# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Shi, Zhan' _publ_contact_author_email zshi@mail.jlu.edu.cn _publ_section_title ; Design and Construction of Coordination Polymers by 2,2'-Dinitro-4,4'-biphenyldicarboxylate and Imidazole-based Ligands: Diverse Structures Based on Different Metal Ions ; loop_ _publ_author_name 'Zhan Shi' 'Baiyan Li' 'Yiming Zhang' 'Guanghua Li' 'Dan Liu' 'Yan Chen' ; Weiwei Hu ; 'Shouhua Feng' data_compound-1 _database_code_depnum_ccdc_archive 'CCDC 782708' #TrackingRef 'CCDC.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C38 H26 Mn2 N8 O16' _chemical_formula_sum 'C38 H26 Mn2 N8 O16' _chemical_formula_weight 960.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 19.249(4) _cell_length_b 7.6441(15) _cell_length_c 26.522(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3902.4(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4428 _cell_measurement_theta_min 3.07 _cell_measurement_theta_max 27.40 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.635 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1952 _exptl_absorpt_coefficient_mu 0.735 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method omega-scan _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 35781 _diffrn_reflns_av_R_equivalents 0.0974 _diffrn_reflns_av_sigmaI/netI 0.0497 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 27.40 _reflns_number_total 4428 _reflns_number_gt 3536 _reflns_threshold_expression >2sigma(I) _computing_data_collection Process-auto _computing_cell_refinement Process-auto _computing_data_reduction Process-auto _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^)+(0.0314P)^2^+8.9717P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4428 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0674 _refine_ls_R_factor_gt 0.0508 _refine_ls_wR_factor_ref 0.1086 _refine_ls_wR_factor_gt 0.1018 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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 Mn1 Mn 0.19805(2) 0.27632(5) 0.020216(15) 0.01060(12) Uani 1 1 d . . . O1 O 0.16877(11) 0.0927(3) 0.07784(7) 0.0191(4) Uani 1 1 d . . . O2 O 0.20951(10) -0.1729(3) 0.05771(7) 0.0171(4) Uani 1 1 d . . . O3 O 0.17210(10) -0.6101(3) 0.46050(7) 0.0152(4) Uani 1 1 d . . . O4 O 0.27503(10) -0.4753(3) 0.46383(7) 0.0150(4) Uani 1 1 d . . . O5 O 0.09914(11) 0.0208(3) 0.30600(7) 0.0244(5) Uani 1 1 d . . . O6 O 0.12291(11) 0.2286(3) 0.25287(8) 0.0212(5) Uani 1 1 d . . . O7 O 0.00451(13) -0.4504(5) 0.33564(10) 0.0678(12) Uani 1 1 d . . . O8 O 0.03646(11) -0.3704(4) 0.26180(8) 0.0354(6) Uani 1 1 d . . . N1 N 0.12057(12) 0.0730(3) 0.26489(8) 0.0157(5) Uani 1 1 d . . . N2 N 0.04905(13) -0.4009(4) 0.30590(9) 0.0266(6) Uani 1 1 d . . . N3 N 0.10997(12) 0.4277(3) 0.04533(9) 0.0153(5) Uani 1 1 d . . . N4 N 0.03736(12) 0.6491(3) 0.05579(9) 0.0160(5) Uani 1 1 d . . . C1 C 0.16109(14) -0.2277(4) 0.24313(10) 0.0142(6) Uani 1 1 d . . . C2 C 0.14454(13) -0.0583(4) 0.22807(10) 0.0127(6) Uani 1 1 d . . . C3 C 0.15035(13) -0.0044(4) 0.17807(10) 0.0132(6) Uani 1 1 d . . . H3 H 0.1400 0.1104 0.1692 0.080 Uiso 1 1 calc . . . C4 C 0.17167(13) -0.1232(4) 0.14159(10) 0.0118(5) Uani 1 1 d . . . C5 C 0.18550(14) -0.2962(4) 0.15541(10) 0.0167(6) Uani 1 1 d . . . H5 H 0.1980 -0.3776 0.1310 0.080 Uiso 1 1 calc . . . C6 C 0.18058(15) -0.3470(4) 0.20561(11) 0.0178(6) Uani 1 1 d . . . H6 H 0.1904 -0.4621 0.2144 0.080 Uiso 1 1 calc . . . C7 C 0.18383(13) -0.0629(4) 0.08798(10) 0.0126(6) Uani 1 1 d . . . C8 C 0.16958(14) -0.2872(4) 0.29673(10) 0.0137(6) Uani 1 1 d . . . C9 C 0.11989(14) -0.3764(4) 0.32531(10) 0.0162(6) Uani 1 1 d . . . C10 C 0.13431(14) -0.4419(4) 0.37291(10) 0.0161(6) Uani 1 1 d . . . H10 H 0.0999 -0.4993 0.3911 0.080 Uiso 1 1 calc . . . C11 C 0.20028(14) -0.4218(3) 0.39348(10) 0.0122(5) Uani 1 1 d . . . C12 C 0.25044(14) -0.3300(4) 0.36628(9) 0.0126(5) Uani 1 1 d . . . H12 H 0.2945 -0.3136 0.3799 0.080 Uiso 1 1 calc . . . C13 C 0.23483(14) -0.2629(4) 0.31881(10) 0.0140(6) Uani 1 1 d . . . H13 H 0.2686 -0.2005 0.3014 0.080 Uiso 1 1 calc . . . C14 C 0.21749(14) -0.5065(3) 0.44330(10) 0.0113(5) Uani 1 1 d . . . C15 C 0.08924(14) 0.5815(4) 0.02749(11) 0.0166(6) Uani 1 1 d . . . H15 H 0.1080 0.6357 -0.0008 0.080 Uiso 1 1 calc . . . C16 C 0.06866(16) 0.3953(4) 0.08738(11) 0.0211(7) Uani 1 1 d . . . H16 H 0.0711 0.2962 0.1076 0.080 Uiso 1 1 calc . . . C17 C 0.02423(16) 0.5313(4) 0.09415(11) 0.0226(7) Uani 1 1 d . . . H17 H -0.0086 0.5429 0.1196 0.080 Uiso 1 1 calc . . . C18 C 0.00216(15) 0.8195(4) 0.05006(11) 0.0194(6) Uani 1 1 d . . . H18A H 0.0143 0.8934 0.0785 0.080 Uiso 1 1 calc . . . H18B H -0.0477 0.8011 0.0509 0.080 Uiso 1 1 calc . . . C19 C 0.02074(15) 0.9138(4) 0.00186(11) 0.0187(6) Uani 1 1 d . . . H19A H 0.0101 0.8400 -0.0269 0.080 Uiso 1 1 calc . . . H19B H 0.0701 0.9389 0.0014 0.080 Uiso 1 1 calc . . . 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 0.0124(2) 0.0114(2) 0.00805(19) -0.00077(16) 0.00037(16) 0.00074(16) O1 0.0274(11) 0.0162(11) 0.0136(10) 0.0048(8) 0.0020(9) 0.0027(9) O2 0.0179(10) 0.0217(11) 0.0118(9) -0.0020(8) 0.0039(8) -0.0002(8) O3 0.0185(10) 0.0162(10) 0.0110(9) 0.0023(8) 0.0003(8) -0.0021(8) O4 0.0160(9) 0.0190(11) 0.0100(9) -0.0033(8) -0.0034(8) 0.0035(8) O5 0.0301(12) 0.0313(13) 0.0119(10) 0.0026(9) 0.0052(9) 0.0097(10) O6 0.0263(11) 0.0165(11) 0.0207(10) -0.0015(9) -0.0014(9) 0.0031(9) O7 0.0148(12) 0.154(3) 0.0347(15) 0.0460(19) -0.0052(11) -0.0249(17) O8 0.0201(11) 0.0670(19) 0.0191(12) 0.0168(12) -0.0080(9) -0.0068(12) N1 0.0130(11) 0.0234(14) 0.0106(11) -0.0007(10) -0.0017(9) 0.0046(10) N2 0.0127(12) 0.0477(18) 0.0194(13) 0.0146(13) -0.0013(10) -0.0054(12) N3 0.0156(12) 0.0142(12) 0.0163(12) 0.0000(10) 0.0020(10) 0.0020(10) N4 0.0126(11) 0.0162(12) 0.0192(12) 0.0003(10) 0.0031(10) 0.0030(10) C1 0.0107(12) 0.0212(15) 0.0109(13) 0.0027(11) -0.0004(10) 0.0000(11) C2 0.0102(12) 0.0162(14) 0.0117(12) -0.0008(11) 0.0001(10) 0.0007(11) C3 0.0091(12) 0.0186(14) 0.0120(13) 0.0017(11) -0.0013(10) -0.0008(11) C4 0.0085(12) 0.0163(14) 0.0105(12) 0.0030(11) 0.0004(10) -0.0023(11) C5 0.0166(14) 0.0192(15) 0.0142(13) -0.0008(12) 0.0023(11) 0.0019(12) C6 0.0183(14) 0.0173(15) 0.0177(14) 0.0040(12) 0.0037(12) 0.0053(12) C7 0.0073(12) 0.0171(14) 0.0133(13) 0.0012(11) -0.0003(10) -0.0030(10) C8 0.0143(13) 0.0163(14) 0.0105(13) 0.0000(11) 0.0011(11) 0.0037(11) C9 0.0099(13) 0.0254(16) 0.0133(13) 0.0039(12) -0.0005(11) -0.0002(12) C10 0.0127(13) 0.0222(15) 0.0132(13) 0.0047(12) 0.0013(11) -0.0010(12) C11 0.0151(13) 0.0126(13) 0.0089(12) -0.0017(10) 0.0017(11) 0.0013(11) C12 0.0132(13) 0.0133(14) 0.0114(12) -0.0025(11) -0.0028(11) -0.0003(11) C13 0.0149(13) 0.0140(14) 0.0131(13) 0.0004(11) 0.0027(11) 0.0001(11) C14 0.0132(13) 0.0108(13) 0.0098(12) -0.0023(10) 0.0018(10) 0.0030(10) C15 0.0141(13) 0.0165(15) 0.0191(14) -0.0012(12) 0.0014(11) 0.0015(11) C16 0.0225(16) 0.0230(16) 0.0177(14) 0.0030(13) 0.0090(12) 0.0026(13) C17 0.0216(15) 0.0250(17) 0.0210(15) 0.0019(13) 0.0055(13) 0.0020(13) C18 0.0173(14) 0.0167(15) 0.0241(15) -0.0014(12) 0.0055(12) 0.0060(12) C19 0.0169(14) 0.0176(15) 0.0217(15) -0.0007(12) 0.0036(12) 0.0014(12) _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 2.0749(19) 8_665 ? Mn1 O3 2.0908(19) 7 ? Mn1 O1 2.150(2) . ? Mn1 N3 2.158(2) . ? Mn1 O4 2.1949(19) 2_554 ? O1 C7 1.254(3) . ? O2 C7 1.263(3) . ? O2 Mn1 2.0749(19) 8_655 ? O3 C14 1.265(3) . ? O3 Mn1 2.0908(19) 7_556 ? O4 C14 1.257(3) . ? O4 Mn1 2.1949(19) 2 ? O5 N1 1.232(3) . ? O6 N1 1.232(3) . ? O7 N2 1.225(3) . ? O8 N2 1.217(3) . ? N1 C2 1.475(3) . ? N2 C9 1.469(4) . ? N3 C15 1.329(4) . ? N3 C16 1.392(4) . ? N4 C15 1.352(4) . ? N4 C17 1.382(4) . ? N4 C18 1.476(4) . ? C1 C2 1.393(4) . ? C1 C6 1.401(4) . ? C1 C8 1.501(4) . ? C2 C3 1.393(4) . ? C3 C4 1.389(4) . ? C3 H3 0.9300 . ? C4 C5 1.398(4) . ? C4 C7 1.513(4) . ? C5 C6 1.390(4) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C8 C13 1.398(4) . ? C8 C9 1.398(4) . ? C9 C10 1.386(4) . ? C10 C11 1.391(4) . ? C10 H10 0.9300 . ? C11 C12 1.395(4) . ? C11 C14 1.508(4) . ? C12 C13 1.392(4) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.358(4) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.510(4) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C19 1.544(6) 5_575 ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Mn1 O3 132.96(8) 8_665 7 ? O2 Mn1 O1 90.36(8) 8_665 . ? O3 Mn1 O1 94.54(8) 7 . ? O2 Mn1 N3 115.19(8) 8_665 . ? O3 Mn1 N3 111.83(8) 7 . ? O1 Mn1 N3 85.69(8) . . ? O2 Mn1 O4 89.69(8) 8_665 2_554 ? O3 Mn1 O4 87.78(8) 7 2_554 ? O1 Mn1 O4 176.78(8) . 