1 C8 1.250(2) . ? O2 C8 1.251(2) . ? O2 Mn1 2.1164(14) 4_565 ? O3 C11 1.273(2) . ? O4 C11 1.245(2) . ? O4 Mn1 2.1759(14) 4_565 ? O5 C3 1.367(2) . ? O5 H5 0.8200 . ? O6 H6A 0.845(9) . ? O6 H6B 0.847(9) . ? O7 H7B 0.84(3) . ? O7 H7A 0.854(18) . ? O8 H8B 0.828(9) . ? O8 H8A 0.833(9) . ? N1 C7 1.331(2) . ? N1 C10 1.383(2) . ? N2 C7 1.359(3) . ? N2 C9 1.374(2) . ? N2 H2 0.8600 . ? C1 C2 1.378(3) . ? C1 C6 1.394(3) . ? C1 H1 0.9300 . ? C2 C3 1.383(3) . ? C2 H2A 0.9300 . ? C3 C4 1.397(3) . ? C4 C5 1.383(3) . ? C4 H4 0.9300 . ? C5 C6 1.393(3) . ? C5 H5A 0.9300 . ? C6 C7 1.464(3) . ? C8 C9 1.496(3) . ? C9 C10 1.372(3) . ? C10 C11 1.487(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 O2 Mn1 O6 92.83(6) 4_566 . ? O2 Mn1 O4 87.51(6) 4_566 4_566 ? O6 Mn1 O4 176.60(7) . 4_566 ? O2 Mn1 O3 178.09(5) 4_566 . ? O6 Mn1 O3 88.96(6) . . ? O4 Mn1 O3 90.75(5) 4_566 . ? O2 Mn1 O7 93.36(7) 4_566 . ? O6 Mn1 O7 96.39(8) . . ? O4 Mn1 O7 80.21(6) 4_566 . ? O3 Mn1 O7 87.12(6) . . ? O2 Mn1 N1 104.70(6) 4_566 . ? O6 Mn1 N1 98.26(7) . . ? O4 Mn1 N1 84.92(6) 4_566 . ? O3 Mn1 N1 74.34(5) . . ? O7 Mn1 N1 156.05(7) . . ? C8 O2 Mn1 137.13(14) . 4_565 ? C11 O3 Mn1 114.81(11) . . ? C11 O4 Mn1 131.66(13) . 4_565 ? C3 O5 H5 109.5 . . ? Mn1 O6 H6A 124.3(13) . . ? Mn1 O6 H6B 125.1(13) . . ? H6A O6 H6B 105.6(17) . . ? Mn1 O7 H7B 121(2) . . ? Mn1 O7 H7A 109(2) . . ? H7B O7 H7A 107(3) . . ? H8B O8 H8A 114.6(19) . . ? C7 N1 C10 106.09(17) . . ? C7 N1 Mn1 135.74(13) . . ? C10 N1 Mn1 104.78(12) . . ? C7 N2 C9 108.68(16) . . ? C7 N2 H2 125.7 . . ? C9 N2 H2 125.7 . . ? C2 C1 C6 121.3(2) . . ? C2 C1 H1 119.4 . . ? C6 C1 H1 119.4 . . ? C1 C2 C3 119.79(19) . . ? C1 C2 H2A 120.1 . . ? C3 C2 H2A 120.1 . . ? O5 C3 C2 121.52(19) . . ? O5 C3 C4 118.4(2) . . ? C2 C3 C4 120.06(19) . . ? C5 C4 C3 119.5(2) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? C4 C5 C6 121.04(19) . . ? C4 C5 H5A 119.5 . . ? C6 C5 H5A 119.5 . . ? C5 C6 C1 118.32(18) . . ? C5 C6 C7 121.08(18) . . ? C1 C6 C7 120.59(19) . . ? N1 C7 N2 110.03(17) . . ? N1 C7 C6 126.07(19) . . ? N2 C7 C6 123.86(18) . . ? O1 C8 O2 124.2(2) . . ? O1 C8 C9 115.95(17) . . ? O2 C8 C9 119.85(17) . . ? C10 C9 N2 105.19(17) . . ? C10 C9 C8 135.23(18) . . ? N2 C9 C8 119.55(17) . . ? C9 C10 N1 109.94(16) . . ? C9 C10 C11 131.41(18) . . ? N1 C10 C11 118.54(17) . . ? O4 C11 O3 124.30(18) . . ? O4 C11 C10 119.97(18) . . ? O3 C11 C10 115.72(16) . . ? 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 Mn1 O3 C11 -33.8(19) 4_566 . . . ? O6 Mn1 O3 C11 125.13(15) . . . . ? O4 Mn1 O3 C11 -58.26(14) 4_566 . . . ? O7 Mn1 O3 C11 -138.42(15) . . . . ? N1 Mn1 O3 C11 26.25(14) . . . . ? O2 Mn1 N1 C7 17.0(2) 4_566 . . . ? O6 Mn1 N1 C7 112.1(2) . . . . ? O4 Mn1 N1 C7 -69.11(19) 4_566 . . . ? O3 Mn1 N1 C7 -161.3(2) . . . . ? O7 Mn1 N1 C7 -120.8(2) . . . . ? O2 Mn1 N1 C10 149.92(11) 4_566 . . . ? O6 Mn1 N1 C10 -114.95(12) . . . . ? O4 Mn1 N1 C10 63.83(12) 4_566 . . . ? O3 Mn1 N1 C10 -28.37(12) . . . . ? O7 Mn1 N1 C10 12.2(2) . . . . ? C6 C1 C2 C3 0.3(3) . . . . ? C1 C2 C3 O5 178.9(2) . . . . ? C1 C2 C3 C4 -1.7(3) . . . . ? O5 C3 C4 C5 -179.3(2) . . . . ? C2 C3 C4 C5 1.3(3) . . . . ? C3 C4 C5 C6 0.5(3) . . . . ? C4 C5 C6 C1 -1.8(3) . . . . ? C4 C5 C6 C7 179.0(2) . . . . ? C2 C1 C6 C5 1.5(3) . . . . ? C2 C1 C6 C7 -179.38(18) . . . . ? C10 N1 C7 N2 -2.8(2) . . . . ? Mn1 N1 C7 N2 129.75(17) . . . . ? C10 N1 C7 C6 174.89(18) . . . . ? Mn1 N1 C7 C6 -52.6(3) . . . . ? C9 N2 C7 N1 2.7(2) . . . . ? C9 N2 C7 C6 -175.05(17) . . . . ? C5 C6 C7 N1 -6.4(3) . . . . ? C1 C6 C7 N1 174.50(18) . . . . ? C5 C6 C7 N2 171.0(2) . . . . ? C1 C6 C7 N2 -8.1(3) . . . . ? Mn1 O2 C8 O1 165.07(17) 4_565 . . . ? Mn1 O2 C8 C9 -17.1(3) 4_565 . . . ? C7 N2 C9 C10 -1.4(2) . . . . ? C7 N2 C9 C8 -179.71(17) . . . . ? O1 C8 C9 C10 -140.3(2) . . . . ? O2 C8 C9 C10 41.7(3) . . . . ? O1 C8 C9 N2 37.4(3) . . . . ? O2 C8 C9 N2 -140.6(2) . . . . ? N2 C9 C10 N1 -0.3(2) . . . . ? C8 C9 C10 N1 177.6(2) . . . . ? N2 C9 C10 C11 -176.42(19) . . . . ? C8 C9 C10 C11 1.5(4) . . . . ? C7 N1 C10 C9 1.9(2) . . . . ? Mn1 N1 C10 C9 -145.96(13) . . . . ? C7 N1 C10 C11 178.59(16) . . . . ? Mn1 N1 C10 C11 30.72(19) . . . . ? Mn1 O4 C11 O3 138.17(17) 4_565 . . . ? Mn1 O4 C11 C10 -40.5(3) 4_565 . . . ? Mn1 O3 C11 O4 163.24(15) . . . . ? Mn1 O3 C11 C10 -18.0(2) . . . . ? C9 C10 C11 O4 -16.1(3) . . . . ? N1 C10 C11 O4 168.04(17) . . . . ? C9 C10 C11 O3 165.0(2) . . . . ? N1 C10 C11 O3 -10.8(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 O5 H5 O3 0.82 1.89 2.702(2) 169.8 1_656 N2 H2 O8 0.86 2.04 2.896(3) 174.8 4_566 O6 H6A O1 0.845(9) 1.928(10) 2.770(2) 174.0(18) 4_565 O6 H6B O5 0.847(9) 1.943(10) 2.783(2) 171(2) 3_766 O8 H8B O7 0.828(9) 2.327(13) 3.117(3) 160(2) 1_655 O8 H8A O8 0.833(9) 2.40(2) 2.974(5) 127(2) 3_765 O7 H7B O1 0.84(3) 1.81(3) 2.648(2) 169(3) 2_655 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.312 _refine_diff_density_min -0.445 _refine_diff_density_rms 0.060 data_y _database_code_depnum_ccdc_archive 'CCDC 855101' #TrackingRef '32.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C11 H8 N2 O5 Sr' _chemical_formula_weight 335.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 14.030(9) _cell_length_b 6.614(4) _cell_length_c 12.613(8) _cell_angle_alpha 90.00 _cell_angle_beta 103.620(8) _cell_angle_gamma 90.00 _cell_volume 1137.6(13) _cell_formula_units_Z 4 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 3000 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25.2 _exptl_crystal_description prismatic _exptl_crystal_colour ? _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.961 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 664 _exptl_absorpt_coefficient_mu 4.759 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4208 _exptl_absorpt_correction_T_max 0.4813 _exptl_absorpt_process_details SADABS(2009) _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(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 P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8016 _diffrn_reflns_av_R_equivalents 0.0932 _diffrn_reflns_av_sigmaI/netI 0.0883 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 25.50 _reflns_number_total 2109 _reflns_number_gt 1478 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SAINT v7.53A (Bruker, 2008)' _computing_cell_refinement 'SAINT v7.53A (Bruker, 2008)' _computing_data_reduction 'SAINT v7.53A (Bruker, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0917P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2109 _refine_ls_number_parameters 175 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0964 _refine_ls_R_factor_gt 0.0572 _refine_ls_wR_factor_ref 0.1498 _refine_ls_wR_factor_gt 0.1367 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.008 _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 Sr1 Sr 0.47257(5) 0.06587(9) 0.16225(5) 0.0126(2) Uani 1 1 d . . . O2 O 0.5853(4) -0.3660(7) 0.5400(4) 0.0211(12) Uani 1 1 d . . . O3 O 0.5282(3) -0.0660(7) 0.3704(4) 0.0146(11) Uani 1 1 d . . . O4 O 0.5998(4) 0.2150(7) 0.3379(3) 0.0158(11) Uani 1 1 d . . . N1 N 0.7307(4) 0.0353(8) 0.6851(4) 0.0136(13) Uani 1 1 d . . . O5 O 0.2686(4) 0.0752(8) 0.1016(4) 0.0242(12) Uani 1 1 d D . . H5A H 0.3028 0.1377 0.1564 0.029 Uiso 1 1 d RD . . O1 O 0.6150(4) -0.2846(7) 0.7130(4) 0.0186(11) Uani 1 1 d . . . N2 N 0.7158(4) 0.2326(8) 0.5419(4) 0.0154(13) Uani 1 1 d . . . H2 H 0.7236 0.3340 0.5022 0.018 Uiso 1 1 calc R . . C1 C 0.6204(5) -0.2492(10) 0.6173(5) 0.0106(15) Uani 1 1 d . . . C2 C 0.6693(5) -0.0556(10) 0.5981(5) 0.0138(15) Uani 1 1 d . . . C3 C 0.6585(5) 0.0649(10) 0.5071(5) 0.0124(14) Uani 1 1 d . . . C4 C 0.5915(5) 0.0693(10) 0.3988(5) 0.0128(15) Uani 1 1 d . . . C5 C 0.7573(5) 0.2103(11) 0.6488(5) 0.0150(15) Uani 1 1 d . . . C6 C 0.8198(5) 0.3627(11) 0.7136(6) 0.0161(16) Uani 1 1 d . . . C7 C 0.8626(6) 0.5155(12) 0.6655(7) 0.031(2) Uani 1 1 d . . . H7 H 0.8542 0.5185 0.5902 0.038 Uiso 1 1 calc R . . C8 C 0.9176(6) 0.6631(13) 0.7290(7) 0.038(2) Uani 1 1 d . . . H8 H 0.9454 0.7660 0.6960 0.046 Uiso 1 1 calc R . . C9 C 0.9318(6) 0.6598(14) 0.8399(8) 0.042(2) Uani 1 1 d . . . H9 H 0.9687 0.7603 0.8822 0.051 Uiso 1 1 calc R . . C10 C 0.8918(7) 0.5093(14) 0.8876(8) 0.041(2) Uani 1 1 d . . . H10 H 0.9022 0.5055 0.9632 0.050 Uiso 1 1 calc R . . C11 C 0.8356(5) 0.3609(13) 0.8251(6) 0.029(2) Uani 1 1 d . . . H11 H 0.8081 0.2589 0.8591 0.034 Uiso 1 1 calc R . . H5B H 0.308(2) 0.035(11) 0.064(4) 0.034 Uiso 1 1 d 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 0.0237(4) 0.0048(3) 0.0077(3) 0.0001(3) 0.0001(2) 0.0007(3) O2 0.043(3) 0.008(2) 0.010(3) -0.001(2) 0.003(2) -0.009(2) O3 0.023(3) 0.010(2) 0.009(2) 0.001(2) 0.000(2) -0.002(2) O4 0.026(3) 0.005(2) 0.016(3) 0.004(2) 0.004(2) 0.006(2) N1 0.012(3) 0.016(3) 0.010(3) 0.002(2) -0.002(2) -0.001(3) O5 0.027(3) 0.028(3) 0.017(3) -0.010(2) 0.004(2) -0.001(3) O1 0.030(3) 0.014(2) 0.012(2) 0.003(2) 0.005(2) -0.004(2) N2 0.017(3) 0.013(3) 0.013(3) 0.005(2) -0.002(2) -0.005(3) C1 0.008(4) 0.013(4) 0.009(3) 0.000(3) -0.001(3) 0.003(3) C2 0.024(4) 0.011(4) 0.006(3) -0.001(3) 0.003(3) 0.004(3) C3 0.010(4) 0.010(3) 0.017(4) -0.007(3) 0.005(3) 0.001(3) C4 0.015(4) 0.009(3) 0.014(4) -0.003(3) 0.001(3) 0.002(3) C5 0.011(4) 0.018(4) 0.015(4) 0.000(3) 0.000(3) -0.003(3) C6 0.006(4) 0.016(4) 0.022(4) -0.003(3) -0.006(3) 0.000(3) C7 0.031(5) 0.026(4) 0.030(5) 0.005(4) -0.005(4) -0.008(4) C8 0.033(5) 0.028(5) 0.048(6) -0.001(4) 0.000(4) -0.014(4) C9 0.025(5) 0.039(5) 0.056(6) -0.015(5) -0.004(4) -0.015(5) C10 0.039(6) 0.048(6) 0.030(5) -0.015(4) -0.006(4) -0.014(5) C11 0.017(5) 0.038(5) 0.028(5) -0.007(4) 0.001(4) -0.015(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 Sr1 O3 2.469(5) 2_655 ? Sr1 O2 2.528(5) 2_655 ? Sr1 O4 2.533(5) 2_645 ? Sr1 O1 2.643(5) 3_656 ? Sr1 O4 2.685(5) . ? Sr1 O1 2.695(5) 4 ? Sr1 O3 2.702(5) . ? Sr1 O5 2.784(6) . ? Sr1 O2 2.789(5) 4 ? Sr1 C4 3.057(7) . ? Sr1 C1 3.093(7) 4 ? Sr1 Sr1 3.953(2) 2_655 ? Sr1 H5A 2.4135 . ? Sr1 H5B 2.37(4) . ? O2 C1 1.251(8) . ? O2 Sr1 2.528(5) 2_645 ? O2 Sr1 2.789(5) 4_556 ? O3 C4 1.253(8) . ? O3 Sr1 2.469(5) 2_645 ? O4 C4 1.255(8) . ? O4 Sr1 2.533(5) 2_655 ? N1 C5 1.329(9) . ? N1 C2 1.365(8) . ? O5 H5A 0.8506 . ? O5 H5B 0.850(10) . ? O1 C1 1.251(8) . ? O1 Sr1 2.643(5) 3_656 ? O1 Sr1 2.695(5) 4_556 ? N2 C5 1.345(8) . ? N2 C3 1.379(8) . ? N2 H2 0.8600 . ? C1 C2 1.499(9) . ? C1 Sr1 3.093(7) 4_556 ? C2 C3 1.376(9) . ? C3 C4 1.464(9) . ? C5 C6 1.455(9) . ? C6 C11 1.372(10) . ? C6 C7 1.386(11) . ? C7 C8 1.378(11) . ? C7 H7 0.9300 . ? C8 C9 1.365(12) . ? C8 H8 0.9300 . ? C9 C10 1.352(13) . ? C9 H9 0.9300 . ? C10 C11 1.384(11) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Sr1 O2 70.61(15) 2_655 2_655 ? O3 Sr1 O4 156.55(16) 2_655 2_645 ? O2 Sr1 O4 97.42(15) 2_655 2_645 ? O3 Sr1 O1 64.87(15) 2_655 3_656 ? O2 Sr1 O1 114.77(15) 2_655 3_656 ? O4 Sr1 O1 105.04(15) 2_645 3_656 ? O3 Sr1 O4 75.59(14) 2_655 . ? O2 Sr1 O4 139.47(16) 2_655 . ? O4 Sr1 O4 121.74(13) 2_645 . ? O1 Sr1 O4 67.65(15) 3_656 . ? O3 Sr1 O1 133.96(16) 2_655 4 ? O2 Sr1 O1 114.01(15) 2_655 4 ? O4 Sr1 O1 69.05(16) 2_645 4 ? O1 Sr1 O1 131.22(8) 3_656 4 ? O4 Sr1 O1 75.27(14) . 4 ? O3 Sr1 O3 118.00(13) 2_655 . ? O2 Sr1 O3 171.36(14) 2_655 . ? O4 Sr1 O3 74.28(14) 2_645 . ? O1 Sr1 O3 70.52(15) 3_656 . ? O4 Sr1 O3 48.15(14) . . ? O1 Sr1 O3 61.18(14) 4 . ? O3 Sr1 O5 88.21(16) 2_655 . ? O2 Sr1 O5 69.74(16) 2_655 . ? O4 Sr1 O5 68.52(15) 2_645 . ? O1 Sr1 O5 63.88(15) 3_656 . ? O4 Sr1 O5 131.28(14) . . ? O1 Sr1 O5 137.51(16) 4 . ? O3 Sr1 O5 108.49(15) . . ? O3 Sr1 O2 110.85(15) 2_655 4 ? O2 Sr1 O2 67.39(18) 2_655 4 ? O4 Sr1 O2 81.06(15) 2_645 4 ? O1 Sr1 O2 172.85(15) 3_656 4 ? O4 Sr1 O2 106.10(15) . 4 ? O1 Sr1 O2 47.07(14) 4 4 ? O3 Sr1 O2 108.25(14) . 4 ? O5 Sr1 O2 122.58(15) . 4 ? O3 Sr1 C4 97.79(16) 2_655 . ? O2 Sr1 C4 162.77(18) 2_655 . ? O4 Sr1 C4 97.72(16) 2_645 . ? O1 Sr1 C4 68.81(17) 3_656 . ? O4 Sr1 C4 24.15(16) . . ? O1 Sr1 C4 64.48(16) 4 . ? O3 Sr1 C4 24.13(16) . . ? O5 Sr1 C4 123.91(17) . . ? O2 Sr1 C4 107.04(16) 4 . ? O3 Sr1 C1 127.86(16) 2_655 4 ? O2 Sr1 C1 90.31(17) 2_655 4 ? O4 Sr1 C1 70.47(17) 2_645 4 ? O1 Sr1 C1 154.91(15) 3_656 4 ? O4 Sr1 C1 93.20(16) . 4 ? O1 Sr1 C1 23.69(15) 4 4 ? O3 Sr1 C1 84.67(15) . 4 ? O5 Sr1 C1 130.92(16) . 4 ? O2 Sr1 C1 23.84(14) 4 4 ? C4 Sr1 C1 87.05(17) . 4 ? O3 Sr1 Sr1 42.36(11) 2_655 2_655 ? O2 Sr1 Sr1 112.93(11) 2_655 2_655 ? O4 Sr1 Sr1 142.38(11) 2_645 2_655 ? O1 Sr1 Sr1 42.72(11) 3_656 2_655 ? O4 Sr1 Sr1 39.33(10) . 2_655 ? O1 Sr1 Sr1 114.13(11) 4 2_655 ? O3 Sr1 Sr1 75.65(10) . 2_655 ? O5 Sr1 Sr1 100.81(10) . 2_655 ? O2 Sr1 Sr1 130.20(11) 4 2_655 ? C4 Sr1 Sr1 57.16(13) . 2_655 ? C1 Sr1 Sr1 128.22(12) 4 2_655 ? O3 Sr1 H5A 80.5 2_655 . ? O2 Sr1 H5A 81.6 2_655 . ? O4 Sr1 H5A 77.7 2_645 . ? O1 Sr1 H5A 46.9 3_656 . ? O4 Sr1 H5A 114.4 . . ? O1 Sr1 H5A 144.6 4 . ? O3 Sr1 H5A 98.6 . . ? O5 Sr1 H5A 17.0 . . ? O2 Sr1 H5A 139.5 4 . ? C4 Sr1 H5A 109.7 . . ? C1 Sr1 H5A 145.9 4 . ? Sr1 Sr1 H5A 85.0 2_655 . ? O3 Sr1 H5B 91.9(19) 2_655 . ? O2 Sr1 H5B 56.1(14) 2_655 . ? O4 Sr1 H5B 65(2) 2_645 . ? O1 Sr1 H5B 80.0(5) 3_656 . ? O4 Sr1 H5B 147.6(4) . . ? O1 Sr1 H5B 130.1(16) 4 . ? O3 Sr1 H5B 120.4(16) . . ? O5 Sr1 H5B 16.6(4) . . ? O2 Sr1 H5B 106.3(4) 4 . ? C4 Sr1 H5B 139.1(11) . . ? C1 Sr1 H5B 117.4(10) 4 . ? Sr1 Sr1 H5B 113.8(12) 2_655 . ? H5A Sr1 H5B 33.3 . . ? C1 O2 Sr1 150.5(4) . 2_645 ? C1 O2 Sr1 91.9(4) . 4_556 ? Sr1 O2 Sr1 112.61(18) 2_645 4_556 ? C4 O3 Sr1 136.6(4) . 2_645 ? C4 O3 Sr1 94.0(4) . . ? Sr1 O3 Sr1 99.62(15) 2_645 . ? C4 O4 Sr1 127.5(4) . 2_655 ? C4 O4 Sr1 94.8(4) . . ? Sr1 O4 Sr1 98.47(15) 2_655 . ? C5 N1 C2 106.4(6) . . ? Sr1 O5 H5A 56.0 . . ? Sr1 O5 H5B 53(3) . . ? H5A O5 H5B 107.2 . . ? C1 O1 Sr1 128.0(4) . 3_656 ? C1 O1 Sr1 96.3(4) . 4_556 ? Sr1 O1 Sr1 95.56(16) 3_656 4_556 ? C5 N2 C3 108.3(6) . . ? C5 N2 H2 125.8 . . ? C3 N2 H2 125.8 . . ? O1 C1 O2 122.3(6) . . ? O1 C1 C2 116.8(6) . . ? O2 C1 C2 120.9(6) . . ? O1 C1 Sr1 60.0(3) . 4_556 ? O2 C1 Sr1 64.3(4) . 4_556 ? C2 C1 Sr1 163.8(5) . 4_556 ? N1 C2 C3 109.9(6) . . ? N1 C2 C1 118.2(6) . . ? C3 C2 C1 131.6(6) . . ? C2 C3 N2 104.9(6) . . ? C2 C3 C4 135.2(6) . . ? N2 C3 C4 118.6(6) . . ? O3 C4 O4 122.4(6) . . ? O3 C4 C3 120.6(6) . . ? O4 C4 C3 117.0(6) . . ? O3 C4 Sr1 61.8(3) . . ? O4 C4 Sr1 61.1(3) . . ? C3 C4 Sr1 173.3(5) . . ? N1 C5 N2 110.5(6) . . ? N1 C5 C6 126.2(6) . . ? N2 C5 C6 123.3(6) . . ? C11 C6 C7 118.2(7) . . ? C11 C6 C5 120.0(7) . . ? C7 C6 C5 121.7(7) . . ? C8 C7 C6 120.2(8) . . ? C8 C7 H7 119.9 . . ? C6 C7 H7 119.9 . . ? C9 C8 C7 120.7(8) . . ? C9 C8 H8 119.6 . . ? C7 C8 H8 119.6 . . ? C10 C9 C8 119.5(8) . . ? C10 C9 H9 120.3 . . ? C8 C9 H9 120.3 . . ? C9 C10 C11 120.6(9) . . ? C9 C10 H10 119.7 . . ? C11 C10 H10 119.7 . . ? C6 C11 C10 120.7(8) . . ? C6 C11 H11 119.6 . . ? C10 C11 H11 119.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Sr1 O3 C4 -35.8(3) 2_655 . . . ? O2 Sr1 O3 C4 149.4(10) 2_655 . . . ? O4 Sr1 O3 C4 165.9(4) 2_645 . . . ? O1 Sr1 O3 C4 -81.5(4) 3_656 . . . ? O4 Sr1 O3 C4 -4.5(4) . . . . ? O1 Sr1 O3 C4 91.5(4) 4 . . . ? O5 Sr1 O3 C4 -133.8(4) . . . . ? O2 Sr1 O3 C4 91.1(4) 4 . . . ? C1 Sr1 O3 C4 94.7(4) 4 . . . ? Sr1 Sr1 O3 C4 -37.0(4) 2_655 . . . ? O3 Sr1 O3 Sr1 -174.4(2) 2_655 . . 2_645 ? O2 Sr1 O3 Sr1 10.8(11) 2_655 . . 2_645 ? O4 Sr1 O3 Sr1 27.19(16) 2_645 . . 2_645 ? O1 Sr1 O3 Sr1 139.87(19) 3_656 . . 2_645 ? O4 Sr1 O3 Sr1 -143.1(3) . . . 2_645 ? O1 Sr1 O3 Sr1 -47.20(16) 4 . . 2_645 ? O5 Sr1 O3 Sr1 87.50(17) . . . 2_645 ? O2 Sr1 O3 Sr1 -47.57(19) 4 . . 2_645 ? C4 Sr1 O3 Sr1 -138.7(5) . . . 2_645 ? C1 Sr1 O3 Sr1 -43.99(17) 4 . . 2_645 ? Sr1 Sr1 O3 Sr1 -175.69(16) 2_655 . . 2_645 ? O3 Sr1 O4 C4 156.2(4) 2_655 . . . ? O2 Sr1 O4 C4 -169.7(4) 2_655 . . . ? O4 Sr1 O4 C4 -6.5(4) 2_645 . . . ? O1 Sr1 O4 C4 87.8(4) 3_656 . . . ? O1 Sr1 O4 C4 -59.8(4) 4 . . . ? O3 Sr1 O4 C4 4.5(4) . . . . ? O5 Sr1 O4 C4 81.8(4) . . . . ? O2 Sr1 O4 C4 -95.8(4) 4 . . . ? C1 Sr1 O4 C4 -75.5(4) 4 . . . ? Sr1 Sr1 O4 C4 129.1(5) 2_655 . . . ? O3 Sr1 O4 Sr1 27.10(15) 2_655 . . 2_655 ? O2 Sr1 O4 Sr1 61.2(3) 2_655 . . 2_655 ? O4 Sr1 O4 Sr1 -135.6(2) 2_645 . . 2_655 ? O1 Sr1 O4 Sr1 -41.28(14) 3_656 . . 2_655 ? O1 Sr1 O4 Sr1 171.07(19) 4 . . 2_655 ? O3 Sr1 O4 Sr1 -124.6(2) . . . 2_655 ? O5 Sr1 O4 Sr1 -47.3(2) . . . 2_655 ? O2 Sr1 O4 Sr1 135.06(15) 4 . . 2_655 ? C4 Sr1 O4 Sr1 -129.1(5) . . . 2_655 ? C1 Sr1 O4 Sr1 155.44(17) 4 . . 2_655 ? Sr1 O1 C1 O2 -118.7(6) 3_656 . . . ? Sr1 O1 C1 O2 -16.5(7) 4_556 . . . ? Sr1 O1 C1 C2 59.8(7) 3_656 . . . ? Sr1 O1 C1 C2 161.9(5) 4_556 . . . ? Sr1 O1 C1 Sr1 -102.1(4) 3_656 . . 4_556 ? Sr1 O2 C1 O1 163.0(6) 2_645 . . . ? Sr1 O2 C1 O1 15.9(7) 4_556 . . . ? Sr1 O2 C1 C2 -15.4(13) 2_645 . . . ? Sr1 O2 C1 C2 -162.5(6) 4_556 . . . ? Sr1 O2 C1 Sr1 147.1(10) 2_645 . . 4_556 ? C5 N1 C2 C3 0.4(8) . . . . ? C5 N1 C2 C1 -174.7(6) . . . . ? O1 C1 C2 N1 20.6(9) . . . . ? O2 C1 C2 N1 -160.9(6) . . . . ? Sr1 C1 C2 N1 94.8(16) 4_556 . . . ? O1 C1 C2 C3 -153.2(7) . . . . ? O2 C1 C2 C3 25.3(11) . . . . ? Sr1 C1 C2 C3 -79.0(18) 4_556 . . . ? N1 C2 C3 N2 0.0(8) . . . . ? C1 C2 C3 N2 174.2(7) . . . . ? N1 C2 C3 C4 -166.7(7) . . . . ? C1 C2 C3 C4 7.5(14) . . . . ? C5 N2 C3 C2 -0.4(7) . . . . ? C5 N2 C3 C4 169.0(6) . . . . ? Sr1 O3 C4 O4 117.0(6) 2_645 . . . ? Sr1 O3 C4 O4 8.4(7) . . . . ? Sr1 O3 C4 C3 -64.2(9) 2_645 . . . ? Sr1 O3 C4 C3 -172.8(5) . . . . ? Sr1 O3 C4 Sr1 108.6(5) 2_645 . . . ? Sr1 O4 C4 O3 96.0(7) 2_655 . . . ? Sr1 O4 C4 O3 -8.5(7) . . . . ? Sr1 O4 C4 C3 -82.8(7) 2_655 . . . ? Sr1 O4 C4 C3 172.7(5) . . . . ? Sr1 O4 C4 Sr1 104.5(4) 2_655 . . . ? C2 C3 C4 O3 -4.0(12) . . . . ? N2 C3 C4 O3 -169.3(6) . . . . ? C2 C3 C4 O4 174.9(7) . . . . ? N2 C3 C4 O4 9.5(9) . . . . ? C2 C3 C4 Sr1 -113(4) . . . . ? N2 C3 C4 Sr1 81(4) . . . . ? O3 Sr1 C4 O3 148.6(3) 2_655 . . . ? O2 Sr1 C4 O3 -165.0(5) 2_655 . . . ? O4 Sr1 C4 O3 -13.7(4) 2_645 . . . ? O1 Sr1 C4 O3 89.5(4) 3_656 . . . ? O4 Sr1 C4 O3 171.9(7) . . . . ? O1 Sr1 C4 O3 -76.1(4) 4 . . . ? O5 Sr1 C4 O3 55.5(4) . . . . ? O2 Sr1 C4 O3 -96.7(4) 4 . . . ? C1 Sr1 C4 O3 -83.6(4) 4 . . . ? Sr1 Sr1 C4 O3 136.0(4) 2_655 . . . ? O3 Sr1 C4 O4 -23.2(4) 2_655 . . . ? O2 Sr1 C4 O4 23.1(8) 2_655 . . . ? O4 Sr1 C4 O4 174.4(3) 2_645 . . . ? O1 Sr1 C4 O4 -82.4(4) 3_656 . . . ? O1 Sr1 C4 O4 112.1(4) 4 . . . ? O3 Sr1 C4 O4 -171.9(7) . . . . ? O5 Sr1 C4 O4 -116.3(4) . . . . ? O2 Sr1 C4 O4 91.4(4) 4 . . . ? C1 Sr1 C4 O4 104.6(4) 4 . . . ? Sr1 Sr1 C4 O4 -35.8(3) 2_655 . . . ? O3 Sr1 C4 C3 -99(4) 2_655 . . . ? O2 Sr1 C4 C3 -52(4) 2_655 . . . ? O4 Sr1 C4 C3 99(4) 2_645 . . . ? O1 Sr1 C4 C3 -158(4) 3_656 . . . ? O4 Sr1 C4 C3 -75(4) . . . . ? O1 Sr1 C4 C3 37(4) 4 . . . ? O3 Sr1 C4 C3 113(4) . . . . ? O5 Sr1 C4 C3 168(4) . . . . ? O2 Sr1 C4 C3 16(4) 4 . . . ? C1 Sr1 C4 C3 29(4) 4 . . . ? Sr1 Sr1 C4 C3 -111(4) 2_655 . . . ? C2 N1 C5 N2 -0.6(8) . . . . ? C2 N1 C5 C6 177.6(7) . . . . ? C3 N2 C5 N1 0.6(8) . . . . ? C3 N2 C5 C6 -177.7(6) . . . . ? N1 C5 C6 C11 -17.8(11) . . . . ? N2 C5 C6 C11 160.3(7) . . . . ? N1 C5 C6 C7 164.1(8) . . . . ? N2 C5 C6 C7 -17.9(11) . . . . ? C11 C6 C7 C8 -1.3(12) . . . . ? C5 C6 C7 C8 176.9(7) . . . . ? C6 C7 C8 C9 0.8(14) . . . . ? C7 C8 C9 C10 0.4(15) . . . . ? C8 C9 C10 C11 -1.0(15) . . . . ? C7 C6 C11 C10 0.7(12) . . . . ? C5 C6 C11 C10 -177.5(8) . . . . ? C9 C10 C11 C6 0.5(14) . . . . ? 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 H5B N2 0.850(10) 2.38(4) 2.941(7) 124(4) 2_645 O5 H5B O2 0.850(10) 2.31(5) 3.044(7) 145(7) 2_655 O5 H5A O1 0.85 2.02 2.874(7) 179.5 3_656 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.686 _refine_diff_density_min -1.581 _refine_diff_density_rms 0.182 data_43 _database_code_depnum_ccdc_archive 'CCDC 855102' #TrackingRef '43.