2_554 ? N3 Mn1 O4 91.39(8) . 2_554 ? C7 O1 Mn1 135.34(18) . . ? C7 O2 Mn1 139.86(18) . 8_655 ? C14 O3 Mn1 119.26(17) . 7_556 ? C14 O4 Mn1 129.40(17) . 2 ? O6 N1 O5 123.6(2) . . ? O6 N1 C2 118.3(2) . . ? O5 N1 C2 118.0(2) . . ? O8 N2 O7 122.6(3) . . ? O8 N2 C9 119.8(2) . . ? O7 N2 C9 117.6(2) . . ? C15 N3 C16 105.7(2) . . ? C15 N3 Mn1 126.90(19) . . ? C16 N3 Mn1 126.92(19) . . ? C15 N4 C17 107.2(2) . . ? C15 N4 C18 128.3(2) . . ? C17 N4 C18 124.5(2) . . ? C2 C1 C6 117.6(2) . . ? C2 C1 C8 125.3(3) . . ? C6 C1 C8 116.5(2) . . ? C1 C2 C3 122.0(3) . . ? C1 C2 N1 121.0(2) . . ? C3 C2 N1 117.0(2) . . ? C4 C3 C2 119.6(3) . . ? C4 C3 H3 120.2 . . ? C2 C3 H3 120.2 . . ? C3 C4 C5 119.5(2) . . ? C3 C4 C7 120.1(2) . . ? C5 C4 C7 120.3(2) . . ? C6 C5 C4 120.1(3) . . ? C6 C5 H5 119.9 . . ? C4 C5 H5 119.9 . . ? C5 C6 C1 121.1(3) . . ? C5 C6 H6 119.4 . . ? C1 C6 H6 119.4 . . ? O1 C7 O2 125.9(3) . . ? O1 C7 C4 117.1(2) . . ? O2 C7 C4 117.1(2) . . ? C13 C8 C9 116.9(2) . . ? C13 C8 C1 117.0(2) . . ? C9 C8 C1 125.9(2) . . ? C10 C9 C8 122.2(3) . . ? C10 C9 N2 117.3(2) . . ? C8 C9 N2 120.5(2) . . ? C9 C10 C11 120.0(3) . . ? C9 C10 H10 120.0 . . ? C11 C10 H10 120.0 . . ? C10 C11 C12 119.0(2) . . ? C10 C11 C14 119.8(2) . . ? C12 C11 C14 121.1(2) . . ? C13 C12 C11 120.2(2) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C12 C13 C8 121.6(2) . . ? C12 C13 H13 119.2 . . ? C8 C13 H13 119.2 . . ? O4 C14 O3 124.9(2) . . ? O4 C14 C11 119.4(2) . . ? O3 C14 C11 115.7(2) . . ? N3 C15 N4 111.2(2) . . ? N3 C15 H15 124.4 . . ? N4 C15 H15 124.4 . . ? C17 C16 N3 109.3(3) . . ? C17 C16 H16 125.4 . . ? N3 C16 H16 125.4 . . ? C16 C17 N4 106.6(2) . . ? C16 C17 H17 126.7 . . ? N4 C17 H17 126.7 . . ? N4 C18 C19 113.5(2) . . ? N4 C18 H18A 108.9 . . ? C19 C18 H18A 108.9 . . ? N4 C18 H18B 108.9 . . ? C19 C18 H18B 108.9 . . ? H18A C18 H18B 107.7 . . ? C18 C19 C19 109.8(3) . 5_575 ? C18 C19 H19A 109.7 . . ? C19 C19 H19A 109.7 5_575 . ? C18 C19 H19B 109.7 . . ? C19 C19 H19B 109.7 5_575 . ? H19A C19 H19B 108.2 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.40 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.495 _refine_diff_density_min -0.492 _refine_diff_density_rms 0.087 data_compound-2 _database_code_depnum_ccdc_archive 'CCDC 782709' #TrackingRef 'CCDC.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C43 H37 Co2 N10 O18' _chemical_formula_sum 'C43 H37 Co2 N10 O18' _chemical_formula_weight 1099.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.405(3) _cell_length_b 14.088(3) _cell_length_c 15.765(3) _cell_angle_alpha 63.53(3) _cell_angle_beta 72.82(3) _cell_angle_gamma 68.38(3) _cell_volume 2264.0(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 10195 _cell_measurement_theta_min 3.03 _cell_measurement_theta_max 27.46 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.613 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1126 _exptl_absorpt_coefficient_mu 0.823 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method omega-scan _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 22307 _diffrn_reflns_av_R_equivalents 0.0673 _diffrn_reflns_av_sigmaI/netI 0.0912 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 27.46 _reflns_number_total 10195 _reflns_number_gt 7186 _reflns_threshold_expression >2sigma(I) _computing_data_collection Process-auto _computing_cell_refinement Process-auto _computing_data_reduction Process-auto _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^)+(0.0761P)^2^+2.1102P] 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 10195 _refine_ls_number_parameters 692 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0967 _refine_ls_R_factor_gt 0.0619 _refine_ls_wR_factor_ref 0.1609 _refine_ls_wR_factor_gt 0.1423 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.18444(5) 0.07490(4) 0.05006(3) 0.01263(14) Uani 1 1 d . . . Co2 Co 0.30761(5) -0.04950(4) 0.23946(3) 0.01320(14) Uani 1 1 d . . . O1 O 0.2356(2) 0.2200(2) -0.01942(18) 0.0169(6) Uani 1 1 d . . . O2 O 0.0567(2) 0.3394(2) -0.0084(2) 0.0208(6) Uani 1 1 d . . . O3 O 0.5859(2) 0.9496(2) -0.21822(19) 0.0197(6) Uani 1 1 d . . . O4 O 0.5020(2) 0.9112(2) -0.06373(19) 0.0201(6) Uani 1 1 d . . . O5 O 0.5617(3) 0.5068(3) -0.1061(2) 0.0309(7) Uani 1 1 d . . . O6 O 0.5787(3) 0.3613(2) -0.1300(2) 0.0301(7) Uani 1 1 d . . . O7 O 0.5049(4) 0.7725(3) -0.3920(2) 0.0578(12) Uani 1 1 d . . . O8 O 0.4669(4) 0.6172(3) -0.3087(2) 0.0505(11) Uani 1 1 d . . . O9 O 0.1767(2) 0.0939(2) 0.17950(18) 0.0138(6) Uani 1 1 d . . . O10 O -0.0120(2) 0.1257(2) 0.24849(19) 0.0181(6) Uani 1 1 d . . . O11 O 0.2102(2) 0.8474(2) 0.26083(18) 0.0178(6) Uani 1 1 d . . . O12 O 0.1541(2) 0.9219(2) 0.11608(18) 0.0157(6) Uani 1 1 d . . . O13 O -0.1571(3) 0.3933(3) 0.4052(3) 0.0543(12) Uani 1 1 d . . . O14 O -0.1199(3) 0.5491(2) 0.3129(2) 0.0310(8) Uani 1 1 d . . . O15 O 0.1725(9) 0.3696(10) 0.4138(8) 0.021(3) Uani 0.50 1 d PU . . O15' O 0.2241(17) 0.362(3) 0.397(2) 0.025(6) Uani 0.20 1 d PU . . O15" O 0.1247(16) 0.3812(19) 0.4324(14) 0.023(4) Uani 0.30 1 d PU . . O16 O 0.1295(3) 0.4888(3) 0.4800(2) 0.0399(9) Uani 1 1 d . . . O17 O 0.3588(2) -0.0165(2) 0.07964(18) 0.0158(6) Uani 1 1 d D . . O18 O -0.0004(2) 0.1563(2) 0.05692(19) 0.0171(6) Uani 1 1 d D . . N1 N 0.5196(3) 0.4463(3) -0.1151(2) 0.0221(8) Uani 1 1 d . . . N2 N 0.4735(4) 0.7036(3) -0.3152(3) 0.0305(9) Uani 1 1 d . . . N3 N -0.0966(3) 0.4484(3) 0.3403(3) 0.0265(8) Uani 1 1 d . . . N4 N 0.1470(4) 0.4645(3) 0.4103(3) 0.0333(10) Uani 1 1 d . . . N5 N 0.1904(3) 0.0725(3) -0.0828(2) 0.0172(7) Uani 1 1 d . . . N6 N 0.1854(3) 0.1347(3) -0.2372(2) 0.0199(7) Uani 1 1 d . . . N7 N 0.2423(3) -0.0472(3) -0.6222(2) 0.0173(7) Uani 1 1 d . . . N8 N 0.1894(3) 0.0194(3) -0.5083(2) 0.0230(8) Uani 1 1 d . . . N9 N 0.4487(3) -0.1857(3) 0.2797(2) 0.0179(7) Uani 1 1 d . . . N10 N 0.5673(3) -0.3293(3) 0.3731(2) 0.0227(8) Uani 1 1 d . . . C1 C 0.3223(4) 0.5840(3) -0.1318(3) 0.0159(8) Uani 1 1 d . . . C2 C 0.3912(3) 0.4740(3) -0.1075(3) 0.0148(8) Uani 1 1 d . . . C3 C 0.3436(4) 0.3869(3) -0.0755(3) 0.0158(8) Uani 1 1 d . . . H3 H 0.3916 0.3147 -0.0590 0.080 Uiso 1 1 calc . . . C4 C 0.2228(3) 0.4088(3) -0.0684(3) 0.0153(8) Uani 1 1 d . . . C5 C 0.1533(3) 0.5181(3) -0.0954(3) 0.0172(8) Uani 1 1 d . . . H5 H 0.0729 0.5335 -0.0924 0.080 Uiso 1 1 calc . . . C6 C 0.2029(4) 0.6035(3) -0.1265(3) 0.0186(8) Uani 1 1 d . . . H6 H 0.1551 0.6757 -0.1444 0.080 Uiso 1 1 calc . . . C7 C 0.1675(4) 0.3152(3) -0.0292(3) 0.0152(8) Uani 1 1 d . . . C8 C 0.3671(3) 0.6770(3) -0.1487(3) 0.0162(8) Uani 1 1 d . . . C9 C 0.4391(4) 0.7306(3) -0.2290(3) 0.0189(9) Uani 1 1 d . . . C10 C 0.4838(4) 0.8087(3) -0.2315(3) 0.0202(9) Uani 1 1 d . . . H10 H 0.5324 0.8421 -0.2858 0.080 Uiso 1 1 calc . . . C11 C 0.4551(3) 0.8366(3) -0.1515(3) 0.0158(8) Uani 1 1 d . . . C12 C 0.3744(4) 0.7925(3) -0.0745(3) 0.0201(9) Uani 1 1 d . . . H12 H 0.3495 0.8153 -0.0231 0.080 Uiso 1 1 calc . . . C13 C 0.3311(4) 0.7151(3) -0.0740(3) 0.0193(9) Uani 1 1 d . . . H13 H 0.2763 0.6873 -0.0222 0.080 Uiso 1 1 calc . . . C14 C 0.5176(3) 0.9059(3) -0.1444(3) 0.0159(8) Uani 1 1 d . . . C15 C 0.1056(4) 0.4346(3) 0.2450(3) 0.0150(8) Uani 1 1 d . . . C16 C 0.0090(3) 0.3907(3) 0.2900(3) 0.0164(8) Uani 1 1 d . . . C17 C 0.0031(4) 0.2968(3) 0.2858(3) 0.0177(8) Uani 1 1 d . . . H17 H -0.0624 0.2704 0.3170 0.080 Uiso 1 1 calc . . . C18 C 0.0965(3) 0.2422(3) 0.2341(3) 0.0134(8) Uani 1 1 d . . . C19 C 0.1932(4) 0.2830(3) 0.1882(3) 0.0195(9) Uani 1 1 d . . . H19 H 0.2556 0.2470 0.1533 0.080 Uiso 1 1 calc . . . C20 C 0.1982(3) 0.3772(3) 0.1935(3) 0.0176(8) Uani 1 1 d . . . H20 H 0.2642 0.4028 0.1624 0.080 Uiso 1 1 calc . . . C21 C 0.0836(4) 0.1458(3) 0.2227(3) 0.0152(8) Uani 1 1 d . . . C22 C 0.1146(3) 0.5391(3) 0.2416(3) 0.0144(8) Uani 1 1 d . . . C23 C 0.1382(4) 0.5543(3) 