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C47 H30 Cd2 N8 O11' _chemical_formula_weight 1107.59 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 21.363(2) _cell_length_b 10.5184(11) _cell_length_c 20.465(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4598.6(9) _cell_formula_units_Z 4 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 678 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25.1 _exptl_crystal_description prismatic _exptl_crystal_colour ? _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.600 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2208 _exptl_absorpt_coefficient_mu 0.995 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7963 _exptl_absorpt_correction_T_max 0.8183 _exptl_absorpt_process_details SADABS(2009) _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(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 P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24625 _diffrn_reflns_av_R_equivalents 0.0472 _diffrn_reflns_av_sigmaI/netI 0.0616 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 26.39 _reflns_number_total 9315 _reflns_number_gt 6064 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction 'SAINT v7.53A (Bruker, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _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^)+(0.0707P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(3) _refine_ls_number_reflns 9315 _refine_ls_number_parameters 618 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0924 _refine_ls_R_factor_gt 0.0516 _refine_ls_wR_factor_ref 0.1391 _refine_ls_wR_factor_gt 0.1193 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _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 0.43227(2) 0.86061(5) 0.44756(2) 0.06133(17) Uani 1 1 d . . . Cd2 Cd 0.43417(2) 0.54280(5) 0.16476(3) 0.06111(17) Uani 1 1 d . . . O1 O 0.5551(4) 0.6480(7) 0.7258(3) 0.104(2) Uani 1 1 d . . . O2 O 0.5371(5) 0.8561(7) 0.7173(3) 0.129(3) Uani 1 1 d . . . O3 O 0.4557(3) 0.9982(6) 0.5371(3) 0.0747(16) Uani 1 1 d . . . O4 O 0.4910(4) 1.0019(6) 0.6378(3) 0.095(2) Uani 1 1 d . . . O5 O 0.4766(8) 0.2364(13) 0.3507(6) 0.091(3) Uani 0.531(11) 1 d P A 1 H5 H 0.4833 0.2597 0.3131 0.136 Uiso 0.531(11) 1 calc PR A 1 O6 O 0.5240(3) 0.9525(6) 0.3959(4) 0.094(2) Uani 1 1 d . . . O7 O 0.5876(3) 0.9302(6) 0.3122(3) 0.0840(18) Uani 1 1 d . . . O8 O 0.5359(3) 0.6570(6) 0.1598(3) 0.0827(18) Uani 1 1 d . . . O9 O 0.5953(2) 0.7984(6) 0.2112(3) 0.0762(16) Uani 1 1 d . . . O10 O 0.1825(3) 0.4730(9) 0.3767(5) 0.131(3) Uani 1 1 d . . . H10 H 0.1539 0.4981 0.3533 0.196 Uiso 1 1 calc R . . C47 C 0.3491(17) 0.498(3) 0.6697(15) 0.187(14) Uiso 0.50 1 d PD . . O12 O 0.6182(17) 0.227(3) 0.288(2) 0.275(15) Uiso 0.50 1 d P . . N1 N 0.4853(3) 0.7435(6) 0.5223(3) 0.0569(16) Uani 1 1 d . . . N2 N 0.5228(3) 0.6066(6) 0.5978(3) 0.0602(16) Uani 1 1 d . . . N3 N 0.4418(3) 0.7779(6) 0.3467(3) 0.0510(14) Uani 1 1 d . . . N4 N 0.4443(3) 0.6678(6) 0.2537(3) 0.0524(15) Uani 1 1 d . . . N5 N 0.3360(4) 0.7914(8) 0.4939(4) 0.078(2) Uani 1 1 d . . . N6 N 0.3519(5) 0.9944(8) 0.4134(5) 0.097(3) Uani 1 1 d . . . N7 N 0.3262(3) 0.4991(6) 0.1607(4) 0.0658(16) Uani 1 1 d . . . N8 N 0.3848(3) 0.6929(6) 0.0991(3) 0.0551(14) Uani 1 1 d . . . C1 C 0.5367(6) 0.7416(11) 0.6938(5) 0.092(3) Uani 1 1 d . . . C2 C 0.5174(4) 0.7245(8) 0.6245(4) 0.062(2) Uani 1 1 d . . . C3 C 0.4953(4) 0.8062(8) 0.5807(4) 0.060(2) Uani 1 1 d . . . C4 C 0.4795(4) 0.9434(9) 0.5839(4) 0.073(2) Uani 1 1 d . . . C5 C 0.5014(3) 0.6234(8) 0.5360(4) 0.0559(19) Uani 1 1 d . . . C6 C 0.4993(3) 0.5206(7) 0.4864(4) 0.0523(18) Uani 1 1 d . A . C7 C 0.5168(3) 0.5426(7) 0.4229(4) 0.0582(19) Uani 1 1 d . . . H7 H 0.5295 0.6237 0.4107 0.070 Uiso 1 1 calc R . . C8 C 0.5160(5) 0.4466(9) 0.3766(4) 0.076(3) Uani 1 1 d . A . H8 H 0.5287 0.4633 0.3340 0.092 Uiso 1 1 calc R . . C9 C 0.4967(7) 0.3281(11) 0.3934(5) 0.114(4) Uani 1 1 d . . . C10 C 0.4774(6) 0.3037(9) 0.4575(5) 0.099(4) Uani 1 1 d . A . H10A H 0.4646 0.2223 0.4693 0.119 Uiso 1 1 calc R . . C11 C 0.4774(5) 0.3967(9) 0.5019(4) 0.076(3) Uani 1 1 d . . . H11 H 0.4628 0.3800 0.5438 0.091 Uiso 1 1 calc R A . C12 C 0.5446(4) 0.7296(10) 0.2053(4) 0.067(2) Uani 1 1 d . . . C13 C 0.4973(3) 0.7413(7) 0.2570(3) 0.0518(18) Uani 1 1 d . . . C14 C 0.4949(3) 0.8110(8) 0.3143(4) 0.0524(18) Uani 1 1 d . . . C15 C 0.5383(4) 0.9041(8) 0.3433(4) 0.065(2) Uani 1 1 d . . . C16 C 0.4123(3) 0.6924(7) 0.3078(4) 0.0497(15) Uani 1 1 d . . . C17 C 0.3514(3) 0.6361(7) 0.3249(3) 0.0521(17) Uani 1 1 d . . . C18 C 0.3487(4) 0.5444(12) 0.3697(6) 0.126(5) Uani 1 1 d . . . H18 H 0.3852 0.5167 0.3899 0.151 Uiso 1 1 calc R . . C19 C 0.2915(4) 0.4895(11) 0.3863(6) 0.106(4) Uani 1 1 d . . . H19 H 0.2905 0.4225 0.4159 0.128 Uiso 1 1 calc R . . C20 C 0.2368(4) 0.5329(9) 0.3597(4) 0.072(2) Uani 1 1 d . . . C21 C 0.2399(4) 0.6294(10) 0.3198(6) 0.093(3) Uani 1 1 d . . . H21 H 0.2031 0.6642 0.3033 0.112 Uiso 1 1 calc R . . C22 C 0.2970(4) 0.6809(9) 0.3016(6) 0.080(3) Uani 1 1 d . . . H22 H 0.2976 0.7486 0.2724 0.096 Uiso 1 1 calc R . . C23 C 0.2952(5) 0.4046(10) 0.1927(5) 0.087(3) Uani 1 1 d . . . H23 H 0.3180 0.3452 0.2166 0.104 Uiso 1 1 calc R . . C24 C 0.2319(6) 0.3956(11) 0.1905(6) 0.106(4) Uani 1 1 d . . . H24 H 0.2123 0.3318 0.2145 0.128 Uiso 1 1 calc R . . C25 C 0.1972(5) 0.4735(12) 0.1557(7) 0.101(3) Uani 1 1 d . . . H25 H 0.1539 0.4648 0.1550 0.121 Uiso 1 1 calc R . . C26 C 0.2269(4) 0.5714(10) 0.1193(5) 0.077(3) Uani 1 1 d . . . C27 C 0.2903(4) 0.5811(8) 0.1234(4) 0.061(2) Uani 1 1 d . . . C28 C 0.3214(4) 0.6819(7) 0.0914(4) 0.0565(18) Uani 1 1 d . . . C29 C 0.2869(4) 0.7681(9) 0.0551(4) 0.076(2) Uani 1 1 d . . . C30 C 0.3193(6) 0.8634(11) 0.0206(6) 0.104(3) Uani 1 1 d . . . H30 H 0.2981 0.9195 -0.0067 0.125 Uiso 1 1 calc R . . C31 C 0.3838(5) 0.8712(10) 0.0286(5) 0.097(3) Uani 1 1 d . . . H31 H 0.4065 0.9339 0.0069 0.116 Uiso 1 1 calc R . . C32 C 0.4132(4) 0.7873(8) 0.0678(4) 0.069(2) Uani 1 1 d . . . H32 H 0.4562 0.7963 0.0734 0.083 Uiso 1 1 calc R . . C33 C 0.1919(4) 0.6589(14) 0.0823(6) 0.103(4) Uani 1 1 d . . . H33 H 0.1484 0.6533 0.0811 0.124 Uiso 1 1 calc R . . C34 C 0.2204(5) 0.7470(14) 0.0501(6) 0.110(4) Uani 1 1 d . . . H34 H 0.1972 0.7990 0.0226 0.132 Uiso 1 1 calc R . . C35 C 0.3288(6) 0.6969(12) 0.5340(6) 0.100(3) Uani 1 1 d . . . H35 H 0.3638 0.6515 0.5475 0.120 Uiso 1 1 calc R . . C36 C 0.2695(7) 0.6613(16) 0.5576(8) 0.139(5) Uani 1 1 d . . . H36 H 0.2659 0.5925 0.5859 0.167 Uiso 1 1 calc R . . C37 C 0.2177(7) 0.726(2) 0.5396(8) 0.130(6) Uani 1 1 d . . . H37 H 0.1782 0.7027 0.5546 0.156 Uiso 1 1 calc R . . C38 C 0.2252(5) 0.8268(16) 0.4990(8) 0.116(4) Uani 1 1 d D . . C39 C 0.2858(4) 0.8578(12) 0.4756(5) 0.086(3) Uani 1 1 d . . . C40 C 0.2927(5) 0.9643(11) 0.4341(6) 0.096(4) Uani 1 1 d . . . C41 C 0.2412(6) 1.0408(14) 0.4145(8) 0.131(5) Uani 1 1 d D . . C42 C 0.2553(10) 1.1349(19) 0.3737(11) 0.185(7) Uani 1 1 d U . . H42 H 0.2220 1.1853 0.3599 0.223 Uiso 1 1 calc R . . C43 C 0.3108(12) 1.165(2) 0.3507(11) 0.204(9) Uani 1 1 d U . . H43 H 0.3165 1.2317 0.3217 0.244 Uiso 1 1 calc R . . C44 C 0.3630(7) 1.0870(12) 0.3733(8) 0.144(6) Uani 1 1 d . . . H44 H 0.4036 1.1036 0.3592 0.173 Uiso 1 1 calc R . . C45 C 0.1728(7) 0.897(2) 0.4794(9) 0.181(10) Uani 1 1 d D . . H45 H 0.1330 0.8713 0.4924 0.217 Uiso 1 1 calc R . . C46 C 0.1801(6) 1.0041(17) 0.4407(12) 0.190(11) Uani 1 1 d D . . H46 H 0.1453 1.0538 0.4311 0.228 Uiso 1 1 calc R . . O11 O 0.3061(12) 0.451(3) 0.7164(15) 0.210(11) Uiso 0.50 1 d PD . . C48 C 0.3728(16) 0.584(3) 0.722(2) 0.196(15) Uiso 0.50 1 d PD . . O5A O 0.5250(9) 0.2291(16) 0.3501(7) 0.091(3) Uani 0.469(11) 1 d P A 2 H5A H 0.5555 0.1975 0.3683 0.136 Uiso 0.469(11) 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 0.0566(3) 0.0674(4) 0.0600(3) -0.0032(3) 0.0045(4) 0.0087(3) Cd2 0.0627(3) 0.0692(4) 0.0515(3) -0.0058(3) -0.0040(4) 0.0084(3) O1 0.169(7) 0.092(5) 0.051(3) 0.006(4) -0.003(4) 0.034(5) O2 0.234(10) 0.094(6) 0.059(4) -0.020(4) -0.012(5) 0.044(6) O3 0.086(4) 0.062(3) 0.076(4) -0.005(3) -0.008(3) 0.023(3) O4 0.148(6) 0.068(4) 0.071(4) -0.014(3) -0.001(4) 0.028(4) O5 0.115(9) 0.096(6) 0.061(5) -0.023(4) -0.013(8) -0.025(9) O6 0.066(4) 0.108(5) 0.107(5) -0.049(4) 0.020(4) -0.023(3) O7 0.048(3) 0.111(5) 0.093(4) -0.028(4) 0.014(3) -0.021(3) O8 0.060(3) 0.126(5) 0.062(4) -0.032(4) 0.009(3) -0.015(3) O9 0.045(3) 0.113(5) 0.071(4) -0.011(3) 0.005(3) -0.009(3) O10 0.056(4) 0.186(8) 0.150(7) 0.117(6) 0.008(4) 0.000(5) N1 0.057(4) 0.053(4) 0.060(4) -0.003(3) 0.001(3) 0.008(3) N2 0.070(4) 0.060(4) 0.050(4) 0.005(3) 0.010(3) 0.008(3) N3 0.050(3) 0.051(3) 0.052(3) -0.003(3) 0.004(3) -0.003(3) N4 0.046(3) 0.067(4) 0.044(3) -0.003(3) -0.002(2) 0.001(3) N5 0.067(5) 0.095(6) 0.070(5) -0.018(4) 0.010(4) 0.001(4) N6 0.106(7) 0.070(5) 0.114(7) -0.024(5) -0.056(6) 0.033(5) N7 0.080(4) 0.057(4) 0.060(4) 0.001(4) 0.001(4) -0.014(3) N8 0.060(4) 0.051(3) 0.054(3) 0.002(3) -0.003(3) -0.001(3) C1 0.153(10) 0.077(7) 0.047(5) -0.009(5) 0.004(6) 0.030(7) C2 0.071(5) 0.063(5) 0.054(5) -0.002(4) 0.014(4) 0.011(4) C3 0.064(5) 0.052(5) 0.065(5) -0.002(4) 0.011(4) 0.012(4) C4 0.084(6) 0.079(6) 0.057(5) 0.005(5) 0.008(5) 0.015(5) C5 0.050(4) 0.067(5) 0.051(5) 0.001(4) 0.008(3) 0.009(4) C6 0.046(4) 0.059(5) 0.052(5) 0.002(4) -0.008(3) 0.005(4) C7 0.046(4) 0.051(5) 0.077(5) 0.008(4) -0.008(4) 0.011(3) C8 0.100(7) 0.081(7) 0.048(5) -0.002(5) -0.014(5) -0.002(5) C9 0.204(14) 0.079(8) 0.058(6) -0.006(6) -0.021(7) -0.044(8) C10 0.172(10) 0.070(6) 0.054(6) 0.012(5) -0.037(6) -0.041(6) C11 0.095(7) 0.080(6) 0.053(5) 0.019(5) -0.012(5) -0.017(5) C12 0.035(4) 0.102(7) 0.064(5) -0.014(5) -0.003(3) 0.000(5) C13 0.046(4) 0.067(5) 0.042(4) 0.001(4) 0.001(3) 0.005(4) C14 0.040(4) 0.060(5) 0.057(5) 0.007(4) -0.002(4) 0.004(4) C15 0.047(4) 0.071(5) 0.077(6) -0.032(5) -0.001(4) 0.008(4) C16 0.042(3) 0.058(4) 0.050(4) 0.003(3) -0.003(4) 0.008(4) C17 0.047(4) 0.057(4) 0.052(4) 0.009(3) -0.004(3) -0.001(3) C18 0.044(5) 0.166(11) 0.166(11) 0.110(10) -0.002(6) 0.002(6) C19 0.050(5) 0.127(9) 0.142(10) 0.079(8) 0.016(6) 0.004(6) C20 0.044(4) 0.099(7) 0.072(5) 0.043(5) 0.001(4) 0.004(4) C21 0.043(5) 0.104(7) 0.133(9) 0.039(7) -0.009(5) 0.005(5) C22 0.052(4) 0.081(6) 0.108(7) 0.041(6) -0.010(5) -0.003(5) C23 0.092(7) 0.078(6) 0.090(7) 0.022(5) 0.018(5) -0.019(6) C24 0.110(10) 0.088(8) 0.120(9) 0.024(7) 0.031(8) -0.025(7) C25 0.077(6) 0.109(8) 0.117(9) -0.030(8) -0.003(7) -0.028(6) C26 0.068(6) 0.097(7) 0.065(5) -0.007(5) 0.004(5) -0.020(6) C27 0.061(5) 0.072(5) 0.050(4) -0.011(4) 0.000(4) 0.002(4) C28 0.057(5) 0.060(5) 0.052(4) 0.003(4) 0.000(4) -0.002(4) C29 0.074(6) 0.092(7) 0.061(5) 0.008(5) -0.002(4) 0.011(5) C30 0.114(9) 0.108(9) 0.090(7) 0.032(6) -0.011(7) 0.016(7) C31 0.098(8) 0.092(7) 0.099(8) 0.036(6) -0.004(6) -0.013(6) C32 0.072(5) 0.063(5) 0.072(5) 0.006(4) 0.003(4) -0.003(4) C33 0.048(5) 0.172(12) 0.089(7) -0.014(8) 0.003(5) -0.010(7) C34 0.070(7) 0.170(12) 0.089(7) 0.020(8) -0.007(6) 0.034(8) C35 0.090(8) 0.111(8) 0.098(8) 0.010(7) 0.025(6) 0.002(7) C36 0.117(11) 0.183(15) 0.118(11) -0.012(10) 0.027(9) -0.033(11) C37 0.079(9) 0.188(17) 0.124(12) -0.049(11) 0.032(8) -0.037(10) C38 0.049(6) 0.161(12) 0.137(11) -0.064(10) 0.005(7) -0.010(7) C39 0.053(5) 0.119(9) 0.087(7) -0.044(7) 0.000(5) 0.002(6) C40 0.069(6) 0.100(8) 0.120(9) -0.020(7) -0.037(6) 0.030(6) C41 0.088(9) 0.131(12) 0.172(15) -0.013(9) -0.065(9) 0.003(8) C42 0.157(10) 0.181(17) 0.22(2) 0.075(14) -0.056(12) 0.033(13) C43 0.203(9) 0.204(9) 0.204(9) 0.0004(10) -0.0005(10) 0.0001(10) C44 0.163(12) 0.083(8) 0.185(14) 0.018(9) -0.086(11) 0.042(9) C45 0.057(8) 0.29(3) 0.20(2) -0.10(2) -0.008(9) 0.001(14) C46 0.064(9) 0.168(15) 0.34(3) -0.107(19) -0.066(14) 0.038(10) O5A 0.115(9) 0.096(6) 0.061(5) -0.023(4) -0.013(8) -0.025(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 Cd1 N3 2.250(6) . ? Cd1 N1 2.267(6) . ? Cd1 N6 2.328(8) . ? Cd1 N5 2.378(8) . ? Cd1 O3 2.388(6) . ? Cd1 O6 2.427(6) . ? Cd2 N4 2.256(6) . ? Cd2 N2 2.279(6) 2_664 ? Cd2 N8 2.327(6) . ? Cd2 N7 2.354(7) . ? Cd2 O1 2.376(7) 2_664 ? Cd2 O8 2.486(6) . ? O1 C1 1.246(12) . ? O1 Cd2 2.376(7) 2_665 ? O2 C1 1.297(12) . ? O3 C4 1.228(10) . ? O4 C4 1.286(11) . ? O5 C9 1.371(15) . ? O5 H5 0.8200 . ? O6 C15 1.231(10) . ? O7 C15 1.260(10) . ? O8 C12 1.217(10) . ? O9 C12 1.309(10) . ? O10 C20 1.366(10) . ? O10 H10 0.8200 . ? C47 O11 1.413(19) . ? C47 C48 1.489(10) . ? N1 C5 1.339(9) . ? N1 C3 1.383(10) . ? N2 C5 1.357(10) . ? N2 C2 1.359(10) . ? N2 Cd2 2.279(6) 2_665 ? N3 C16 1.357(10) . ? N3 C14 1.359(9) . ? N4 C16 1.326(10) . ? N4 C13 1.373(10) . ? N5 C35 1.298(13) . ? N5 C39 1.333(13) . ? N6 C44 1.295(16) . ? N6 C40 1.370(15) . ? N7 C23 1.361(11) . ? N7 C27 1.384(11) . ? N8 C32 1.328(10) . ? N8 C28 1.369(9) . ? C1 C2 1.488(13) . ? C2 C3 1.328(11) . ? C3 C4 1.483(12) . ? C5 C6 1.483(11) . ? C6 C7 1.373(11) . ? C6 C11 1.420(12) . ? C7 C8 1.384(12) . ? C7 H7 0.9300 . ? C8 C9 1.357(13) . ? C8 H8 0.9300 . ? C9 C10 1.398(15) . ? C9 O5A 1.50(2) . ? C10 C11 1.335(13) . ? C10 H10A 0.9300 . ? C11 H11 0.9300 . ? C12 C13 1.469(11) . ? C13 C14 1.383(11) . ? C14 C15 1.474(11) . ? C16 C17 1.470(9) . ? C17 C18 1.331(11) . ? C17 C22 1.343(10) . ? C18 C19 1.395(13) . ? C18 H18 0.9300 . ? C19 C20 1.368(12) . ? C19 H19 0.9300 . ? C20 C21 1.304(12) . ? C21 C22 1.387(12) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C24 1.357(15) . ? C23 H23 0.9300 . ? C24 C25 1.315(15) . ? C24 H24 0.9300 . ? C25 C26 1.421(15) . ? C25 H25 0.9300 . ? C26 C27 1.359(12) . ? C26 C33 1.407(15) . ? C27 C28 1.413(11) . ? C28 C29 1.384(11) . ? C29 C30 1.407(14) . ? C29 C34 1.442(14) . ? C30 C31 1.390(14) . ? C30 H30 0.9300 . ? C31 C32 1.349(13) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 C34 1.290(16) . ? C33 H33 0.9300 . ? C34 H34 0.9300 . ? C35 C36 1.406(16) . ? C35 H35 0.9300 . ? C36 C37 1.35(2) . ? C36 H36 0.9300 . ? C37 C38 1.36(2) . ? C37 H37 0.9300 . ? C38 C45 1.398(15) . ? C38 C39 1.418(16) . ? C39 C40 1.415(15) . ? C40 C41 1.421(15) . ? C41 C42 1.33(2) . ? C41 C46 1.464(15) . ? C42 C43 1.31(2) . ? C42 H42 0.9300 . ? C43 C44 1.46(2) . ? C43 H43 0.9300 . ? C44 H44 0.9300 . ? C45 C46 1.389(16) . ? C45 H45 0.9300 . ? C46 H46 0.9300 . ? O5A H5A 0.8200 . ? 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 N3 Cd1 N1 111.3(2) . . ? N3 Cd1 N6 91.4(3) . . ? N1 Cd1 N6 154.2(3) . . ? N3 Cd1 N5 109.0(2) . . ? N1 Cd1 N5 89.8(3) . . ? N6 Cd1 N5 70.6(4) . . ? N3 Cd1 O3 156.9(2) . . ? N1 Cd1 O3 72.9(2) . . ? N6 Cd1 O3 91.1(2) . . ? N5 Cd1 O3 93.5(2) . . ? N3 Cd1 O6 71.4(2) . . ? N1 Cd1 O6 96.1(3) . . ? N6 Cd1 O6 102.9(4) . . ? N5 Cd1 O6 173.4(3) . . ? O3 Cd1 O6 85.6(2) . . ? N4 Cd2 N2 148.1(2) . 2_664 ? N4 Cd2 N8 96.6(2) . . ? N2 Cd2 N8 107.7(2) 2_664 . ? N4 Cd2 N7 103.7(2) . . ? N2 Cd2 N7 103.8(2) 2_664 . ? N8 Cd2 N7 70.6(2) . . ? N4 Cd2 O1 93.4(2) . 2_664 ? N2 Cd2 O1 72.2(2) 2_664 2_664 ? N8 Cd2 O1 157.1(3) . 2_664 ? N7 Cd2 O1 87.0(3) . 2_664 ? N4 Cd2 O8 70.6(2) . . ? N2 Cd2 O8 87.5(2) 2_664 . ? N8 Cd2 O8 92.6(2) . . ? N7 Cd2 O8 161.8(2) . . ? O1 Cd2 O8 110.2(3) 2_664 . ? C1 O1 Cd2 114.9(6) . 2_665 ? C4 O3 Cd1 113.7(6) . . ? C9 O5 H5 109.5 . . ? C15 O6 Cd1 114.7(5) . . ? C12 O8 Cd2 113.9(5) . . ? C20 O10 H10 109.5 . . ? O11 C47 C48 86.9(10) . . ? C5 N1 C3 103.2(6) . . ? C5 N1 Cd1 141.5(5) . . ? C3 N1 Cd1 113.7(5) . . ? C5 N2 C2 103.1(7) . . ? C5 N2 Cd2 141.8(5) . 2_665 ? C2 N2 Cd2 114.9(5) . 2_665 ? C16 N3 C14 105.8(6) . . ? C16 N3 Cd1 138.8(5) . . ? C14 N3 Cd1 115.1(5) . . ? C16 N4 C13 105.9(6) . . ? C16 N4 Cd2 137.5(5) . . ? C13 N4 Cd2 116.5(5) . . ? C35 N5 C39 118.8(10) . . ? C35 N5 Cd1 126.1(7) . . ? C39 N5 Cd1 115.1(7) . . ? C44 N6 C40 122.6(10) . . ? C44 N6 Cd1 120.6(9) . . ? C40 N6 Cd1 116.6(7) . . ? C23 N7 C27 116.8(8) . . ? C23 N7 Cd2 126.9(6) . . ? C27 N7 Cd2 116.2(5) . . ? C32 N8 C28 117.4(7) . . ? C32 N8 Cd2 125.4(5) . . ? C28 N8 Cd2 117.2(5) . . ? O1 C1 O2 122.4(9) . . ? O1 C1 C2 119.5(9) . . ? O2 C1 C2 117.9(9) . . ? C3 C2 N2 110.5(7) . . ? C3 C2 C1 131.5(9) . . ? N2 C2 C1 118.0(8) . . ? C2 C3 N1 109.2(7) . . ? C2 C3 C4 132.9(8) . . ? N1 C3 C4 117.8(7) . . ? O3 C4 O4 121.5(8) . . ? O3 C4 C3 121.1(8) . . ? O4 C4 C3 117.4(8) . . ? N1 C5 N2 113.9(7) . . ? N1 C5 C6 122.4(7) . . ? N2 C5 C6 123.6(7) . . ? C7 C6 C11 117.0(8) . . ? C7 C6 C5 121.1(7) . . ? C11 C6 C5 121.8(7) . . ? C6 C7 C8 121.5(8) . . ? C6 C7 H7 119.3 . . ? C8 C7 H7 119.3 . . ? C9 C8 C7 120.0(9) . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C8 C9 O5 125.4(11) . . ? C8 C9 C10 119.7(10) . . ? O5 C9 C10 112.1(11) . . ? C8 C9 O5A 111.5(12) . . ? O5 C9 O5A 42.1(8) . . ? C10 C9 O5A 123.2(12) . . ? C11 C10 C9 120.2(9) . . ? C11 C10 H10A 119.9 . . ? C9 C10 H10A 119.9 . . ? C10 C11 C6 121.5(8) . . ? C10 C11 H11 119.3 . . ? C6 C11 H11 119.3 . . ? O8 C12 O9 123.0(8) . . ? O8 C12 C13 119.9(8) . . ? O9 C12 C13 117.1(7) . . ? N4 C13 C14 108.0(6) . . ? N4 C13 C12 119.0(7) . . ? C14 C13 C12 132.9(7) . . ? N3 C14 C13 108.0(7) . . ? N3 C14 C15 119.9(7) . . ? C13 C14 C15 132.1(7) . . ? O6 C15 O7 124.0(7) . . ? O6 C15 C14 118.1(7) . . ? O7 C15 C14 117.8(7) . . ? N4 C16 N3 112.3(6) . . ? N4 C16 C17 125.2(7) . . ? N3 C16 C17 122.6(7) . . ? C18 C17 C22 117.5(7) . . ? C18 C17 C16 119.6(7) . . ? C22 C17 C16 122.6(7) . . ? C17 C18 C19 120.4(9) . . ? C17 C18 H18 119.8 . . ? C19 C18 H18 119.8 . . ? C20 C19 C18 120.9(9) . . ? C20 C19 H19 119.5 . . ? C18 C19 H19 119.5 . . ? C21 C20 O10 124.2(7) . . ? C21 C20 C19 117.7(8) . . ? O10 C20 C19 118.1(7) . . ? C20 C21 C22 121.1(8) . . ? C20 C21 H21 119.4 . . ? C22 C21 H21 119.4 . . ? C17 C22 C21 122.0(8) . . ? C17 C22 H22 119.0 . . ? C21 C22 H22 119.0 . . ? C24 C23 N7 121.3(10) . . ? C24 C23 H23 119.4 . . ? N7 C23 H23 119.4 . . ? C25 C24 C23 122.5(10) . . ? C25 C24 H24 118.8 . . ? C23 C24 H24 118.8 . . ? C24 C25 C26 118.9(10) . . ? C24 C25 H25 120.5 . . ? C26 C25 H25 120.5 . . ? C27 C26 C33 120.9(9) . . ? C27 C26 C25 117.8(10) . . ? C33 C26 C25 121.2(10) . . ? C26 C27 N7 122.6(8) . . ? C26 C27 C28 119.7(8) . . ? N7 C27 C28 117.6(7) . . ? N8 C28 C29 122.2(7) . . ? N8 C28 C27 118.4(7) . . ? C29 C28 C27 119.4(8) . . ? C28 C29 C30 118.4(9) . . ? C28 C29 C34 117.4(9) . . ? C30 C29 C34 123.9(10) . . ? C31 C30 C29 118.0(9) . . ? C31 C30 H30 121.0 . . ? C29 C30 H30 121.0 . . ? C32 C31 C30 119.6(10) . . ? C32 C31 H31 120.2 . . ? C30 C31 H31 120.2 . . ? N8 C32 C31 124.3(9) . . ? N8 C32 H32 117.9 . . ? C31 C32 H32 117.9 . . ? C34 C33 C26 119.5(9) . . ? C34 C33 H33 120.3 . . ? C26 C33 H33 120.3 . . ? C33 C34 C29 122.8(10) . . ? C33 C34 H34 118.6 . . ? C29 C34 H34 118.6 . . ? N5 C35 C36 121.9(13) . . ? N5 C35 H35 119.0 . . ? C36 C35 H35 119.0 . . ? C37 C36 C35 120.6(16) . . ? C37 C36 H36 119.7 . . ? C35 C36 H36 119.7 . . ? C36 C37 C38 117.6(13) . . ? C36 C37 H37 121.2 . . ? C38 C37 H37 121.2 . . ? C37 C38 C45 119.4(15) . . ? C37 C38 C39 119.7(13) . . ? C45 C38 C39 120.9(16) . . ? N5 C39 C40 120.0(9) . . ? N5 C39 C38 121.3(12) . . ? C40 C39 C38 118.7(12) . . ? N6 C40 C39 117.7(9) . . ? N6 C40 C41 119.7(12) . . ? C39 C40 C41 122.6(13) . . ? C42 C41 C40 115.1(15) . . ? C42 C41 C46 128.9(16) . . ? C40 C41 C46 115.9(14) . . ? C43 C42 C41 127.3(19) . . ? C43 C42 H42 116.4 . . ? C41 C42 H42 116.4 . . ? C42 C43 C44 116(2) . . ? C42 C43 H43 121.8 . . ? C44 C43 H43 121.8 . . ? N6 C44 C43 118.8(17) . . ? N6 C44 H44 120.6 . . ? C43 C44 H44 120.6 . . ? C46 C45 C38 120.1(17) . . ? C46 C45 H45 119.9 . . ? C38 C45 H45 119.9 . . ? C45 C46 C41 121.6(15) . . ? C45 C46 H46 119.2 . . ? C41 C46 H46 119.2 . . ? C9 O5A H5A 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 N3 Cd1 O3 C4 -110.8(8) . . . . ? N1 Cd1 O3 C4 -6.3(6) . . . . ? N6 Cd1 O3 C4 153.0(7) . . . . ? N5 Cd1 O3 C4 82.4(7) . . . . ? O6 Cd1 O3 C4 -104.1(7) . . . . ? N3 Cd1 O6 C15 -7.9(6) . . . . ? N1 Cd1 O6 C15 102.6(7) . . . . ? N6 Cd1 O6 C15 -95.0(7) . . . . ? N5 Cd1 O6 C15 -103(2) . . . . ? O3 Cd1 O6 C15 174.9(7) . . . . ? N4 Cd2 O8 C12 -1.9(6) . . . . ? N2 Cd2 O8 C12 -158.2(7) 2_664 . . . ? N8 Cd2 O8 C12 94.2(7) . . . . ? N7 Cd2 O8 C12 72.5(11) . . . . ? O1 Cd2 O8 C12 -88.2(7) 2_664 . . . ? N3 Cd1 N1 C5 -34.2(9) . . . . ? N6 Cd1 N1 C5 115.9(9) . . . . ? N5 Cd1 N1 C5 76.2(8) . . . . ? O3 Cd1 N1 C5 169.9(9) . . . . ? O6 Cd1 N1 C5 -106.6(8) . . . . ? N3 Cd1 N1 C3 163.6(5) . . . . ? N6 Cd1 N1 C3 -46.3(9) . . . . ? N5 Cd1 N1 C3 -86.0(5) . . . . ? O3 Cd1 N1 C3 7.7(5) . . . . ? O6 Cd1 N1 C3 91.2(5) . . . . ? N1 Cd1 N3 C16 89.4(7) . . . . ? N6 Cd1 N3 C16 -78.0(8) . . . . ? N5 Cd1 N3 C16 -8.1(8) . . . . ? O3 Cd1 N3 C16 -174.1(6) . . . . ? O6 Cd1 N3 C16 178.8(8) . . . . ? N1 Cd1 N3 C14 -82.9(5) . . . . ? N6 Cd1 N3 C14 109.6(6) . . . . ? N5 Cd1 N3 C14 179.5(5) . . . . ? O3 Cd1 N3 C14 13.5(8) . . . . ? O6 Cd1 N3 C14 6.5(5) . . . . ? N2 Cd2 N4 C16 -127.6(7) 2_664 . . . ? N8 Cd2 N4 C16 92.8(7) . . . . ? N7 Cd2 N4 C16 21.2(8) . . . . ? O1 Cd2 N4 C16 -66.6(7) 2_664 . . . ? O8 Cd2 N4 C16 -176.8(8) . . . . ? N2 Cd2 N4 C13 51.6(7) 2_664 . . . ? N8 Cd2 N4 C13 -88.0(5) . . . . ? N7 Cd2 N4 C13 -159.6(5) . . . . ? O1 Cd2 N4 C13 112.7(5) 2_664 . . . ? O8 Cd2 N4 C13 2.4(5) . . . . ? N3 Cd1 N5 C35 97.8(8) . . . . ? N1 Cd1 N5 C35 -14.8(8) . . . . ? N6 Cd1 N5 C35 -177.6(9) . . . . ? O3 Cd1 N5 C35 -87.7(8) . . . . ? O6 Cd1 N5 C35 -169.6(18) . . . . ? N3 Cd1 N5 C39 -81.9(6) . . . . ? N1 Cd1 N5 C39 165.5(6) . . . . ? N6 Cd1 N5 C39 2.7(6) . . . . ? O3 Cd1 N5 C39 92.6(6) . . . . ? O6 Cd1 N5 C39 11(2) . . . . ? N3 Cd1 N6 C44 -68.2(9) . . . . ? N1 Cd1 N6 C44 139.5(10) . . . . ? N5 Cd1 N6 C44 -177.9(9) . . . . ? O3 Cd1 N6 C44 88.8(9) . . . . ? O6 Cd1 N6 C44 3.1(9) . . . . ? N3 Cd1 N6 C40 107.4(7) . . . . ? N1 Cd1 N6 C40 -44.9(10) . . . . ? N5 Cd1 N6 C40 -2.3(7) . . . . ? O3 Cd1 N6 C40 -95.6(7) . . . . ? O6 Cd1 N6 C40 178.6(7) . . . . ? N4 Cd2 N7 C23 -85.6(7) . . . . ? N2 Cd2 N7 C23 78.0(8) 2_664 . . . ? N8 Cd2 N7 C23 -177.9(8) . . . . ? O1 Cd2 N7 C23 7.1(7) 2_664 . . . ? O8 Cd2 N7 C23 -154.8(8) . . . . ? N4 Cd2 N7 C27 91.9(6) . . . . ? N2 Cd2 N7 C27 -104.4(6) 2_664 . . . ? N8 Cd2 N7 C27 -0.3(5) . . . . ? O1 Cd2 N7 C27 -175.3(6) 2_664 . . . ? O8 Cd2 N7 C27 22.8(11) . . . . ? N4 Cd2 N8 C32 78.8(6) . . . . ? N2 Cd2 N8 C32 -80.1(6) 2_664 . . . ? N7 Cd2 N8 C32 -179.0(7) . . . . ? O1 Cd2 N8 C32 -166.1(6) 2_664 . . . ? O8 Cd2 N8 C32 8.1(6) . . . . ? N4 Cd2 N8 C28 -102.0(5) . . . . ? N2 Cd2 N8 C28 99.0(5) 2_664 . . . ? N7 Cd2 N8 C28 0.2(5) . . . . ? O1 Cd2 N8 C28 13.1(9) 2_664 . . . ? O8 Cd2 N8 C28 -172.8(5) . . . . ? Cd2 O1 C1 O2 -169.7(10) 2_665 . . . ? Cd2 O1 C1 C2 6.0(14) 2_665 . . . ? C5 N2 C2 C3 -1.2(9) . . . . ? Cd2 N2 C2 C3 176.4(6) 2_665 . . . ? C5 N2 C2 C1 179.6(9) . . . . ? Cd2 N2 C2 C1 -2.9(10) 2_665 . . . ? O1 C1 C2 C3 178.6(10) . . . . ? O2 C1 C2 C3 -5.4(18) . . . . ? O1 C1 C2 N2 -2.3(16) . . . . ? O2 C1 C2 N2 173.6(10) . . . . ? N2 C2 C3 N1 -0.1(10) . . . . ? C1 C2 C3 N1 179.0(10) . . . . ? N2 C2 C3 C4 178.6(9) . . . . ? C1 C2 C3 C4 -2.3(17) . . . . ? C5 N1 C3 C2 1.4(9) . . . . ? Cd1 N1 C3 C2 170.1(5) . . . . ? C5 N1 C3 C4 -177.6(7) . . . . ? Cd1 N1 C3 C4 -8.9(9) . . . . ? Cd1 O3 C4 O4 -175.0(7) . . . . ? Cd1 O3 C4 C3 3.9(11) . . . . ? C2 C3 C4 O3 -175.4(9) . . . . ? N1 C3 C4 O3 3.3(12) . . . . ? C2 C3 C4 O4 3.6(15) . . . . ? N1 C3 C4 O4 -177.7(8) . . . . ? C3 N1 C5 N2 -2.2(9) . . . . ? Cd1 N1 C5 N2 -165.5(5) . . . . ? C3 N1 C5 C6 -178.8(7) . . . . ? Cd1 N1 C5 C6 17.9(12) . . . . ? C2 N2 C5 N1 2.1(9) . . . . ? Cd2 N2 C5 N1 -174.2(5) 2_665 . . . ? C2 N2 C5 C6 178.7(7) . . . . ? Cd2 N2 C5 C6 2.3(13) 2_665 . . . ? N1 C5 C6 C7 38.6(11) . . . . ? N2 C5 C6 C7 -137.7(8) . . . . ? N1 C5 C6 C11 -139.6(8) . . . . ? N2 C5 C6 C11 44.1(11) . . . . ? C11 C6 C7 C8 -2.9(12) . . . . ? C5 C6 C7 C8 178.8(7) . . . . ? C6 C7 C8 C9 1.0(14) . . . . ? C7 C8 C9 O5 160.2(14) . . . . ? C7 C8 C9 C10 0.2(18) . . . . ? C7 C8 C9 O5A -154.1(11) . . . . ? C8 C9 C10 C11 1(2) . . . . ? O5 C9 C10 C11 -161.8(13) . . . . ? O5A C9 C10 C11 151.9(13) . . . . ? C9 C10 C11 C6 -2.7(17) . . . . ? C7 C6 C11 C10 3.8(13) . . . . ? C5 C6 C11 C10 -177.9(9) . . . . ? Cd2 O8 C12 O9 -179.9(7) . . . . ? Cd2 O8 C12 C13 1.0(11) . . . . ? C16 N4 C13 C14 -0.8(8) . . . . ? Cd2 N4 C13 C14 179.7(5) . . . . ? C16 N4 C13 C12 176.5(7) . . . . ? Cd2 N4 C13 C12 -3.0(9) . . . . ? O8 C12 C13 N4 1.2(12) . . . . ? O9 C12 C13 N4 -178.0(7) . . . . ? O8 C12 C13 C14 177.7(9) . . . . ? O9 C12 C13 C14 -1.5(14) . . . . ? C16 N3 C14 C13 -1.8(8) . . . . ? Cd1 N3 C14 C13 173.0(5) . . . . ? C16 N3 C14 C15 179.8(7) . . . . ? Cd1 N3 C14 C15 -5.4(9) . . . . ? N4 C13 C14 N3 1.6(8) . . . . ? C12 C13 C14 N3 -175.1(8) . . . . ? N4 C13 C14 C15 179.8(8) . . . . ? C12 C13 C14 C15 3.1(15) . . . . ? Cd1 O6 C15 O7 -172.9(7) . . . . ? Cd1 O6 C15 C14 7.9(10) . . . . ? N3 C14 C15 O6 -2.1(12) . . . . ? C13 C14 C15 O6 179.9(9) . . . . ? N3 C14 C15 O7 178.7(8) . . . . ? C13 C14 C15 O7 0.7(13) . . . . ? C13 N4 C16 N3 -0.3(8) . . . . ? Cd2 N4 C16 N3 179.0(5) . . . . ? C13 N4 C16 C17 179.1(7) . . . . ? Cd2 N4 C16 C17 -1.6(12) . . . . ? C14 N3 C16 N4 1.3(8) . . . . ? Cd1 N3 C16 N4 -171.5(5) . . . . ? C14 N3 C16 C17 -178.1(6) . . . . ? Cd1 N3 C16 C17 9.1(11) . . . . ? N4 C16 C17 C18 103.9(11) . . . . ? N3 C16 C17 C18 -76.7(12) . . . . ? N4 C16 C17 C22 -82.3(11) . . . . ? N3 C16 C17 C22 97.1(10) . . . . ? C22 C17 C18 C19 6.1(19) . . . . ? C16 C17 C18 C19 -179.7(11) . . . . ? C17 C18 C19 C20 -3(2) . . . . ? C18 C19 C20 C21 -1.9(19) . . . . ? C18 C19 C20 O10 178.4(13) . . . . ? O10 C20 C21 C22 -176.2(11) . . . . ? C19 C20 C21 C22 4.2(17) . . . . ? C18 C17 C22 C21 -4.0(16) . . . . ? C16 C17 C22 C21 -178.0(9) . . . . ? C20 C21 C22 C17 -1.3(18) . . . . ? C27 N7 C23 C24 -3.0(14) . . . . ? Cd2 N7 C23 C24 174.6(8) . . . . ? N7 C23 C24 C25 2.6(18) . . . . ? C23 C24 C25 C26 -0.3(19) . . . . ? C24 C25 C26 C27 -1.4(16) . . . . ? C24 C25 C26 C33 -178.7(11) . . . . ? C33 C26 C27 N7 178.2(8) . . . . ? C25 C26 C27 N7 0.9(13) . . . . ? C33 C26 C27 C28 1.3(13) . . . . ? C25 C26 C27 C28 -176.0(8) . . . . ? C23 N7 C27 C26 1.3(12) . . . . ? Cd2 N7 C27 C26 -176.6(7) . . . . ? C23 N7 C27 C28 178.2(7) . . . . ? Cd2 N7 C27 C28 0.3(9) . . . . ? C32 N8 C28 C29 -2.8(11) . . . . ? Cd2 N8 C28 C29 178.0(6) . . . . ? C32 N8 C28 C27 179.1(7) . . . . ? Cd2 N8 C28 C27 -0.1(9) . . . . ? C26 C27 C28 N8 176.8(7) . . . . ? N7 C27 C28 N8 -0.2(11) . . . . ? C26 C27 C28 C29 -1.3(12) . . . . ? N7 C27 C28 C29 -178.3(8) . . . . ? N8 C28 C29 C30 5.5(13) . . . . ? C27 C28 C29 C30 -176.5(9) . . . . ? N8 C28 C29 C34 179.8(9) . . . . ? C27 C28 C29 C34 -2.2(13) . . . . ? C28 C29 C30 C31 -4.4(16) . . . . ? C34 C29 C30 C31 -178.3(11) . . . . ? C29 C30 C31 C32 0.9(17) . . . . ? C28 N8 C32 C31 -1.0(13) . . . . ? Cd2 N8 C32 C31 178.1(8) . . . . ? C30 C31 C32 N8 2.0(17) . . . . ? C27 C26 C33 C34 2.4(16) . . . . ? C25 C26 C33 C34 179.6(11) . . . . ? C26 C33 C34 C29 -6.2(19) . . . . ? C28 C29 C34 C33 6.1(17) . . . . ? C30 C29 C34 C33 -180.0(12) . . . . ? C39 N5 C35 C36 1.2(16) . . . . ? Cd1 N5 C35 C36 -178.4(9) . . . . ? N5 C35 C36 C37 -1(2) . . . . ? C35 C36 C37 C38 -1(2) . . . . ? C36 C37 C38 C45 -179.8(14) . . . . ? C36 C37 C38 C39 2(2) . . . . ? C35 N5 C39 C40 177.4(9) . . . . ? Cd1 N5 C39 C40 -2.9(11) . . . . ? C35 N5 C39 C38 -0.1(14) . . . . ? Cd1 N5 C39 C38 179.6(7) . . . . ? C37 C38 C39 N5 -1.5(17) . . . . ? C45 C38 C39 N5 -179.8(12) . . . . ? C37 C38 C39 C40 -179.0(12) . . . . ? C45 C38 C39 C40 2.6(18) . . . . ? C44 N6 C40 C39 177.2(10) . . . . ? Cd1 N6 C40 C39 1.8(12) . . . . ? C44 N6 C40 C41 -3.7(17) . . . . ? Cd1 N6 C40 C41 -179.2(8) . . . . ? N5 C39 C40 N6 0.8(14) . . . . ? C38 C39 C40 N6 178.4(9) . . . . ? N5 C39 C40 C41 -178.2(10) . . . . ? C38 C39 C40 C41 -0.6(16) . . . . ? N6 C40 C41 C42 3.1(19) . . . . ? C39 C40 C41 C42 -177.9(14) . . . . ? N6 C40 C41 C46 -178.1(12) . . . . ? C39 C40 C41 C46 0.9(19) . . . . ? C40 C41 C42 C43 -1(3) . . . . ? C46 C41 C42 C43 -179(2) . . . . ? C41 C42 C43 C44 -1(4) . . . . ? C40 N6 C44 C43 2(2) . . . . ? Cd1 N6 C44 C43 177.1(12) . . . . ? C42 C43 C44 N6 1(3) . . . . ? C37 C38 C45 C46 176.6(18) . . . . ? C39 C38 C45 C46 -5(3) . . . . ? C38 C45 C46 C41 5(3) . . . . ? C42 C41 C46 C45 175(2) . . . . ? C40 C41 C46 C45 -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 O5 H5 O1 0.82 2.19 2.910(16) 146.3 2_664 O5 H5 O2 0.82 2.35 2.912(15) 126.5 2_664 O10 H10 O7 0.82 1.81 2.626(8) 170.9 4_465 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.39 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.622 _refine_diff_density_min -0.394 _refine_diff_density_rms 0.079 data_a _database_code_depnum_ccdc_archive 'CCDC 855103' #TrackingRef '44.cif' _audit_creation_date 2011-05-16 _audit_creation_method ; Olex2 1.1 (compiled 2011.02.15 svn.r1672, GUI svn.r3494) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C42 H26 Cd2 N8 O10, H2 O' _chemical_formula_sum 'C42 H28 Cd2 N8 O11' _chemical_formula_weight 1045.52 _chemical_melting_point ? 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' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y+1/2, -z+1/2' 3 '-x, -y, -z' 4 'x, -y-1/2, z-1/2' _cell_length_a 9.4315(11) _cell_length_b 20.990(3) _cell_length_c 20.452(2) _cell_angle_alpha 90.00 _cell_angle_beta 103.1830(10) _cell_angle_gamma 90.00 _cell_volume 3942.3(8) _cell_formula_units_Z 4 _cell_measurement_reflns_used 6033 _cell_measurement_temperature 291.15 _cell_measurement_theta_max 26.041 _cell_measurement_theta_min 2.193 _exptl_absorpt_coefficient_mu 1.154 _exptl_absorpt_correction_T_max 0.8192 _exptl_absorpt_correction_T_min 0.8020 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS(2009) _exptl_crystal_colour ? _exptl_crystal_density_diffrn 1.762 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description ? _exptl_crystal_F_000 2080 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0370 _diffrn_reflns_av_unetI/netI 0.0480 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 21783 _diffrn_reflns_theta_full 26.42 _diffrn_reflns_theta_max 26.42 _diffrn_reflns_theta_min 1.41 _diffrn_ambient_temperature 291.15 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 6252 _reflns_number_total 8080 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ? _computing_data_collection ? _computing_data_reduction 'SAINT v7.53A (Bruker, 2008)' _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'A short history of SHELX (Sheldrick, 2007)' _refine_diff_density_max 0.814 _refine_diff_density_min -0.444 _refine_diff_density_rms 0.085 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_hydrogen_treatment CONSTR _refine_ls_matrix_type full _refine_ls_number_parameters 570 _refine_ls_number_reflns 8080 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0521 _refine_ls_R_factor_gt 0.0357 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0432P)^2^+0.6311P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0834 _refine_ls_wR_factor_ref 0.0909 _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 0.73608(3) 0.771373(12) 0.062081(13) 0.03183(9) Uani 1 1 d . . . Cd2 Cd 0.88745(3) 0.493872(12) 0.233812(12) 0.02861(8) Uani 1 1 d . . . O1 O 0.9199(3) 0.72753(13) 0.01568(13) 0.0406(7) Uani 1 1 d . . . O2 O 1.0705(3) 0.64505(14) 0.01946(14) 0.0508(8) Uani 1 1 d . . . O3 O 1.1316(3) 0.54624(13) 0.08271(14) 0.0460(7) Uani 1 1 d . . . O4 O 1.0634(3) 0.49413(12) 0.16516(13) 0.0377(6) Uani 1 1 d . . . O5 O 0.2913(3) 0.6376(2) 0.28456(17) 0.0681(10) Uani 1 1 d . . . H5 H 0.3201 0.6306 0.3248 0.102 Uiso 1 1 calc R . . O6 O 0.9817(3) 0.55792(12) 0.33412(12) 0.0381(6) Uani 1 1 d . . . O7 O 1.1072(3) 0.55174(12) 0.44016(13) 0.0442(7) Uani 1 1 d . . . O8 O 1.2430(3) 0.47197(14) 0.51672(13) 0.0533(8) Uani 1 1 d . . . O9 O 1.3089(3) 0.37115(14) 0.51260(13) 0.0575(9) Uani 1 1 d . . . O10 O 1.0190(3) 0.18627(13) 0.11562(13) 0.0468(7) Uani 1 1 d . . . H10 H 1.0092 0.1504 0.1299 0.070 Uiso 1 1 calc R . . O11 O 0.3836(4) 0.60329(17) 0.41729(17) 0.0740(10) Uani 1 1 d D . . H11A H 0.3038 0.5885 0.4235 0.089 Uiso 1 1 d RD . . H11B H 0.4401 0.5913 0.4535 0.089 Uiso 1 1 d RD . . N1 N 0.7838(3) 0.67051(13) 0.10726(14) 0.0282(6) Uani 1 1 d . . . N2 N 0.8499(3) 0.58290(13) 0.16981(14) 0.0280(6) Uani 1 1 d . . . N3 N 1.0266(3) 0.43012(13) 0.31193(13) 0.0269(6) Uani 1 1 d . . . N4 N 1.1472(3) 0.35635(13) 0.38269(14) 0.0288(7) Uani 1 1 d . . . N5 N 0.5617(3) 0.74591(15) -0.03264(15) 0.0376(7) Uani 1 1 d . . . N6 N 0.5062(3) 0.78811(15) 0.08436(16) 0.0384(8) Uani 1 1 d . . . N7 N 0.7143(3) 0.44579(14) 0.14354(15) 0.0350(7) Uani 1 1 d . . . N8 N 0.6674(3) 0.47666(15) 0.26474(15) 0.0330(7) Uani 1 1 d . . . C1 C 0.9668(4) 0.67437(19) 0.03770(18) 0.0359(9) Uani 1 1 d . . . C2 C 0.9015(4) 0.64330(17) 0.08858(16) 0.0290(8) Uani 1 1 d . . . C3 C 0.9419(4) 0.58940(17) 0.12695(17) 0.0284(8) Uani 1 1 d . . . C4 C 1.0523(4) 0.53993(18) 0.12573(18) 0.0327(8) Uani 1 1 d . . . C5 C 0.7565(4) 0.63218(16) 0.15589(17) 0.0280(8) Uani 1 1 d . . . C6 C 0.6363(4) 0.63992(16) 0.18984(17) 0.0299(8) Uani 1 1 d . . . C7 C 0.6617(4) 0.63386(18) 0.25907(18) 0.0336(8) Uani 1 1 d . . . H7 H 0.7568 0.6291 0.2839 0.040 Uiso 1 1 calc R . . C8 C 0.5501(4) 0.63466(18) 0.29186(19) 0.0378(9) Uani 1 1 d . . . H8 H 0.5701 0.6312 0.3384 0.045 Uiso 1 1 calc R . . C9 C 0.4071(4) 0.6406(2) 0.2555(2) 0.0425(10) Uani 1 1 d . . . C10 C 0.3804(4) 0.6492(2) 0.1868(2) 0.0470(11) Uani 1 1 d . . . H10A H 0.2854 0.6554 0.1624 0.056 Uiso 1 1 calc R . . C11 C 0.4931(4) 0.64858(18) 0.15407(19) 0.0362(9) Uani 1 1 d . . . H11 H 0.4733 0.6540 0.1077 0.043 Uiso 1 1 calc R . . C12 C 1.0533(4) 0.52714(18) 0.38331(18) 0.0325(8) Uani 1 1 d . . . C13 C 1.0781(3) 0.45829(16) 0.37370(16) 0.0259(7) Uani 1 1 d . . . C14 C 1.1526(4) 0.41283(16) 0.41708(16) 0.0268(7) Uani 1 1 d . . . C15 C 1.2406(4) 0.41767(19) 0.48697(18) 0.0397(9) Uani 1 1 d . . . C16 C 1.0704(3) 0.36929(16) 0.31971(16) 0.0260(7) Uani 1 1 d . . . C17 C 1.0477(3) 0.32166(16) 0.26598(16) 0.0264(7) Uani 1 1 d . . . C18 C 1.0139(4) 0.25893(17) 0.27760(17) 0.0291(8) Uani 1 1 d . . . H18 H 0.9979 0.2477 0.3193 0.035 Uiso 1 1 calc R . . C19 C 1.0035(4) 0.21299(17) 0.22865(18) 0.0322(8) Uani 1 1 d . . . H19 H 0.9813 0.1712 0.2375 0.039 Uiso 1 1 calc R . . C20 C 1.0264(4) 0.22931(17) 0.16565(18) 0.0321(8) Uani 1 1 d . . . C21 C 1.0550(4) 0.29194(17) 0.15286(18) 0.0339(8) Uani 1 1 d . . . H21 H 1.0671 0.3033 0.1105 0.041 Uiso 1 1 calc R . . C22 C 1.0660(4) 0.33799(18) 0.20199(17) 0.0323(8) Uani 1 1 d . . . H22 H 1.0856 0.3800 0.1926 0.039 Uiso 1 1 calc R . . C23 C 0.5947(5) 0.7281(2) -0.0897(2) 0.0510(11) Uani 1 1 d . . . H23 H 0.6922 0.7251 -0.0913 0.061 Uiso 1 1 calc R . . C24 C 0.4887(6) 0.7139(2) -0.1470(2) 0.0593(13) Uani 1 1 d . . . H24 H 0.5136 0.7029 -0.1870 0.071 Uiso 1 1 calc R . . C25 C 0.3466(6) 0.7168(2) -0.1426(3) 0.0713(16) Uani 1 1 d . . . H25 H 0.2730 0.7061 -0.1795 0.086 Uiso 1 1 calc R . . C26 C 0.3123(5) 0.7354(2) -0.0842(3) 0.0619(14) Uani 1 1 d . . . H26 H 0.2156 0.7373 -0.0810 0.074 Uiso 1 1 calc R . . C27 C 0.4224(4) 0.75134(18) -0.0300(2) 0.0383(9) Uani 1 1 d . . . C28 C 0.3911(4) 0.77683(18) 0.0335(2) 0.0385(9) Uani 1 1 d . . . C29 C 0.2502(5) 0.7906(2) 0.0395(3) 0.0598(13) Uani 1 1 d . . . H29 H 0.1711 0.7839 0.0036 0.072 Uiso 1 1 calc R . . C30 C 0.2302(6) 0.8145(3) 0.1000(3) 0.0708(15) Uani 1 1 d . . . H30 H 0.1371 0.8240 0.1051 0.085 Uiso 1 1 calc R . . C31 C 0.3473(6) 0.8237(2) 0.1515(3) 0.0624(13) Uani 1 1 d . . . H31 H 0.3355 0.8390 0.1926 0.075 Uiso 1 1 calc R . . C32 C 0.4824(5) 0.8103(2) 0.1422(2) 0.0510(11) Uani 1 1 d . . . H32 H 0.5621 0.8170 0.1777 0.061 Uiso 1 1 calc R . . C33 C 0.7429(5) 0.4308(2) 0.0842(2) 0.0457(10) Uani 1 1 d . . . H33 H 0.8395 0.4270 0.0813 0.055 Uiso 1 1 calc R . . C34 C 0.6351(5) 0.4208(2) 0.0275(2) 0.0559(12) Uani 1 1 d . . . H34 H 0.6583 0.4094 -0.0128 0.067 Uiso 1 1 calc R . . C35 C 0.4939(5) 0.4277(2) 0.0312(2) 0.0524(12) Uani 1 1 d . . . H35 H 0.4194 0.4217 -0.0068 0.063 Uiso 1 1 calc R . . C36 C 0.4614(4) 0.4437(2) 0.0917(2) 0.0470(10) Uani 1 1 d . . . H36 H 0.3653 0.4490 0.0947 0.056 Uiso 1 1 calc R . . C37 C 0.5747(4) 0.45169(17) 0.14770(18) 0.0332(8) Uani 1 1 d . . . C38 C 0.5477(4) 0.46423(18) 0.21597(18) 0.0339(8) Uani 1 1 d . . . C39 C 0.4118(4) 0.4625(2) 0.2285(2) 0.0492(11) Uani 1 1 d . . . H39 H 0.3308 0.4555 0.1937 0.059 Uiso 1 1 calc R . . C40 C 0.3952(5) 0.4710(2) 0.2928(2) 0.0554(12) Uani 1 1 d . . . H40 H 0.3031 0.4697 0.3019 0.066 Uiso 1 1 calc R . . C41 C 0.5161(5) 0.4815(2) 0.3435(2) 0.0478(11) Uani 1 1 d . . . H41 H 0.5078 0.4862 0.3877 0.057 Uiso 1 1 calc R . . C42 C 0.6491(5) 0.4849(2) 0.3275(2) 0.0439(10) Uani 1 1 d . . . H42 H 0.7306 0.4933 0.3616 0.053 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.03043(15) 0.02856(15) 0.03230(15) -0.00126(11) -0.00160(11) -0.00120(11) Cd2 0.02656(14) 0.02903(15) 0.02855(14) 0.00418(11) 0.00276(10) 0.00105(11) O1 0.0464(16) 0.0405(16) 0.0373(15) 0.0118(13) 0.0148(13) 0.0049(13) O2 0.0569(19) 0.0540(19) 0.0521(17) 0.0123(15) 0.0343(15) 0.0152(15) O3 0.0449(16) 0.0451(17) 0.0559(17) 0.0065(14) 0.0277(14) 0.0099(13) O4 0.0353(14) 0.0337(15) 0.0460(15) 0.0101(13) 0.0131(12) 0.0082(12) O5 0.0368(17) 0.100(3) 0.076(2) -0.003(2) 0.0304(16) 0.0062(18) O6 0.0457(16) 0.0296(14) 0.0347(14) 0.0036(12) 0.0000(12) 0.0057(12) O7 0.0604(18) 0.0317(15) 0.0352(15) -0.0090(12) -0.0005(13) 0.0026(13) O8 0.076(2) 0.0409(17) 0.0329(15) -0.0116(13) -0.0080(14) 0.0077(16) O9 0.079(2) 0.0461(18) 0.0322(15) -0.0032(13) -0.0184(15) 0.0210(17) O10 0.067(2) 0.0322(15) 0.0370(15) -0.0071(12) 0.0041(14) 0.0030(15) O11 0.060(2) 0.098(3) 0.069(2) -0.010(2) 0.0270(18) -0.010(2) N1 0.0288(15) 0.0271(16) 0.0285(15) 0.0021(13) 0.0064(12) 0.0006(13) N2 0.0278(15) 0.0263(16) 0.0292(15) 0.0004(13) 0.0053(12) 0.0005(12) N3 0.0267(15) 0.0266(16) 0.0257(15) -0.0014(12) 0.0021(12) 0.0031(12) N4 0.0290(15) 0.0274(16) 0.0275(15) 0.0014(13) 0.0015(12) 0.0036(13) N5 0.0365(18) 0.0367(18) 0.0358(18) -0.0027(15) 0.0007(14) 0.0004(15) N6 0.0379(18) 0.0360(18) 0.0389(18) -0.0026(15) 0.0040(15) 0.0020(15) N7 0.0354(17) 0.0318(17) 0.0374(17) -0.0062(14) 0.0076(14) -0.0010(14) N8 0.0279(16) 0.0361(18) 0.0359(17) -0.0031(14) 0.0089(13) -0.0016(14) C1 0.039(2) 0.040(2) 0.0297(19) 0.0019(17) 0.0089(17) -0.0030(18) C2 0.0308(18) 0.0310(19) 0.0253(17) -0.0015(15) 0.0067(15) -0.0017(15) C3 0.0274(18) 0.0283(19) 0.0290(18) 0.0005(15) 0.0054(15) -0.0001(15) C4 0.0257(18) 0.033(2) 0.039(2) -0.0021(17) 0.0084(16) 0.0005(16) C5 0.0284(18) 0.0250(18) 0.0300(18) -0.0011(15) 0.0056(15) -0.0024(15) C6 0.0306(19) 0.0245(18) 0.0345(19) -0.0004(15) 0.0072(16) -0.0003(15) C7 0.0270(18) 0.038(2) 0.036(2) -0.0014(17) 0.0070(16) 0.0029(16) C8 0.039(2) 0.042(2) 0.035(2) -0.0023(18) 0.0143(17) 0.0030(18) C9 0.033(2) 0.043(2) 0.054(3) -0.005(2) 0.0178(19) 0.0024(18) C10 0.028(2) 0.050(3) 0.061(3) -0.001(2) 0.0048(19) 0.0046(19) C11 0.036(2) 0.040(2) 0.031(2) -0.0014(17) 0.0052(17) 0.0008(17) C12 0.0286(19) 0.031(2) 0.037(2) -0.0002(17) 