0.3155(3) 0.0180(8) Uani 1 1 d . . . C24 C 0.1548(4) 0.6520(3) 0.3037(3) 0.0170(8) Uani 1 1 d . . . H24 H 0.1727 0.6581 0.3540 0.080 Uiso 1 1 calc . . . C25 C 0.1446(3) 0.7406(3) 0.2160(3) 0.0137(8) Uani 1 1 d . . . C26 C 0.1157(4) 0.7291(3) 0.1426(3) 0.0167(8) Uani 1 1 d . . . H26 H 0.1052 0.7888 0.0846 0.080 Uiso 1 1 calc . . . C27 C 0.1023(4) 0.6299(3) 0.1550(3) 0.0183(8) Uani 1 1 d . . . H27 H 0.0848 0.6239 0.1045 0.080 Uiso 1 1 calc . . . C28 C 0.1713(3) 0.8465(3) 0.1955(3) 0.0137(8) Uani 1 1 d . . . C29 C 0.2203(4) 0.1439(3) -0.1682(3) 0.0220(9) Uani 1 1 d . . . H29 H 0.2601 0.1939 -0.1797 0.080 Uiso 1 1 calc . . . C30 C 0.1312(4) 0.0171(3) -0.0983(3) 0.0202(9) Uani 1 1 d . . . H30 H 0.0980 -0.0376 -0.0504 0.080 Uiso 1 1 calc . . . C31 C 0.1284(4) 0.0535(3) -0.1926(3) 0.0194(9) Uani 1 1 d . . . H31 H 0.0947 0.0289 -0.2216 0.080 Uiso 1 1 calc . . . C32 C 0.2057(5) 0.2027(4) -0.3409(3) 0.0300(11) Uani 1 1 d . . . H32A H 0.2210 0.2692 -0.3492 0.080 Uiso 1 1 calc . . . H32B H 0.1354 0.2244 -0.3678 0.080 Uiso 1 1 calc . . . C33 C 0.3083(5) 0.1411(4) -0.3949(3) 0.0339(11) Uani 1 1 d . . . H33A H 0.3747 0.1095 -0.3610 0.080 Uiso 1 1 calc . . . H33B H 0.3299 0.1939 -0.4578 0.080 Uiso 1 1 calc . . . C34 C 0.2865(4) 0.0487(4) -0.4081(3) 0.0273(10) Uani 1 1 d . . . H34A H 0.3561 0.0163 -0.4449 0.080 Uiso 1 1 calc . . . H34B H 0.2730 -0.0085 -0.3457 0.080 Uiso 1 1 calc . . . C35 C 0.1818(4) 0.0893(4) -0.4591(3) 0.0292(11) Uani 1 1 d . . . H35A H 0.1104 0.0912 -0.4125 0.080 Uiso 1 1 calc . . . H35B H 0.1771 0.1640 -0.5056 0.080 Uiso 1 1 calc . . . C36 C 0.2462(4) 0.0294(3) -0.5975(3) 0.0206(9) Uani 1 1 d . . . H36 H 0.2840 0.0839 -0.6372 0.080 Uiso 1 1 calc . . . C37 C 0.1810(4) -0.1114(4) -0.5434(3) 0.0252(10) Uani 1 1 d . . . H37 H 0.1642 -0.1725 -0.5394 0.080 Uiso 1 1 calc . . . C38 C 0.1483(4) -0.0722(4) -0.4718(3) 0.0277(10) Uani 1 1 d . . . H38 H 0.1069 -0.1013 -0.4110 0.080 Uiso 1 1 calc . . . C39 C 0.4781(4) -0.2368(3) 0.3661(3) 0.0222(9) Uani 1 1 d . . . H39 H 0.4418 -0.2121 0.4161 0.080 Uiso 1 1 calc . . . C40 C 0.5226(4) -0.2503(4) 0.2286(3) 0.0273(10) Uani 1 1 d . . . H40 H 0.5230 -0.2346 0.1646 0.080 Uiso 1 1 calc . . . C41 C 0.5942(4) -0.3399(4) 0.2862(3) 0.0278(10) Uani 1 1 d . . . H41 H 0.6503 -0.3972 0.2702 0.080 Uiso 1 1 calc . . . C42 C 0.6105(4) -0.4129(4) 0.4615(3) 0.0277(10) Uani 1 1 d . . . H42A H 0.5834 -0.3827 0.5111 0.080 Uiso 1 1 calc . . . H42B H 0.6957 -0.4345 0.4507 0.080 Uiso 1 1 calc . . . C43 C 0.5664(4) -0.5135(4) 0.4943(3) 0.0283(10) Uani 1 1 d . . . H43A H 0.6024 -0.5485 0.4480 0.080 Uiso 1 1 calc . . . H43B H 0.5915 -0.5661 0.5552 0.080 Uiso 1 1 calc . . . H2A H -0.035(4) 0.137(4) 0.1250(16) 0.042(14) Uiso 1 1 d D . . H2B H 0.009(7) 0.231(3) 0.038(4) 0.12(3) Uiso 1 1 d D . . H1A H 0.397(4) -0.061(4) 0.042(4) 0.064(18) Uiso 1 1 d D . . H1B H 0.410(4) 0.026(4) 0.073(4) 0.054(17) 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 0.0187(3) 0.0105(3) 0.0118(3) -0.0047(2) -0.0017(2) -0.0073(2) Co2 0.0178(3) 0.0126(3) 0.0128(3) -0.0060(2) -0.0016(2) -0.0072(2) O1 0.0204(14) 0.0144(13) 0.0192(14) -0.0089(12) -0.0014(11) -0.0064(12) O2 0.0229(16) 0.0133(14) 0.0286(16) -0.0065(13) -0.0042(13) -0.0092(12) O3 0.0275(16) 0.0182(14) 0.0181(14) -0.0076(12) -0.0003(12) -0.0131(13) O4 0.0249(16) 0.0231(15) 0.0210(14) -0.0145(13) 0.0043(12) -0.0143(13) O5 0.0239(17) 0.0274(17) 0.047(2) -0.0108(16) -0.0085(15) -0.0152(14) O6 0.0229(16) 0.0276(17) 0.0410(19) -0.0185(16) -0.0031(14) -0.0028(14) O7 0.103(3) 0.062(3) 0.0243(18) -0.0235(19) 0.024(2) -0.058(3) O8 0.098(3) 0.047(2) 0.0290(19) -0.0265(18) 0.016(2) -0.050(2) O9 0.0176(14) 0.0113(13) 0.0132(13) -0.0069(11) -0.0004(11) -0.0037(11) O10 0.0201(15) 0.0216(14) 0.0193(14) -0.0131(12) 0.0036(11) -0.0114(12) O11 0.0270(16) 0.0151(14) 0.0172(13) -0.0062(12) -0.0043(12) -0.0112(12) O12 0.0241(15) 0.0106(13) 0.0146(13) -0.0019(11) -0.0058(11) -0.0087(12) O13 0.052(2) 0.043(2) 0.073(3) -0.041(2) 0.037(2) -0.031(2) O14 0.0278(17) 0.0213(16) 0.046(2) -0.0230(16) 0.0016(15) -0.0016(14) O15 0.034(9) 0.008(5) 0.016(7) -0.003(4) -0.002(7) -0.004(8) O15' 0.017(12) 0.012(8) 0.041(13) -0.005(8) -0.015(10) 0.003(10) O15" 0.049(12) 0.005(6) 0.008(6) -0.004(5) 0.012(7) -0.011(9) O16 0.062(2) 0.042(2) 0.0195(16) -0.0003(15) -0.0153(16) -0.0266(19) O17 0.0209(15) 0.0144(13) 0.0157(13) -0.0097(12) 0.0011(11) -0.0067(12) O18 0.0213(15) 0.0160(14) 0.0182(14) -0.0079(12) -0.0031(12) -0.0079(12) N1 0.0211(18) 0.0209(18) 0.0230(18) -0.0061(16) -0.0020(15) -0.0084(16) N2 0.049(3) 0.036(2) 0.0203(19) -0.0143(18) 0.0069(17) -0.031(2) N3 0.026(2) 0.0233(19) 0.039(2) -0.0220(18) 0.0051(17) -0.0119(17) N4 0.058(3) 0.022(2) 0.029(2) -0.0002(17) -0.023(2) -0.020(2) N5 0.0211(18) 0.0171(17) 0.0180(17) -0.0112(15) -0.0001(14) -0.0067(15) N6 0.032(2) 0.0165(17) 0.0139(16) -0.0069(14) -0.0003(15) -0.0108(16) N7 0.0232(18) 0.0177(17) 0.0150(16) -0.0066(14) -0.0043(14) -0.0083(15) N8 0.037(2) 0.0203(18) 0.0153(16) -0.0103(15) -0.0024(15) -0.0084(16) N9 0.0200(18) 0.0160(17) 0.0197(17) -0.0077(15) -0.0016(14) -0.0072(15) N10 0.0241(19) 0.0196(18) 0.0195(18) -0.0062(15) -0.0059(15) -0.0005(16) C1 0.024(2) 0.0157(19) 0.0116(18) -0.0048(16) 0.0013(16) -0.0135(17) C2 0.0135(19) 0.019(2) 0.0142(18) -0.0076(16) 0.0002(15) -0.0068(16) C3 0.024(2) 0.0093(17) 0.0156(18) -0.0056(16) -0.0015(16) -0.0070(16) C4 0.021(2) 0.0170(19) 0.0131(18) -0.0075(16) -0.0031(15) -0.0079(17) C5 0.020(2) 0.0153(19) 0.019(2) -0.0071(17) -0.0040(16) -0.0064(17) C6 0.023(2) 0.0137(19) 0.021(2) -0.0056(17) -0.0041(17) -0.0082(17) C7 0.025(2) 0.0133(19) 0.0118(18) -0.0052(16) -0.0030(16) -0.0098(17) C8 0.021(2) 0.0162(19) 0.0153(18) -0.0055(16) -0.0028(16) -0.0097(17) C9 0.025(2) 0.019(2) 0.0173(19) -0.0104(17) 0.0026(17) -0.0105(18) C10 0.029(2) 0.016(2) 0.018(2) -0.0045(17) -0.0043(17) -0.0125(18) C11 0.020(2) 0.0136(18) 0.0164(19) -0.0068(16) -0.0027(16) -0.0056(17) C12 0.020(2) 0.023(2) 0.021(2) -0.0107(18) -0.0015(17) -0.0093(18) C13 0.020(2) 0.021(2) 0.019(2) -0.0080(17) 0.0039(16) -0.0122(18) C14 0.018(2) 0.0123(18) 0.019(2) -0.0083(17) -0.0023(16) -0.0047(16) C15 0.024(2) 0.0113(18) 0.0137(18) -0.0051(16) -0.0041(16) -0.0071(17) C16 0.017(2) 0.0139(19) 0.0178(19) -0.0098(17) -0.0009(16) -0.0010(16) C17 0.021(2) 0.0133(19) 0.022(2) -0.0091(17) -0.0041(17) -0.0047(17) C18 0.019(2) 0.0087(17) 0.0121(17) -0.0014(15) -0.0060(15) -0.0032(16) C19 0.027(2) 0.0143(19) 0.0177(19) -0.0077(17) -0.0001(17) -0.0064(18) C20 0.020(2) 0.0148(19) 0.0178(19) -0.0045(17) -0.0005(16) -0.0083(17) C21 0.023(2) 0.0127(18) 0.0113(17) -0.0018(16) -0.0050(16) -0.0083(17) C22 0.017(2) 0.0083(17) 0.0200(19) -0.0086(16) -0.0034(16) -0.0010(16) C23 0.030(2) 0.0096(18) 0.0144(18) 0.0000(16) -0.0076(17) -0.0085(17) C24 0.023(2) 0.018(2) 0.0141(18) -0.0060(16) -0.0054(16) -0.0084(17) C25 0.0142(19) 0.0105(18) 0.0186(19) -0.0070(16) -0.0024(15) -0.0039(15) C26 0.022(2) 0.0111(18) 0.0156(18) -0.0037(16) -0.0038(16) -0.0038(17) C27 0.025(2) 0.019(2) 0.0161(19) -0.0068(17) -0.0041(17) -0.0107(18) C28 0.0131(19) 0.0120(18) 0.0169(19) -0.0068(16) 0.0001(15) -0.0047(16) C29 0.032(2) 0.026(2) 0.0150(19) -0.0100(18) 0.0021(17) -0.017(2) C30 0.025(2) 0.019(2) 0.021(2) -0.0102(18) -0.0030(17) -0.0082(18) C31 0.024(2) 0.019(2) 0.019(2) -0.0086(18) -0.0019(17) -0.0093(18) C32 0.057(3) 0.025(2) 0.0118(19) -0.0053(18) -0.002(2) -0.020(2) C33 0.046(3) 0.044(3) 0.020(2) -0.016(2) 0.003(2) -0.023(3) C34 0.033(3) 0.030(2) 0.026(2) -0.019(2) -0.007(2) -0.005(2) C35 0.044(3) 0.026(2) 0.024(2) -0.018(2) -0.005(2) -0.005(2) C36 0.029(2) 0.020(2) 0.0164(19) -0.0070(18) -0.0053(17) -0.0095(19) C37 0.034(3) 0.023(2) 0.021(2) -0.0086(19) 0.0015(19) -0.015(2) C38 0.043(3) 0.028(2) 0.017(2) -0.0083(19) 0.0050(19) -0.022(2) C39 0.024(2) 0.023(2) 0.018(2) -0.0088(18) -0.0003(17) -0.0062(19) C40 0.030(3) 0.027(2) 0.028(2) -0.017(2) -0.007(2) -0.002(2) C41 0.027(2) 0.028(2) 0.031(2) -0.019(2) -0.006(2) -0.001(2) C42 0.028(2) 0.027(2) 0.023(2) -0.0045(19) -0.0035(19) -0.008(2) C43 0.023(2) 0.027(2) 0.026(2) -0.002(2) -0.0056(19) -0.005(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O12 2.059(3) 1_545 ? Co1 