0.0058(16) -0.0005(16) C13 0.0248(17) 0.0256(18) 0.0270(17) -0.0025(15) 0.0054(14) 0.0009(14) C14 0.0284(18) 0.0289(19) 0.0222(16) -0.0019(15) 0.0040(14) 0.0011(15) C15 0.047(2) 0.040(2) 0.0276(19) -0.0023(18) -0.0007(17) 0.0062(19) C16 0.0227(17) 0.0256(18) 0.0292(18) 0.0012(15) 0.0049(14) 0.0015(14) C17 0.0204(16) 0.0285(19) 0.0269(18) -0.0015(15) -0.0017(14) 0.0025(14) C18 0.0251(17) 0.036(2) 0.0245(17) 0.0058(15) 0.0014(14) 0.0003(15) C19 0.0330(19) 0.0238(19) 0.037(2) 0.0045(16) 0.0029(16) 0.0003(15) C20 0.0302(19) 0.032(2) 0.0299(19) -0.0062(16) -0.0020(15) 0.0060(16) C21 0.043(2) 0.035(2) 0.0249(18) -0.0003(16) 0.0092(16) 0.0003(17) C22 0.0333(19) 0.0278(19) 0.035(2) 0.0016(16) 0.0064(16) -0.0018(16) C23 0.054(3) 0.059(3) 0.038(2) -0.007(2) 0.006(2) 0.002(2) C24 0.082(4) 0.053(3) 0.036(2) -0.006(2) -0.001(2) 0.005(3) C25 0.069(4) 0.058(3) 0.064(3) -0.010(3) -0.032(3) 0.009(3) C26 0.040(2) 0.064(3) 0.071(3) -0.014(3) -0.011(2) 0.006(2) C27 0.035(2) 0.029(2) 0.046(2) 0.0056(18) 0.0003(18) -0.0018(17) C28 0.032(2) 0.032(2) 0.048(2) 0.0073(18) 0.0027(18) 0.0007(17) C29 0.034(2) 0.062(3) 0.082(4) 0.010(3) 0.010(2) 0.001(2) C30 0.056(3) 0.073(4) 0.093(4) 0.003(3) 0.038(3) 0.013(3) C31 0.069(3) 0.060(3) 0.069(3) -0.002(3) 0.037(3) 0.009(3) C32 0.055(3) 0.052(3) 0.046(3) -0.007(2) 0.011(2) 0.001(2) C33 0.041(2) 0.055(3) 0.040(2) -0.009(2) 0.0085(19) -0.003(2) C34 0.056(3) 0.069(3) 0.042(2) -0.013(2) 0.011(2) -0.006(2) C35 0.048(3) 0.068(3) 0.035(2) -0.004(2) -0.0039(19) -0.009(2) C36 0.036(2) 0.061(3) 0.041(2) 0.001(2) 0.0017(18) -0.001(2) C37 0.0299(19) 0.030(2) 0.038(2) -0.0004(17) 0.0040(16) -0.0036(16) C38 0.033(2) 0.032(2) 0.036(2) -0.0007(17) 0.0069(16) 0.0006(17) C39 0.028(2) 0.063(3) 0.056(3) -0.004(2) 0.0076(19) -0.002(2) C40 0.038(2) 0.064(3) 0.072(3) -0.007(3) 0.029(2) -0.005(2) C41 0.056(3) 0.050(3) 0.046(2) -0.009(2) 0.030(2) -0.004(2) C42 0.042(2) 0.053(3) 0.037(2) -0.0034(19) 0.0097(18) -0.006(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 Cd1 O1 2.346(3) . ? Cd1 O9 2.570(3) 2_755 ? Cd1 N1 2.313(3) . ? Cd1 N4 2.259(3) 2_755 ? Cd1 N5 2.300(3) . ? Cd1 N6 2.341(3) . ? Cd2 O4 2.406(3) . ? Cd2 O6 2.444(2) . ? Cd2 N2 2.263(3) . ? Cd2 N3 2.260(3) . ? Cd2 N7 2.391(3) . ? Cd2 N8 2.332(3) . ? O1 C1 1.246(4) . ? O2 C1 1.281(5) . ? O3 C4 1.285(4) . ? O4 C4 1.244(4) . ? O5 H5 0.8200 . ? O5 C9 1.359(5) . ? O6 C12 1.255(4) . ? O7 C12 1.268(4) . ? O8 C15 1.290(4) . ? O9 Cd1 2.570(3) 2_745 ? O9 C15 1.220(4) . ? O10 H10 0.8200 . ? O10 C20 1.355(4) . ? O11 H11A 0.8498 . ? O11 H11B 0.8464 . ? N1 C2 1.377(4) . ? N1 C5 1.349(4) . ? N2 C3 1.373(4) . ? N2 C5 1.346(4) . ? N3 C13 1.379(4) . ? N3 C16 1.340(4) . ? N4 Cd1 2.259(3) 2_745 ? N4 C14 1.374(4) . ? N4 C16 1.354(4) . ? N5 C23 1.327(5) . ? N5 C27 1.333(5) . ? N6 C28 1.342(5) . ? N6 C32 1.337(5) . ? N7 C33 1.339(5) . ? N7 C37 1.345(4) . ? N8 C38 1.351(4) . ? N8 C42 1.344(5) . ? C1 C2 1.477(5) . ? C2 C3 1.380(5) . ? C3 C4 1.475(5) . ? C5 C6 1.467(5) . ? C6 C7 1.387(5) . ? C6 C11 1.394(5) . ? C7 H7 0.9300 . ? C7 C8 1.371(5) . ? C8 H8 0.9300 . ? C8 C9 1.389(5) . ? C9 C10 1.381(6) . ? C10 H10A 0.9300 . ? C10 C11 1.380(5) . ? C11 H11 0.9300 . ? C12 C13 1.484(5) . ? C13 C14 1.381(5) . ? C14 C15 1.484(5) . ? C16 C17 1.465(5) . ? C17 C18 1.388(5) . ? C17 C22 1.401(5) . ? C18 H18 0.9300 . ? C18 C19 1.377(5) . ? C19 H19 0.9300 . ? C19 C20 1.397(5) . ? C20 C21 1.379(5) . ? C21 H21 0.9300 . ? C21 C22 1.381(5) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C23 C24 1.388(6) . ? C24 H24 0.9300 . ? C24 C25 1.364(7) . ? C25 H25 0.9300 . ? C25 C26 1.364(7) . ? C26 H26 0.9300 . ? C26 C27 1.376(6) . ? C27 C28 1.495(6) . ? C28 C29 1.392(6) . ? C29 H29 0.9300 . ? C29 C30 1.386(7) . ? C30 H30 0.9300 . ? C30 C31 1.356(7) . ? C31 H31 0.9300 . ? C31 C32 1.360(6) . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? C33 C34 1.374(6) . ? C34 H34 0.9300 . ? C34 C35 1.359(6) . ? C35 H35 0.9300 . ? C35 C36 1.381(6) . ? C36 H36 0.9300 . ? C36 C37 1.387(5) . ? C37 C38 1.499(5) . ? C38 C39 1.364(5) . ? C39 H39 0.9300 . ? C39 C40 1.370(6) . ? C40 H40 0.9300 . ? C40 C41 1.373(6) . ? C41 H41 0.9300 . ? C41 C42 1.369(6) . ? C42 H42 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cd1 O9 96.68(10) . 2_755 ? N1 Cd1 O1 73.02(9) . . ? N1 Cd1 O9 166.96(10) . 2_755 ? N1 Cd1 N6 99.45(10) . . ? N4 Cd1 O1 101.03(10) 2_755 . ? N4 Cd1 O9 69.47(9) 2_755 2_755 ? N4 Cd1 N1 119.65(10) 2_755 . ? N4 Cd1 N5 141.08(11) 2_755 . ? N4 Cd1 N6 98.71(11) 2_755 . ? N5 Cd1 O1 91.17(11) . . ? N5 Cd1 O9 72.50(10) . 2_755 ? N5 Cd1 N1 99.24(11) . . ? N5 Cd1 N6 71.51(11) . . ? N6 Cd1 O1 160.07(10) . . ? N6 Cd1 O9 87.63(11) . 2_755 ? O4 Cd2 O6 108.74(9) . . ? N2 Cd2 O4 72.44(9) . . ? N2 Cd2 O6 90.59(9) . . ? N2 Cd2 N7 84.99(10) . . ? N2 Cd2 N8 104.68(10) . . ? N3 Cd2 O4 92.71(9) . . ? N3 Cd2 O6 72.00(9) . . ? N3 Cd2 N2 152.49(10) . . ? N3 Cd2 N7 118.68(10) . . ? N3 Cd2 N8 97.22(10) . . ? N7 Cd2 O4 89.47(10) . . ? N7 Cd2 O6 159.03(9) . . ? N8 Cd2 O4 159.03(10) . . ? N8 Cd2 O6 91.91(10) . . ? N8 Cd2 N7 69.56(10) . . ? C1 O1 Cd1 116.1(2) . . ? C4 O4 Cd2 114.4(2) . . ? C9 O5 H5 109.5 . . ? C12 O6 Cd2 114.6(2) . . ? C15 O9 Cd1 113.4(2) . 2_745 ? C20 O10 H10 109.5 . . ? H11A O11 H11B 99.3 . . ? C2 N1 Cd1 111.4(2) . . ? C5 N1 Cd1 142.0(2) . . ? C5 N1 C2 105.0(3) . . ? C3 N2 Cd2 114.4(2) . . ? C5 N2 Cd2 139.9(2) . . ? C5 N2 C3 105.5(3) . . ? C13 N3 Cd2 114.8(2) . . ? C16 N3 Cd2 139.6(2) . . ? C16 N3 C13 105.4(3) . . ? C14 N4 Cd1 117.9(2) . 2_745 ? C16 N4 Cd1 136.8(2) . 2_745 ? C16 N4 C14 105.3(3) . . ? C23 N5 Cd1 122.7(3) . . ? C23 N5 C27 119.4(4) . . ? C27 N5 Cd1 117.9(3) . . ? C28 N6 Cd1 116.4(3) . . ? C32 N6 Cd1 125.1(3) . . ? C32 N6 C28 118.5(4) . . ? C33 N7 Cd2 123.8(3) . . ? C33 N7 C37 118.8(3) . . ? C37 N7 Cd2 114.7(2) . . ? C38 N8 Cd2 118.4(2) . . ? C42 N8 Cd2 123.7(3) . . ? C42 N8 C38 117.5(3) . . ? O1 C1 O2 123.8(3) . . ? O1 C1 C2 118.6(3) . . ? O2 C1 C2 117.5(3) . . ? N1 C2 C1 120.3(3) . . ? N1 C2 C3 108.5(3) . . ? C3 C2 C1 131.1(3) . . ? N2 C3 C2 108.2(3) . . ? N2 C3 C4 119.5(3) . . ? C2 C3 C4 132.2(3) . . ? O3 C4 C3 117.6(3) . . ? O4 C4 O3 123.2(3) . . ? O4 C4 C3 119.2(3) . . ? N1 C5 C6 125.5(3) . . ? N2 C5 N1 112.9(3) . . ? N2 C5 C6 121.6(3) . . ? C7 C6 C5 120.1(3) . . ? C7 C6 C11 117.9(3) . . ? C11 C6 C5 121.8(3) . . ? C6 C7 H7 119.1 . . ? C8 C7 C6 121.7(3) . . ? C8 C7 H7 119.1 . . ? C7 C8 H8 120.0 . . ? C7 C8 C9 119.9(4) . . ? C9 C8 H8 120.0 . . ? O5 C9 C8 122.7(4) . . ? O5 C9 C10 118.2(4) . . ? C10 C9 C8 119.1(4) . . ? C9 C10 H10A 119.7 . . ? C11 C10 C9 120.7(4) . . ? C11 C10 H10A 119.7 . . ? C6 C11 H11 119.7 . . ? C10 C11 C6 120.5(4) . . ? C10 C11 H11 119.7 . . ? O6 C12 O7 123.7(3) . . ? O6 C12 C13 117.8(3) . . ? O7 C12 C13 118.4(3) . . ? N3 C13 C12 120.4(3) . . ? N3 C13 C14 108.3(3) . . ? C14 C13 C12 131.3(3) . . ? N4 C14 C13 108.3(3) . . ? N4 C14 C15 120.0(3) . . ? C13 C14 C15 131.5(3) . . ? O8 C15 C14 117.4(3) . . ? O9 C15 O8 123.6(3) . . ? O9 C15 C14 118.9(3) . . ? N3 C16 N4 112.8(3) . . ? N3 C16 C17 125.0(3) . . ? N4 C16 C17 122.1(3) . . ? C18 C17 C16 121.3(3) . . ? C18 C17 C22 118.3(3) . . ? C22 C17 C16 120.4(3) . . ? C17 C18 H18 119.3 . . ? C19 C18 C17 121.4(3) . . ? C19 C18 H18 119.3 . . ? C18 C19 H19 120.1 . . ? C18 C19 C20 119.9(3) . . ? C20 C19 H19 120.1 . . ? O10 C20 C19 122.7(3) . . ? O10 C20 C21 118.1(3) . . ? C21 C20 C19 119.1(3) . . ? C20 C21 H21 119.5 . . ? C20 C21 C22 121.0(3) . . ? C22 C21 H21 119.5 . . ? C17 C22 H22 119.9 . . ? C21 C22 C17 120.2(3) . . ? C21 C22 H22 119.9 . . ? N5 C23 H23 118.8 . . ? N5 C23 C24 122.3(5) . . ? C24 C23 H23 118.8 . . ? C23 C24 H24 121.2 . . ? C25 C24 C23 117.6(5) . . ? C25 C24 H24 121.2 . . ? C24 C25 H25 119.9 . . ? C26 C25 C24 120.2(4) . . ? C26 C25 H25 119.9 . . ? C25 C26 H26 120.4 . . ? C25 C26 C27 119.3(5) . . ? C27 C26 H26 120.4 . . ? N5 C27 C26 121.1(4) . . ? N5 C27 C28 117.3(3) . . ? C26 C27 C28 121.7(4) . . ? N6 C28 C27 116.8(3) . . ? N6 C28 C29 121.0(4) . . ? C29 C28 C27 122.1(4) . . ? C28 C29 H29 120.6 . . ? C30 C29 C28 118.7(5) . . ? C30 C29 H29 120.6 . . ? C29 C30 H30 120.2 . . ? C31 C30 C29 119.5(5) . . ? C31 C30 H30 120.2 . . ? C30 C31 H31 120.5 . . ? C30 C31 C32 118.9(5) . . ? C32 C31 H31 120.5 . . ? N6 C32 C31 123.3(4) . . ? N6 C32 H32 118.4 . . ? C31 C32 H32 118.4 . . ? N7 C33 H33 118.7 . . ? N7 C33 C34 122.6(4) . . ? C34 C33 H33 118.7 . . ? C33 C34 H34 120.6 . . ? C35 C34 C33 118.8(4) . . ? C35 C34 H34 120.6 . . ? C34 C35 H35 120.1 . . ? C34 C35 C36 119.8(4) . . ? C36 C35 H35 120.1 . . ? C35 C36 H36 120.6 . . ? C35 C36 C37 118.9(4) . . ? C37 C36 H36 120.6 . . ? N7 C37 C36 121.1(3) . . ? N7 C37 C38 116.9(3) . . ? C36 C37 C38 121.9(3) . . ? N8 C38 C37 115.5(3) . . ? N8 C38 C39 122.0(3) . . ? C39 C38 C37 122.5(3) . . ? C38 C39 H39 120.2 . . ? C38 C39 C40 119.7(4) . . ? C40 C39 H39 120.2 . . ? C39 C40 H40 120.3 . . ? C39 C40 C41 119.3(4) . . ? C41 C40 H40 120.3 . . ? C40 C41 H41 120.8 . . ? C42 C41 C40 118.4(4) . . ? C42 C41 H41 120.8 . . ? N8 C42 C41 123.1(4) . . ? N8 C42 H42 118.4 . . ? C41 C42 H42 118.4 . . ? 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 O11 0.82 1.94 2.751(5) 173.2 . O10 H10 O6 0.82 2.07 2.884(4) 171.1 2_745 O10 H10 O7 0.82 2.61 3.174(4) 126.8 2_745 O11 H11A O7 0.85 2.11 2.956(4) 179.3 1_455 O11 H11B O9 0.85 2.44 2.976(5) 121.9 3_766 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 Cd1 O1 C1 O2 -177.4(3) . . . . ? Cd1 O1 C1 C2 1.7(4) . . . . ? Cd1 O9 C15 O8 177.4(3) 2_745 . . . ? Cd1 O9 C15 C14 -4.4(5) 2_745 . . . ? Cd1 N1 C2 C1 -8.5(4) . . . . ? Cd1 N1 C2 C3 168.5(2) . . . . ? Cd1 N1 C5 N2 -162.2(3) . . . . ? Cd1 N1 C5 C6 19.9(6) . . . . ? Cd1 N4 C14 C13 178.5(2) 2_745 . . . ? Cd1 N4 C14 C15 3.7(4) 2_745 . . . ? Cd1 N4 C16 N3 -177.8(2) 2_745 . . . ? Cd1 N4 C16 C17 -1.5(5) 2_745 . . . ? Cd1 N5 C23 C24 -178.8(3) . . . . ? Cd1 N5 C27 C26 -178.4(3) . . . . ? Cd1 N5 C27 C28 3.1(4) . . . . ? Cd1 N6 C28 C27 3.4(4) . . . . ? Cd1 N6 C28 C29 -174.3(3) . . . . ? Cd1 N6 C32 C31 175.1(3) . . . . ? Cd2 O4 C4 O3 -176.2(3) . . . . ? Cd2 O4 C4 C3 2.9(4) . . . . ? Cd2 O6 C12 O7 -178.0(3) . . . . ? Cd2 O6 C12 C13 3.2(4) . . . . ? Cd2 N2 C3 C2 176.5(2) . . . . ? Cd2 N2 C3 C4 0.4(4) . . . . ? Cd2 N2 C5 N1 -175.1(2) . . . . ? Cd2 N2 C5 C6 2.9(5) . . . . ? Cd2 N3 C13 C12 -5.8(4) . . . . ? Cd2 N3 C13 C14 176.2(2) . . . . ? Cd2 N3 C16 N4 -174.4(2) . . . . ? Cd2 N3 C16 C17 9.3(6) . . . . ? Cd2 N7 C33 C34 -160.7(3) . . . . ? Cd2 N7 C37 C36 160.8(3) . . . . ? Cd2 N7 C37 C38 -21.9(4) . . . . ? Cd2 N8 C38 C37 10.2(4) . . . . ? Cd2 N8 C38 C39 -170.6(3) . . . . ? Cd2 N8 C42 C41 172.5(3) . . . . ? O1 Cd1 N1 C2 6.5(2) . . . . ? O1 Cd1 N1 C5 168.7(4) . . . . ? O1 Cd1 N5 C23 -13.1(3) . . . . ? O1 Cd1 N5 C27 169.0(3) . . . . ? O1 Cd1 N6 C28 -32.3(5) . . . . ? O1 Cd1 N6 C32 150.8(3) . . . . ? O1 C1 C2 N1 4.9(5) . . . . ? O1 C1 C2 C3 -171.3(4) . . . . ? O2 C1 C2 N1 -176.0(3) . . . . ? O2 C1 C2 C3 7.8(6) . . . . ? O4 Cd2 O6 C12 -91.2(2) . . . . ? O4 Cd2 N2 C3 0.7(2) . . . . ? O4 Cd2 N2 C5 174.7(4) . . . . ? O4 Cd2 N3 C13 114.0(2) . . . . ? O4 Cd2 N3 C16 -72.1(3) . . . . ? O4 Cd2 N7 C33 0.4(3) . . . . ? O4 Cd2 N7 C37 -160.6(3) . . . . ? O4 Cd2 N8 C38 -15.9(5) . . . . ? O4 Cd2 N8 C42 171.4(3) . . . . ? O5 C9 C10 C11 -176.0(4) . . . . ? O6 Cd2 O4 C4 -86.5(3) . . . . ? O6 Cd2 N2 C3 110.2(2) . . . . ? O6 Cd2 N2 C5 -75.8(4) . . . . ? O6 Cd2 N3 C13 5.1(2) . . . . ? O6 Cd2 N3 C16 179.1(4) . . . . ? O6 Cd2 N7 C33 151.3(3) . . . . ? O6 Cd2 N7 C37 -9.7(4) . . . . ? O6 Cd2 N8 C38 154.4(3) . . . . ? O6 Cd2 N8 C42 -18.3(3) . . . . ? O6 C12 C13 N3 1.6(5) . . . . ? O6 C12 C13 C14 179.1(4) . . . . ? O7 C12 C13 N3 -177.3(3) . . . . ? O7 C12 C13 C14 0.1(6) . . . . ? O9 Cd1 O1 C1 -176.3(3) 2_755 . . . ? O9 Cd1 N1 C2 45.3(5) 2_755 . . . ? O9 Cd1 N1 C5 -152.5(4) 2_755 . . . ? O9 Cd1 N5 C23 83.5(3) 2_755 . . . ? O9 Cd1 N5 C27 -94.4(3) 2_755 . . . ? O9 Cd1 N6 C28 70.9(3) 2_755 . . . ? O9 Cd1 N6 C32 -106.1(3) 2_755 . . . ? O10 C20 C21 C22 -179.1(3) . . . . ? N1 Cd1 O1 C1 -4.5(3) . . . . ? N1 Cd1 N5 C23 -86.1(3) . . . . ? N1 Cd1 N5 C27 96.0(3) . . . . ? N1 Cd1 N6 C28 -98.1(3) . . . . ? N1 Cd1 N6 C32 84.9(3) . . . . ? N1 C2 C3 N2 -0.2(4) . . . . ? N1 C2 C3 C4 175.3(3) . . . . ? N1 C5 C6 C7 -135.1(4) . . . . ? N1 C5 C6 C11 49.9(5) . . . . ? N2 Cd2 O4 C4 -2.0(2) . . . . ? N2 Cd2 O6 C12 -162.9(3) . . . . ? N2 Cd2 N3 C13 58.2(3) . . . . ? N2 Cd2 N3 C16 -127.8(3) . . . . ? N2 Cd2 N7 C33 72.8(3) . . . . ? N2 Cd2 N7 C37 -88.2(3) . . . . ? N2 Cd2 N8 C38 63.3(3) . . . . ? N2 Cd2 N8 C42 -109.4(3) . . . . ? N2 C3 C4 O3 176.8(3) . . . . ? N2 C3 C4 O4 -2.3(5) . . . . ? N2 C5 C6 C7 47.2(5) . . . . ? N2 C5 C6 C11 -127.8(4) . . . . ? N3 Cd2 O4 C4 -158.4(3) . . . . ? N3 Cd2 O6 C12 -4.6(2) . . . . ? N3 Cd2 N2 C3 60.7(3) . . . . ? N3 Cd2 N2 C5 -125.3(3) . . . . ? N3 Cd2 N7 C33 -92.4(3) . . . . ? N3 Cd2 N7 C37 106.6(3) . . . . ? N3 Cd2 N8 C38 -133.5(3) . . . . ? N3 Cd2 N8 C42 53.8(3) . . . . ? N3 C13 C14 N4 -0.3(4) . . . . ? N3 C13 C14 C15 173.7(4) . . . . ? N3 C16 C17 C18 -141.7(3) . . . . ? N3 C16 C17 C22 41.0(5) . . . . ? N4 Cd1 O1 C1 113.4(3) 2_755 . . . ? N4 Cd1 N1 C2 -86.8(2) 2_755 . . . ? N4 Cd1 N1 C5 75.5(4) 2_755 . . . ? N4 Cd1 N5 C23 96.1(3) 2_755 . . . ? N4 Cd1 N5 C27 -81.8(3) 2_755 . . . ? N4 Cd1 N6 C28 139.7(3) 2_755 . . . ? N4 Cd1 N6 C32 -37.3(3) 2_755 . . . ? N4 C14 C15 O8 179.3(3) . . . . ? N4 C14 C15 O9 1.0(6) . . . . ? N4 C16 C17 C18 42.3(5) . . . . ? N4 C16 C17 C22 -134.9(3) . . . . ? N5 Cd1 O1 C1 -103.8(3) . . . . ? N5 Cd1 N1 C2 94.9(2) . . . . ? N5 Cd1 N1 C5 -102.9(4) . . . . ? N5 Cd1 N6 C28 -1.4(3) . . . . ? N5 Cd1 N6 C32 -178.4(4) . . . . ? N5 C23 C24 C25 -2.1(7) . . . . ? N5 C27 C28 N6 -4.4(5) . . . . ? N5 C27 C28 C29 173.3(4) . . . . ? N6 Cd1 O1 C1 -74.7(4) . . . . ? N6 Cd1 N1 C2 167.5(2) . . . . ? N6 Cd1 N1 C5 -30.3(4) . . . . ? N6 Cd1 N5 C23 176.9(3) . . . . ? N6 Cd1 N5 C27 -1.0(3) . . . . ? N6 C28 C29 C30 -2.0(7) . . . . ? N7 Cd2 O4 C4 82.9(3) . . . . ? N7 Cd2 O6 C12 119.7(3) . . . . ? N7 Cd2 N2 C3 -90.3(2) . . . . ? N7 Cd2 N2 C5 83.7(4) . . . . ? N7 Cd2 N3 C13 -155.2(2) . . . . ? N7 Cd2 N3 C16 18.8(4) . . . . ? N7 Cd2 N8 C38 -15.5(3) . . . . ? N7 Cd2 N8 C42 171.8(3) . . . . ? N7 C33 C34 C35 1.5(7) . . . . ? N7 C37 C38 N8 8.4(5) . . . . ? N7 C37 C38 C39 -170.8(4) . . . . ? N8 Cd2 O4 C4 83.2(4) . . . . ? N8 Cd2 O6 C12 92.4(3) . . . . ? N8 Cd2 N2 C3 -157.6(2) . . . . ? N8 Cd2 N2 C5 16.3(4) . . . . ? N8 Cd2 N3 C13 -84.5(2) . . . . ? N8 Cd2 N3 C16 89.4(4) . . . . ? N8 Cd2 N7 C33 -179.5(3) . . . . ? N8 Cd2 N7 C37 19.6(2) . . . . ? N8 C38 C39 C40 -2.6(7) . . . . ? C1 C2 C3 N2 176.3(3) . . . . ? C1 C2 C3 C4 -8.2(7) . . . . ? C2 N1 C5 N2 0.7(4) . . . . ? C2 N1 C5 C6 -177.2(3) . . . . ? C2 C3 C4 O3 1.7(6) . . . . ? C2 C3 C4 O4 -177.4(4) . . . . ? C3 N2 C5 N1 -0.8(4) . . . . ? C3 N2 C5 C6 177.2(3) . . . . ? C5 N1 C2 C1 -177.2(3) . . . . ? C5 N1 C2 C3 -0.3(4) . . . . ? C5 N2 C3 C2 0.6(4) . . . . ? C5 N2 C3 C4 -175.6(3) . . . . ? C5 C6 C7 C8 -173.6(3) . . . . ? C5 C6 C11 C10 173.3(4) . . . . ? C6 C7 C8 C9 1.1(6) . . . . ? C7 C6 C11 C10 -1.8(6) . . . . ? C7 C8 C9 O5 175.7(4) . . . . ? C7 C8 C9 C10 -3.5(6) . . . . ? C8 C9 C10 C11 3.3(6) . . . . ? C9 C10 C11 C6 -0.6(6) . . . . ? C11 C6 C7 C8 1.6(6) . . . . ? C12 C13 C14 N4 -178.0(3) . . . . ? C12 C13 C14 C15 -4.0(6) . . . . ? C13 N3 C16 N4 -0.1(4) . . . . ? C13 N3 C16 C17 -176.3(3) . . . . ? C13 C14 C15 O8 5.9(6) . . . . ? C13 C14 C15 O9 -172.4(4) . . . . ? C14 N4 C16 N3 -0.1(4) . . . . ? C14 N4 C16 C17 176.3(3) . . . . ? C16 N3 C13 C12 178.2(3) . . . . ? C16 N3 C13 C14 0.2(4) . . . . ? C16 N4 C14 C13 0.2(4) . . . . ? C16 N4 C14 C15 -174.6(3) . . . . ? C16 C17 C18 C19 -175.0(3) . . . . ? C16 C17 C22 C21 175.3(3) . . . . ? C17 C18 C19 C20 -0.4(5) . . . . ? C18 C17 C22 C21 -2.1(5) . . . . ? C18 C19 C20 O10 179.4(3) . . . . ? C18 C19 C20 C21 -1.9(5) . . . . ? C19 C20 C21 C22 2.2(5) . . . . ? C20 C21 C22 C17 -0.2(5) . . . . ? C22 C17 C18 C19 2.3(5) . . . . ? C23 N5 C27 C26 3.7(6) . . . . ? C23 N5 C27 C28 -174.9(4) . . . . ? C23 C24 C25 C26 2.4(8) . . . . ? C24 C25 C26 C27 0.2(8) . . . . ? C25 C26 C27 N5 -3.3(7) . . . . ? C25 C26 C27 C28 175.2(4) . . . . ? C26 C27 C28 N6 177.1(4) . . . . ? C26 C27 C28 C29 -5.2(6) . . . . ? C27 N5 C23 C24 -0.9(6) . . . . ? C27 C28 C29 C30 -179.6(4) . . . . ? C28 N6 C32 C31 -1.8(7) . . . . ? C28 C29 C30 C31 0.0(8) . . . . ? C29 C30 C31 C32 1.1(8) . . . . ? C30 C31 C32 N6 -0.2(8) . . . . ? C32 N6 C28 C27 -179.4(3) . . . . ? C32 N6 C28 C29 2.9(6) . . . . ? C33 N7 C37 C36 -1.2(6) . . . . ? C33 N7 C37 C38 176.1(3) . . . . ? C33 C34 C35 C36 -0.9(7) . . . . ? C34 C35 C36 C37 -0.6(7) . . . . ? C35 C36 C37 N7 1.7(6) . . . . ? C35 C36 C37 C38 -175.4(4) . . . . ? C36 C37 C38 N8 -174.3(4) . . . . ? C36 C37 C38 C39 6.5(6) . . . . ? C37 N7 C33 C34 -0.5(6) . . . . ? C37 C38 C39 C40 176.5(4) . . . . ? C38 N8 C42 C41 -0.3(6) . . . . ? C38 C39 C40 C41 0.3(7) . . . . ? C39 C40 C41 C42 1.8(7) . . . . ? C40 C41 C42 N8 -1.9(7) . . . . ? C42 N8 C38 C37 -176.6(3) . . . . ? C42 N8 C38 C39 2.6(6) . . . . ? data_yzl47 _database_code_depnum_ccdc_archive 'CCDC 855104' #TrackingRef '47.cif' _audit_creation_date 2011-05-11 _audit_creation_method ; Olex2 1.1 (compiled 2011.02.15 svn.r1672, GUI svn.r3494) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'Sr, C12 H8 N2 O4, H2 O' _chemical_formula_sum 'C12 H10 N2 O5 Sr' _chemical_formula_weight 349.84 _chemical_melting_point ? _chemical_oxdiff_formula 'C11 H10 S O2' 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' O O 0.0106 0.0060 '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' Sr Sr -1.5307 3.2498 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y+1/2, -z+1/2' 3 '-x, -y, -z' 4 'x, -y-1/2, z-1/2' _cell_length_a 14.9469(7) _cell_length_b 6.6581(2) _cell_length_c 12.6986(5) _cell_angle_alpha 90.00 _cell_angle_beta 103.505(5) _cell_angle_gamma 90.00 _cell_volume 1228.80(9) _cell_formula_units_Z 4 _cell_measurement_reflns_used 2384 _cell_measurement_temperature 290.5 _cell_measurement_theta_max 26.3151 _cell_measurement_theta_min 2.8957 _exptl_absorpt_coefficient_mu 4.410 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.70336 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour ? _exptl_crystal_density_diffrn 1.891 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description ? _exptl_crystal_F_000 696 _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0320 _diffrn_reflns_av_unetI/netI 0.0847 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 5692 _diffrn_reflns_theta_full 26.37 _diffrn_reflns_theta_max 26.3151 _diffrn_reflns_theta_min 2.8957 _diffrn_ambient_temperature 290.5 _diffrn_detector_area_resol_mean 16.2312 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -92.00 -67.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - -17.1323 157.0000 157.0000 25 #__ type_ start__ end____ width___ exp.time_ 2 omega -53.00 -5.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - 19.7885 -37.0000 120.0000 48 #__ type_ start__ end____ width___ exp.time_ 3 omega 12.00 45.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - 19.7885 -37.0000 120.0000 33 #__ type_ start__ end____ width___ exp.time_ 4 omega -6.00 87.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - 19.7885 37.0000 -60.0000 93 #__ type_ start__ end____ width___ exp.time_ 5 omega 9.00 34.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - 19.7885 77.0000 150.0000 25 #__ type_ start__ end____ width___ exp.time_ 6 omega -50.00 -25.