O1 2.081(3) . ? Co1 N5 2.089(3) . ? Co1 O17 2.135(3) . ? Co1 O9 2.144(2) . ? Co1 O18 2.147(3) . ? Co2 N9 2.060(3) . ? Co2 O11 2.074(3) 1_545 ? Co2 O9 2.097(3) . ? Co2 N7 2.101(3) 1_556 ? Co2 O3 2.127(3) 2_665 ? Co2 O17 2.279(3) . ? O1 C7 1.262(4) . ? O2 C7 1.266(5) . ? O3 C14 1.271(5) . ? O3 Co2 2.127(3) 2_665 ? O4 C14 1.260(4) . ? O5 N1 1.224(4) . ? O6 N1 1.236(4) . ? O7 N2 1.229(5) . ? O8 N2 1.207(4) . ? O9 C21 1.299(5) . ? O10 C21 1.230(5) . ? O11 C28 1.265(4) . ? O11 Co2 2.074(3) 1_565 ? O12 C28 1.244(4) . ? O12 Co1 2.059(3) 1_565 ? O13 N3 1.216(5) . ? O14 N3 1.228(4) . ? O15 O15" 0.577(15) . ? O15 O15' 0.606(18) . ? O15 N4 1.234(13) . ? O15' O15" 1.18(3) . ? O15' N4 1.48(3) . ? O15" N4 1.18(3) . ? O16 N4 1.229(5) . ? O17 H1A 0.952(19) . ? O17 H1B 0.972(19) . ? O18 H2A 0.983(19) . ? O18 H2B 0.992(19) . ? N1 C2 1.475(5) . ? N2 C9 1.474(5) . ? N3 C16 1.477(5) . ? N4 C23 1.468(5) . ? N5 C29 1.317(5) . ? N5 C30 1.381(5) . ? N6 C29 1.354(5) . ? N6 C31 1.373(5) . ? N6 C32 1.481(5) . ? N7 C36 1.320(5) . ? N7 C37 1.374(5) . ? N7 Co2 2.101(3) 1_554 ? N8 C36 1.344(5) . ? N8 C38 1.380(5) . ? N8 C35 1.466(5) . ? N9 C39 1.317(5) . ? N9 C40 1.386(5) . ? N10 C39 1.347(5) . ? N10 C41 1.374(5) . ? N10 C42 1.459(5) . ? C1 C6 1.387(6) . ? C1 C2 1.402(5) . ? C1 C8 1.494(5) . ? C2 C3 1.384(5) . ? C3 C4 1.395(6) . ? C3 H3 0.9300 . ? C4 C5 1.396(5) . ? C4 C7 1.509(5) . ? C5 C6 1.381(5) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C8 C9 1.396(5) . ? C8 C13 1.398(5) . ? C9 C10 1.384(5) . ? C10 C11 1.394(5) . ? C10 H10 0.9300 . ? C11 C12 1.390(5) . ? C11 C14 1.509(5) . ? C12 C13 1.377(5) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C15 C16 1.405(5) . ? C15 C20 1.407(5) . ? C15 C22 1.494(5) . ? C16 C17 1.383(5) . ? C17 C18 1.394(5) . ? C17 H17 0.9300 . ? C18 C19 1.385(6) . ? C18 C21 1.516(5) . ? C19 C20 1.391(5) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C22 C27 1.395(5) . ? C22 C23 1.399(5) . ? C23 C24 1.390(5) . ? C24 C25 1.390(5) . ? C24 H24 0.9300 . ? C25 C26 1.395(5) . ? C25 C28 1.521(5) . ? C26 C27 1.389(5) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C29 H29 0.9300 . ? C30 C31 1.345(5) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 C33 1.517(6) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.531(6) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C35 1.522(6) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 H36 0.9300 . ? C37 C38 1.365(6) . ? C37 H37 0.9300 . ? C38 H38 0.9300 . ? C39 H39 0.9300 . ? C40 C41 1.354(6) . ? C40 H40 0.9300 . ? C41 H41 0.9300 . ? C42 C43 1.526(6) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 C43 1.522(9) 2_646 ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O12 Co1 O1 173.37(11) 1_545 . ? O12 Co1 N5 89.14(12) 1_545 . ? O1 Co1 N5 89.87(12) . . ? O12 Co1 O17 83.81(11) 1_545 . ? O1 Co1 O17 90.02(11) . . ? N5 Co1 O17 102.54(12) . . ? O12 Co1 O9 96.13(10) 1_545 . ? O1 Co1 O9 85.06(10) . . ? N5 Co1 O9 174.55(11) . . ? O17 Co1 O9 79.51(10) . . ? O12 Co1 O18 91.58(11) 1_545 . ? O1 Co1 O18 94.98(11) . . ? N5 Co1 O18 90.34(12) . . ? O17 Co1 O18 166.22(10) . . ? O9 Co1 O18 88.12(10) . . ? N9 Co2 O11 89.31(12) . 1_545 ? N9 Co2 O9 172.19(11) . . ? O11 Co2 O9 93.03(11) 1_545 . ? N9 Co2 N7 95.10(13) . 1_556 ? O11 Co2 N7 92.38(12) 1_545 1_556 ? O9 Co2 N7 92.24(12) . 1_556 ? N9 Co2 O3 88.26(12) . 2_665 ? O11 Co2 O3 177.54(11) 1_545 2_665 ? O9 Co2 O3 89.32(11) . 2_665 ? N7 Co2 O3 88.26(12) 1_556 2_665 ? N9 Co2 O17 95.19(12) . . ? O11 Co2 O17 92.13(10) 1_545 . ? O9 Co2 O17 77.29(10) . . ? N7 Co2 O17 168.80(11) 1_556 . ? O3 Co2 O17 87.67(10) 2_665 . ? C7 O1 Co1 124.9(2) . . ? C14 O3 Co2 130.5(2) . 2_665 ? C21 O9 Co2 128.9(2) . . ? C21 O9 Co1 124.7(2) . . ? Co2 O9 Co1 98.84(10) . . ? C28 O11 Co2 124.9(2) . 1_565 ? C28 O12 Co1 132.2(2) . 1_565 ? O15" O15 O15' 171(5) . . ? O15" O15 N4 71(3) . . ? O15' O15 N4 101(4) . . ? O15 O15' O15" 5(2) . . ? O15 O15' N4 55(3) . . ? O15" O15' N4 51(2) . . ? O15 O15" O15' 5(3) . . ? O15 O15" N4 81(3) . . ? O15' O15" N4 77(3) . . ? Co1 O17 Co2 93.67(10) . . ? Co1 O17 H1A 111(3) . . ? Co2 O17 H1A 136(3) . . ? Co1 O17 H1B 117(3) . . ? Co2 O17 H1B 90(3) . . ? H1A O17 H1B 109(3) . . ? Co1 O18 H2A 108(3) . . ? Co1 O18 H2B 95(5) . . ? H2A O18 H2B 103(2) . . ? O5 N1 O6 123.8(4) . . ? O5 N1 C2 119.3(3) . . ? O6 N1 C2 116.9(3) . . ? O8 N2 O7 122.6(4) . . ? O8 N2 C9 119.5(3) . . ? O7 N2 C9 117.9(3) . . ? O13 N3 O14 123.8(4) . . ? O13 N3 C16 117.8(3) . . ? O14 N3 C16 118.4(4) . . ? O15" N4 O16 111.6(10) . . ? O15" N4 O15 27.5(7) . . ? O16 N4 O15 124.8(6) . . ? O15" N4 C23 124.0(12) . . ? O16 N4 C23 118.1(3) . . ? O15 N4 C23 117.1(6) . . ? O15" N4 O15' 51.2(12) . . ? O16 N4 O15' 128.0(13) . . ? O15 N4 O15' 23.8(10) . . ? C23 N4 O15' 108.2(12) . . ? C29 N5 C30 105.4(3) . . ? C29 N5 Co1 127.1(3) . . ? C30 N5 Co1 125.0(3) . . ? C29 N6 C31 107.4(3) . . ? C29 N6 C32 124.6(3) . . ? C31 N6 C32 128.0(3) . . ? C36 N7 C37 105.2(3) . . ? C36 N7 Co2 123.2(3) . 1_554 ? C37 N7 Co2 131.4(3) . 1_554 ? C36 N8 C38 106.8(3) . . ? C36 N8 C35 125.2(4) . . ? C38 N8 C35 127.9(3) . . ? C39 N9 C40 105.4(3) . . ? C39 N9 Co2 125.3(3) . . ? C40 N9 Co2 128.9(3) . . ? C39 N10 C41 107.0(3) . . ? C39 N10 C42 125.8(3) . . ? C41 N10 C42 126.1(3) . . ? C6 C1 C2 117.0(3) . . ? C6 C1 C8 118.8(4) . . ? C2 C1 C8 123.6(4) . . ? C3 C2 C1 122.6(4) . . ? C3 C2 N1 116.8(3) . . ? C1 C2 N1 120.6(3) . . ? C2 C3 C4 119.1(4) . . ? C2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? C3 C4 C5 119.1(4) . . ? C3 C4 C7 120.4(3) . . ? C5 C4 C7 120.5(4) . . ? C6 C5 C4 120.6(4) . . ? C6 C5 H5 119.7 . . ? C4 C5 H5 119.7 . . ? C5 C6 C1 121.6(4) . . ? C5 C6 H6 119.2 . . ? C1 C6 H6 119.2 . . ? O1 C7 O2 125.8(3) . . ? O1 C7 C4 117.3(3) . . ? O2 C7 C4 116.8(3) . . ? C9 C8 C13 116.1(3) . . ? C9 C8 C1 128.7(3) . . ? C13 C8 C1 115.2(3) . . ? C10 C9 C8 122.6(3) . . ? C10 C9 N2 116.8(3) . . ? C8 C9 N2 120.5(3) . . ? C9 C10 C11 119.3(4) . . ? C9 C10 H10 120.4 . . ? C11 C10 H10 120.4 . . ? C12 C11 C10 119.1(3) . . ? C12 C11 C14 119.8(3) . . ? C10 C11 C14 120.9(3) . . ? C13 C12 C11 120.2(3) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C12 C13 C8 122.1(4) . . ? C12 C13 H13 119.0 . . ? C8 C13 H13 119.0 . . ? O4 C14 O3 125.3(3) . . ? O4 C14 C11 116.8(3) . . ? O3 C14 C11 117.8(3) . . ? C16 C15 C20 115.8(3) . . ? C16 C15 C22 126.0(3) . . ? C20 C15 C22 118.0(3) . . ? C17 C16 C15 123.3(3) . . ? C17 C16 N3 116.1(4) . . ? C15 C16 N3 120.5(3) . . ? C16 C17 C18 119.2(4) . . ? C16 C17 H17 120.4 . . ? C18 C17 H17 120.4 . . ? C19 C18 C17 119.4(3) . . ? C19 C18 C21 122.0(3) . . ? C17 C18 C21 118.4(3) . . ? C18 C19 C20 120.7(4) . . ? C18 C19 H19 119.6 . . ? C20 C19 H19 119.6 . . ? C19 C20 C15 121.6(4) . . ? C19 C20 H20 119.2 . . ? C15 C20 H20 119.2 . . ? O10 C21 O9 124.7(3) . . ? O10 C21 C18 120.0(3) . . ? O9 C21 C18 115.2(3) . . ? C27 C22 C23 116.6(3) . . ? C27 C22 C15 116.8(3) . . ? C23 C22 C15 126.6(3) . . ? C24 C23 C22 122.8(3) . . ? C24 C23 N4 117.1(3) . . ? C22 C23 N4 120.1(3) . . ? C23 C24 C25 119.5(3) . . ? C23 C24 H24 120.2 . . ? C25 C24 H24 120.2 . . ? C24 C25 C26 118.7(3) . . ? C24 C25 C28 122.2(3) . . ? C26 C25 C28 119.0(3) . . ? C27 C26 C25 121.0(4) . . ? C27 C26 H26 119.5 . . ? C25 C26 H26 119.5 . . ? C26 C27 C22 121.4(3) . . ? C26 C27 H27 119.3 . . ? C22 C27 H27 119.3 . . ? O12 C28 O11 127.4(3) . . ? O12 C28 C25 116.4(3) . . ? O11 C28 C25 116.2(3) . . ? N5 C29 N6 111.0(3) . . ? N5 C29 H29 124.5 . . ? N6 C29 H29 124.5 . . ? C31 C30 N5 110.3(4) . . ? C31 C30 H30 124.8 . . ? N5 C30 H30 124.8 . . ? C30 C31 N6 105.9(3) . . ? C30 C31 H31 127.1 . . ? N6 C31 H31 127.1 . . ? N6 C32 C33 112.0(4) . . ? N6 C32 H32A 109.2 . . ? C33 C32 H32A 109.2 . . ? N6 C32 H32B 109.2 . . ? C33 C32 H32B 109.2 . . ? H32A C32 H32B 107.9 . . ? C32 C33 C34 115.6(4) . . ? C32 C33 H33A 108.4 . . ? C34 C33 H33A 108.4 . . ? C32 C33 H33B 108.4 . . ? C34 C33 H33B 108.4 . . ? H33A C33 H33B 107.4 . . ? C35 C34 C33 112.6(4) . . ? C35 C34 H34A 109.1 . . ? C33 C34 H34A 109.1 . . ? C35 C34 H34B 109.1 . . ? C33 C34 H34B 109.1 . . ? H34A C34 H34B 107.8 . . ? N8 C35 C34 112.6(4) . . ? N8 C35 H35A 109.1 . . ? C34 C35 H35A 109.1 . . ? N8 C35 H35B 109.1 . . ? C34 C35 H35B 109.1 . . ? H35A C35 H35B 107.8 . . ? N7 C36 N8 112.2(4) . . ? N7 C36 H36 123.9 . . ? N8 C36 H36 123.9 . . ? C38 C37 N7 110.0(4) . . ? C38 C37 H37 125.0 . . ? N7 C37 H37 125.0 . . ? C37 C38 N8 105.8(3) . . ? C37 C38 H38 127.1 . . ? N8 C38 H38 127.1 . . ? N9 C39 N10 111.7(3) . . ? N9 C39 H39 124.2 . . ? N10 C39 H39 124.2 . . ? C41 C40 N9 109.5(4) . . ? C41 C40 H40 125.3 . . ? N9 C40 H40 125.3 . . ? C40 C41 N10 106.4(4) . . ? C40 C41 H41 126.8 . . ? N10 C41 H41 126.8 . . ? N10 C42 C43 110.0(4) . . ? N10 C42 H42A 109.7 . . ? C43 C42 H42A 109.7 . . ? N10 C42 H42B 109.7 . . ? C43 C42 H42B 109.7 . . ? H42A C42 H42B 108.2 . . ? C43 C43 C42 113.7(5) 2_646 . ? C43 C43 H43A 108.8 2_646 . ? C42 C43 H43A 108.8 . . ? C43 C43 H43B 108.8 2_646 . ? C42 C43 H43B 108.8 . . ? H43A C43 H43B 107.7 . . ? 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 O18 H2A O10 0.983(19) 1.98(3) 2.821(4) 142(4) . O18 H2B O2 0.992(19) 1.63(2) 2.601(4) 165(6) . O17 H1A O4 0.952(19) 1.89(3) 2.766(4) 152(4) 1_545 O17 H1B O4 0.972(19) 1.59(2) 2.559(4) 177(5) 2_665 O17 H1B O3 0.972(19) 2.48(4) 3.054(4) 118(4) 2_665 _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.765 _refine_diff_density_min -0.563 _refine_diff_density_rms 0.112 data_compound-3 _database_code_depnum_ccdc_archive 'CCDC 782710' #TrackingRef 'CCDC.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C43 H37 N10 Ni2 O18' _chemical_formula_sum 'C43 H37 N10 Ni2 O18' _chemical_formula_weight 1099.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.7703(7) _cell_length_b 14.1255(8) _cell_length_c 15.8443(9) _cell_angle_alpha 116.321(3) _cell_angle_beta 90.408(4) _cell_angle_gamma 111.164(3) _cell_volume 2340.7(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 11490 _cell_measurement_theta_min 1.67 _cell_measurement_theta_max 28.29 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.560 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1130 _exptl_absorpt_coefficient_mu 0.892 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.807 _exptl_absorpt_correction_T_max 0.837 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 9.00cm _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 17080 _diffrn_reflns_av_R_equivalents 0.0518 _diffrn_reflns_av_sigmaI/netI 0.1254 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 28.29 _reflns_number_total 11490 _reflns_number_gt 5846 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXP-97 _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0990P)^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 11490 _refine_ls_number_parameters 655 _refine_ls_number_restraints 116 _refine_ls_R_factor_all 0.1323 _refine_ls_R_factor_gt 0.0658 _refine_ls_wR_factor_ref 0.1989 _refine_ls_wR_factor_gt 0.1673 _refine_ls_goodness_of_fit_ref 0.936 _refine_ls_restrained_S_all 0.934 _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 Ni1 Ni 0.69891(5) 0.69300(5) 0.73490(4) 0.02610(17) Uani 1 1 d . . . Ni2 Ni 0.81687(5) 0.62731(5) 0.55059(4) 0.02536(17) Uani 1 1 d D . . O1 O 0.8286(3) 0.7761(2) 0.6772(2) 0.0276(7) Uani 1 1 d . . . O2 O 1.0158(3) 0.8760(3) 0.7464(3) 0.0391(9) Uani 1 1 d . . . O3 O 0.7921(3) 1.6115(3) 0.7597(2) 0.0334(8) Uani 1 1 d . . . O4 O 0.8527(3) 1.5459(3) 0.6190(2) 0.0336(8) Uani 1 1 d . . . N1 N 1.0893(11) 1.2995(11) 0.8625(9) 0.0591(11) Uani 0.50 1 d PU A 1 O5 O 1.1414(8) 1.3125(7) 0.9341(7) 0.0591(11) Uani 0.50 1 d PU A 1 O6 O 1.1113(8) 1.3791(8) 0.8463(7) 0.0591(11) Uani 0.50 1 d PU A 1 N1' N 1.1107(11) 1.2873(11) 0.8280(9) 0.0591(11) Uani 0.50 1 d PU A 2 O5' O 1.1804(8) 1.2983(7) 0.8879(7) 0.0591(11) Uani 0.50 1 d PU A 2 O6' O 1.1344(8) 1.3580(8) 0.8012(7) 0.0591(11) Uani 0.50 1 d PU A 2 N2 N 0.8548(10) 1.3746(11) 0.9112(10) 0.0655(8) Uani 0.50 1 d PU A 1 O7 O 0.8244(8) 1.4410(8) 0.9695(7) 0.0655(8) Uani 0.50 1 d PU A 1 O8 O 0.9037(8) 1.3340(8) 0.9406(7) 0.0655(8) Uani 0.50 1 d PU A 1 N2' N 0.8088(10) 1.3425(11) 0.8886(10) 0.0655(8) Uani 0.50 1 d PU A 2 O7' O 0.7414(8) 1.3727(8) 0.9247(7) 0.0655(8) Uani 0.50 1 d PU A 2 O8' O 0.8293(9) 1.2849(8) 0.9128(7) 0.0655(8) Uani 0.50 1 d PU A 2 O9 O 0.7651(3) 0.7005(3) 0.4794(2) 0.0319(8) Uani 1 1 d . . . O10 O 0.9380(3) 0.8255(3) 0.4867(3) 0.0457(10) Uani 1 1 d . . . O11 O 0.4928(3) 1.3504(3) 0.4446(3) 0.0403(9) Uani 1 1 d . B . O12 O 0.4056(3) 1.2313(3) 0.2897(3) 0.0349(8) Uani 1 1 d . . . O13 O 0.4267(4) 0.7334(4) 0.3619(4) 0.0778(16) Uani 1 1 d . . . O14 O 0.4436(4) 0.9012(5) 0.3870(5) 0.0884(19) Uani 1 1 d . . . O15 O 0.5165(8) 0.9020(8) 0.1028(7) 0.0655(8) Uani 0.50 1 d PU B 1 O16 O 0.5329(8) 0.8164(8) 0.1915(7) 0.0655(8) Uani 0.50 1 d PU B 1 O15' O 0.4626(8) 0.8784(8) 0.1187(7) 0.0655(8) Uani 0.50 1 d PU B 2 O16' O 0.5912(8) 0.8439(8) 0.1756(7) 0.0655(8) Uani 0.50 1 d PU B 2 O17 O 0.6497(3) 0.5695(3) 0.5782(2) 0.0283(7) Uani 1 1 d D . . O18 O 0.9919(3) 0.7074(3) 0.5537(3) 0.0346(8) Uani 1 1 d D . . N3 N 0.4851(4) 0.8317(5) 0.3776(4) 0.0518(13) Uani 1 1 d . . . N4 N 0.5337(6) 0.9019(5) 0.1847(4) 0.080(2) Uani 1 1 d . . . N5 N 0.7661(4) 0.8326(3) 0.8713(3) 0.0345(10) Uani 1 1 d . . . N6 N 0.8137(5) 1.0100(4) 0.9881(4) 0.0555(14) Uani 1 1 d . . . N7 N 0.8026(4) 1.4881(3) 1.4210(3) 0.0357(10) Uani 1 1 d . . . N8 N 0.8066(5) 1.3941(4) 1.2673(4) 0.0594(14) Uani 1 1 d . . . N9 N 0.5655(4) 0.5989(3) 0.7742(3) 0.0348(10) Uani 1 1 d . . . N10 N 0.4518(4) 0.5490(4) 0.8653(4) 0.0501(12) Uani 1 1 d . . . C1 C 0.9012(4) 1.1852(4) 0.7482(4) 0.0305(11) Uani 1 1 d . A . C2 C 0.9965(4) 1.1862(4) 0.7927(4) 0.0390(13) Uani 1 1 d . . . C3 C 1.0027(4) 1.0867(4) 0.7863(4) 0.0354(12) Uani 1 1 d . A . H3 H 1.0682 1.0916 0.8169 0.080 Uiso 1 1 calc . . . C4 C 0.9107(4) 0.9802(4) 0.7340(3) 0.0258(10) Uani 1 1 d . . . C5 C 0.8141(4) 0.9775(4) 0.6901(4) 0.0344(12) Uani 1 1 d . A . H5 H 0.7510 0.9074 0.6560 0.080 Uiso 1 1 calc . . . C6 C 0.8095(4) 1.0775(4) 0.6958(4) 0.0383(13) Uani 1 1 d . . . H6 H 0.7443 1.0723 0.6642 0.080 Uiso 1 1 calc . . . C7 C 0.9206(4) 0.8704(4) 0.7203(3) 0.0273(10) Uani 1 1 d . A . C8 C 0.8928(4) 1.2875(4) 0.7449(4) 0.0307(11) Uani 1 1 d . . . C9 C 0.8548(5) 1.3658(5) 0.8117(4) 0.0419(14) Uani 1 1 d . A . C10 C 0.8367(5) 1.4512(4) 0.7996(4) 0.0396(13) Uani 1 1 d . . . H10 H 0.8090 1.4999 0.8456 0.080 Uiso 1 1 calc . . . C11 C 0.8602(4) 1.4628(4) 0.7191(4) 0.0266(10) Uani 1 1 d . A . C12 C 0.9012(5) 1.3873(5) 0.6516(4) 0.0389(13) Uani 1 1 d . . . H12 H 0.9197 1.3953 0.5978 0.080 Uiso 1 1 calc . . . C13 C 0.9149(5) 1.3003(5) 0.6637(4) 0.0408(13) Uani 1 1 d . A . H13 H 0.9395 1.2494 0.6163 0.080 Uiso 1 1 calc . . . C14 C 0.8335(4) 1.5482(4) 0.6977(4) 0.0260(10) Uani 1 1 d . . . C15 C 0.6775(4) 0.9570(4) 0.3697(4) 0.0326(11) Uani 1 1 d . B . C16 C 0.6104(4) 0.8686(4) 0.3898(4) 0.0337(11) Uani 1 1 d . . . C17 C 0.6575(4) 0.8109(4) 0.4198(4) 0.0360(12) Uani 1 1 d . . . H17 H 0.6105 0.7528 0.4325 0.080 Uiso 1 1 calc . . . C18 C 0.7768(4) 0.8410(4) 0.4308(3) 0.0279(10) Uani 1 1 d . . . C19 C 0.8438(4) 0.9265(4) 0.4089(4) 0.0377(12) Uani 1 1 d . . . H19 H 0.9223 0.9463 0.4146 0.080 Uiso 1 1 calc . . . C20 C 0.7953(4) 0.9823(5) 0.3788(4) 0.0405(13) Uani 1 1 d . . . H20 H 0.8423 1.0384 0.3640 0.080 Uiso 1 1 calc . . . C21 C 0.8316(4) 0.7851(4) 0.4682(3) 0.0294(11) Uani 1 1 d . . . C22 C 0.6347(4) 1.0358(4) 0.3550(4) 0.0346(12) Uani 1 1 d . . . C23 C 0.5628(5) 1.0111(4) 0.2740(4) 0.0426(13) Uani 1 1 d . B . C24 C 0.5151(5) 1.0858(5) 0.2737(4) 0.0411(13) Uani 1 1 d . . . H24 H 0.4677 1.0661 0.2184 0.080 Uiso 1 1 calc . . . C25 C 0.5393(4) 1.1905(4) 0.3572(4) 0.0315(11) Uani 1 1 d . B . C26 C 0.6198(5) 1.2220(4) 0.4348(4) 0.0425(13) Uani 1 1 d . . . H26 H 0.6432 1.2950 0.4879 0.080 Uiso 1 1 calc . . . C27 C 0.6659(5) 1.1462(5) 0.4348(4) 0.0431(13) Uani 1 1 d . B . H27 H 0.7183 1.1691 0.4884 0.080 Uiso 1 1 calc . . . C28 C 0.4753(4) 1.2641(4) 0.3630(4) 0.0306(11) Uani 1 1 d . . . C29 C 0.7623(5) 0.9343(5) 0.8981(4) 0.0445(14) Uani 1 1 d . . . H29 H 0.7270 0.9504 0.8577 0.080 Uiso 1 1 calc . . . C30 C 0.8250(6) 0.8460(5) 0.9500(5) 0.0625(19) Uani 1 1 d . . . H30 H 0.8419 0.7890 0.9537 0.080 Uiso 1 1 calc . . . C31 C 0.8556(8) 0.9554(6) 1.0231(5) 0.086(3) Uani 1 1 d . . . H31 H 0.8968 0.9867 1.0846 0.080 Uiso 1 1 calc . . . C32 C 0.8216(8) 