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - 19.7885 -77.0000 -30.0000 25 ; _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0316708000 _diffrn_orient_matrix_UB_12 0.0811659000 _diffrn_orient_matrix_UB_13 0.0084718000 _diffrn_orient_matrix_UB_21 -0.0364341000 _diffrn_orient_matrix_UB_22 0.0676215000 _diffrn_orient_matrix_UB_23 -0.0209630000 _diffrn_orient_matrix_UB_31 -0.0070439000 _diffrn_orient_matrix_UB_32 0.0138304000 _diffrn_orient_matrix_UB_33 0.0528499000 _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_source 'Enhance (Mo) X-ray Source' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 2067 _reflns_number_total 2506 _reflns_odcompleteness_completeness 99.82 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'A short history of SHELX (Sheldrick, 2007)' _refine_diff_density_max 0.808 _refine_diff_density_min -0.751 _refine_diff_density_rms 0.093 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 180 _refine_ls_number_reflns 2506 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0481 _refine_ls_R_factor_gt 0.0346 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0372P)^2^+0.9528P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0779 _refine_ls_wR_factor_ref 0.0836 _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 0.47417(2) 0.06495(5) 0.32338(2) 0.01799(12) Uani 1 1 d . . . O1 O 0.60844(17) -0.2856(4) -0.15237(17) 0.0228(5) Uani 1 1 d . . . O2 O 0.58015(18) -0.3662(4) 0.00501(18) 0.0266(6) Uani 1 1 d . . . O3 O 0.52613(16) -0.0675(3) 0.14438(18) 0.0189(5) Uani 1 1 d . . . O4 O 0.59363(16) 0.2151(3) 0.21377(18) 0.0217(5) Uani 1 1 d . . . O5 O 0.28224(18) 0.0764(4) 0.27725(19) 0.0298(6) Uani 1 1 d D . . H5A H 0.3204 0.0929 0.3378 0.036 Uiso 1 1 d RD . . N1 N 0.7178(2) 0.0350(4) -0.0643(2) 0.0206(6) Uani 1 1 d . . . N2 N 0.7027(2) 0.2295(5) 0.0704(2) 0.0214(7) Uani 1 1 d . . . C1 C 0.6135(2) -0.2501(5) -0.0537(2) 0.0182(7) Uani 1 1 d . . . C2 C 0.6595(2) -0.0569(5) -0.0101(2) 0.0172(7) Uani 1 1 d . . . C3 C 0.6486(2) 0.0629(5) 0.0741(3) 0.0168(7) Uani 1 1 d . . . C4 C 0.5856(2) 0.0670(5) 0.1496(2) 0.0170(7) Uani 1 1 d . . . C5 C 0.7423(2) 0.2084(5) -0.0144(3) 0.0202(7) Uani 1 1 d . . . C6 C 0.8021(2) 0.3619(5) -0.0455(3) 0.0240(8) Uani 1 1 d . . . C7 C 0.8403(3) 0.5151(6) 0.0236(4) 0.0394(10) Uani 1 1 d . . . H7 H 0.8307 0.5188 0.0934 0.047 Uiso 1 1 calc R . . C8 C 0.8922(3) 0.6626(7) -0.0091(4) 0.0491(12) Uani 1 1 d . . . H8 H 0.9176 0.7635 0.0393 0.059 Uiso 1 1 calc R . . C9 C 0.9075(3) 0.6644(7) -0.1118(4) 0.0513(9) Uani 1 1 d U . . C10 C 0.8695(3) 0.5127(7) -0.1809(4) 0.0431(11) Uani 1 1 d . . . H10 H 0.8790 0.5111 -0.2508 0.052 Uiso 1 1 calc R . . C11 C 0.8169(3) 0.3604(6) -0.1494(3) 0.0368(10) Uani 1 1 d . . . H11 H 0.7920 0.2589 -0.1977 0.044 Uiso 1 1 calc R . . C12 C 0.9642(3) 0.8298(7) -0.1479(4) 0.0513(9) Uani 1 1 d U . . H12A H 0.9354 0.9574 -0.1436 0.077 Uiso 1 1 calc R . . H12B H 0.9680 0.8055 -0.2213 0.077 Uiso 1 1 calc R . . H12C H 1.0250 0.8306 -0.1017 0.077 Uiso 1 1 calc R . . H5B H 0.2735 0.0368 0.2122 0.062 Uiso 1 1 d RD . . H2 H 0.705(3) 0.326(7) 0.106(3) 0.035(13) 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 0.0321(2) 0.00899(17) 0.01538(17) 0.00037(14) 0.01060(13) 0.00105(15) O1 0.0373(14) 0.0169(12) 0.0156(12) -0.0024(10) 0.0094(10) -0.0040(11) O2 0.0451(16) 0.0176(13) 0.0200(12) -0.0014(11) 0.0133(12) -0.0078(12) O3 0.0279(13) 0.0113(11) 0.0194(11) 0.0016(10) 0.0095(10) -0.0027(11) O4 0.0346(14) 0.0122(11) 0.0212(12) -0.0043(10) 0.0122(11) -0.0007(11) O5 0.0430(15) 0.0311(15) 0.0161(12) -0.0012(12) 0.0084(11) -0.0020(13) N1 0.0298(16) 0.0156(15) 0.0185(14) -0.0020(12) 0.0102(12) -0.0017(13) N2 0.0300(17) 0.0143(15) 0.0210(15) -0.0054(14) 0.0084(13) -0.0053(13) C1 0.0258(18) 0.0144(17) 0.0154(16) 0.0013(14) 0.0067(14) 0.0049(14) C2 0.0249(17) 0.0148(16) 0.0123(15) 0.0031(14) 0.0051(13) 0.0018(15) C3 0.0232(17) 0.0117(15) 0.0160(15) 0.0006(14) 0.0057(13) -0.0008(15) C4 0.0240(17) 0.0129(16) 0.0144(16) 0.0035(15) 0.0048(13) 0.0042(15) C5 0.0240(18) 0.0203(18) 0.0161(16) -0.0041(15) 0.0045(14) -0.0013(15) C6 0.0253(19) 0.0226(18) 0.0257(18) 0.0008(16) 0.0093(15) -0.0007(16) C7 0.051(3) 0.034(2) 0.037(2) -0.010(2) 0.018(2) -0.016(2) C8 0.058(3) 0.036(3) 0.057(3) -0.009(2) 0.021(2) -0.022(2) C9 0.0450(19) 0.042(2) 0.069(2) 0.0107(19) 0.0183(17) -0.0154(17) C10 0.047(3) 0.044(3) 0.046(3) 0.010(2) 0.026(2) -0.007(2) C11 0.048(3) 0.034(2) 0.033(2) -0.0019(19) 0.0184(19) -0.009(2) C12 0.0450(19) 0.042(2) 0.069(2) 0.0107(19) 0.0183(17) -0.0154(17) _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 Sr1 3.9779(3) 2_645 ? Sr1 O1 2.700(2) 4_556 ? Sr1 O1 2.673(2) 3_655 ? Sr1 O2 2.539(2) 2_655 ? Sr1 O2 2.806(2) 4_556 ? Sr1 O3 2.481(2) 2_655 ? Sr1 O3 2.715(2) . ? Sr1 O4 2.540(2) 2_645 ? Sr1 O4 2.699(2) . ? Sr1 O5 2.792(3) . ? Sr1 H5A 2.3558 . ? Sr1 C1 3.107(3) 4_556 ? Sr1 C4 3.059(3) . ? O1 Sr1 2.700(2) 4 ? O1 Sr1 2.673(2) 3_655 ? O1 C1 1.259(4) . ? O2 Sr1 2.806(2) 4 ? O2 Sr1 2.539(2) 2_645 ? O2 C1 1.256(4) . ? O3 Sr1 2.481(2) 2_645 ? O3 C4 1.252(4) . ? O4 Sr1 2.540(2) 2_655 ? O4 C4 1.266(4) . ? O5 H5A 0.8504 . ? O5 H5B 0.8479 . ? N1 C2 1.375(4) . ? N1 C5 1.327(4) . ? N2 C3 1.380(4) . ? N2 C5 1.352(4) . ? N2 H2 0.79(4) . ? C1 Sr1 3.107(3) 4 ? C1 C2 1.501(5) . ? C2 C3 1.374(4) . ? C3 C4 1.493(4) . ? C5 C6 1.471(5) . ? C6 C7 1.380(5) . ? C6 C11 1.388(5) . ? C7 H7 0.9300 . ? C7 C8 1.375(6) . ? C8 H8 0.9300 . ? C8 C9 1.375(6) . ? C9 C10 1.371(7) . ? C9 C12 1.524(6) . ? C10 H10 0.9300 . ? C10 C11 1.398(6) . ? C11 H11 0.9300 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 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 Sr1 Sr1 H5A 113.7 2_645 . ? O1 Sr1 Sr1 41.99(5) 4_556 2_645 ? O1 Sr1 Sr1 100.53(5) 3_655 2_645 ? O1 Sr1 O1 131.39(4) 3_655 4_556 ? O1 Sr1 O2 172.69(7) 3_655 4_556 ? O1 Sr1 O2 47.13(6) 4_556 4_556 ? O1 Sr1 O3 61.42(7) 4_556 . ? O1 Sr1 O3 70.53(7) 3_655 . ? O1 Sr1 O4 67.25(7) 3_655 . ? O1 Sr1 O5 63.73(7) 3_655 . ? O1 Sr1 O5 137.96(7) 4_556 . ? O1 Sr1 H5A 139.3 4_556 . ? O1 Sr1 H5A 75.3 3_655 . ? O1 Sr1 C1 23.75(7) 4_556 4_556 ? O1 Sr1 C1 155.13(7) 3_655 4_556 ? O1 Sr1 C4 64.55(7) 4_556 . ? O1 Sr1 C4 68.74(8) 3_655 . ? O2 Sr1 Sr1 133.57(6) 2_655 2_645 ? O2 Sr1 Sr1 81.74(5) 4_556 2_645 ? O2 Sr1 O1 113.87(7) 2_655 4_556 ? O2 Sr1 O1 114.73(7) 2_655 3_655 ? O2 Sr1 O2 67.16(9) 2_655 4_556 ? O2 Sr1 O3 171.35(7) 2_655 . ? O2 Sr1 O4 139.33(8) 2_655 . ? O2 Sr1 O4 97.54(8) 2_655 2_645 ? O2 Sr1 O5 69.89(8) 2_655 . ? O2 Sr1 H5A 53.5 2_655 . ? O2 Sr1 H5A 110.3 4_556 . ? O2 Sr1 C1 90.12(8) 2_655 4_556 ? O2 Sr1 C1 23.83(7) 4_556 4_556 ? O2 Sr1 C4 107.29(8) 4_556 . ? O2 Sr1 C4 162.84(9) 2_655 . ? O3 Sr1 Sr1 37.93(5) . 2_645 ? O3 Sr1 Sr1 155.60(5) 2_655 2_645 ? O3 Sr1 O1 133.65(8) 2_655 4_556 ? O3 Sr1 O1 64.77(7) 2_655 3_655 ? O3 Sr1 O2 70.55(7) 2_655 2_655 ? O3 Sr1 O2 110.60(7) 2_655 4_556 ? O3 Sr1 O2 108.55(7) . 4_556 ? O3 Sr1 O3 118.06(6) 2_655 . ? O3 Sr1 O4 75.33(7) 2_655 . ? O3 Sr1 O4 156.79(8) 2_655 2_645 ? O3 Sr1 O5 88.07(7) 2_655 . ? O3 Sr1 O5 108.30(7) . . ? O3 Sr1 H5A 82.5 2_655 . ? O3 Sr1 H5A 124.5 . . ? O3 Sr1 C1 127.55(8) 2_655 4_556 ? O3 Sr1 C1 84.95(7) . 4_556 ? O3 Sr1 C4 24.12(8) . . ? O3 Sr1 C4 97.86(8) 2_655 . ? O4 Sr1 Sr1 42.11(5) 2_645 2_645 ? O4 Sr1 Sr1 81.04(5) . 2_645 ? O4 Sr1 O1 75.54(7) . 4_556 ? O4 Sr1 O1 105.34(7) 2_645 3_655 ? O4 Sr1 O1 69.10(7) 2_645 4_556 ? O4 Sr1 O2 81.05(7) 2_645 4_556 ? O4 Sr1 O2 106.50(7) . 4_556 ? O4 Sr1 O3 74.12(7) 2_645 . ? O4 Sr1 O3 48.36(7) . . ? O4 Sr1 O4 121.81(6) 2_645 . ? O4 Sr1 O5 130.75(7) . . ? O4 Sr1 O5 68.92(8) 2_645 . ? O4 Sr1 H5A 74.5 2_645 . ? O4 Sr1 H5A 141.8 . . ? O4 Sr1 C1 93.57(8) . 4_556 ? O4 Sr1 C1 70.49(8) 2_645 4_556 ? O4 Sr1 C4 24.40(8) . . ? O4 Sr1 C4 97.52(8) 2_645 . ? O5 Sr1 Sr1 103.12(5) . 2_645 ? O5 Sr1 O2 122.72(7) . 4_556 ? O5 Sr1 H5A 16.4 . . ? O5 Sr1 C1 131.26(8) . 4_556 ? O5 Sr1 C4 123.66(8) . . ? C1 Sr1 Sr1 59.33(6) 4_556 2_645 ? C1 Sr1 H5A 124.5 4_556 . ? C4 Sr1 Sr1 57.86(6) . 2_645 ? C4 Sr1 H5A 139.6 . . ? C4 Sr1 C1 87.21(8) . 4_556 ? Sr1 O1 Sr1 95.50(8) 3_655 4 ? C1 O1 Sr1 96.5(2) . 4 ? C1 O1 Sr1 127.9(2) . 3_655 ? Sr1 O2 Sr1 112.84(9) 2_645 4 ? C1 O2 Sr1 91.64(19) . 4 ? C1 O2 Sr1 150.7(2) . 2_645 ? Sr1 O3 Sr1 99.80(7) 2_645 . ? C4 O3 Sr1 93.51(18) . . ? C4 O3 Sr1 136.5(2) . 2_645 ? Sr1 O4 Sr1 98.75(7) 2_655 . ? C4 O4 Sr1 93.92(19) . . ? C4 O4 Sr1 128.3(2) . 2_655 ? Sr1 O5 H5A 51.3 . . ? Sr1 O5 H5B 96.5 . . ? H5A O5 H5B 147.1 . . ? C5 N1 C2 106.5(3) . . ? C3 N2 H2 126(3) . . ? C5 N2 C3 108.2(3) . . ? C5 N2 H2 125(3) . . ? O1 C1 Sr1 59.72(17) . 4 ? O1 C1 C2 116.4(3) . . ? O2 C1 Sr1 64.53(18) . 4 ? O2 C1 O1 122.3(3) . . ? O2 C1 C2 121.3(3) . . ? C2 C1 Sr1 163.4(2) . 4 ? N1 C2 C1 119.1(3) . . ? C3 C2 N1 109.6(3) . . ? C3 C2 C1 131.1(3) . . ? N2 C3 C4 118.0(3) . . ? C2 C3 N2 105.3(3) . . ? C2 C3 C4 135.8(3) . . ? O3 C4 Sr1 62.37(16) . . ? O3 C4 O4 123.4(3) . . ? O3 C4 C3 119.9(3) . . ? O4 C4 Sr1 61.68(16) . . ? O4 C4 C3 116.6(3) . . ? C3 C4 Sr1 173.9(2) . . ? N1 C5 N2 110.4(3) . . ? N1 C5 C6 126.3(3) . . ? N2 C5 C6 123.3(3) . . ? C7 C6 C5 122.0(3) . . ? C7 C6 C11 118.4(3) . . ? C11 C6 C5 119.5(3) . . ? C6 C7 H7 119.5 . . ? C8 C7 C6 121.0(4) . . ? C8 C7 H7 119.5 . . ? C7 C8 H8 119.2 . . ? C9 C8 C7 121.6(4) . . ? C9 C8 H8 119.2 . . ? C8 C9 C12 121.3(4) . . ? C10 C9 C8 117.7(4) . . ? C10 C9 C12 121.0(4) . . ? C9 C10 H10 119.1 . . ? C9 C10 C11 121.8(4) . . ? C11 C10 H10 119.1 . . ? C6 C11 C10 119.5(4) . . ? C6 C11 H11 120.3 . . ? C10 C11 H11 120.3 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? 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 H5A O2 0.85 2.21 3.060(4) 179.6 2_655 O5 H5B N1 0.85 1.97 2.803(4) 167.0 3_655 N2 H2 O5 0.79(4) 2.20(4) 2.987(4) 174(4) 2_655 loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Sr1 Sr1 O3 C4 -138.4(2) 2_645 . . . ? Sr1 Sr1 O4 Sr1 146.79(7) 2_645 . . 2_655 ? Sr1 Sr1 O4 C4 17.03(18) 2_645 . . . ? Sr1 Sr1 C4 O3 28.80(15) 2_645 . . . ? Sr1 Sr1 C4 O4 -160.0(2) 2_645 . . . ? Sr1 Sr1 C4 C3 -85(2) 2_645 . . . ? Sr1 O1 C1 Sr1 102.2(2) 3_655 . . 4 ? Sr1 O1 C1 O2 16.5(3) 4 . . . ? Sr1 O1 C1 O2 118.7(3) 3_655 . . . ? Sr1 O1 C1 C2 -161.7(2) 4 . . . ? Sr1 O1 C1 C2 -59.5(4) 3_655 . . . ? Sr1 O2 C1 Sr1 -147.6(5) 2_645 . . 4 ? Sr1 O2 C1 O1 -163.4(3) 2_645 . . . ? Sr1 O2 C1 O1 -15.8(3) 4 . . . ? Sr1 O2 C1 C2 14.7(7) 2_645 . . . ? Sr1 O2 C1 C2 162.4(3) 4 . . . ? Sr1 O3 C4 Sr1 -108.2(3) 2_645 . . . ? Sr1 O3 C4 O4 -9.3(3) . . . . ? Sr1 O3 C4 O4 -117.5(3) 2_645 . . . ? Sr1 O3 C4 C3 173.6(3) . . . . ? Sr1 O3 C4 C3 65.4(4) 2_645 . . . ? Sr1 O4 C4 Sr1 -104.4(2) 2_655 . . . ? Sr1 O4 C4 O3 9.4(3) . . . . ? Sr1 O4 C4 O3 -95.0(3) 2_655 . . . ? Sr1 O4 C4 C3 -173.4(2) . . . . ? Sr1 O4 C4 C3 82.2(3) 2_655 . . . ? Sr1 C1 C2 N1 -92.9(8) 4 . . . ? Sr1 C1 C2 C3 80.7(8) 4 . . . ? O1 Sr1 O3 Sr1 -140.28(9) 3_655 . . 2_645 ? O1 Sr1 O3 Sr1 47.32(8) 4_556 . . 2_645 ? O1 Sr1 O3 C4 -91.10(19) 4_556 . . . ? O1 Sr1 O3 C4 81.30(18) 3_655 . . . ? O1 Sr1 O4 Sr1 -170.64(9) 4_556 . . 2_655 ? O1 Sr1 O4 Sr1 41.31(7) 3_655 . . 2_655 ? O1 Sr1 O4 C4 59.60(19) 4_556 . . . ? O1 Sr1 O4 C4 -88.45(19) 3_655 . . . ? O1 Sr1 C4 O3 -89.62(18) 3_655 . . . ? O1 Sr1 C4 O3 76.50(18) 4_556 . . . ? O1 Sr1 C4 O4 -112.3(2) 4_556 . . . ? O1 Sr1 C4 O4 81.55(19) 3_655 . . . ? O1 Sr1 C4 C3 156(2) 3_655 . . . ? O1 Sr1 C4 C3 -37(2) 4_556 . . . ? O1 C1 C2 N1 -20.8(5) . . . . ? O1 C1 C2 C3 152.8(3) . . . . ? O2 Sr1 O3 Sr1 -11.5(5) 2_655 . . 2_645 ? O2 Sr1 O3 Sr1 47.39(9) 4_556 . . 2_645 ? O2 Sr1 O3 C4 -149.9(5) 2_655 . . . ? O2 Sr1 O3 C4 -91.02(18) 4_556 . . . ? O2 Sr1 O4 Sr1 -134.65(7) 4_556 . . 2_655 ? O2 Sr1 O4 Sr1 -60.70(14) 2_655 . . 2_655 ? O2 Sr1 O4 C4 95.58(19) 4_556 . . . ? O2 Sr1 O4 C4 169.54(17) 2_655 . . . ? O2 Sr1 C4 O3 96.89(18) 4_556 . . . ? O2 Sr1 C4 O3 165.2(2) 2_655 . . . ? O2 Sr1 C4 O4 -91.94(19) 4_556 . . . ? O2 Sr1 C4 O4 -23.6(4) 2_655 . . . ? O2 Sr1 C4 C3 51(2) 2_655 . . . ? O2 Sr1 C4 C3 -17(2) 4_556 . . . ? O2 C1 C2 N1 160.9(3) . . . . ? O2 C1 C2 C3 -25.4(6) . . . . ? O3 Sr1 O3 Sr1 174.22(10) 2_655 . . 2_645 ? O3 Sr1 O3 C4 35.80(17) 2_655 . . . ? O3 Sr1 O4 Sr1 124.95(12) . . . 2_655 ? O3 Sr1 O4 Sr1 -27.09(7) 2_655 . . 2_655 ? O3 Sr1 O4 C4 -156.8(2) 2_655 . . . ? O3 Sr1 O4 C4 -4.81(17) . . . . ? O3 Sr1 C4 O3 -148.59(15) 2_655 . . . ? O3 Sr1 C4 O4 22.58(19) 2_655 . . . ? O3 Sr1 C4 O4 171.2(3) . . . . ? O3 Sr1 C4 C3 -114(2) . . . . ? O3 Sr1 C4 C3 98(2) 2_655 . . . ? O4 Sr1 O3 Sr1 143.28(12) . . . 2_645 ? O4 Sr1 O3 Sr1 -27.17(8) 2_645 . . 2_645 ? O4 Sr1 O3 C4 -165.59(19) 2_645 . . . ? O4 Sr1 O3 C4 4.87(17) . . . . ? O4 Sr1 O4 Sr1 135.76(10) 2_645 . . 2_655 ? O4 Sr1 O4 C4 6.00(18) 2_645 . . . ? O4 Sr1 C4 O3 13.97(19) 2_645 . . . ? O4 Sr1 C4 O3 -171.2(3) . . . . ? O4 Sr1 C4 O4 -174.86(16) 2_645 . . . ? O4 Sr1 C4 C3 75(2) . . . . ? O4 Sr1 C4 C3 -100(2) 2_645 . . . ? O5 Sr1 O3 Sr1 -87.97(9) . . . 2_645 ? O5 Sr1 O3 C4 133.62(18) . . . . ? O5 Sr1 O4 Sr1 47.15(11) . . . 2_655 ? O5 Sr1 O4 C4 -82.6(2) . . . . ? O5 Sr1 C4 O3 -55.7(2) . . . . ? O5 Sr1 C4 O4 115.50(18) . . . . ? O5 Sr1 C4 C3 -170(2) . . . . ? N1 C2 C3 N2 -0.6(4) . . . . ? N1 C2 C3 C4 168.0(3) . . . . ? N1 C5 C6 C7 -165.3(4) . . . . ? N1 C5 C6 C11 18.4(6) . . . . ? N2 C3 C4 Sr1 -79(2) . . . . ? N2 C3 C4 O3 169.7(3) . . . . ? N2 C3 C4 O4 -7.6(4) . . . . ? N2 C5 C6 C7 16.2(6) . . . . ? N2 C5 C6 C11 -160.1(4) . . . . ? C1 Sr1 O3 Sr1 43.96(8) 4_556 . . 2_645 ? C1 Sr1 O3 C4 -94.46(19) 4_556 . . . ? C1 Sr1 O4 Sr1 -155.03(8) 4_556 . . 2_655 ? C1 Sr1 O4 C4 75.21(19) 4_556 . . . ? C1 Sr1 C4 O3 83.87(18) 4_556 . . . ? C1 Sr1 C4 O4 -104.96(19) 4_556 . . . ? C1 Sr1 C4 C3 -30(2) 4_556 . . . ? C1 C2 C3 N2 -174.7(3) . . . . ? C1 C2 C3 C4 -6.1(7) . . . . ? C2 N1 C5 N2 0.7(4) . . . . ? C2 N1 C5 C6 -178.0(3) . . . . ? C2 C3 C4 Sr1 113(2) . . . . ? C2 C3 C4 O3 2.2(6) . . . . ? C2 C3 C4 O4 -175.1(4) . . . . ? C3 N2 C5 N1 -1.1(4) . . . . ? C3 N2 C5 C6 177.7(3) . . . . ? C4 Sr1 O3 Sr1 138.4(2) . . . 2_645 ? C4 Sr1 O4 Sr1 129.8(2) . . . 2_655 ? C5 N1 C2 C1 174.9(3) . . . . ? C5 N1 C2 C3 -0.1(4) . . . . ? C5 N2 C3 C2 1.0(4) . . . . ? C5 N2 C3 C4 -170.0(3) . . . . ? C5 C6 C7 C8 -176.7(4) . . . . ? C5 C6 C11 C10 176.4(4) . . . . ? C6 C7 C8 C9 0.6(8) . . . . ? C7 C6 C11 C10 0.0(6) . . . . ? C7 C8 C9 C10 -0.4(8) . . . . ? C7 C8 C9 C12 179.3(5) . . . . ? C8 C9 C10 C11 0.0(7) . . . . ? C9 C10 C11 C6 0.2(7) . . . . ? C11 C6 C7 C8 -0.4(7) . . . . ? C12 C9 C10 C11 -179.7(4) . . . . ? data_cxj53 _database_code_depnum_ccdc_archive 'CCDC 855105' #TrackingRef '53.cif' _audit_creation_date 2011-07-12 _audit_creation_method ; Olex2 1.1 (compiled 2011.02.15 svn.r1672, GUI svn.r3494) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C83 H69 Cd4 N15 O17' _chemical_formula_sum 'C83 H69 Cd4 N15 O17' _chemical_formula_weight 1998.13 _chemical_melting_point ? _chemical_oxdiff_formula 'C11 H10 S O2' 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' O O 0.0106 0.0060 '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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, -y, -z' _cell_length_a 15.0195(7) _cell_length_b 15.2813(7) _cell_length_c 19.1307(10) _cell_angle_alpha 103.351(4) _cell_angle_beta 91.289(4) _cell_angle_gamma 93.269(4) _cell_volume 4262.3(4) _cell_formula_units_Z 2 _cell_measurement_reflns_used 10987 _cell_measurement_temperature 291.15 _cell_measurement_theta_max 26.3139 _cell_measurement_theta_min 2.8876 _exptl_absorpt_coefficient_mu 1.059 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.71486 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour ? _exptl_crystal_density_diffrn 1.557 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description ? _exptl_crystal_F_000 2000 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0379 _diffrn_reflns_av_unetI/netI 0.0616 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 35366 _diffrn_reflns_theta_full 26.37 _diffrn_reflns_theta_max 26.37 _diffrn_reflns_theta_min 2.89 _diffrn_ambient_temperature 291.15 _diffrn_detector_area_resol_mean 16.2312 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -52.00 -18.00 1.0000 46.0000 omega____ theta____ kappa____ phi______ frames - -17.1383 123.0000 13.0000 34 #__ type_ start__ end____ width___ exp.time_ 2 omega -53.00 -27.00 1.0000 46.0000 omega____ theta____ kappa____ phi______ frames - -17.1383 -37.0000 -90.0000 26 #__ type_ start__ end____ width___ exp.time_ 3 omega 42.00 74.00 1.0000 46.0000 omega____ theta____ kappa____ phi______ frames - 19.7164 -123.0000 166.0000 32 #__ type_ start__ end____ width___ exp.time_ 4 omega -53.00 42.00 1.0000 46.0000 omega____ theta____ kappa____ phi______ frames - 19.7164 -37.0000 90.0000 95 #__ type_ start__ end____ width___ exp.time_ 5 omega 5.00 31.00 1.0000 46.0000 omega____ theta____ kappa____ phi______ frames - 19.7164 -37.0000 120.0000 26 #__ type_ start__ end____ width___ exp.time_ 6 omega -44.00 47.00 1.0000 46.0000 omega____ theta____ kappa____ phi______ frames - 19.7164 -77.0000 -120.0000 91 #__ type_ start__ end____ width___ exp.time_ 7 omega -9.00 88.00 1.0000 46.0000 omega____ theta____ kappa____ phi______ frames - 19.7164 77.0000 0.0000 97 #__ type_ start__ end____ width___ exp.time_ 8 omega -10.00 26.00 1.0000 46.0000 omega____ theta____ kappa____ phi______ frames - 19.7164 77.0000 -150.0000 36 ; _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0041839000 _diffrn_orient_matrix_UB_12 -0.0110926000 _diffrn_orient_matrix_UB_13 0.0338879000 _diffrn_orient_matrix_UB_21 -0.0052946000 _diffrn_orient_matrix_UB_22 -0.0464840000 _diffrn_orient_matrix_UB_23 -0.0171201000 _diffrn_orient_matrix_UB_31 0.0468505000 _diffrn_orient_matrix_UB_32 -0.0011730000 _diffrn_orient_matrix_UB_33 -0.0035467000 _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_source 'Enhance (Mo) X-ray Source' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 12155 _reflns_number_total 17371 _reflns_odcompleteness_completeness 99.80 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'A short history of SHELX (Sheldrick, 2007)' _refine_diff_density_max 0.575 _refine_diff_density_min -0.622 _refine_diff_density_rms 0.080 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 1085 _refine_ls_number_reflns 17371 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0741 _refine_ls_R_factor_gt 0.0432 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0358P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0854 _refine_ls_wR_factor_ref 0.0996 _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 1.039230(17) 0.07768(2) 0.727280(14) 0.04016(9) Uani 1 1 d D . . Cd2 Cd 0.680576(17) 0.12527(2) 0.941288(15) 0.04112(9) Uani 1 1 d . . . Cd3 Cd 0.783180(18) 0.27737(2) 0.520605(15) 0.04126(9) Uani 1 1 d . . . Cd4 Cd 0.432891(18) 0.35032(2) 0.741253(15) 0.04205(9) Uani 1 1 d . . . O1 O 0.9149(2) -0.0852(2) 0.52595(15) 0.0560(8) Uani 1 1 d . . . H1 H 0.8768 -0.0632 0.5052 0.084 Uiso 1 1 calc R . . O2 O 1.00194(19) -0.0430(2) 0.62415(15) 0.0554(8) Uani 1 1 d . . . O3 O 0.81061(18) -0.0136(2) 0.45786(13) 0.0482(7) Uani 1 1 d . . . O4 O 0.76858(18) 0.1243(2) 0.45724(14) 0.0512(8) Uani 1 1 d . . . O5 O 1.17438(16) 0.1051(2) 0.68153(14) 0.0593(9) Uani 1 1 d D . . O6 O 1.09036(16) 0.1925(2) 0.82660(13) 0.0473(7) Uani 1 1 d . . . O7 O 1.05458(17) 0.2756(2) 0.93222(15) 0.0620(9) Uani 1 1 d . . . O8 O 0.92640(19) 0.2942(2) 1.01147(15) 0.0687(10) Uani 1 1 d . . . H8 H 0.9691 0.2879 0.9852 0.103 Uiso 1 1 calc R . . O9 O 0.78923(17) 0.2336(2) 1.01126(14) 0.0559(9) Uani 1 1 d . . . O10 O 0.56548(19) 0.0166(2) 0.88813(16) 0.0582(8) Uani 1 1 d . . . O11 O 0.4422(2) -0.0081(2) 0.81946(16) 0.0669(9) Uani 1 1 d . . . H11 