1.1323(5) 1.0402(5) 0.081(2) Uani 1 1 d . . . H32A H 0.8266 1.1620 0.9950 0.080 Uiso 1 1 calc . . . H32B H 0.8911 1.1806 1.0893 0.080 Uiso 1 1 calc . . . C33 C 0.7181(7) 1.1396(6) 1.0871(6) 0.080(2) Uani 1 1 d . C . H33A H 0.7313 1.1436 1.1492 0.080 Uiso 1 1 calc . . . H33B H 0.6508 1.0695 1.0475 0.080 Uiso 1 1 calc . . . C34 C 0.6940(8) 1.2458(7) 1.1012(6) 0.095(3) Uani 1 1 d . . . C35 C 0.8172(12) 1.3669(14) 1.1613(13) 0.0655(8) Uani 0.50 1 d PU C 1 C35' C 0.7730(12) 1.3554(15) 1.1625(13) 0.0655(8) Uani 0.50 1 d PU C 2 C36 C 0.7740(6) 1.4729(5) 1.3356(4) 0.0590(18) Uani 1 1 d . . . H36 H 0.7357 1.5113 1.3227 0.080 Uiso 1 1 calc . . . C37 C 0.8557(5) 1.4149(5) 1.4069(4) 0.0439(14) Uani 1 1 d . . . H37 H 0.8864 1.4074 1.4558 0.080 Uiso 1 1 calc . . . C38 C 0.8578(6) 1.3554(5) 1.3136(4) 0.0525(16) Uani 1 1 d . C . H38 H 0.8877 1.2999 1.2864 0.080 Uiso 1 1 calc . . . C39 C 0.5387(5) 0.6346(5) 0.8604(5) 0.0550(16) Uani 1 1 d . . . H39 H 0.5754 0.7093 0.9112 0.080 Uiso 1 1 calc . . . C40 C 0.4932(7) 0.4856(6) 0.7246(6) 0.077(2) Uani 1 1 d . . . H40 H 0.4917 0.4361 0.6612 0.080 Uiso 1 1 calc . . . C41 C 0.4237(7) 0.4548(6) 0.7802(6) 0.074(2) Uani 1 1 d . . . H41 H 0.3672 0.3819 0.7624 0.080 Uiso 1 1 calc . . . C42 C 0.4055(6) 0.5556(6) 0.9522(5) 0.0654(19) Uani 1 1 d . . . H42A H 0.3227 0.5271 0.9375 0.080 Uiso 1 1 calc . . . H42B H 0.4354 0.6355 1.0024 0.080 Uiso 1 1 calc . . . C43 C 0.4395(6) 0.4821(9) 0.9884(7) 0.094(3) Uani 1 1 d . . . H43A H 0.4078 0.4873 1.0450 0.080 Uiso 1 1 calc . . . H43B H 0.4056 0.4017 0.9391 0.080 Uiso 1 1 calc . . . H1B H 0.610(4) 0.4854(17) 0.548(4) 0.080 Uiso 1 1 d D . . H2B H 0.993(2) 0.766(4) 0.530(4) 0.080 Uiso 1 1 d D . . H1A H 0.595(4) 0.596(4) 0.563(5) 0.080 Uiso 1 1 d D . . H2A H 1.026(2) 0.762(4) 0.6244(15) 0.080 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 Ni1 0.0335(3) 0.0216(3) 0.0279(4) 0.0117(3) 0.0047(3) 0.0162(3) Ni2 0.0346(3) 0.0211(3) 0.0272(3) 0.0134(3) 0.0045(3) 0.0160(3) O1 0.0337(17) 0.0184(15) 0.0314(19) 0.0119(14) 0.0058(15) 0.0112(14) O2 0.042(2) 0.0292(18) 0.043(2) 0.0122(17) -0.0077(17) 0.0188(16) O3 0.049(2) 0.0318(18) 0.034(2) 0.0187(16) 0.0113(17) 0.0282(16) O4 0.052(2) 0.0370(19) 0.035(2) 0.0263(17) 0.0165(17) 0.0301(17) N1 0.0598(11) 0.0582(11) 0.0598(12) 0.0290(6) 0.0106(4) 0.0236(6) O5 0.0598(11) 0.0582(11) 0.0598(12) 0.0290(6) 0.0106(4) 0.0236(6) O6 0.0598(11) 0.0582(11) 0.0598(12) 0.0290(6) 0.0106(4) 0.0236(6) N1' 0.0598(11) 0.0582(11) 0.0598(12) 0.0290(6) 0.0106(4) 0.0236(6) O5' 0.0598(11) 0.0582(11) 0.0598(12) 0.0290(6) 0.0106(4) 0.0236(6) O6' 0.0598(11) 0.0582(11) 0.0598(12) 0.0290(6) 0.0106(4) 0.0236(6) N2 0.0665(9) 0.0653(9) 0.0655(9) 0.0316(5) 0.0129(3) 0.0272(4) O7 0.0665(9) 0.0653(9) 0.0655(9) 0.0316(5) 0.0129(3) 0.0272(4) O8 0.0665(9) 0.0653(9) 0.0655(9) 0.0316(5) 0.0129(3) 0.0272(4) N2' 0.0665(9) 0.0653(9) 0.0655(9) 0.0316(5) 0.0129(3) 0.0272(4) O7' 0.0665(9) 0.0653(9) 0.0655(9) 0.0316(5) 0.0129(3) 0.0272(4) O8' 0.0665(9) 0.0653(9) 0.0655(9) 0.0316(5) 0.0129(3) 0.0272(4) O9 0.0375(19) 0.0324(18) 0.036(2) 0.0224(17) 0.0044(16) 0.0175(15) O10 0.036(2) 0.051(2) 0.075(3) 0.046(2) 0.010(2) 0.0231(18) O11 0.042(2) 0.0314(19) 0.043(2) 0.0096(18) -0.0055(17) 0.0221(16) O12 0.042(2) 0.0325(18) 0.038(2) 0.0174(17) -0.0006(17) 0.0233(16) O13 0.041(2) 0.068(3) 0.125(5) 0.056(3) 0.003(3) 0.011(2) O14 0.052(3) 0.101(4) 0.172(6) 0.102(4) 0.031(3) 0.046(3) O15 0.0665(9) 0.0653(9) 0.0655(9) 0.0316(5) 0.0129(3) 0.0272(4) O16 0.0665(9) 0.0653(9) 0.0655(9) 0.0316(5) 0.0129(3) 0.0272(4) O15' 0.0665(9) 0.0653(9) 0.0655(9) 0.0316(5) 0.0129(3) 0.0272(4) O16' 0.0665(9) 0.0653(9) 0.0655(9) 0.0316(5) 0.0129(3) 0.0272(4) O17 0.0322(17) 0.0206(16) 0.0337(19) 0.0131(15) 0.0021(15) 0.0124(14) O18 0.0408(19) 0.0350(19) 0.039(2) 0.0215(17) 0.0080(17) 0.0216(16) N3 0.038(3) 0.061(3) 0.070(4) 0.044(3) 0.004(3) 0.019(3) N4 0.136(5) 0.056(3) 0.050(4) 0.006(3) -0.025(4) 0.067(4) N5 0.045(2) 0.029(2) 0.030(2) 0.0125(19) 0.003(2) 0.0176(19) N6 0.093(4) 0.032(3) 0.035(3) 0.007(2) 0.004(3) 0.029(3) N7 0.050(3) 0.028(2) 0.031(2) 0.015(2) 0.004(2) 0.018(2) N8 0.099(4) 0.048(3) 0.036(3) 0.013(3) 0.010(3) 0.043(3) N9 0.040(2) 0.032(2) 0.034(3) 0.016(2) 0.009(2) 0.017(2) N10 0.046(3) 0.059(3) 0.043(3) 0.031(3) 0.011(2) 0.010(2) C1 0.039(3) 0.025(2) 0.041(3) 0.023(2) 0.011(2) 0.018(2) C2 0.039(3) 0.018(2) 0.054(4) 0.017(2) -0.008(3) 0.006(2) C3 0.036(3) 0.025(2) 0.047(3) 0.019(2) -0.004(2) 0.013(2) C4 0.033(2) 0.021(2) 0.027(3) 0.013(2) 0.005(2) 0.013(2) C5 0.037(3) 0.026(2) 0.040(3) 0.016(2) 0.000(2) 0.012(2) C6 0.039(3) 0.033(3) 0.053(4) 0.025(3) 0.002(3) 0.019(2) C7 0.040(3) 0.022(2) 0.026(3) 0.014(2) 0.006(2) 0.016(2) C8 0.041(3) 0.027(2) 0.038(3) 0.023(2) 0.010(2) 0.020(2) C9 0.074(4) 0.040(3) 0.042(3) 0.033(3) 0.031(3) 0.037(3) C10 0.065(4) 0.034(3) 0.042(3) 0.024(3) 0.027(3) 0.036(3) C11 0.030(2) 0.021(2) 0.035(3) 0.016(2) 0.005(2) 0.015(2) C12 0.059(3) 0.047(3) 0.042(3) 0.033(3) 0.026(3) 0.038(3) C13 0.066(4) 0.043(3) 0.043(3) 0.029(3) 0.027(3) 0.042(3) C14 0.029(2) 0.019(2) 0.032(3) 0.013(2) 0.004(2) 0.0121(19) C15 0.041(3) 0.029(2) 0.036(3) 0.018(2) 0.001(2) 0.019(2) C16 0.030(3) 0.036(3) 0.042(3) 0.021(3) 0.005(2) 0.018(2) C17 0.040(3) 0.029(3) 0.043(3) 0.023(3) 0.005(2) 0.013(2) C18 0.035(3) 0.027(2) 0.030(3) 0.015(2) 0.007(2) 0.019(2) C19 0.036(3) 0.041(3) 0.054(4) 0.032(3) 0.013(3) 0.023(2) C20 0.039(3) 0.044(3) 0.060(4) 0.037(3) 0.014(3) 0.024(3) C21 0.041(3) 0.029(2) 0.028(3) 0.015(2) 0.006(2) 0.021(2) C22 0.043(3) 0.030(3) 0.042(3) 0.022(2) 0.005(2) 0.020(2) C23 0.063(4) 0.034(3) 0.034(3) 0.012(3) 0.001(3) 0.030(3) C24 0.056(3) 0.039(3) 0.038(3) 0.018(3) -0.002(3) 0.030(3) C25 0.035(3) 0.030(3) 0.036(3) 0.016(2) 0.007(2) 0.019(2) C26 0.052(3) 0.029(3) 0.045(3) 0.011(3) -0.005(3) 0.024(2) C27 0.051(3) 0.037(3) 0.042(3) 0.015(3) -0.007(3) 0.025(3) C28 0.032(3) 0.023(2) 0.042(3) 0.018(2) 0.004(2) 0.014(2) C29 0.072(4) 0.033(3) 0.028(3) 0.010(3) 0.007(3) 0.026(3) C30 0.095(5) 0.044(4) 0.045(4) 0.014(3) -0.015(4) 0.034(4) C31 0.145(7) 0.050(4) 0.040(4) 0.008(3) -0.034(4) 0.036(4) C32 0.135(7) 0.034(4) 0.052(5) 0.008(3) 0.010(5) 0.026(4) C33 0.093(6) 0.042(4) 0.078(6) 0.005(4) 0.005(5) 0.031(4) C34 0.139(8) 0.061(5) 0.061(5) 0.000(4) -0.020(5) 0.053(5) C35 0.0665(9) 0.0653(9) 0.0655(9) 0.0316(5) 0.0129(3) 0.0272(4) C35' 0.0665(9) 0.0653(9) 0.0655(9) 0.0316(5) 0.0129(3) 0.0272(4) C36 0.107(5) 0.046(3) 0.036(3) 0.012(3) 0.002(4) 0.052(4) C37 0.063(4) 0.040(3) 0.040(3) 0.019(3) 0.013(3) 0.032(3) C38 0.083(4) 0.050(4) 0.043(4) 0.022(3) 0.016(3) 0.046(3) C39 0.058(4) 0.045(3) 0.059(4) 0.024(3) 0.017(3) 0.018(3) C40 0.087(5) 0.047(4) 0.072(5) 0.023(4) 0.029(5) 0.009(4) C41 0.084(5) 0.047(4) 0.061(5) 0.024(4) 0.018(4) -0.002(4) C42 0.064(4) 0.073(5) 0.056(4) 0.032(4) 0.017(4) 0.024(4) C43 0.068(5) 0.161(9) 0.089(6) 0.093(7) 0.027(5) 0.041(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N9 2.042(4) . ? Ni1 N5 2.065(4) . ? Ni1 O3 2.068(3) 1_545 ? Ni1 O12 2.114(3) 2_676 ? Ni1 O1 2.127(3) . ? Ni1 O17 2.225(3) . ? Ni2 O4 2.045(3) 1_545 ? Ni2 N7 2.067(4) 1_544 ? Ni2 O9 2.072(3) . ? Ni2 O18 2.098(3) . ? Ni2 O17 2.118(3) . ? Ni2 O1 2.120(3) . ? O1 C7 1.293(5) . ? O2 C7 1.243(5) . ? O3 C14 1.270(5) . ? O3 Ni1 2.068(3) 1_565 ? O4 C14 1.262(5) . ? O4 Ni2 2.045(3) 1_565 ? N1 O6 1.199(14) . ? N1 O5 1.217(14) . ? N1 C2 1.494(14) . ? N1' O6' 1.195(14) . ? N1' O5' 1.214(14) . ? N1' C2 1.502(13) . ? N2 O7 1.176(15) . ? N2 O8 1.194(15) . ? N2 C9 1.526(15) . ? N2' O7' 1.142(14) . ? N2' O8' 1.143(15) . ? N2' C9 1.472(15) . ? O9 C21 1.281(5) . ? O10 C21 1.243(6) . ? O11 C28 1.269(6) . ? O12 C28 1.252(6) . ? O12 Ni1 2.114(3) 2_676 ? O13 N3 1.221(6) . ? O14 N3 1.230(6) . ? O15 N4 1.316(11) . ? O16 N4 1.256(10) . ? O15' N4 1.220(10) . ? O16' N4 1.249(10) . ? O17 H1B 0.976(19) . ? O17 H1A 0.980(19) . ? O18 H2B 1.037(19) . ? O18 H2A 1.012(19) . ? N3 C16 1.475(6) . ? N4 C23 1.470(7) . ? N5 C29 1.325(6) . ? N5 C30 1.354(7) . ? N6 C29 1.317(7) . ? N6 C31 1.365(8) . ? N6 C32 1.511(8) . ? N7 C36 1.299(7) . ? N7 C37 1.371(6) . ? N7 Ni2 2.067(4) 1_566 ? N8 C36 1.363(7) . ? N8 C38 1.367(7) . ? N8 C35' 1.503(18) . ? N8 C35 1.567(18) . ? N9 C39 1.326(7) . ? N9 C40 1.356(8) . ? N10 C41 1.332(8) . ? N10 C39 1.347(7) . ? N10 C42 1.481(8) . ? C1 C2 1.395(7) . ? C1 C6 1.399(7) . ? C1 C8 1.511(6) . ? C2 C3 1.394(6) . ? C3 C4 1.390(6) . ? C3 H3 0.9300 . ? C4 C5 1.393(6) . ? C4 C7 1.522(6) . ? C5 C6 1.397(6) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C8 C9 1.390(7) . ? C8 C13 1.394(7) . ? C9 C10 1.397(6) . ? C10 C11 1.379(7) . ? C10 H10 0.9300 . ? C11 C12 1.398(6) . ? C11 C14 1.530(6) . ? C12 C13 1.393(6) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C15 C20 1.406(7) . ? C15 C16 1.407(7) . ? C15 C22 1.503(6) . ? C16 C17 1.394(6) . ? C17 C18 1.413(7) . ? C17 H17 0.9300 . ? C18 C19 1.392(6) . ? C18 C21 1.508(6) . ? C19 C20 1.384(6) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C22 C23 1.402(7) . ? C22 C27 1.409(7) . ? C23 C24 1.398(7) . ? C24 C25 1.401(7) . ? C24 H24 0.9300 . ? C25 C26 1.390(7) . ? C25 C28 1.512(6) . ? C26 C27 1.396(7) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C29 H29 0.9300 . ? C30 C31 1.361(9) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 C33 1.535(11) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.559(10) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C35' 1.372(18) . ? C34 C35 1.703(18) . ? C36 H36 0.9300 . ? C37 C38 1.344(8) . ? C37 H37 0.9300 . ? C38 H38 0.9300 . ? C39 H39 0.9300 . ? C40 C41 1.351(9) . ? C40 H40 0.9300 . ? C41 H41 0.9300 . ? C42 C43 1.564(11) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 C43 1.428(15) 2_667 ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N9 Ni1 N5 94.90(17) . . ? N9 Ni1 O3 87.87(15) . 1_545 ? N5 Ni1 O3 92.05(15) . 1_545 ? N9 Ni1 O12 88.61(15) . 2_676 ? N5 Ni1 O12 88.94(15) . 2_676 ? O3 Ni1 O12 176.41(13) 1_545 2_676 ? N9 Ni1 O1 173.37(15) . . ? N5 Ni1 O1 91.65(14) . . ? O3 Ni1 O1 92.91(12) 1_545 . ? O12 Ni1 O1 90.51(12) 2_676 . ? N9 Ni1 O17 96.84(15) . . ? N5 Ni1 O17 167.68(14) . . ? O3 Ni1 O17 92.09(12) 1_545 . ? O12 Ni1 O17 87.64(12) 2_676 . ? O1 Ni1 O17 76.55(12) . . ? O4 Ni2 N7 88.55(15) 1_545 1_544 ? O4 Ni2 O9 174.84(14) 1_545 . ? N7 Ni2 O9 90.66(15) 1_544 . ? O4 Ni2 O18 90.24(13) 1_545 . ? N7 Ni2 O18 89.54(15) 1_544 . ? O9 Ni2 O18 94.86(13) . . ? O4 Ni2 O17 85.85(13) 1_545 . ? N7 Ni2 O17 101.41(15) 1_544 . ? O9 Ni2 O17 89.31(12) . . ? O18 Ni2 O17 168.25(14) . . ? O4 Ni2 O1 96.01(13) 1_545 . ? N7 Ni2 O1 175.44(14) 1_544 . ? O9 Ni2 O1 84.80(12) . . ? O18 Ni2 O1 90.39(13) . . ? O17 Ni2 O1 79.03(12) . . ? C7 O1 Ni2 124.2(3) . . ? C7 O1 Ni1 130.2(3) . . ? Ni2 O1 Ni1 98.32(12) . . ? C14 O3 Ni1 125.9(3) . 1_565 ? C14 O4 Ni2 131.6(3) . 1_565 ? O6 N1 O5 120.2(13) . . ? O6 N1 C2 117.9(11) . . ? O5 N1 C2 122.0(11) . . ? O6' N1' O5' 119.2(12) . . ? O6' N1' C2 122.9(11) . . ? O5' N1' C2 118.0(10) . . ? O7 N2 O8 115.4(14) . . ? O7 N2 C9 119.6(12) . . ? O8 N2 C9 123.4(12) . . ? O7' N2' O8' 113.1(14) . . ? O7' N2' C9 122.9(13) . . ? O8' N2' C9 123.7(13) . . ? C21 O9 Ni2 125.2(3) . . ? C28 O12 Ni1 130.6(3) . 2_676 ? Ni2 O17 Ni1 95.43(12) . . ? Ni2 O17 H1B 113(3) . . ? Ni1 O17 H1B 127(4) . . ? Ni2 O17 H1A 119(4) . . ? Ni1 O17 H1A 96(4) . . ? H1B O17 H1A 106(3) . . ? Ni2 O18 H2B 101.7(15) . . ? Ni2 O18 H2A 104.0(15) . . ? H2B O18 H2A 100(2) . . ? O13 N3 O14 122.5(5) . . ? O13 N3 C16 117.8(5) . . ? O14 N3 C16 119.6(5) . . ? O15' N4 O16' 122.5(8) . . ? O15' N4 O16 114.8(8) . . ? O16' N4 O16 37.5(5) . . ? O15' N4 O15 34.0(5) . . ? O16' N4 O15 107.9(8) . . ? O16 N4 O15 124.2(7) . . ? O15' N4 C23 118.0(6) . . ? O16' N4 C23 118.9(7) . . ? O16 N4 C23 117.9(7) . . ? O15 N4 C23 117.8(6) . . ? C29 N5 C30 104.6(5) . . ? C29 N5 Ni1 124.5(4) . . ? C30 N5 Ni1 130.9(4) . . ? C29 N6 C31 106.5(5) . . ? C29 N6 C32 125.5(5) . . ? C31 N6 C32 128.1(6) . . ? C36 N7 C37 104.4(4) . . ? C36 N7 Ni2 126.9(3) . 1_566 ? C37 N7 Ni2 125.7(4) . 1_566 ? C36 N8 C38 106.7(5) . . ? C36 N8 C35' 121.0(8) . . ? C38 N8 C35' 131.9(8) . . ? C36 N8 C35 131.2(7) . . ? C38 N8 C35 120.6(7) . . ? C35' N8 C35 19.8(7) . . ? C39 N9 C40 104.3(5) . . ? C39 N9 Ni1 126.0(4) . . ? C40 N9 Ni1 129.3(4) . . ? C41 N10 C39 107.1(5) . . ? C41 N10 C42 126.5(5) . . ? C39 N10 C42 126.1(6) . . ? C2 C1 C6 116.3(4) . . ? C2 C1 C8 125.8(4) . . ? C6 C1 C8 117.7(4) . . ? C3 C2 C1 123.1(4) . . ? C3 C2 N1 117.2(6) . . ? C1 C2 N1 119.0(6) . . ? C3 C2 N1' 113.6(6) . . ? C1 C2 N1' 121.3(6) . . ? N1 C2 N1' 23.0(6) . . ? C4 C3 C2 120.0(4) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C4 C5 117.9(4) . . ? C3 C4 C7 120.1(4) . . ? C5 C4 C7 121.9(4) . . ? C4 C5 C6 121.7(5) . . ? C4 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? C5 C6 C1 121.1(5) . . ? C5 C6 H6 119.5 . . ? C1 C6 H6 119.5 . . ? O2 C7 O1 124.9(4) . . ? O2 C7 C4 118.8(4) . . ? O1 C7 C4 116.2(4) . . ? C9 C8 C13 115.7(4) . . ? C9 C8 C1 126.2(4) . . ? C13 C8 C1 117.8(4) . . ? C8 C9 C10 123.7(5) . . ? C8 C9 N2' 117.7(7) . . ? C10 C9 N2' 117.4(7) . . ? C8 C9 N2 118.1(7) . . ? C10 C9 N2 117.1(7) . . ? N2' C9 N2 22.3(6) . . ? C11 C10 C9 119.6(4) . . ? C11 C10 H10 120.2 . . ? C9 C10 H10 120.2 . . ? C10 C11 C12 118.2(4) . . ? C10 C11 C14 122.1(4) . . ? C12 C11 C14 119.5(4) . . ? C13 C12 C11 121.2(4) . . ? C13 C12 H12 119.4 . . ? C11 C12 H12 119.4 . . ? C12 C13 C8 121.6(4) . . ? C12 C13 H13 119.2 . . ? C8 C13 H13 119.2 . . ? O4 C14 O3 127.1(4) . . ? O4 C14 C11 116.0(4) . . ? O3 C14 C11 116.9(4) . . ? C20 C15 C16 116.2(4) . . ? C20 C15 C22 119.0(4) . . ? C16 C15 C22 124.1(4) . . ? C17 C16 C15 122.5(4) . . ? C17 C16 N3 117.2(4) . . ? C15 C16 N3 120.2(4) . . ? C16 C17 C18 119.6(4) . . ? C16 C17 H17 120.2 . . ? C18 C17 H17 120.2 . . ? C19 C18 C17 118.5(4) . . ? C19 C18 C21 120.3(4) . . ? C17 C18 C21 121.1(4) . . ? C20 C19 C18 120.9(4) . . ? C20 C19 H19 119.5 . . ? C18 C19 H19 119.5 . . ? C19 C20 C15 122.2(4) . . ? C19 C20 H20 118.9 . . ? C15 C20 H20 118.9 . . ? O10 C21 O9 124.9(4) . . ? O10 C21 C18 117.5(4) . . ? O9 C21 C18 117.6(4) . . ? C23 C22 C27 116.2(4) . . ? C23 C22 C15 128.1(5) . . ? C27 C22 C15 115.6(4) . . ? C24 C23 C22 122.9(5) . . ? C24 C23 N4 117.2(5) . . ? C22 C23 N4 119.9(4) . . ? C23 C24 C25 119.5(5) . . ? C23 C24 H24 120.3 . . ? C25 C24 H24 120.3 . . ? C26 C25 C24 118.3(4) . . ? C26 C25 C28 121.5(4) . . ? C24 C25 C28 120.2(4) . . ? C25 C26 C27 121.4(5) . . ? C25 C26 H26 119.3 . . ? C27 C26 H26 119.3 . . ? C26 C27 C22 121.2(5) . . ? C26 C27 H27 119.4 . . ? C22 C27 H27 119.4 . . ? O12 C28 O11 125.9(4) . . ? O12 C28 C25 117.9(4) . . ? O11 C28 C25 116.0(4) . . ? N6 C29 N5 112.9(5) . . ? N6 C29 H29 123.6 . . ? N5 C29 H29 123.6 . . ? N5 C30 C31 109.8(5) . . ? N5 C30 H30 125.1 . . ? C31 C30 H30 125.1 . . ? C30 C31 N6 106.3(6) . . ? C30 C31 H31 126.9 . . ? N6 C31 H31 126.9 . . ? N6 C32 C33 112.2(6) . . ? N6 C32 H32A 109.2 . . ? C33 C32 H32A 109.2 . . ? N6 C32 H32B 109.2 . . ? C33 C32 H32B 109.2 . . ? H32A C32 H32B 107.9 . . ? C32 C33 C34 113.5(7) . . ? C32 C33 H33A 108.9 . . ? C34 C33 H33A 108.9 . . ? C32 C33 H33B 108.9 . . ? C34 C33 H33B 108.9 . . ? H33A C33 H33B 107.7 . . ? C35' C34 C33 119.6(10) . . ? C35' C34 C35 15.6(9) . . ? C33 C34 C35 108.2(8) . . ? N8 C35 C34 99.8(9) . . ? C34 C35' N8 121.0(13) . . ? N7 C36 N8 112.1(5) . . ? N7 C36 H36 124.0 . . ? N8 C36 H36 124.0 . . ? C38 C37 N7 111.7(5) . . ? C38 C37 H37 124.2 . . ? N7 C37 H37 124.2 . . ? C37 C38 N8 105.2(5) . . ? C37 C38 H38 127.4 . . ? N8 C38 H38 127.4 . . ? N9 C39 N10 111.5(6) . . ? N9 C39 H39 124.3 . . ? N10 C39 H39 124.3 . . ? C41 C40 N9 110.4(6) . . ? C41 C40 H40 124.8 . . ? N9 C40 H40 124.8 . . ? N10 C41 C40 106.8(6) . . ? N10 C41 H41 126.6 . . ? C40 C41 H41 126.6 . . ? N10 C42 C43 110.5(6) . . ? N10 C42 H42A 109.6 . . ? C43 C42 H42A 109.6 . . ? N10 C42 H42B 109.6 . . ? C43 C42 H42B 109.6 . . ? H42A C42 H42B 108.1 . . ? C43 C43 C42 113.5(9) 2_667 . ? C43 C43 H43A 108.9 2_667 . ? C42 C43 H43A 108.9 . . ? C43 C43 H43B 108.9 2_667 . ? C42 C43 H43B 108.9 . . ? H43A C43 H43B 107.7 . . ? 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 O17 H1B O11 0.976(19) 1.92(4) 2.780(5) 145(5) 1_545 O18 H2B O10 1.037(19) 1.62(2) 2.603(4) 156(2) . O17 H1A O11 0.980(19) 1.59(2) 2.561(4) 171(6) 2_676 O17 H1A O12 0.980(19) 2.52(6) 3.005(4) 110(4) 2_676 O18 H2A O2 1.012(19) 1.94(3) 2.846(5) 148(4) . O18 H2A O1 1.012(19) 2.72(3) 2.993(4) 95.9(19) . _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.187 _refine_diff_density_min -0.944 _refine_diff_density_rms 0.105 data_compound-4 _database_code_depnum_ccdc_archive 'CCDC 782711' #TrackingRef 'CCDC.