H 0.3964 0.0157 0.8337 0.100 Uiso 1 1 calc R . . O12 O 0.34537(18) 0.0786(2) 0.76054(16) 0.0630(9) Uani 1 1 d . . . O13 O 0.34373(17) 0.2146(2) 0.73865(14) 0.0528(8) Uani 1 1 d . . . O14 O 0.50008(17) 0.5044(2) 0.75270(15) 0.0522(8) Uani 1 1 d . . . O15 O 0.61561(19) 0.5828(2) 0.72222(16) 0.0568(8) Uani 1 1 d . . . H15 H 0.6578 0.5732 0.6957 0.085 Uiso 1 1 calc R . . O16 O 0.74244(18) 0.5543(2) 0.64332(16) 0.0596(9) Uani 1 1 d . . . O17 O 0.79716(17) 0.4391(2) 0.56634(15) 0.0536(8) Uani 1 1 d . . . N1 N 0.87028(19) 0.1997(2) 0.58082(15) 0.0347(7) Uani 1 1 d . . . N2 N 0.96523(19) 0.1348(2) 0.64351(15) 0.0357(8) Uani 1 1 d . . . N3 N 1.0896(3) -0.0425(3) 0.7714(2) 0.0602(10) Uani 1 1 d . . . N4 N 0.92611(19) 0.0960(2) 0.81033(16) 0.0424(9) Uani 1 1 d . . . N5 N 0.81150(19) 0.1102(2) 0.88455(16) 0.0416(8) Uani 1 1 d . . . N6 N 0.7155(2) 0.0075(3) 0.99808(18) 0.0513(10) Uani 1 1 d . . . N7 N 0.5864(2) 0.1973(3) 1.03063(18) 0.0492(9) Uani 1 1 d . . . N8 N 0.5985(2) 0.1870(2) 0.86087(17) 0.0422(8) Uani 1 1 d . . . N9 N 0.5076(2) 0.2663(2) 0.80768(16) 0.0419(8) Uani 1 1 d . . . N10 N 0.3383(2) 0.4273(3) 0.82638(19) 0.0563(10) Uani 1 1 d . . . N11 N 0.3314(3) 0.3593(3) 0.64639(19) 0.0551(10) Uani 1 1 d . . . N12 N 0.55216(19) 0.3461(2) 0.66951(16) 0.0410(8) Uani 1 1 d . . . N13 N 0.67210(19) 0.3174(2) 0.60254(16) 0.0411(8) Uani 1 1 d . . . N14 N 0.6831(3) 0.2953(3) 0.4280(2) 0.0653(12) Uani 1 1 d . . . N15 N 0.9043(2) 0.3132(3) 0.45295(18) 0.0491(9) Uani 1 1 d . . . C1 C 0.9503(3) -0.0239(3) 0.5801(2) 0.0440(10) Uani 1 1 d . . . C2 C 0.9261(2) 0.0692(3) 0.58799(18) 0.0335(9) Uani 1 1 d . . . C3 C 0.8680(2) 0.1092(3) 0.55021(18) 0.0328(9) Uani 1 1 d . . . C4 C 0.8114(2) 0.0715(3) 0.48382(19) 0.0396(10) Uani 1 1 d . . . C5 C 0.9309(2) 0.2117(3) 0.63700(19) 0.0362(9) Uani 1 1 d . . . C6 C 1.0766(4) 0.4082(4) 0.7406(3) 0.0865(18) Uani 1 1 d . . . H6 H 1.1360 0.4206 0.7563 0.104 Uiso 1 1 calc R . . C7 C 1.0474(3) 0.3217(4) 0.7059(3) 0.0687(15) Uani 1 1 d . . . H7 H 1.0872 0.2763 0.6993 0.082 Uiso 1 1 calc R . . C8 C 0.9594(3) 0.3011(3) 0.68050(19) 0.0406(10) Uani 1 1 d . . . C9 C 0.9014(3) 0.3692(3) 0.6949(2) 0.0584(13) Uani 1 1 d . . . H9 H 0.8413 0.3568 0.6813 0.070 Uiso 1 1 calc R . . C10 C 0.9322(4) 0.4568(3) 0.7299(3) 0.0700(15) Uani 1 1 d . . . H10 H 0.8927 0.5025 0.7381 0.084 Uiso 1 1 calc R . . C11 C 1.0194(4) 0.4760(4) 0.7522(3) 0.0743(16) Uani 1 1 d . . . C12 C 1.0531(4) 0.5739(4) 0.7873(3) 0.118(2) Uani 1 1 d . . . H12A H 1.1102 0.5866 0.7690 0.176 Uiso 1 1 calc R . . H12B H 1.0586 0.5815 0.8385 0.176 Uiso 1 1 calc R . . H12C H 1.0114 0.6145 0.7762 0.176 Uiso 1 1 calc R . . C13 C 1.1743(4) -0.0577(5) 0.7741(4) 0.105(2) Uani 1 1 d . . . H13 H 1.2148 -0.0217 0.7552 0.126 Uiso 1 1 calc R . . C14 C 1.2066(5) -0.1243(6) 0.8035(5) 0.127(3) Uani 1 1 d . . . H14 H 1.2675 -0.1320 0.8052 0.152 Uiso 1 1 calc R . . C15 C 1.1481(7) -0.1791(6) 0.8302(4) 0.125(3) Uani 1 1 d . . . H15A H 1.1679 -0.2256 0.8492 0.150 Uiso 1 1 calc R . . C16 C 1.0613(6) -0.1635(6) 0.8281(4) 0.134(3) Uani 1 1 d . . . H16 H 1.0195 -0.1986 0.8466 0.161 Uiso 1 1 calc R . . C17 C 1.0343(4) -0.0943(5) 0.7980(4) 0.104(2) Uani 1 1 d . . . H17 H 0.9738 -0.0844 0.7967 0.125 Uiso 1 1 calc R . . C18 C 1.0367(2) 0.2140(3) 0.8752(2) 0.0431(10) Uani 1 1 d . . . C19 C 0.9484(2) 0.1648(3) 0.86862(19) 0.0381(10) Uani 1 1 d . . . C20 C 0.8773(2) 0.1740(3) 0.91413(19) 0.0389(10) Uani 1 1 d . . . C21 C 0.8623(3) 0.2371(3) 0.9831(2) 0.0470(11) Uani 1 1 d . . . C22 C 0.8433(2) 0.0647(3) 0.8220(2) 0.0413(10) Uani 1 1 d . . . C23 C 0.7625(3) -0.1008(5) 0.6533(3) 0.095(2) Uani 1 1 d . . . H23 H 0.7699 -0.1080 0.6042 0.113 Uiso 1 1 calc R . . C24 C 0.8026(3) -0.0252(4) 0.7009(3) 0.087(2) Uani 1 1 d . . . H24 H 0.8346 0.0179 0.6827 0.104 Uiso 1 1 calc R . . C25 C 0.7963(3) -0.0128(3) 0.7735(2) 0.0501(12) Uani 1 1 d . . . C26 C 0.7484(5) -0.0767(5) 0.7970(3) 0.143(3) Uani 1 1 d . . . H26 H 0.7428 -0.0714 0.8461 0.171 Uiso 1 1 calc R . . C27 C 0.7065(5) -0.1519(6) 0.7474(4) 0.162(4) Uani 1 1 d . . . H27 H 0.6731 -0.1949 0.7647 0.194 Uiso 1 1 calc R . . C28 C 0.7136(4) -0.1628(4) 0.6768(3) 0.0810(18) Uani 1 1 d . . . C29 C 0.6672(5) -0.2436(5) 0.6232(4) 0.138(3) Uani 1 1 d . . . H29A H 0.7060 -0.2925 0.6143 0.207 Uiso 1 1 calc R . . H29B H 0.6537 -0.2268 0.5790 0.207 Uiso 1 1 calc R . . H29C H 0.6130 -0.2621 0.6429 0.207 Uiso 1 1 calc R . . C30 C 0.8009(4) -0.0029(4) 1.0146(3) 0.0837(17) Uani 1 1 d . . . H30 H 0.8444 0.0396 1.0073 0.100 Uiso 1 1 calc R . . C31 C 0.8274(4) -0.0744(5) 1.0423(4) 0.112(2) Uani 1 1 d . . . H31 H 0.8874 -0.0800 1.0524 0.135 Uiso 1 1 calc R . . C32 C 0.7637(4) -0.1361(5) 1.0542(4) 0.101(2) Uani 1 1 d . . . H32 H 0.7791 -0.1838 1.0738 0.122 Uiso 1 1 calc R . . C33 C 0.6771(4) -0.1263(4) 1.0369(3) 0.0807(17) Uani 1 1 d . . . H33 H 0.6324 -0.1678 1.0437 0.097 Uiso 1 1 calc R . . C34 C 0.6566(3) -0.0546(4) 1.0092(3) 0.0677(15) Uani 1 1 d . . . H34 H 0.5970 -0.0493 0.9975 0.081 Uiso 1 1 calc R . . C35 C 0.5598(3) 0.1614(3) 1.0840(2) 0.0614(13) Uani 1 1 d . . . H35 H 0.5815 0.1069 1.0879 0.074 Uiso 1 1 calc R . . C36 C 0.5011(4) 0.2021(4) 1.1341(3) 0.0801(17) Uani 1 1 d . . . H36 H 0.4835 0.1749 1.1708 0.096 Uiso 1 1 calc R . . C37 C 0.4694(3) 0.2818(4) 1.1294(3) 0.0774(18) Uani 1 1 d . . . H37 H 0.4298 0.3102 1.1626 0.093 Uiso 1 1 calc R . . C38 C 0.4969(4) 0.3194(4) 1.0752(3) 0.0895(19) Uani 1 1 d . . . H38 H 0.4772 0.3746 1.0708 0.107 Uiso 1 1 calc R . . C39 C 0.5540(4) 0.2744(4) 1.0273(3) 0.0810(17) Uani 1 1 d . . . H39 H 0.5712 0.3000 0.9896 0.097 Uiso 1 1 calc R . . C40 C 0.5110(3) 0.0435(3) 0.8493(2) 0.0479(11) Uani 1 1 d . . . C41 C 0.5228(2) 0.1331(3) 0.8352(2) 0.0397(10) Uani 1 1 d . . . C42 C 0.4681(2) 0.1829(3) 0.8024(2) 0.0396(10) Uani 1 1 d . . . C43 C 0.3798(3) 0.1571(3) 0.7644(2) 0.0448(11) Uani 1 1 d . . . C44 C 0.5870(2) 0.2651(3) 0.8426(2) 0.0412(10) Uani 1 1 d . . . C45 C 0.6938(5) 0.5012(5) 0.8911(3) 0.106(2) Uani 1 1 d . . . H45 H 0.6759 0.5600 0.9022 0.128 Uiso 1 1 calc R . . C46 C 0.6297(4) 0.4297(4) 0.8757(3) 0.0811(17) Uani 1 1 d . . . H46 H 0.5696 0.4412 0.8768 0.097 Uiso 1 1 calc R . . C47 C 0.6541(3) 0.3418(3) 0.8586(2) 0.0485(11) Uani 1 1 d . . . C48 C 0.7444(3) 0.3273(4) 0.8556(3) 0.0715(15) Uani 1 1 d . . . H48 H 0.7628 0.2689 0.8421 0.086 Uiso 1 1 calc R . . C49 C 0.8075(4) 0.3997(5) 0.8726(3) 0.091(2) Uani 1 1 d . . . H49 H 0.8677 0.3888 0.8719 0.109 Uiso 1 1 calc R . . C50 C 0.7832(5) 0.4866(5) 0.8905(3) 0.095(2) Uani 1 1 d . . . C51 C 0.8515(5) 0.5692(6) 0.9078(4) 0.180(4) Uani 1 1 d . . . H51A H 0.8317 0.6136 0.9476 0.271 Uiso 1 1 calc R . . H51B H 0.8565 0.5946 0.8665 0.271 Uiso 1 1 calc R . . H51C H 0.9086 0.5506 0.9200 0.271 Uiso 1 1 calc R . . C52 C 0.2779(4) 0.3821(4) 0.8562(3) 0.0842(18) Uani 1 1 d . . . H52 H 0.2778 0.3195 0.8453 0.101 Uiso 1 1 calc R . . C53 C 0.2154(4) 0.4225(5) 0.9021(3) 0.110(2) Uani 1 1 d . . . H53 H 0.1734 0.3878 0.9207 0.132 Uiso 1 1 calc R . . C54 C 0.2160(4) 0.5127(5) 0.9198(3) 0.089(2) Uani 1 1 d . . . H54 H 0.1760 0.5418 0.9522 0.107 Uiso 1 1 calc R . . C55 C 0.2760(3) 0.5604(4) 0.8893(3) 0.0847(18) Uani 1 1 d . . . H55 H 0.2770 0.6230 0.8997 0.102 Uiso 1 1 calc R . . C56 C 0.3357(3) 0.5155(4) 0.8428(3) 0.0771(17) Uani 1 1 d . . . H56 H 0.3761 0.5492 0.8219 0.093 Uiso 1 1 calc R . . C57 C 0.2662(3) 0.2988(5) 0.6183(3) 0.0881(19) Uani 1 1 d . . . H57 H 0.2589 0.2477 0.6367 0.106 Uiso 1 1 calc R . . C58 C 0.2085(4) 0.3069(5) 0.5634(3) 0.101(2) Uani 1 1 d . . . H58 H 0.1639 0.2620 0.5456 0.121 Uiso 1 1 calc R . . C59 C 0.2169(5) 0.3792(5) 0.5359(4) 0.116(3) Uani 1 1 d . . . H59 H 0.1770 0.3874 0.5005 0.140 Uiso 1 1 calc R . . C60 C 0.2846(6) 0.4397(6) 0.5611(5) 0.164(4) Uani 1 1 d U . . H60 H 0.2945 0.4896 0.5416 0.196 Uiso 1 1 calc R . . C61 C 0.3405(5) 0.4271(5) 0.6172(4) 0.142(3) Uani 1 1 d . . . H61 H 0.3868 0.4703 0.6343 0.171 Uiso 1 1 calc R . . C62 C 0.5692(3) 0.5091(3) 0.7186(2) 0.0436(10) Uani 1 1 d . . . C63 C 0.5990(2) 0.4251(3) 0.67297(19) 0.0373(9) Uani 1 1 d . . . C64 C 0.6732(2) 0.4076(3) 0.6307(2) 0.0394(10) Uani 1 1 d . . . C65 C 0.7421(2) 0.4694(3) 0.6118(2) 0.0441(10) Uani 1 1 d . . . C66 C 0.5982(2) 0.2823(3) 0.6270(2) 0.0416(10) Uani 1 1 d . . . C67 C 0.4450(4) 0.0724(4) 0.5905(3) 0.0761(16) Uani 1 1 d . . . H67 H 0.3849 0.0566 0.5785 0.091 Uiso 1 1 calc R . . C68 C 0.4779(3) 0.1603(4) 0.5970(3) 0.0694(14) Uani 1 1 d . . . H68 H 0.4390 0.2031 0.5901 0.083 Uiso 1 1 calc R . . C69 C 0.5668(3) 0.1865(3) 0.6132(2) 0.0476(11) Uani 1 1 d . . . C70 C 0.6222(4) 0.1223(4) 0.6221(4) 0.102(2) Uani 1 1 d . . . H70 H 0.6827 0.1373 0.6325 0.123 Uiso 1 1 calc R . . C71 C 0.5882(5) 0.0343(5) 0.6154(4) 0.129(3) Uani 1 1 d . . . H71 H 0.6266 -0.0096 0.6206 0.155 Uiso 1 1 calc R . . C72 C 0.4984(4) 0.0107(4) 0.6012(3) 0.0871(18) Uani 1 1 d . . . C73 C 0.4612(5) -0.0863(5) 0.5973(4) 0.144(3) Uani 1 1 d . . . H73A H 0.4087 -0.0994 0.5663 0.216 Uiso 1 1 calc R . . H73B H 0.4464 -0.0924 0.6446 0.216 Uiso 1 1 calc R . . H73C H 0.5054 -0.1276 0.5787 0.216 Uiso 1 1 calc R . . C74 C 0.6076(4) 0.3359(4) 0.4415(3) 0.0826(17) Uani 1 1 d . . . H74 H 0.5920 0.3540 0.4892 0.099 Uiso 1 1 calc R . . C75 C 0.5511(4) 0.3530(4) 0.3895(4) 0.097(2) Uani 1 1 d . . . H75 H 0.4994 0.3828 0.4018 0.116 Uiso 1 1 calc R . . C76 C 0.5724(5) 0.3255(5) 0.3209(4) 0.121(3) Uani 1 1 d . . . H76 H 0.5358 0.3360 0.2842 0.146 Uiso 1 1 calc R . . C77 C 0.6454(6) 0.2836(7) 0.3062(4) 0.175(5) Uani 1 1 d . . . H77 H 0.6605 0.2633 0.2586 0.210 Uiso 1 1 calc R . . C78 C 0.7012(5) 0.2690(6) 0.3617(3) 0.135(3) Uani 1 1 d . . . H78 H 0.7531 0.2393 0.3499 0.162 Uiso 1 1 calc R . . C79 C 0.9242(4) 0.3940(4) 0.4435(3) 0.0832(18) Uani 1 1 d . . . H79 H 0.8874 0.4397 0.4628 0.100 Uiso 1 1 calc R . . C80 C 0.9972(4) 0.4153(4) 0.4062(3) 0.094(2) Uani 1 1 d . . . H80 H 1.0092 0.4740 0.4015 0.112 Uiso 1 1 calc R . . C81 C 1.0505(3) 0.3497(4) 0.3768(3) 0.0747(16) Uani 1 1 d . . . H81 H 1.0993 0.3617 0.3506 0.090 Uiso 1 1 calc R . . C82 C 1.0312(3) 0.2667(5) 0.3865(3) 0.089(2) Uani 1 1 d . . . H82 H 1.0674 0.2203 0.3675 0.107 Uiso 1 1 calc R . . C83 C 0.9579(3) 0.2501(4) 0.4247(3) 0.0714(15) Uani 1 1 d . . . H83 H 0.9458 0.1920 0.4309 0.086 Uiso 1 1 calc R . . H5A H 1.2211(12) 0.125(4) 0.7069(13) 0.107 Uiso 1 1 d D . . H5B H 1.1898(18) 0.076(3) 0.6407(13) 0.107 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.03263(15) 0.0474(2) 0.04088(16) 0.01045(14) 0.00059(12) 0.00603(13) Cd2 0.03035(15) 0.0523(2) 0.04396(17) 0.01659(15) 0.00292(12) 0.00716(14) Cd3 0.03852(16) 0.0428(2) 0.04518(17) 0.01324(14) 0.00560(13) 0.01178(14) Cd4 0.03488(16) 0.0489(2) 0.04644(17) 0.01801(15) 0.00517(12) 0.00727(14) O1 0.069(2) 0.0379(19) 0.0563(18) 0.0003(15) -0.0134(15) 0.0118(16) O2 0.0630(19) 0.044(2) 0.0582(18) 0.0086(15) -0.0139(15) 0.0182(16) O3 0.0601(18) 0.0390(19) 0.0405(15) -0.0002(14) -0.0071(13) 0.0032(15) O4 0.0524(17) 0.047(2) 0.0536(17) 0.0104(15) -0.0117(14) 0.0097(15) O5 0.0342(15) 0.090(3) 0.0425(16) -0.0050(17) -0.0017(12) -0.0041(16) O6 0.0331(14) 0.057(2) 0.0484(16) 0.0066(14) 0.0057(12) -0.0046(14) O7 0.0436(16) 0.070(2) 0.0579(18) -0.0096(17) 0.0022(14) -0.0185(16) O8 0.0519(19) 0.082(3) 0.0553(19) -0.0151(18) 0.0096(15) -0.0081(19) O9 0.0407(16) 0.070(2) 0.0512(17) 0.0012(16) 0.0101(13) 0.0055(15) O10 0.0564(19) 0.047(2) 0.079(2) 0.0335(17) -0.0174(16) -0.0026(15) O11 0.0588(19) 0.057(2) 0.088(2) 0.0322(18) -0.0185(17) -0.0213(17) O12 0.0475(18) 0.065(2) 0.078(2) 0.0289(18) -0.0216(15) -0.0214(17) O13 0.0395(16) 0.066(2) 0.0571(18) 0.0238(16) -0.0096(13) 0.0029(15) O14 0.0480(16) 0.046(2) 0.0641(18) 0.0111(15) 0.0217(14) 0.0109(14) O15 0.0568(19) 0.039(2) 0.073(2) 0.0065(16) 0.0253(15) 0.0059(16) O16 0.0546(18) 0.036(2) 0.087(2) 0.0104(17) 0.0240(16) 0.0011(15) O17 0.0489(17) 0.048(2) 0.0671(19) 0.0162(16) 0.0245(14) 0.0083(15) N1 0.0366(17) 0.031(2) 0.0352(17) 0.0051(15) -0.0005(13) 0.0031(14) N2 0.0340(17) 0.033(2) 0.0383(17) 0.0044(15) -0.0011(13) 0.0039(15) N3 0.060(3) 0.057(3) 0.066(2) 0.022(2) -0.006(2) 0.003(2) N4 0.0316(17) 0.050(2) 0.0425(18) 0.0044(17) 0.0016(14) -0.0010(16) N5 0.0329(17) 0.050(2) 0.0410(18) 0.0091(17) 0.0025(14) 0.0011(16) N6 0.044(2) 0.058(3) 0.056(2) 0.0212(19) -0.0029(17) 0.0073(19) N7 0.045(2) 0.050(3) 0.052(2) 0.0104(19) 0.0125(16) 0.0077(18) N8 0.0330(18) 0.047(2) 0.052(2) 0.0239(17) -0.0075(15) -0.0014(16) N9 0.0364(18) 0.048(2) 0.0444(19) 0.0194(17) -0.0061(14) -0.0010(16) N10 0.052(2) 0.060(3) 0.057(2) 0.012(2) 0.0182(18) 0.004(2) N11 0.061(2) 0.050(3) 0.060(2) 0.025(2) -0.0109(19) 0.003(2) N12 0.0352(17) 0.042(2) 0.0482(19) 0.0143(17) 0.0063(15) 0.0064(16) N13 0.0374(18) 0.038(2) 0.050(2) 0.0127(17) 0.0121(15) 0.0080(16) N14 0.063(3) 0.068(3) 0.067(3) 0.016(2) -0.011(2) 0.019(2) N15 0.055(2) 0.040(2) 0.057(2) 0.0176(19) 0.0169(17) 0.0133(19) C1 0.042(2) 0.036(3) 0.050(2) 0.003(2) 0.0000(19) 0.007(2) C2 0.0311(19) 0.031(2) 0.037(2) 0.0043(18) 0.0012(16) 0.0026(17) C3 0.0291(19) 0.032(2) 0.035(2) 0.0047(18) 0.0033(15) 0.0010(17) C4 0.034(2) 0.048(3) 0.035(2) 0.006(2) 0.0025(17) 0.0020(19) C5 0.033(2) 0.039(3) 0.035(2) 0.0054(18) 0.0035(16) 0.0042(18) C6 0.073(4) 0.067(4) 0.106(4) -0.002(4) -0.019(3) -0.015(3) C7 0.059(3) 0.055(4) 0.083(4) 0.002(3) -0.011(3) -0.001(3) C8 0.050(2) 0.035(3) 0.037(2) 0.0102(19) -0.0021(18) 0.001(2) C9 0.064(3) 0.047(3) 0.057(3) -0.001(2) -0.012(2) 0.010(2) C10 0.089(4) 0.044(3) 0.071(3) -0.001(3) -0.017(3) 0.014(3) C11 0.103(4) 0.043(3) 0.069(3) 0.003(3) -0.019(3) -0.007(3) C12 0.144(6) 0.054(4) 0.139(6) 0.000(4) -0.039(5) -0.015(4) C13 0.068(4) 0.103(6) 0.160(6) 0.057(5) 0.005(4) 0.034(4) C14 0.113(6) 0.114(8) 0.167(8) 0.058(6) -0.021(5) 0.039(5) C15 0.202(10) 0.082(6) 0.101(5) 0.034(4) -0.028(6) 0.050(7) C16 0.143(7) 0.101(7) 0.183(8) 0.083(6) 0.007(6) 0.011(6) C17 0.092(5) 0.074(5) 0.167(7) 0.068(5) 0.012(4) 0.010(4) C18 0.036(2) 0.044(3) 0.049(2) 0.012(2) -0.0011(19) 0.0016(19) C19 0.030(2) 0.045(3) 0.040(2) 0.0118(19) -0.0002(16) 0.0021(18) C20 0.034(2) 0.041(3) 0.042(2) 0.0086(19) -0.0008(17) 0.0035(18) C21 0.044(2) 0.054(3) 0.042(2) 0.008(2) -0.0017(19) 0.005(2) C22 0.031(2) 0.049(3) 0.043(2) 0.009(2) 0.0010(17) -0.0015(19) C23 0.071(4) 0.119(6) 0.069(3) -0.024(4) 0.013(3) -0.027(4) C24 0.067(3) 0.116(6) 0.062(3) -0.004(3) 0.008(3) -0.034(3) C25 0.037(2) 0.059(3) 0.050(3) 0.004(2) 0.0134(19) -0.003(2) C26 0.186(7) 0.125(7) 0.084(4) -0.020(4) 0.046(5) -0.090(6) C27 0.195(8) 0.136(8) 0.120(6) -0.015(5) 0.059(6) -0.113(7) C28 0.077(4) 0.068(4) 0.081(4) -0.014(3) 0.018(3) -0.018(3) C29 0.156(7) 0.081(6) 0.146(6) -0.029(5) 0.010(5) -0.030(5) C30 0.063(3) 0.088(5) 0.109(4) 0.046(4) -0.025(3) -0.003(3) C31 0.075(4) 0.117(7) 0.165(7) 0.078(5) -0.044(4) 0.008(4) C32 0.088(5) 0.101(6) 0.140(6) 0.080(5) -0.026(4) 0.005(4) C33 0.070(4) 0.083(5) 0.099(4) 0.044(4) -0.007(3) 0.000(3) C34 0.057(3) 0.080(4) 0.073(3) 0.030(3) -0.002(2) 0.010(3) C35 0.076(3) 0.051(3) 0.059(3) 0.015(3) 0.020(2) 0.012(3) C36 0.103(4) 0.060(4) 0.074(4) 0.005(3) 0.041(3) 0.003(3) C37 0.074(3) 0.073(4) 0.072(4) -0.016(3) 0.024(3) 0.013(3) C38 0.112(5) 0.078(5) 0.086(4) 0.020(4) 0.029(4) 0.051(4) C39 0.108(4) 0.069(4) 0.075(4) 0.027(3) 0.031(3) 0.032(4) C40 0.044(2) 0.046(3) 0.058(3) 0.024(2) -0.003(2) -0.001(2) C41 0.034(2) 0.043(3) 0.044(2) 0.014(2) -0.0031(17) -0.0026(19) C42 0.032(2) 0.045(3) 0.043(2) 0.016(2) -0.0031(17) -0.0031(19) C43 0.034(2) 0.055(3) 0.047(2) 0.017(2) -0.0038(18) -0.003(2) C44 0.037(2) 0.046(3) 0.043(2) 0.016(2) -0.0044(17) -0.0026(19) C45 0.122(6) 0.063(4) 0.120(5) 0.004(4) 0.002(4) -0.037(4) C46 0.076(4) 0.055(4) 0.108(4) 0.016(3) -0.009(3) -0.012(3) C47 0.043(2) 0.057(3) 0.049(2) 0.024(2) -0.0147(19) -0.011(2) C48 0.051(3) 0.078(4) 0.093(4) 0.040(3) -0.005(3) -0.014(3) C49 0.053(3) 0.120(6) 0.108(5) 0.055(5) -0.020(3) -0.036(4) C50 0.099(5) 0.094(6) 0.084(4) 0.019(4) -0.009(4) -0.052(4) C51 0.189(8) 0.178(10) 0.140(7) 0.000(6) -0.002(6) -0.125(8) C52 0.097(4) 0.073(4) 0.083(4) 0.015(3) 0.043(3) 0.004(3) C53 0.110(5) 0.094(6) 0.120(5) 0.010(5) 0.069(4) -0.003(4) C54 0.081(4) 0.097(6) 0.079(4) -0.005(4) 0.034(3) 0.013(4) C55 0.077(4) 0.062(4) 0.107(4) 0.001(3) 0.038(3) 0.006(3) C56 0.072(3) 0.054(4) 0.102(4) 0.009(3) 0.039(3) 0.004(3) C57 0.070(4) 0.112(6) 0.101(4) 0.070(4) -0.016(3) -0.015(4) C58 0.087(4) 0.114(6) 0.108(5) 0.053(4) -0.045(4) -0.017(4) C59 0.126(6) 0.093(6) 0.131(6) 0.037(5) -0.081(5) 0.006(5) C60 0.203(7) 0.135(7) 0.174(6) 0.099(5) -0.096(6) -0.030(6) C61 0.193(8) 0.080(5) 0.163(7) 0.075(5) -0.121(6) -0.054(5) C62 0.044(2) 0.042(3) 0.048(2) 0.013(2) 0.0083(19) 0.007(2) C63 0.035(2) 0.038(3) 0.040(2) 0.0114(19) 0.0029(17) 0.0046(18) C64 0.040(2) 0.031(2) 0.049(2) 0.0115(19) 0.0072(18) 0.0104(18) C65 0.036(2) 0.049(3) 0.053(2) 0.021(2) 0.0073(19) 0.004(2) C66 0.038(2) 0.044(3) 0.045(2) 0.012(2) 0.0017(18) 0.010(2) C67 0.067(3) 0.057(4) 0.099(4) 0.010(3) 0.005(3) -0.008(3) C68 0.061(3) 0.049(3) 0.097(4) 0.014(3) 0.001(3) 0.002(3) C69 0.045(2) 0.037(3) 0.060(3) 0.008(2) 0.011(2) 0.005(2) C70 0.067(4) 0.047(4) 0.194(7) 0.033(4) -0.023(4) -0.003(3) C71 0.097(5) 0.049(4) 0.243(9) 0.043(5) -0.033(5) 0.001(4) C72 0.091(4) 0.051(4) 0.115(5) 0.013(4) 0.007(4) -0.013(3) C73 0.160(7) 0.067(5) 0.208(8) 0.050(5) -0.023(6) -0.035(5) C74 0.073(4) 0.089(5) 0.090(4) 0.028(3) -0.010(3) 0.011(3) C75 0.082(4) 0.093(5) 0.116(5) 0.024(4) -0.030(4) 0.028(4) C76 0.143(7) 0.132(7) 0.088(5) 0.014(5) -0.034(5) 0.066(6) C77 0.186(8) 0.271(13) 0.068(4) 0.013(6) -0.024(5) 0.136(9) C78 0.134(6) 0.205(9) 0.065(4) 0.009(5) -0.011(4) 0.099(6) C79 0.114(5) 0.054(4) 0.088(4) 0.022(3) 0.050(3) 0.020(3) C80 0.134(5) 0.056(4) 0.090(4) 0.015(3) 0.055(4) -0.014(4) C81 0.065(3) 0.087(5) 0.071(3) 0.019(3) 0.021(3) -0.014(3) C82 0.066(3) 0.086(5) 0.124(5) 0.034(4) 0.049(3) 0.024(3) C83 0.068(3) 0.050(3) 0.104(4) 0.029(3) 0.040(3) 0.019(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 Cd1 O2 2.400(3) . ? Cd1 O5 2.284(3) . ? Cd1 O6 2.349(3) . ? Cd1 N2 2.289(3) . ? Cd1 N3 2.346(4) . ? Cd1 N4 2.337(3) . ? Cd2 O9 2.401(3) . ? Cd2 O10 2.365(3) . ? Cd2 N5 2.265(3) . ? Cd2 N6 2.383(4) . ? Cd2 N7 2.356(3) . ? Cd2 N8 2.343(3) . ? Cd3 O4 2.369(3) . ? Cd3 O17 2.419(3) . ? Cd3 N1 2.278(3) . ? Cd3 N13 2.325(3) . ? Cd3 N14 2.372(4) . ? Cd3 N15 2.368(3) . ? Cd4 O13 2.394(3) . ? Cd4 O14 2.469(3) . ? Cd4 N9 2.319(3) . ? Cd4 N10 2.337(3) . ? Cd4 N11 2.377(4) . ? Cd4 N12 2.276(3) . ? O1 H1 0.8200 . ? O1 C1 1.306(4) . ? O2 C1 1.227(5) . ? O3 C4 1.280(5) . ? O4 C4 1.247(5) . ? O5 H5A 0.845(10) . ? O5 H5B 0.851(10) . ? O6 C18 1.242(4) . ? O7 C18 1.278(4) . ? O8 H8 0.8200 . ? O8 C21 1.282(5) . ? O9 C21 1.237(4) . ? O10 C40 1.242(5) . ? O11 H11 0.8200 . ? O11 C40 1.299(5) . ? O12 C43 1.263(5) . ? O13 C43 1.245(5) . ? O14 C62 1.246(4) . ? O15 H15 0.8200 . ? O15 C62 1.277(5) . ? O16 C65 1.298(5) . ? O17 C65 1.243(4) . ? N1 C3 1.369(5) . ? N1 C5 1.365(4) . ? N2 C2 1.375(4) . ? N2 C5 1.341(5) . ? N3 C13 1.309(6) . ? N3 C17 1.306(7) . ? N4 C19 1.365(5) . ? N4 C22 1.349(4) . ? N5 C20 1.363(5) . ? N5 C22 1.349(4) . ? N6 C30 1.342(6) . ? N6 C34 1.316(6) . ? N7 C35 1.325(5) . ? N7 C39 1.315(6) . ? N8 C41 1.376(5) . ? N8 C44 1.338(5) . ? N9 C42 1.356(5) . ? N9 C44 1.356(5) . ? N10 C52 1.327(6) . ? N10 C56 1.314(6) . ? N11 C57 1.320(6) . ? N11 C61 1.288(7) . ? N12 C63 1.349(5) . ? N12 C66 1.351(5) . ? N13 C64 1.358(5) . ? N13 C66 1.346(5) . ? N14 C74 1.326(6) . ? N14 C78 1.278(6) . ? N15 C79 1.308(6) . ? N15 C83 1.318(5) . ? C1 C2 1.463(5) . ? C2 C3 1.376(5) . ? C3 C4 1.491(5) . ? C5 C8 1.460(5) . ? C6 H6 0.9300 . ? C6 C7 1.376(7) . ? C6 C11 1.366(7) . ? C7 H7 0.9300 . ? C7 C8 1.392(6) . ? C8 C9 1.378(5) . ? C9 H9 0.9300 . ? C9 C10 1.399(6) . ? C10 H10 0.9300 . ? C10 C11 1.362(7) . ? C11 C12 1.542(7) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13 0.9300 . ? C13 C14 1.377(9) . ? C14 H14 0.9300 . ? C14 C15 1.366(10) . ? C15 H15A 0.9300 . ? C15 C16 1.341(10) . ? C16 H16 0.9300 . ? C16 C17 1.391(9) . ? C17 H17 0.9300 . ? C18 C19 1.476(5) . ? C19 C20 1.385(5) . ? C20 C21 1.474(5) . ? C22 C25 1.459(6) . ? C23 H23 0.9300 . ? C23 C24 1.391(7) . ? C23 C28 1.332(8) . ? C24 H24 0.9300 . ? C24 C25 1.363(6) . ? C25 C26 1.346(8) . ? C26 H26 0.9300 . ? C26 C27 1.416(8) . ? C27 H27 0.9300 . ? C27 C28 1.329(8) . ? C28 C29 1.531(7) . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30 0.9300 . ? C30 C31 1.392(8) . ? C31 H31 0.9300 . ? C31 C32 1.367(8) . ? C32 H32 0.9300 . ? C32 C33 1.360(7) . ? C33 H33 0.9300 . ? C33 C34 1.369(7) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C35 C36 1.381(6) . ? C36 H36 0.9300 . ? C36 C37 1.354(8) . ? C37 H37 0.9300 . ? C37 C38 1.358(8) . ? C38 H38 0.9300 . ? C38 C39 1.364(6) . ? C39 H39 0.9300 . ? C40 C41 1.457(6) . ? C41 C42 1.385(5) . ? C42 C43 1.486(5) . ? C44 C47 1.474(6) . ? C45 H45 0.9300 . ? C45 C46 1.388(8) . ? C45 C50 1.373(8) . ? C46 H46 0.9300 . ? C46 C47 1.379(7) . ? C47 C48 1.387(6) . ? C48 H48 0.9300 . ? C48 C49 1.388(7) . ? C49 H49 0.9300 . ? C49 C50 1.365(9) . ? C50 C51 1.550(8) . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C52 H52 0.9300 . ? C52 C53 1.373(7) . ? C53 H53 0.9300 . ? C53 C54 1.341(9) . ? C54 H54 0.9300 . ? C54 C55 1.353(8) . ? C55 H55 0.9300 . ? C55 C56 1.375(6) . ? C56 H56 0.9300 . ? C57 H57 0.9300 . ? C57 C58 1.380(7) . ? C58 H58 0.9300 . ? C58 C59 1.330(9) . ? C59 H59 0.9300 . ? C59 C60 1.335(9) . ? C60 H60 0.9300 . ? C60 C61 1.402(9) . ? C61 H61 0.9300 . ? C62 C63 1.476(5) . ? C63 C64 1.393(5) . ? C64 C65 1.469(6) . ? C66 C69 1.474(6) . ? C67 H67 0.9300 . ? C67 C68 1.383(7) . ? C67 C72 1.320(8) . ? C68 H68 0.9300 . ? C68 C69 1.379(6) . ? C69 C70 1.359(7) . ? C70 H70 0.9300 . ? C70 C71 1.389(8) . ? C71 H71 0.9300 . ? C71 C72 1.381(8) . ? C72 C73 1.538(8) . ? C73 H73A 0.9600 . ? C73 H73B 0.9600 . ? C73 H73C 0.9600 . ? C74 H74 0.9300 . ? C74 C75 1.374(7) . ? C75 H75 0.9300 . ? C75 C76 1.335(8) . ? C76 H76 0.9300 . ? C76 C77 1.304(8) . ? C77 H77 0.9300 . ? C77 C78 1.405(8) . ? C78 H78 0.9300 . ? C79 H79 0.9300 . ? C79 C80 1.384(7) . ? C80 H80 0.9300 . ? C80 C81 1.346(7) . ? C81 H81 0.9300 . ? C81 C82 1.341(8) . ? C82 H82 0.9300 . ? C82 C83 1.379(6) . ? C83 H83 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Cd1 O2 90.62(10) . . ? O5 Cd1 O6 84.55(9) . . ? O5 Cd1 N2 91.96(11) . . ? O5 Cd1 N3 92.74(14) . . ? O5 Cd1 N4 157.15(11) . . ? O6 Cd1 O2 174.40(9) . . ? N2 Cd1 O2 71.64(10) . . ? N2 Cd1 O6 111.29(11) . . ? N2 Cd1 N3 152.23(12) . . ? N2 Cd1 N4 95.90(11) . . ? N3 Cd1 O2 80.96(12) . . ? N3 Cd1 O6 96.40(12) . . ? N4 Cd1 O2 112.21(11) . . ? N4 Cd1 O6 72.60(10) . . ? N4 Cd1 N3 90.23(13) . . ? O10 Cd2 O9 171.89(10) . . ? O10 Cd2 N6 80.84(12) . . ? N5 Cd2 O9 72.03(10) . . ? N5 Cd2 O10 114.46(11) . . ? N5 Cd2 N6 89.52(12) . . ? N5 Cd2 N7 153.49(12) . . ? N5 Cd2 N8 99.76(11) . . ? N6 Cd2 O9 94.67(12) . . ? N7 Cd2 O9 81.68(10) . . ? N7 Cd2 O10 92.03(11) . . ? N7 Cd2 N6 96.08(13) . . ? N8 Cd2 O9 111.82(12) . . ? N8 Cd2 O10 72.69(11) . . ? N8 Cd2 N6 153.47(13) . . ? N8 Cd2 N7 86.66(12) . . ? O4 Cd3 O17 170.74(10) . . ? O4 Cd3 N14 82.74(12) . . ? N1 Cd3 O4 72.91(10) . . ? N1 Cd3 O17 114.34(10) . . ? N1 Cd3 N13 100.85(11) . . ? N1 Cd3 N14 155.64(13) . . ? N1 Cd3 N15 92.00(11) . . ? N13 Cd3 O4 113.54(11) . . ? N13 Cd3 O17 71.68(10) . . ? N13 Cd3 N14 88.84(13) . . ? N13 Cd3 N15 152.20(13) . . ? N14 Cd3 O17 89.88(13) . . ? N15 Cd3 O4 93.72(11) . . ? N15 Cd3 O17 80.57(11) . . ? N15 Cd3 N14 89.35(13) . . ? O13 Cd4 O14 169.39(9) . . ? N9 Cd4 O13 71.46(11) . . ? N9 Cd4 O14 114.24(11) . . ? N9 Cd4 N10 101.46(12) . . ? N9 Cd4 N11 150.61(14) . . ? N10 Cd4 O13 88.53(12) . . ? N10 Cd4 O14 81.61(12) . . ? N10 Cd4 N11 90.78(13) . . ? N11 Cd4 O13 82.39(13) . . ? N11 Cd4 O14 93.79(13) . . ? N12 Cd4 O13 119.57(11) . . ? N12 Cd4 O14 70.33(11) . . ? N12 Cd4 N9 89.14(11) . . ? N12 Cd4 N10 151.90(14) . . ? N12 Cd4 N11 92.40(12) . . ? C1 O1 H1 109.5 . . ? C1 O2 Cd1 114.3(3) . . ? C4 O4 Cd3 115.5(2) . . ? Cd1 O5 H5A 124(2) . . ? Cd1 O5 H5B 122(2) . . ? H5A O5 H5B 108(2) . . ? C18 O6 Cd1 116.2(2) . . ? C21 O8 H8 109.5 . . ? C21 O9 Cd2 114.4(3) . . ? C40 O10 Cd2 114.4(3) . . ? C40 O11 H11 109.5 . . ? C43 O13 Cd4 116.1(3) . . ? C62 O14 Cd4 114.8(3) . . ? C62 O15 H15 109.5 . . ? C65 O17 Cd3 114.9(3) . . ? C3 N1 Cd3 113.6(2) . . ? C5 N1 Cd3 141.9(3) . . ? C5 N1 C3 104.3(3) . . ? C2 N2 Cd1 113.3(3) . . ? C5 N2 Cd1 139.6(2) . . ? C5 N2 C2 105.3(3) . . ? C13 N3 Cd1 121.8(4) . . ? C17 N3 Cd1 121.0(4) . . ? C17 N3 C13 117.0(6) . . ? C19 N4 Cd1 111.5(2) . . ? C22 N4 Cd1 143.2(3) . . ? C22 N4 C19 105.3(3) . . ? C20 N5 Cd2 114.6(2) . . ? C22 N5 Cd2 139.0(3) . . ? C22 N5 C20 105.4(3) . . ? C30 N6 Cd2 119.5(4) . . ? C34 N6 Cd2 124.1(3) . . ? C34 N6 C30 116.2(5) . . ? C35 N7 Cd2 122.9(3) . . ? C39 N7 Cd2 120.4(3) . . ? C39 N7 C35 116.6(4) . . ? C41 N8 Cd2 110.8(3) . . ? C44 N8 Cd2 141.5(3) . . ? C44 N8 C41 105.3(3) . . ? C42 N9 Cd4 113.3(2) . . ? C42 N9 C44 104.4(4) . . ? C44 N9 Cd4 141.2(3) . . ? C52 N10 Cd4 120.3(4) . . ? C56 N10 Cd4 123.3(3) . . ? C56 N10 C52 116.1(4) . . ? C57 N11 Cd4 125.8(4) . . ? C61 N11 Cd4 118.8(4) . . ? C61 N11 C57 115.3(5) . . ? C63 N12 Cd4 116.6(2) . . ? C63 N12 C66 105.9(3) . . ? C66 N12 Cd4 137.0(3) . . ? C64 N13 Cd3 113.0(3) . . ? C66 N13 Cd3 141.0(3) . . ? C66 N13 C64 105.4(3) . . ? C74 N14 Cd3 122.4(4) . . ? C78 N14 Cd3 121.3(4) . . ? C78 N14 C74 116.2(5) . . ? C79 N15 Cd3 123.9(3) . . ? C79 N15 C83 116.6(4) . . ? C83 N15 Cd3 119.5(3) . . ? O1 C1 C2 118.3(4) . . ? O2 C1 O1 121.5(4) . . ? O2 C1 C2 120.2(4) . . ? N2 C2 C1 118.7(3) . . ? N2 C2 C3 108.2(3) . . ? C3 C2 C1 133.1(3) . . ? N1 C3 C2 109.2(3) . . ? N1 C3 C4 119.5(3) . . ? C2 C3 C4 131.2(4) . . ? O3 C4 C3 117.1(4) . . ? O4 C4 O3 124.4(4) . . ? O4 C4 C3 118.5(4) . . ? N1 C5 C8 122.1(4) . . ? N2 C5 N1 112.9(3) . . ? N2 C5 C8 124.8(3) . . ? C7 C6 H6 119.6 . . ? C11 C6 H6 119.6 . . ? C11 C6 C7 120.9(5) . . ? C6 C7 H7 119.5 . . ? C6 C7 C8 121.1(5) . . ? C8 C7 H7 119.5 . . ? C7 C8 C5 121.0(4) . . ? C9 C8 C5 121.3(4) . . ? C9 C8 C7 117.6(4) . . ? C8 C9 H9 119.8 . . ? C8 C9 C10 120.5(4) . . ? C10 C9 H9 119.8 . . ? C9 C10 H10 119.6 . . ? C11 C10 C9 120.8(5) . . ? C11 C10 H10 119.6 . . ? C6 C11 C12 120.9(5) . . ? C10 C11 C6 119.1(5) . . ? C10 C11 C12 120.0(5) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N3 C13 H13 118.4 . . ? N3 C13 C14 123.2(7) . . ? C14 C13 H13 118.4 . . ? C13 C14 H14 120.4 . . ? C15 C14 C13 119.3(8) . . ? C15 C14 H14 120.4 . . ? C14 C15 H15A 121.1 . . ? C16 C15 C14 117.8(8) . . ? C16 C15 H15A 121.1 . . ? C15 C16 H16 120.4 . . ? C15 C16 C17 119.2(8) . . ? C17 C16 H16 120.4 . . ? N3 C17 C16 123.4(7) . . ? N3 C17 H17 118.3 . . ? C16 C17 H17 118.3 . . ? O6 C18 O7 123.4(4) . . ? O6 C18 C19 119.1(4) . . ? O7 C18 C19 117.4(3) . . ? N4 C19 C18 120.5(3) . . ? N4 C19 C20 108.4(3) . . ? C20 C19 C18 131.1(4) . . ? N5 C20 C19 108.3(3) . . ? N5 C20 C21 118.9(3) . . ? C19 C20 C21 132.7(4) . . ? O8 C21 C20 117.9(3) . . ? O9 C21 O8 122.6(4) . . ? O9 C21 C20 119.5(4) . . ? N4 C22 N5 112.5(3) . . ? N4 C22 C25 122.9(3) . . ? N5 C22 C25 124.6(3) . . ? C24 C23 H23 119.4 . . ? C28 C23 H23 119.4 . . ? C28 C23 C24 121.1(6) . . ? C23 C24 H24 119.1 . . ? C25 C24 C23 121.8(6) . . ? C25 C24 H24 119.1 . . ? C24 C25 C22 120.4(4) . . ? C26 C25 C22 122.8(4) . . ? C26 C25 C24 116.7(5) . . ? C25 C26 H26 119.8 . . ? C25 C26 C27 120.3(6) . . ? C27 C26 H26 119.8 . . ? C26 C27 H27 119.0 . . ? C28 C27 C26 122.0(7) . . ? C28 C27 H27 119.0 . . ? C23 C28 C29 120.2(6) . . ? C27 C28 C23 117.9(5) . . ? C27 C28 C29 121.9(6) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29B 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N6 C30 H30 118.5 . . ? N6 C30 C31 122.9(6) . . ? C31 C30 H30 118.5 . . ? C30 C31 H31 120.6 . . ? C32 C31 C30 118.8(6) . . ? C32 C31 H31 120.6 . . ? C31 C32 H32 120.8 . . ? C33 C32 C31 118.4(6) . . ? C33 C32 H32 120.8 . . ? C32 C33 H33 120.4 . . ? C32 C33 C34 119.2(6) . . ? C34 C33 H33 120.4 . . ? N6 C34 C33 124.5(5) . . ? N6 C34 H34 117.8 . . ? C33 C34 H34 117.8 . . ? N7 C35 H35 118.8 . . ? N7 C35 C36 122.4(5) . . ? C36 C35 H35 118.8 . . ? C35 C36 H36 120.3 . . ? C37 C36 C35 119.5(5) . . ? C37 C36 H36 120.3 . . ? C36 C37 H37 120.7 . . ? C36 C37 C38 118.5(5) . . ? C38 C37 H37 120.7 . . ? C37 C38 H38 120.8 . . ? C37 C38 C39 118.5(6) . . ? C39 C38 H38 120.8 . . ? N7 C39 C38 124.5(5) . . ? N7 C39 H39 117.8 . . ? C38 C39 H39 117.8 . . ? O10 C40 O11 120.7(4) . . ? O10 C40 C41 121.2(4) . . ? O11 C40 C41 118.1(4) . . ? N8 C41 C40 119.9(4) . . ? N8 C41 C42 107.3(4) . . ? C42 C41 C40 132.7(4) . . ? N9 C42 C41 109.6(3) . . ? N9 C42 C43 120.4(4) . . ? C41 C42 C43 130.0(4) . . ? O12 C43 C42 118.4(4) . . ? O13 C43 O12 123.9(4) . . ? O13 C43 C42 117.8(4) . . ? N8 C44 N9 113.3(4) . . ? N8 C44 C47 123.2(4) . . ? N9 C44 C47 123.5(4) . . ? C46 C45 H45 119.5 . . ? C50 C45 H45 119.5 . . ? C50 C45 C46 121.0(7) . . ? C45 C46 H46 119.6 . . ? C47 C46 C45 120.9(6) . . ? C47 C46 H46 119.6 . . ? C46 C47 C44 121.6(4) . . ? C46 C47 C48 118.0(5) . . ? C48 C47 C44 120.4(5) . . ? C47 C48 H48 119.9 . . ? C49 C48 C47 120.2(6) . . ? C49 C48 H48 119.9 . . ? C48 C49 H49 119.2 . . ? C50 C49 C48 121.6(6) . . ? C50 C49 H49 119.2 . . ? C45 C50 C51 118.6(8) . . ? C49 C50 C45 118.2(6) . . ? C49 C50 C51 123.2(7) . . ? C50 C51 H51A 109.5 . . ? C50 C51 H51B 109.5 . . ? C50 C51 H51C 109.5 . . ? H51A C51 H51B 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? N10 C52 H52 118.2 . . ? N10 C52 C53 123.7(6) . . ? C53 C52 H52 118.2 . . ? C52 C53 H53 120.5 . . ? C54 C53 C52 119.0(6) . . ? C54 C53 H53 120.5 . . ? C53 C54 H54 120.7 . . ? C53 C54 C55 118.5(5) . . ? C55 C54 H54 120.7 . . ? C54 C55 H55 120.3 . . ? C54 C55 C56 119.3(6) . . ? C56 C55 H55 120.3 . . ? N10 C56 C55 123.3(5) . . ? N10 C56 H56 118.4 . . ? C55 C56 H56 118.4 . . ? N11 C57 H57 118.0 . . ? N11 C57 C58 124.0(6) . . ? C58 C57 H57 118.0 . . ? C57 C58 H58 120.2 . . ? C59 C58 C57 119.7(7) . . ? C59 C58 H58 120.2 . . ? C58 C59 H59 121.1 . . ? C60 C59 C58 117.7(6) . . ? C60 C59 H59 121.1 . . ? C59 C60 H60 120.3 . . ? C59 C60 C61 119.3(8) . . ? C61 C60 H60 120.3 . . ? N11 C61 C60 123.9(7) . . ? N11 C61 H61 118.1 . . ? C60 C61 H61 118.1 . . ? O14 C62 O15 123.0(4) . . ? O14 C62 C63 118.1(4) . . ? O15 C62 C63 118.9(3) . . ? N12 C63 C62 120.0(3) . . ? N12 C63 C64 108.1(3) . . ? C64 C63 C62 131.9(4) . . ? N13 C64 C63 108.4(4) . . ? N13 C64 C65 121.0(3) . . ? C63 C64 C65 130.5(4) . . ? O16 C65 C64 118.1(3) . . ? O17 C65 O16 122.6(4) . . ? O17 C65 C64 119.3(4) . . ? N12 C66 C69 120.5(3) . . ? N13 C66 N12 112.2(4) . . ? N13 C66 C69 127.3(3) . . ? C68 C67 H67 119.9 . . ? C72 C67 H67 119.9 . . ? C72 C67 C68 120.3(5) . . ? C67 C68 H68 119.0 . . ? C69 C68 C67 121.9(5) . . ? C69 C68 H68 119.0 . . ? C68 C69 C66 120.5(4) . . ? C70 C69 C66 121.5(4) . . ? C70 C69 C68 117.8(5) . . ? C69 C70 H70 120.1 . . ? C69 C70 C71 119.7(5) . . ? C71 C70 H70 120.1 . . ? C70 C71 H71 119.4 . . ? C72 C71 C70 121.2(6) . . ? C72 C71 H71 119.4 . . ? C67 C72 C71 119.1(6) . . ? C67 C72 C73 120.5(6) . . ? C71 C72 C73 120.4(6) . . ? C72 C73 H73A 109.5 . . ? C72 C73 H73B 109.5 . . ? C72 C73 H73C 109.5 . . ? H73A C73 H73B 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? N14 C74 H74 118.0 . . ? N14 C74 C75 124.1(5) . . ? C75 C74 H74 118.0 . . ? C74 C75 H75 120.9 . . ? C76 C75 C74 118.1(6) . . ? C76 C75 H75 120.9 . . ? C75 C76 H76 120.6 . . ? C77 C76 C75 118.9(6) . . ? C77 C76 H76 120.6 . . ? C76 C77 H77 119.8 . . ? C76 C77 C78 120.5(7) . . ? C78 C77 H77 119.8 . . ? N14 C78 C77 122.2(6) . . ? N14 C78 H78 118.9 . . ? C77 C78 H78 118.9 . . ? N15 C79 H79 118.2 . . ? N15 C79 C80 123.6(5) . . ? C80 C79 H79 118.2 . . ? C79 C80 H80 120.5 . . ? C81 C80 C79 119.1(6) . . ? C81 C80 H80 120.5 . . ? C80 C81 H81 121.0 . . ? C82 C81 C80 118.0(5) . . ? C82 C81 H81 121.0 . . ? C81 C82 H82 119.9 . . ? C81 C82 C83 120.2(5) . . ? C83 C82 H82 119.9 . . ? N15 C83 C82 122.6(5) . . ? N15 C83 H83 118.7 . . ? C82 C83 H83 118.7 . . ? 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 Cd1 O2 C1 O1 -171.1(3) . . . . ? Cd1 O2 C1 C2 8.0(5) . . . . ? Cd1 O6 C18 O7 -179.5(3) . . . . ? Cd1 O6 C18 C19 2.4(5) . . . . ? Cd1 N2 C2 C1 -12.5(4) . . . . ? Cd1 N2 C2 C3 166.8(2) . . . . ? Cd1 N2 C5 N1 -161.4(3) . . . . ? Cd1 N2 C5 C8 23.6(6) . . . . ? Cd1 N3 C13 C14 176.1(6) . . . . ? Cd1 N3 C17 C16 -176.7(6) . . . . ? Cd1 N4 C19 C18 -3.1(5) . . . . ? Cd1 N4 C19 C20 177.8(3) . . . . ? Cd1 N4 C22 N5 -177.3(3) . . . . ? Cd1 N4 C22 C25 5.6(8) . . . . ? Cd2 O9 C21 O8 176.6(4) . . . . ? Cd2 O9 C21 C20 -3.3(5) . . . . ? Cd2 O10 C40 O11 -176.9(3) . . . . ? Cd2 O10 C40 C41 3.8(5) . . . . ? Cd2 N5 C20 C19 -171.4(3) . . . . ? Cd2 N5 C20 C21 7.8(5) . . . . ? Cd2 N5 C22 N4 167.4(3) . . . . ? Cd2 N5 C22 C25 -15.5(7) . . . . ? Cd2 N6 C30 C31 -174.5(5) . . . . ? Cd2 N6 C34 C33 174.9(4) . . . . ? Cd2 N7 C35 C36 -176.7(4) . . . . ? Cd2 N7 C39 C38 177.8(5) . . . . ? Cd2 N8 C41 C40 -10.3(4) . . . . ? Cd2 N8 C41 C42 166.2(2) . . . . ? Cd2 N8 C44 N9 -158.3(3) . . . . ? Cd2 N8 C44 C47 21.9(6) . . . . ? Cd3 O4 C4 O3 178.8(3) . . . . ? Cd3 O4 C4 C3 -1.4(4) . . . . ? Cd3 O17 C65 O16 177.7(3) . . . . ? Cd3 O17 C65 C64 -2.8(5) . . . . ? Cd3 N1 C3 C2 176.8(2) . . . . ? Cd3 N1 C3 C4 -0.2(4) . . . . ? Cd3 N1 C5 N2 -175.7(3) . . . . ? Cd3 N1 C5 C8 -0.6(6) . . . . ? Cd3 N13 C64 C63 173.9(2) . . . . ? Cd3 N13 C64 C65 -2.9(5) . . . . ? Cd3 N13 C66 N12 -170.1(3) . . . . ? Cd3 N13 C66 C69 11.1(7) . . . . ? Cd3 N14 C74 C75 175.4(5) . . . . ? Cd3 N14 C78 C77 -176.3(7) . . . . ? Cd3 N15 C79 C80 177.4(4) . . . . ? Cd3 N15 C83 C82 -178.1(4) . . . . ? Cd4 O13 C43 O12 -172.6(3) . . . . ? Cd4 O13 C43 C42 8.1(4) . . . . ? Cd4 O14 C62 O15 -175.4(3) . . . . ? Cd4 O14 C62 C63 3.7(5) . . . . ? Cd4 N9 C42 C41 171.9(2) . . . . ? Cd4 N9 C42 C43 -7.1(4) . . . . ? Cd4 N9 C44 N8 -167.7(3) . . . . ? Cd4 N9 C44 C47 12.0(6) . . . . ? Cd4 N10 C52 C53 -174.6(5) . . . . ? Cd4 N10 C56 C55 175.6(4) . . . . ? Cd4 N11 C57 C58 179.7(5) . . . . ? Cd4 N11 C61 C60 -179.8(7) . . . . ? Cd4 N12 C63 C62 -3.3(5) . . . . ? Cd4 N12 C63 C64 174.7(2) . . . . ? Cd4 N12 C66 N13 -172.3(3) . . . . ? Cd4 N12 C66 C69 6.5(6) . . . . ? O1 C1 C2 N2 -177.9(3) . . . . ? O1 C1 C2 C3 2.9(7) . . . . ? O2 Cd1 O6 C18 -152.7(10) . . . . ? O2 Cd1 N2 C2 11.5(2) . . . . ? O2 Cd1 N2 C5 173.0(4) . . . . ? O2 Cd1 N3 C13 102.0(5) . . . . ? O2 Cd1 N3 C17 -81.7(5) . . . . ? O2 Cd1 N4 C19 180.0(3) . . . . ? O2 Cd1 N4 C22 -2.6(5) . . . . ? O2 C1 C2 N2 2.9(6) . . . . ? O2 C1 C2 C3 -176.3(4) . . . . ? O4 Cd3 O17 C65 126.8(5) . . . . ? O4 Cd3 N1 C3 -0.4(2) . . . . ? O4 Cd3 N1 C5 174.3(4) . . . . ? O4 Cd3 N13 C64 -170.8(2) . . . . ? O4 Cd3 N13 C66 -1.1(5) . . . . ? O4 Cd3 N14 C74 127.2(5) . . . . ? O4 Cd3 N14 C78 -55.6(6) . . . . ? O4 Cd3 N15 C79 154.3(4) . . . . ? O4 Cd3 N15 C83 -28.4(4) . . . . ? O5 Cd1 O2 C1 -102.5(3) . . . . ? O5 Cd1 O6 C18 176.7(3) . . . . ? O5 Cd1 N2 C2 101.5(2) . . . . ? O5 Cd1 N2 C5 -97.0(4) . . . . ? O5 Cd1 N3 C13 11.8(5) . . . . ? O5 Cd1 N3 C17 -171.9(5) . . . . ? O5 Cd1 N4 C19 2.0(5) . . . . ? O5 Cd1 N4 C22 179.4(4) . . . . ? O6 Cd1 O2 C1 -133.0(10) . . . . ? O6 Cd1 N2 C2 -173.6(2) . . . . ? O6 Cd1 N2 C5 -12.1(4) . . . . ? O6 Cd1 N3 C13 -73.1(4) . . . . ? O6 Cd1 N3 C17 103.3(5) . . . . ? O6 Cd1 N4 C19 3.0(3) . . . . ? O6 Cd1 N4 C22 -179.6(5) . . . . ? O6 C18 C19 N4 0.6(6) . . . . ? O6 C18 C19 C20 179.4(4) . . . . ? O7 C18 C19 N4 -177.7(4) . . . . ? O7 C18 C19 C20 1.2(7) . . . . ? O9 Cd2 O10 C40 118.2(7) . . . . ? O9 Cd2 N5 C20 -6.6(3) . . . . ? O9 Cd2 N5 C22 -173.1(5) . . . . ? O9 Cd2 N6 C30 -39.5(4) . . . . ? O9 Cd2 N6 C34 146.7(4) . . . . ? O9 Cd2 N7 C35 -103.1(4) . . . . ? O9 Cd2 N7 C39 80.3(4) . . . . ? O9 Cd2 N8 C41 -164.3(2) . . . . ? O9 Cd2 N8 C44 -5.6(4) . . . . ? O10 Cd2 O9 C21 149.3(7) . . . . ? O10 Cd2 N5 C20 178.6(3) . . . . ? O10 Cd2 N5 C22 12.1(5) . . . . ? O10 Cd2 N6 C30 147.3(4) . . . . ? O10 Cd2 N6 C34 -26.5(4) . . . . ? O10 Cd2 N7 C35 71.8(4) . . . . ? O10 Cd2 N7 C39 -104.8(4) . . . . ? O10 Cd2 N8 C41 8.5(2) . . . . ? O10 Cd2 N8 C44 167.3(4) . . . . ? O10 C40 C41 N8 4.7(6) . . . . ? O10 C40 C41 C42 -170.7(4) . . . . ? O11 C40 C41 N8 -174.6(3) . . . . ? O11 C40 C41 C42 10.0(7) . . . . ? O13 Cd4 O14 C62 -163.6(4) . . . . ? O13 Cd4 N9 C42 7.7(2) . . . . ? O13 Cd4 N9 C44 173.2(4) . . . . ? O13 Cd4 N10 C52 9.8(4) . . . . ? O13 Cd4 N10 C56 -164.0(4) . . . . ? O13 Cd4 N11 C57 -2.6(4) . . . . ? O13 Cd4 N11 C61 179.5(6) . . . . ? O13 Cd4 N12 C63 179.3(3) . . . . ? O13 Cd4 N12 C66 -9.7(4) . . . . ? O14 Cd4 O13 C43 -132.9(5) . . . . ? O14 Cd4 N9 C42 178.1(2) . . . . ? O14 Cd4 N9 C44 -16.4(4) . . . . ? O14 Cd4 N10 C52 -174.2(4) . . . . ? O14 Cd4 N10 C56 12.1(4) . . . . ? O14 Cd4 N11 C57 -172.7(4) . . . . ? O14 Cd4 N11 C61 9.5(5) . . . . ? O14 Cd4 N12 C63 3.5(3) . . . . ? O14 Cd4 N12 C66 174.6(4) . . . . ? O14 C62 C63 N12 -0.6(6) . . . . ? O14 C62 C63 C64 -178.0(4) . . . . ? O15 C62 C63 N12 178.6(4) . . . . ? O15 C62 C63 C64 1.2(7) . . . . ? O17 Cd3 O4 C4 143.5(5) . . . . ? O17 Cd3 N1 C3 -174.2(2) . . . . ? O17 Cd3 N1 C5 0.5(4) . . . . ? O17 Cd3 N13 C64 1.0(3) . . . . ? O17 Cd3 N13 C66 170.7(4) . . . . ? O17 Cd3 N14 C74 -58.4(4) . . . . ? O17 Cd3 N14 C78 118.8(6) . . . . ? O17 Cd3 N15 C79 -18.4(4) . . . . ? O17 Cd3 N15 C83 159.0(4) . . . . ? N1 Cd3 O4 C4 1.0(3) . . . . ? N1 Cd3 O17 C65 -92.9(3) . . . . ? N1 Cd3 N13 C64 113.3(3) . . . . ? N1 Cd3 N13 C66 -77.1(4) . . . . ? N1 Cd3 N14 C74 127.6(4) . . . . ? N1 Cd3 N14 C78 -55.2(7) . . . . ? N1 Cd3 N15 C79 -132.8(4) . . . . ? N1 Cd3 N15 C83 44.6(4) . . . . ? N1 C3 C4 O3 -179.1(3) . . . . ? N1 C3 C4 O4 1.1(5) . . . . ? N1 C5 C8 C7 -142.4(4) . . . . ? N1 C5 C8 C9 34.3(6) . . . . ? N2 Cd1 O2 C1 -10.6(3) . . . . ? N2 Cd1 O6 C18 86.7(3) . . . . ? N2 Cd1 N3 C13 111.2(5) . . . . ? N2 Cd1 N3 C17 -72.4(5) . . . . ? N2 Cd1 N4 C19 -107.5(3) . . . . ? N2 Cd1 N4 C22 69.9(5) . . . . ? N2 C2 C3 N1 0.4(4) . . . . ? N2 C2 C3 C4 176.9(4) . . . . ? N2 C5 C8 C7 32.1(6) . . . . ? N2 C5 C8 C9 -151.1(4) . . . . ? N3 Cd1 O2 C1 164.8(3) . . . . ? N3 Cd1 O6 C18 -91.2(3) . . . . ? N3 Cd1 N2 C2 1.9(4) . . . . ? N3 Cd1 N2 C5 163.3(4) . . . . ? N3 Cd1 N4 C19 99.6(3) . . . . ? N3 Cd1 N4 C22 -82.9(5) . . . . ? N3 C13 C14 C15 1.3(13) . . . . ? N4 Cd1 O2 C1 78.3(3) . . . . ? N4 Cd1 O6 C18 -2.9(3) . . . . ? N4 Cd1 N2 C2 -100.0(2) . . . . ? N4 Cd1 N2 C5 61.5(4) . . . . ? N4 Cd1 N3 C13 -145.6(4) . . . . ? N4 Cd1 N3 C17 30.8(5) . . . . ? N4 C19 C20 N5 0.8(5) . . . . ? N4 C19 C20 C21 -178.3(4) . . . . ? N4 C22 C25 C24 -39.0(7) . . . . ? N4 C22 C25 C26 138.2(6) . . . . ? N5 Cd2 O9 C21 5.3(3) . . . . ? N5 Cd2 O10 C40 -99.8(3) . . . . ? N5 Cd2 N6 C30 32.4(4) . . . . ? N5 Cd2 N6 C34 -141.4(4) . . . . ? N5 Cd2 N7 C35 -110.4(4) . . . . ? N5 Cd2 N7 C39 72.9(5) . . . . ? N5 Cd2 N8 C41 121.2(2) . . . . ? N5 Cd2 N8 C44 -80.0(4) . . . . ? N5 C20 C21 O8 177.2(4) . . . . ? N5 C20 C21 O9 -3.0(6) . . . . ? N5 C22 C25 C24 144.3(5) . . . . ? N5 C22 C25 C26 -38.5(8) . . . . ? N6 Cd2 O9 C21 93.3(3) . . . . ? N6 Cd2 O10 C40 175.0(3) . . . . ? N6 Cd2 N5 C20 -101.7(3) . . . . ? N6 Cd2 N5 C22 91.8(4) . . . . ? N6 Cd2 N7 C35 -9.2(4) . . . . ? N6 Cd2 N7 C39 174.2(4) . . . . ? N6 Cd2 N8 C41 12.2(4) . . . . ? N6 Cd2 N8 C44 171.0(4) . . . . ? N6 C30 C31 C32 -1.0(11) . . . . ? N7 Cd2 O9 C21 -171.2(3) . . . . ? N7 Cd2 O10 C40 79.1(3) . . . . ? N7 Cd2 N5 C20 1.0(5) . . . . ? N7 Cd2 N5 C22 -165.4(4) . . . . ? N7 Cd2 N6 C30 -121.6(4) . . . . ? N7 Cd2 N6 C34 64.6(4) . . . . ? N7 Cd2 N8 C41 -84.7(2) . . . . ? N7 Cd2 N8 C44 74.1(4) . . . . ? N7 C35 C36 C37 -0.4(8) . . . . ? N8 Cd2 O9 C21 -88.2(3) . . . . ? N8 Cd2 O10 C40 -6.7(3) . . . . ? N8 Cd2 N5 C20 103.3(3) . . . . ? N8 Cd2 N5 C22 -63.2(5) . . . . ? N8 Cd2 N6 C30 143.7(4) . . . . ? N8 Cd2 N6 C34 -30.1(5) . . . . ? N8 Cd2 N7 C35 144.3(4) . . . . ? N8 Cd2 N7 C39 -32.3(4) . . . . ? N8 C41 C42 N9 -0.6(4) . . . . ? N8 C41 C42 C43 178.3(4) . . . . ? N8 C44 C47 C46 -145.0(5) . . . . ? N8 C44 C47 C48 36.2(6) . . . . ? N9 Cd4 O13 C43 -8.7(3) . . . . ? N9 Cd4 O14 C62 75.8(3) . . . . ? N9 Cd4 N10 C52 -61.0(4) . . . . ? N9 Cd4 N10 C56 125.3(4) . . . . ? N9 Cd4 N11 C57 24.4(5) . . . . ? N9 Cd4 N11 C61 -153.5(5) . . . . ? N9 Cd4 N12 C63 -112.7(3) . . . . ? N9 Cd4 N12 C66 58.4(4) . . . . ? N9 C42 C43 O12 179.9(3) . . . . ? N9 C42 C43 O13 -0.7(5) . . . . ? N9 C44 C47 C46 35.3(6) . . . . ? N9 C44 C47 C48 -143.6(4) . . . . ? N10 Cd4 O13 C43 -111.3(3) . . . . ? N10 Cd4 O14 C62 174.6(3) . . . . ? N10 Cd4 N9 C42 92.2(3) . . . . ? N10 Cd4 N9 C44 -102.3(4) . . . . ? N10 Cd4 N11 C57 -91.0(4) . . . . ? N10 Cd4 N11 C61 91.1(6) . . . . ? N10 Cd4 N12 C63 0.5(4) . . . . ? N10 Cd4 N12 C66 171.6(3) . . . . ? N10 C52 C53 C54 -1.7(11) . . . . ? N11 Cd4 O13 C43 157.7(3) . . . . ? N11 Cd4 O14 C62 -95.1(3) . . . . ? N11 Cd4 N9 C42 -20.6(4) . . . . ? N11 Cd4 N9 C44 144.8(4) . . . . ? N11 Cd4 N10 C52 92.1(4) . . . . ? N11 Cd4 N10 C56 -81.6(4) . . . . ? N11 Cd4 N12 C63 96.7(3) . . . . ? N11 Cd4 N12 C66 -92.3(4) . . . . ? N11 C57 C58 C59 -0.2(11) . . . . ? N12 Cd4 O13 C43 69.2(3) . . . . ? N12 Cd4 O14 C62 -3.9(3) . . . . ? N12 Cd4 N9 C42 -114.0(3) . . . . ? N12 Cd4 N9 C44 51.5(4) . . . . ? N12 Cd4 N10 C52 -171.3(3) . . . . ? N12 Cd4 N10 C56 15.0(6) . . . . ? N12 Cd4 N11 C57 116.9(4) . . . . ? N12 Cd4 N11 C61 -61.0(6) . . . . ? N12 C63 C64 N13 -1.1(5) . . . . ? N12 C63 C64 C65 175.3(4) . . . . ? N12 C66 C69 C68 44.7(6) . . . . ? N12 C66 C69 C70 -129.6(5) . . . . ? N13 Cd3 O4 C4 -93.7(3) . . . . ? N13 Cd3 O17 C65 1.0(3) . . . . ? N13 Cd3 N1 C3 111.1(2) . . . . ? N13 Cd3 N1 C5 -74.2(4) . . . . ? N13 Cd3 N14 C74 13.3(5) . . . . ? N13 Cd3 N14 C78 -169.5(6) . . . . ? N13 Cd3 N15 C79 -14.7(6) . . . . ? N13 Cd3 N15 C83 162.7(3) . . . . ? N13 C64 C65 O16 -176.4(4) . . . . ? N13 C64 C65 O17 4.0(6) . . . . ? N13 C66 C69 C68 -136.6(4) . . . . ? N13 C66 C69 C70 49.1(7) . . . . ? N14 Cd3 O4 C4 -179.2(3) . . . . ? N14 Cd3 O17 C65 89.8(3) . . . . ? N14 Cd3 N1 C3 -0.8(4) . . . . ? N14 Cd3 N1 C5 173.9(4) . . . . ? N14 Cd3 N13 C64 -89.2(3) . . . . ? N14 Cd3 N13 C66 80.4(4) . . . . ? N14 Cd3 N15 C79 71.6(4) . . . . ? N14 Cd3 N15 C83 -111.0(4) . . . . ? N14 C74 C75 C76 1.3(11) . . . . ? N15 Cd3 O4 C4 91.9(3) . . . . ? N15 Cd3 O17 C65 179.2(3) . . . . ? N15 Cd3 N1 C3 -93.6(3) . . . . ? N15 Cd3 N1 C5 81.1(4) . . . . ? N15 Cd3 N13 C64 -2.8(4) . . . . ? N15 Cd3 N13 C66 166.8(4) . . . . ? N15 Cd3 N14 C74 -139.0(5) . . . . ? N15 Cd3 N14 C78 38.3(6) . . . . ? N15 C79 C80 C81 1.0(10) . . . . ? C1 C2 C3 N1 179.7(4) . . . . ? C1 C2 C3 C4 -3.9(7) . . . . ? C2 N2 C5 N1 1.0(4) . . . . ? C2 N2 C5 C8 -174.0(4) . . . . ? C2 C3 C4 O3 4.7(6) . . . . ? C2 C3 C4 O4 -175.1(4) . . . . ? C3 N1 C5 N2 -0.7(4) . . . . ? C3 N1 C5 C8 174.4(3) . . . . ? C5 N1 C3 C2 0.2(4) . . . . ? C5 N1 C3 C4 -176.8(3) . . . . ? C5 N2 C2 C1 179.8(3) . . . . ? C5 N2 C2 C3 -0.8(4) . . . . ? C5 C8 C9 C10 -173.0(4) . . . . ? C6 C7 C8 C5 173.3(5) . . . . ? C6 C7 C8 C9 -3.6(7) . . . . ? C7 C6 C11 C10 0.9(9) . . . . ? C7 C6 C11 C12 -176.6(6) . . . . ? C7 C8 C9 C10 3.9(7) . . . . ? C8 C9 C10 C11 -1.9(8) . . . . ? C9 C10 C11 C6 -0.6(9) . . . . ? C9 C10 C11 C12 176.9(5) . . . . ? C11 C6 C7 C8 1.2(9) . . . . ? C13 N3 C17 C16 -0.2(10) . . . . ? C13 C14 C15 C16 -1.7(13) . . . . ? C14 C15 C16 C17 1.2(13) . . . . ? C15 C16 C17 N3 -0.3(13) . . . . ? C17 N3 C13 C14 -0.3(10) . . . . ? C18 C19 C20 N5 -178.2(4) . . . . ? C18 C19 C20 C21 2.7(8) . . . . ? C19 N4 C22 N5 0.3(5) . . . . ? C19 N4 C22 C25 -176.8(4) . . . . ? C19 C20 C21 O8 -3.8(7) . . . . ? C19 C20 C21 O9 176.0(4) . . . . ? C20 N5 C22 N4 0.2(5) . . . . ? C20 N5 C22 C25 177.2(4) . . . . ? C22 N4 C19 C18 178.5(4) . . . . ? C22 N4 C19 C20 -0.6(5) . . . . ? C22 N5 C20 C19 -0.6(4) . . . . ? C22 N5 C20 C21 178.7(4) . . . . ? C22 C25 C26 C27 -178.0(7) . . . . ? C23 C24 C25 C22 176.6(5) . . . . ? C23 C24 C25 C26 -0.7(9) . . . . ? C24 C23 C28 C27 -2.0(11) . . . . ? C24 C23 C28 C29 177.7(6) . . . . ? C24 C25 C26 C27 -0.7(11) . . . . ? C25 C26 C27 C28 0.9(15) . . . . ? C26 C27 C28 C23 0.5(13) . . . . ? C26 C27 C28 C29 -179.2(8) . . . . ? C28 C23 C24 C25 2.2(10) . . . . ? C30 N6 C34 C33 0.9(7) . . . . ? C30 C31 C32 C33 1.6(11) . . . . ? C31 C32 C33 C34 -1.0(10) . . . . ? C32 C33 C34 N6 -0.3(9) . . . . ? C34 N6 C30 C31 -0.2(8) . . . . ? C35 N7 C39 C38 1.0(8) . . . . ? C35 C36 C37 C38 -0.1(9) . . . . ? C36 C37 C38 C39 1.1(9) . . . . ? C37 C38 C39 N7 -1.6(10) . . . . ? C39 N7 C35 C36 0.0(7) . . . . ? C40 C41 C42 N9 175.2(4) . . . . ? C40 C41 C42 C43 -5.9(7) . . . . ? C41 N8 C44 N9 1.2(4) . . . . ? C41 N8 C44 C47 -178.6(3) . . . . ? C41 C42 C43 O12 1.1(6) . . . . ? C41 C42 C43 O13 -179.6(4) . . . . ? C42 N9 C44 N8 -1.5(4) . . . . ? C42 N9 C44 C47 178.3(3) . . . . ? C44 N8 C41 C40 -176.8(3) . . . . ? C44 N8 C41 C42 -0.3(4) . . . . ? C44 N9 C42 C41 1.2(4) . . . . ? C44 N9 C42 C43 -177.8(3) . . . . ? C44 C47 C48 C49 -178.2(4) . . . . ? C45 C46 C47 C44 179.5(5) . . . . ? C45 C46 C47 C48 -1.6(8) . . . . ? C46 C45 C50 C49 1.4(10) . . . . ? C46 C45 C50 C51 179.7(6) . . . . ? C46 C47 C48 C49 2.9(7) . . . . ? C47 C48 C49 C50 -2.1(9) . . . . ? C48 C49 C50 C45 -0.1(10) . . . . ? C48 C49 C50 C51 -178.3(6) . . . . ? C50 C45 C46 C47 -0.5(10) . . . . ? C52 N10 C56 C55 1.6(8) . . . . ? C52 C53 C54 C55 2.6(11) . . . . ? C53 C54 C55 C56 -1.5(10) . . . . ? C54 C55 C56 N10 -0.7(9) . . . . ? C56 N10 C52 C53 -0.4(9) . . . . ? C57 N11 C61 C60 2.1(12) . . . . ? C57 C58 C59 C60 3.0(12) . . . . ? C58 C59 C60 C61 -3.3(14) . . . . ? C59 C60 C61 N11 0.7(15) . . . . ? C61 N11 C57 C58 -2.4(9) . . . . ? C62 C63 C64 N13 176.5(4) . . . . ? C62 C63 C64 C65 -7.1(8) . . . . ? C63 N12 C66 N13 -0.7(4) . . . . ? C63 N12 C66 C69 178.2(4) . . . . ? C63 C64 C65 O16 7.6(7) . . . . ? C63 C64 C65 O17 -172.0(4) . . . . ? C64 N13 C66 N12 0.0(4) . . . . ? C64 N13 C66 C69 -178.8(4) . . . . ? C66 N12 C63 C62 -176.9(3) . . . . ? C66 N12 C63 C64 1.1(4) . . . . ? C66 N13 C64 C63 0.7(4) . . . . ? C66 N13 C64 C65 -176.1(4) . . . . ? C66 C69 C70 C71 173.7(6) . . . . ? C67 C68 C69 C66 -173.7(4) . . . . ? C67 C68 C69 C70 0.8(8) . . . . ? C68 C67 C72 C71 -3.2(10) . . . . ? C68 C67 C72 C73 177.3(6) . . . . ? C68 C69 C70 C71 -0.8(9) . . . . ? C69 C70 C71 C72 -1.2(12) . . . . ? C70 C71 C72 C67 3.2(11) . . . . ? C70 C71 C72 C73 -177.3(7) . . . . ? C72 C67 C68 C69 1.3(9) . . . . ? C74 N14 C78 C77 1.1(12) . . . . ? C74 C75 C76 C77 0.2(13) . . . . ? C75 C76 C77 C78 -1.0(16) . . . . ? C76 C77 C78 N14 0.4(16) . . . . ? C78 N14 C74 C75 -2.0(10) . . . . ? C79 N15 C83 C82 -0.5(8) . . . . ? C79 C80 C81 C82 -1.4(9) . . . . ? C80 C81 C82 C83 0.9(9) . . . . ? C81 C82 C83 N15 0.0(9) . . . . ? C83 N15 C79 C80 0.0(9) . . . . ? data_a _database_code_depnum_ccdc_archive 'CCDC 885319' #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 Co1.50 N2 O8' _chemical_formula_weight 398.61 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 24.3529(9) _cell_length_b 24.3529(9) _cell_length_c 14.2468(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 7317.3(6) _cell_formula_units_Z 18 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.628 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3609 _exptl_absorpt_coefficient_mu 1.589 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.7417 _exptl_absorpt_correction_T_max 0.7630 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23571 _diffrn_reflns_av_R_equivalents 0.0772 _diffrn_reflns_av_sigmaI/netI 0.0569 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 27.99 _reflns_number_total 3936 _reflns_number_gt 2695 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0599P)^2^+26.0037P] 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 3936 _refine_ls_number_parameters 241 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0745 _refine_ls_R_factor_gt 0.0406 _refine_ls_wR_factor_ref 0.1179 _refine_ls_wR_factor_gt 0.0983 _refine_ls_goodness_of_fit_ref 0.905 _refine_ls_restrained_S_all 0.906 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.74617(2) 0.01353(2) 1.01868(3) 0.02297(13) Uani 1 1 d . . . Co2 Co 0.6667 -0.1667 1.3333 0.03226(19) Uani 1 2 d S . . O1 O 0.73273(11) -0.00930(10) 1.16129(15) 0.0262(5) Uani 1 1 d . . . O4 O 0.71680(12) -0.25685(10) 1.12608(15) 0.0301(5) Uani 1 1 d . . . C9 C 0.8490(3) -0.0588(3) 0.6943(3) 0.0616(13) Uani 1 1 d . . . C12 C 0.71365(16) -0.21064(15) 1.1615(2) 0.0258(7) Uani 1 1 d . . . N1 N 0.75640(13) -0.06672(12) 1.02214(18) 0.0265(6) Uani 1 1 d . . . N2 N 0.74680(13) -0.16291(12) 1.00719(17) 0.0244(6) Uani 1 1 d . . . C11 C 0.72959(15) -0.15718(15) 1.0974(2) 0.0239(7) Uani 1 1 d . . . O2 O 0.71091(15) -0.08485(12) 1.26347(17) 0.0483(8) Uani 1 1 d . . . C6 C 0.73547(16) -0.09802(15) 1.1061(2) 0.0243(7) Uani 1 1 d . . . C7 C 0.72512(15) -0.06331(14) 1.1820(2) 0.0252(7) Uani 1 1 d . . . C1 C 0.76292(16) -0.10756(15) 0.9654(2) 0.0269(7) Uani 1 1 d . . . C2 C 0.79034(19) -0.09034(17) 0.8707(2) 0.0340(8) Uani 1 1 d . . . C4 C 0.8427(2) -0.0306(2) 0.8550(3) 0.0472(10) Uani 1 1 d . . . H4 H 0.8583 -0.0009 0.9033 0.057 Uiso 1 1 calc R . . C10 C 0.7969(3) -0.1167(2) 0.7095(3) 0.0616(14) Uani 1 1 d . . . H10 H 0.7811 -0.1460 0.6607 0.074 Uiso 1 1 calc R . . C8 C 0.8832(3) -0.0411(4) 0.6001(4) 0.101(2) Uani 1 1 d . . . H8A H 0.8884 -0.0755 0.5781 0.151 Uiso 1 1 calc R . . H8B H 0.9241 -0.0039 0.6074 0.151 Uiso 1 1 calc R . . H8C H 0.8587 -0.0328 0.5554 0.151 Uiso 1 1 calc R . . C5 C 0.8716(2) -0.0151(2) 0.7677(3) 0.0631(13) Uani 1 1 d . . . H5 H 0.9066 0.0250 0.7580 0.076 Uiso 1 1 calc R . . C3 C 0.7668(2) -0.13310(19) 0.7964(3) 0.0473(11) Uani 1 1 d . . . H3 H 0.7310 -0.1727 0.8049 0.057 Uiso 1 1 calc R . . O6 O 0.72125(16) 0.08614(14) 1.0521(3) 0.0567(9) Uani 1 1 d . . . H6 H 0.7536 0.1210 1.0540 0.085 Uiso 1 1 calc R . . O7 O 0.64414(13) -0.04351(17) 1.0094(2) 0.0524(8) Uani 1 1 d D . . O8 O 0.7500(2) -0.13117(19) 1.4209(3) 0.0706(10) Uani 1 1 d D . . H8 H 0.7556 -0.1605 1.4360 0.106 Uiso 1 1 calc RD . . O5 O 0.6696(3) 0.1058(2) 0.8567(5) 0.0989(14) Uani 1 1 d D . . O9 O 0.69859(14) -0.21152(12) 1.24561(16) 0.0407(7) Uani 1 1 d . . . H1W H 0.693(3) 0.077(3) 1.098(4) 0.10(2) Uiso 1 1 d . . . H3W H 0.661(4) 0.080(3) 0.812(3) 0.14(4) Uiso 1 1 d D . . H2W H 0.675(5) 0.088(4) 0.905(3) 0.21(6) Uiso 1 1 d D . . H5W H 0.635(3) -0.060(3) 0.955(2) 0.11(2) Uiso 1 1 d D . . H4W H 0.633(6) -0.016(5) 1.018(5) 0.32(7) Uiso 1 1 d D . . H6W H 0.784(2) -0.0987(6) 1.438(7) 0.23(5) Uiso 1 1 d 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 0.0250(2) 0.0227(2) 0.0198(2) 0.00494(17) 0.00277(17) 0.01089(19) Co2 0.0573(5) 0.0272(3) 0.0173(3) 0.0049(3) 0.0101(3) 0.0250(3) O1 0.0398(13) 0.0229(11) 0.0192(11) 0.0037(9) 0.0062(10) 0.0182(10) O4 0.0480(15) 0.0256(12) 0.0216(11) 0.0020(9) 0.0089(10) 0.0221(11) C9 0.092(4) 0.082(4) 0.035(2) 0.017(2) 0.027(2) 0.062(3) C12 0.0333(18) 0.0247(16) 0.0224(16) 0.0022(13) 0.0047(13) 0.0169(14) N1 0.0380(16) 0.0272(14) 0.0172(13) 0.0014(11) 0.0037(11) 0.0184(13) N2 0.0326(15) 0.0257(14) 0.0177(12) 0.0000(10) 0.0040(11) 0.0167(12) C11 0.0311(17) 0.0257(16) 0.0165(14) -0.0006(12) 0.0032(12) 0.0154(14) O2 0.093(2) 0.0307(14) 0.0232(13) 0.0093(11) 0.0249(14) 0.0329(15) C6 0.0344(18) 0.0267(16) 0.0158(14) 0.0013(12) 0.0034(13) 0.0183(14) C7 0.0328(17) 0.0218(16) 0.0199(15) 0.0019(13) 0.0056(13) 0.0129(14) C1 0.0356(18) 0.0282(17) 0.0204(15) 0.0008(13) 0.0025(13) 0.0186(15) C2 0.054(2) 0.039(2) 0.0205(16) 0.0057(14) 0.0103(15) 0.0315(18) C4 0.061(3) 0.047(2) 0.032(2) 0.0051(18) 0.0116(19) 0.025(2) C10 0.109(4) 0.068(3) 0.025(2) -0.002(2) 0.009(2) 0.057(3) C8 0.130(6) 0.145(6) 0.043(3) 0.026(3) 0.048(3) 0.082(5) C5 0.068(3) 0.065(3) 0.048(3) 0.020(2) 0.027(2) 0.027(3) C3 0.079(3) 0.039(2) 0.0263(19) 0.0044(16) 0.0094(19) 0.032(2) O6 0.061(2) 0.0419(16) 0.075(2) 0.0155(17) 0.0369(19) 0.0318(16) O7 0.0321(15) 0.069(2) 0.0404(18) 0.0112(15) -0.0073(13) 0.0132(15) O8 0.086(3) 0.070(2) 0.066(2) -0.015(2) -0.026(2) 0.047(2) O5 0.091(3) 0.095(3) 0.128(4) 0.004(4) 0.014(3) 0.059(3) O9 0.0748(19) 0.0360(14) 0.0216(12) 0.0087(10) 0.0167(12) 0.0354(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1 2.089(2) . ? Co1 N1 2.091(3) . ? Co1 O4 2.093(2) 11_667 ? Co1 N2 2.096(3) 11_667 ? Co1 O7 2.161(3) . ? Co1 O6 2.190(3) . ? Co2 O2 1.994(2) 16_647 ? Co2 O2 1.994(2) . ? Co2 O9 2.052(2) . ? Co2 O9 2.051(2) 16_647 ? Co2 O8 2.161(4) . ? Co2 O8 2.161(4) 16_647 ? O1 C7 1.268(4) . ? O4 C12 1.270(4) . ? O4 Co1 2.093(2) 12_547 ? C9 C10 1.363(7) . ? C9 C5 1.394(7) . ? C9 C8 1.524(6) . ? C12 O9 1.250(4) . ? C12 C11 1.474(4) . ? N1 C1 1.351(4) . ? N1 C6 1.372(4) . ? N2 C1 1.340(4) . ? N2 C11 1.380(4) . ? N2 Co1 2.096(3) 12_547 ? C11 C6 1.380(4) . ? O2 C7 1.249(4) . ? C6 C7 1.471(4) . ? C1 C2 1.471(4) . ? C2 C3 1.391(5) . ? C2 C4 1.393(6) . ? C4 C5 1.385(5) . ? C4 H4 0.9300 . ? C10 C3 1.392(6) . ? C10 H10 0.9300 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C5 H5 0.9300 . ? C3 H3 0.9300 . ? O6 H6 0.8200 . ? O6 H1W 0.89(6) . ? O7 H5W 0.849(10) . ? O7 H4W 0.851(10) . ? O8 H8 0.8200 . ? O8 H6W 0.841(10) . ? O5 H3W 0.845(10) . ? O5 H2W 0.850(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 N1 78.72(9) . . ? O1 Co1 O4 170.37(9) . 11_667 ? N1 Co1 O4 101.08(10) . 11_667 ? O1 Co1 N2 111.31(10) . 11_667 ? N1 Co1 N2 105.74(11) . 11_667 ? O4 Co1 N2 78.11(9) 11_667 11_667 ? O1 Co1 O7 84.94(10) . . ? N1 Co1 O7 92.11(13) . . ? O4 Co1 O7 85.44(10) 11_667 . ? N2 Co1 O7 157.65(11) 11_667 . ? O1 Co1 O6 86.21(11) . . ? N1 Co1 O6 163.84(11) . . ? O4 Co1 O6 92.80(12) 11_667 . ? N2 Co1 O6 85.05(11) 11_667 . ? O7 Co1 O6 80.71(14) . . ? O2 Co2 O2 179.997(1) 16_647 . ? O2 Co2 O9 86.06(10) 16_647 . ? O2 Co2 O9 93.94(10) . . ? O2 Co2 O9 93.94(10) 16_647 16_647 ? O2 Co2 O9 86.06(10) . 16_647 ? O9 Co2 O9 179.999(1) . 16_647 ? O2 Co2 O8 92.39(14) 16_647 . ? O2 Co2 O8 87.61(14) . . ? O9 Co2 O8 91.98(13) . . ? O9 Co2 O8 88.02(13) 16_647 . ? O2 Co2 O8 87.61(14) 16_647 16_647 ? O2 Co2 O8 92.39(14) . 16_647 ? O9 Co2 O8 88.02(13) . 16_647 ? O9 Co2 O8 91.98(13) 16_647 16_647 ? O8 Co2 O8 179.997(1) . 16_647 ? C7 O1 Co1 115.15(19) . . ? C12 O4 Co1 116.89(19) . 12_547 ? C10 C9 C5 118.7(4) . . ? C10 C9 C8 121.8(5) . . ? C5 C9 C8 119.6(5) . . ? O9 C12 O4 120.9(3) . . ? O9 C12 C11 123.6(3) . . ? O4 C12 C11 115.5(3) . . ? C1 N1 C6 105.1(3) . . ? C1 N1 Co1 141.9(2) . . ? C6 N1 Co1 110.8(2) . . ? C1 N2 C11 105.2(2) . . ? C1 N2 Co1 142.7(2) . 12_547 ? C11 N2 Co1 111.9(2) . 12_547 ? C6 C11 N2 108.1(3) . . ? C6 C11 C12 135.3(3) . . ? N2 C11 C12 116.5(3) . . ? C7 O2 Co2 141.4(2) . . ? N1 C6 C11 108.5(3) . . ? N1 C6 C7 116.4(3) . . ? C11 C6 C7 135.0(3) . . ? O2 C7 O1 121.2(3) . . ? O2 C7 C6 122.2(3) . . ? O1 C7 C6 116.5(3) . . ? N2 C1 N1 113.1(3) . . ? N2 C1 C2 123.8(3) . . ? N1 C1 C2 122.9(3) . . ? C3 C2 C4 118.6(3) . . ? C3 C2 C1 121.7(3) . . ? C4 C2 C1 119.6(3) . . ? C5 C4 C2 120.3(4) . . ? C5 C4 H4 119.9 . . ? C2 C4 H4 119.9 . . ? C9 C10 C3 121.5(4) . . ? C9 C10 H10 119.3 . . ? C3 C10 H10 119.3 . . ? C9 C8 H8A 109.5 . . ? C9 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C9 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C5 C9 120.8(5) . . ? C4 C5 H5 119.6 . . ? C9 C5 H5 119.6 . . ? C2 C3 C10 120.1(4) . . ? C2 C3 H3 119.9 . . ? C10 C3 H3 119.9 . . ? Co1 O6 H6 109.5 . . ? Co1 O6 H1W 117(4) . . ? H6 O6 H1W 116.9 . . ? Co1 O7 H5W 108(4) . . ? Co1 O7 H4W 101(9) . . ? H5W O7 H4W 111.9(19) . . ? Co2 O8 H8 109.5 . . ? Co2 O8 H6W 145(3) . . ? H8 O8 H6W 103.6 . . ? H3W O5 H2W 105.4(17) . . ? C12 O9 Co2 139.5(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 N1 Co1 O1 C7 -12.1(2) . . . . ? O4 Co1 O1 C7 77.7(6) 11_667 . . . ? N2 Co1 O1 C7 -114.7(2) 11_667 . . . ? O7 Co1 O1 C7 81.1(2) . . . . ? O6 Co1 O1 C7 162.1(2) . . . . ? Co1 O4 C12 O9 173.4(3) 12_547 . . . ? Co1 O4 C12 C11 -7.4(4) 12_547 . . . ? O1 Co1 N1 C1 172.7(4) . . . . ? O4 Co1 N1 C1 2.5(4) 11_667 . . . ? N2 Co1 N1 C1 -78.1(4) 11_667 . . . ? O7 Co1 N1 C1 88.3(4) . . . . ? O6 Co1 N1 C1 151.3(4) . . . . ? O1 Co1 N1 C6 13.5(2) . . . . ? O4 Co1 N1 C6 -156.7(2) 11_667 . . . ? N2 Co1 N1 C6 122.7(2) 11_667 . . . ? O7 Co1 N1 C6 -70.9(2) . . . . ? O6 Co1 N1 C6 -7.9(6) . . . . ? C1 N2 C11 C6 0.7(4) . . . . ? Co1 N2 C11 C6 -175.2(2) 12_547 . . . ? C1 N2 C11 C12 -175.9(3) . . . . ? Co1 N2 C11 C12 8.2(4) 12_547 . . . ? O9 C12 C11 C6 3.0(6) . . . . ? O4 C12 C11 C6 -176.2(4) . . . . ? O9 C12 C11 N2 178.4(3) . . . . ? O4 C12 C11 N2 -0.8(4) . . . . ? O2 Co2 O2 C7 54(9) 16_647 . . . ? O9 Co2 O2 C7 37.3(4) . . . . ? O9 Co2 O2 C7 -142.7(4) 16_647 . . . ? O8 Co2 O2 C7 129.1(4) . . . . ? O8 Co2 O2 C7 -50.9(4) 16_647 . . . ? C1 N1 C6 C11 -0.3(4) . . . . ? Co1 N1 C6 C11 166.6(2) . . . . ? C1 N1 C6 C7 179.2(3) . . . . ? Co1 N1 C6 C7 -13.9(4) . . . . ? N2 C11 C6 N1 -0.2(4) . . . . ? C12 C11 C6 N1 175.5(4) . . . . ? N2 C11 C6 C7 -179.6(4) . . . . ? C12 C11 C6 C7 -4.0(7) . . . . ? Co2 O2 C7 O1 152.6(3) . . . . ? Co2 O2 C7 C6 -29.0(6) . . . . ? Co1 O1 C7 O2 -173.4(3) . . . . ? Co1 O1 C7 C6 8.1(4) . . . . ? N1 C6 C7 O2 -174.3(3) . . . . ? C11 C6 C7 O2 5.1(6) . . . . ? N1 C6 C7 O1 4.2(4) . . . . ? C11 C6 C7 O1 -176.4(4) . . . . ? C11 N2 C1 N1 -0.9(4) . . . . ? Co1 N2 C1 N1 172.7(3) 12_547 . . . ? C11 N2 C1 C2 173.9(3) . . . . ? Co1 N2 C1 C2 -12.5(6) 12_547 . . . ? C6 N1 C1 N2 0.8(4) . . . . ? Co1 N1 C1 N2 -159.1(3) . . . . ? C6 N1 C1 C2 -174.0(3) . . . . ? Co1 N1 C1 C2 26.0(6) . . . . ? N2 C1 C2 C3 43.5(5) . . . . ? N1 C1 C2 C3 -142.2(4) . . . . ? N2 C1 C2 C4 -134.1(4) . . . . ? N1 C1 C2 C4 40.2(5) . . . . ? C3 C2 C4 C5 -1.9(6) . . . . ? C1 C2 C4 C5 175.8(4) . . . . ? C5 C9 C10 C3 -0.9(8) . . . . ? C8 C9 C10 C3 178.4(5) . . . . ? C2 C4 C5 C9 0.0(7) . . . . ? C10 C9 C5 C4 1.4(8) . . . . ? C8 C9 C5 C4 -177.9(5) . . . . ? C4 C2 C3 C10 2.3(6) . . . . ? C1 C2 C3 C10 -175.3(4) . . . . ? C9 C10 C3 C2 -1.0(7) . . . . ? O4 C12 O9 Co2 -162.2(3) . . . . ? C11 C12 O9 Co2 18.6(6) . . . . ? O2 Co2 O9 C12 149.0(4) 16_647 . . . ? O2 Co2 O9 C12 -31.0(4) . . . . ? O9 Co2 O9 C12 -148(23) 16_647 . . . ? O8 Co2 O9 C12 -118.7(4) . . . . ? O8 Co2 O9 C12 61.3(4) 16_647 . . . ? 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 O8 H8 O5 0.82 2.03 2.846(6) 177.5 14_557 O6 H1W O4 0.89(6) 1.92(6) 2.795(4) 170(6) 15_447 O6 H1W O9 0.89(6) 2.48(6) 3.120(4) 129(5) 15_447 O5 H3W O7 0.845(10) 2.309(15) 3.146(8) 171(7) 9_654 O5 H2W O6 0.850(10) 2.40(4) 3.186(8) 155(8) . O7 H5W O1 0.849(10) 2.06(4) 2.816(4) 148(6) 9_654 O7 H4W O6 0.851(10) 2.38(11) 2.817(5) 113(9) . O7 H4W O9 0.851(10) 2.41(5) 3.213(5) 157(11) 15_447 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.99 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.677 _refine_diff_density_min -0.444 _refine_diff_density_rms 0.085