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C38 H28 Cu3 N8 O18' _chemical_formula_sum 'C38 H28 Cu3 N8 O18' _chemical_formula_weight 1075.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 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 8.2565(17) _cell_length_b 10.422(2) _cell_length_c 23.990(5) _cell_angle_alpha 90.00 _cell_angle_beta 96.68(3) _cell_angle_gamma 90.00 _cell_volume 2050.2(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4667 _cell_measurement_theta_min 3.16 _cell_measurement_theta_max 27.45 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.742 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1086 _exptl_absorpt_coefficient_mu 1.633 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method omega-scan _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 19611 _diffrn_reflns_av_R_equivalents 0.0725 _diffrn_reflns_av_sigmaI/netI 0.0617 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 3.16 _diffrn_reflns_theta_max 27.45 _reflns_number_total 4667 _reflns_number_gt 3306 _reflns_threshold_expression >2sigma(I) _computing_data_collection Process-auto _computing_cell_refinement Process-auto _computing_data_reduction Process-auto _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^)+(0.0788P)^2^+3.6722P] 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 4667 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0937 _refine_ls_R_factor_gt 0.0603 _refine_ls_wR_factor_ref 0.1640 _refine_ls_wR_factor_gt 0.1484 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu -0.64595(6) 0.82533(6) 0.02669(2) 0.03500(19) Uani 1 1 d . . . Cu2 Cu -1.0000 1.0000 0.0000 0.0389(2) Uani 1 2 d S . . O1 O -0.7856(4) 0.7855(4) 0.08668(15) 0.0433(9) Uani 1 1 d . . . O2 O -1.0301(4) 0.8672(4) 0.05430(16) 0.0539(11) Uani 1 1 d . . . O3 O -1.5360(4) 0.6810(3) 0.45691(14) 0.0426(8) Uani 1 1 d . . . O4 O -1.5542(4) 0.4734(3) 0.43143(14) 0.0392(8) Uani 1 1 d . . . O5 O -0.8921(6) 0.6085(6) 0.32444(18) 0.0834(16) Uani 1 1 d . . . O6 O -0.7419(5) 0.5519(5) 0.26239(19) 0.0718(14) Uani 1 1 d . . . O7 O -1.4038(6) 0.3696(5) 0.24632(19) 0.0714(13) Uani 1 1 d . . . O8 O -1.1748(5) 0.4413(4) 0.22641(16) 0.0566(11) Uani 1 1 d . . . O9 O -0.7781(5) 0.9649(5) 0.0025(2) 0.0688(15) Uani 1 1 d . . . N1 N -0.8612(6) 0.6069(5) 0.27685(19) 0.0506(12) Uani 1 1 d . . . N2 N -1.2914(6) 0.4462(4) 0.25286(18) 0.0430(10) Uani 1 1 d . . . N3 N -0.5135(5) 0.6765(4) 0.05465(17) 0.0358(9) Uani 1 1 d . . . N4 N -0.3040(5) 0.5434(4) 0.06331(19) 0.0442(11) Uani 1 1 d . . . C1 C -1.1329(6) 0.6988(4) 0.2411(2) 0.0341(10) Uani 1 1 d . . . C2 C -0.9710(6) 0.6727(5) 0.23363(19) 0.0357(11) Uani 1 1 d . . . C3 C -0.9053(5) 0.7073(5) 0.1853(2) 0.0350(11) Uani 1 1 d . . . H3 H -0.7977 0.6869 0.1811 0.080 Uiso 1 1 calc . . . C4 C -1.0010(5) 0.7728(4) 0.14300(19) 0.0305(10) Uani 1 1 d . . . C5 C -1.1617(5) 0.8021(5) 0.1502(2) 0.0353(11) Uani 1 1 d . . . H5 H -1.2265 0.8467 0.1224 0.080 Uiso 1 1 calc . . . C6 C -1.2258(6) 0.7651(5) 0.1987(2) 0.0391(11) Uani 1 1 d . . . H6 H -1.3335 0.7852 0.2028 0.080 Uiso 1 1 calc . . . C7 C -0.9315(6) 0.8133(5) 0.0906(2) 0.0350(11) Uani 1 1 d . . . C8 C -1.2146(6) 0.6622(5) 0.2910(2) 0.0367(11) Uani 1 1 d . . . C9 C -1.2979(6) 0.5471(5) 0.29524(19) 0.0345(10) Uani 1 1 d . . . C10 C -1.3906(6) 0.5222(5) 0.3387(2) 0.0365(11) Uani 1 1 d . . . H10 H -1.4429 0.4435 0.3405 0.080 Uiso 1 1 calc . . . C11 C -1.4054(6) 0.6140(5) 0.37938(19) 0.0349(10) Uani 1 1 d . . . C12 C -1.3257(7) 0.7309(5) 0.3754(2) 0.0473(13) Uani 1 1 d . . . H12 H -1.3351 0.7942 0.4021 0.080 Uiso 1 1 calc . . . C13 C -1.2329(7) 0.7539(5) 0.3320(2) 0.0494(14) Uani 1 1 d . . . H13 H -1.1813 0.8329 0.3302 0.080 Uiso 1 1 calc . . . C14 C -1.5062(5) 0.5858(5) 0.42627(19) 0.0353(11) Uani 1 1 d . . . C15 C -0.3724(6) 0.6483(5) 0.0370(2) 0.0446(13) Uani 1 1 d . . . H15 H -0.3258 0.6947 0.0098 0.080 Uiso 1 1 calc . . . C16 C -0.5344(6) 0.5870(5) 0.0952(2) 0.0430(12) Uani 1 1 d . . . H16 H -0.6230 0.5837 0.1158 0.080 Uiso 1 1 calc . . . C17 C -0.4068(6) 0.5043(5) 0.1008(2) 0.0466(13) Uani 1 1 d . . . H17 H -0.3921 0.4348 0.1252 0.080 Uiso 1 1 calc . . . C18 C -0.1463(7) 0.4847(6) 0.0558(3) 0.0588(16) Uani 1 1 d . . . H18A H -0.1587 0.3922 0.0539 0.080 Uiso 1 1 calc . . . H18B H -0.0682 0.5048 0.0880 0.080 Uiso 1 1 calc . . . C19 C -0.0818(6) 0.5315(6) 0.0033(3) 0.0502(14) Uani 1 1 d . . . H19A H -0.0686 0.6239 0.0050 0.080 Uiso 1 1 calc . . . H19B H -0.1594 0.5113 -0.0291 0.080 Uiso 1 1 calc . . . H1A H -0.766(9) 1.000(7) -0.026(3) 0.080 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 Cu1 0.0278(3) 0.0479(4) 0.0330(3) 0.0144(3) 0.0194(2) 0.0110(2) Cu2 0.0314(4) 0.0529(5) 0.0357(5) 0.0131(4) 0.0178(3) 0.0105(4) O1 0.0325(16) 0.060(2) 0.042(2) 0.0212(17) 0.0270(15) 0.0192(15) O2 0.0349(18) 0.081(3) 0.049(2) 0.039(2) 0.0208(16) 0.0139(18) O3 0.054(2) 0.045(2) 0.0341(18) -0.0082(16) 0.0285(16) -0.0066(16) O4 0.0415(18) 0.047(2) 0.0325(18) -0.0088(15) 0.0205(15) -0.0154(16) O5 0.085(3) 0.132(5) 0.036(2) 0.033(3) 0.018(2) 0.034(3) O6 0.051(2) 0.097(3) 0.071(3) 0.040(3) 0.022(2) 0.032(2) O7 0.076(3) 0.081(3) 0.063(3) -0.037(2) 0.030(2) -0.024(3) O8 0.075(3) 0.053(2) 0.051(2) -0.0064(19) 0.044(2) 0.003(2) O9 0.0358(19) 0.101(4) 0.075(3) 0.062(3) 0.033(2) 0.032(2) N1 0.048(3) 0.063(3) 0.043(3) 0.023(2) 0.016(2) 0.011(2) N2 0.055(3) 0.045(2) 0.032(2) -0.0034(19) 0.023(2) 0.001(2) N3 0.034(2) 0.041(2) 0.036(2) 0.0084(18) 0.0187(17) 0.0098(17) N4 0.037(2) 0.049(3) 0.049(3) 0.001(2) 0.0146(19) 0.017(2) C1 0.041(2) 0.036(2) 0.029(2) 0.0011(19) 0.022(2) 0.001(2) C2 0.038(2) 0.044(3) 0.028(2) 0.011(2) 0.0136(19) 0.007(2) C3 0.032(2) 0.041(3) 0.035(3) 0.008(2) 0.019(2) 0.007(2) C4 0.030(2) 0.036(2) 0.030(2) 0.008(2) 0.0178(18) 0.0043(19) C5 0.030(2) 0.044(3) 0.035(3) 0.010(2) 0.0163(19) 0.009(2) C6 0.033(2) 0.051(3) 0.037(3) 0.006(2) 0.022(2) 0.009(2) C7 0.034(2) 0.041(3) 0.034(3) 0.013(2) 0.019(2) 0.004(2) C8 0.041(2) 0.042(3) 0.031(2) 0.007(2) 0.023(2) 0.006(2) C9 0.040(2) 0.043(3) 0.025(2) -0.003(2) 0.0185(19) 0.002(2) C10 0.041(3) 0.039(3) 0.032(3) -0.003(2) 0.019(2) -0.004(2) C11 0.040(2) 0.042(3) 0.025(2) -0.001(2) 0.0165(19) -0.004(2) C12 0.068(4) 0.039(3) 0.041(3) -0.006(2) 0.034(3) -0.006(3) C13 0.067(3) 0.039(3) 0.049(3) -0.004(2) 0.034(3) -0.013(3) C14 0.033(2) 0.049(3) 0.026(2) -0.001(2) 0.0140(19) -0.005(2) C15 0.041(3) 0.051(3) 0.047(3) 0.007(3) 0.025(2) 0.013(2) C16 0.038(3) 0.047(3) 0.048(3) 0.012(2) 0.021(2) 0.007(2) C17 0.045(3) 0.051(3) 0.046(3) 0.012(3) 0.017(2) 0.009(2) C18 0.043(3) 0.069(4) 0.067(4) 0.002(3) 0.021(3) 0.029(3) C19 0.031(3) 0.061(3) 0.060(4) -0.014(3) 0.011(2) 0.014(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 Cu1 O9 1.869(4) . ? Cu1 N3 1.970(4) . ? Cu1 O1 1.990(3) . ? Cu1 O3 1.996(3) 4_675 ? Cu1 O4 2.395(4) 2_355 ? Cu2 O9 1.863(4) . ? Cu2 O9 1.863(4) 3_375 ? Cu2 O2 1.936(3) . ? Cu2 O2 1.936(3) 3_375 ? Cu2 H1A 2.10(8) . ? O1 C7 1.253(5) . ? O2 C7 1.254(6) . ? O3 C14 1.275(6) . ? O3 Cu1 1.996(3) 4_476 ? O4 C14 1.248(6) . ? O4 Cu1 2.395(4) 2_345 ? O5 N1 1.199(6) . ? O6 N1 1.224(6) . ? O7 N2 1.220(6) . ? O8 N2 1.215(5) . ? O9 H1A 0.79(8) . ? N1 C2 1.466(6) . ? N2 C9 1.468(6) . ? N3 C15 1.318(6) . ? N3 C16 1.373(6) . ? N4 C15 1.353(7) . ? N4 C17 1.368(6) . ? N4 C18 1.468(6) . ? C1 C6 1.385(7) . ? C1 C2 1.396(6) . ? C1 C8 1.491(6) . ? C2 C3 1.384(6) . ? C3 C4 1.390(7) . ? C3 H3 0.9300 . ? C4 C5 1.392(6) . ? C4 C7 1.501(6) . ? C5 C6 1.388(6) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C8 C9 1.392(7) . ? C8 C13 1.393(7) . ? C9 C10 1.388(6) . ? C10 C11 1.381(6) . ? C10 H10 0.9300 . ? C11 C12 1.394(7) . ? C11 C14 1.504(6) . ? C12 C13 1.382(7) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.356(7) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.504(9) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C19 1.527(9) 3_565 ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O9 Cu1 N3 177.45(15) . . ? O9 Cu1 O1 91.17(15) . . ? N3 Cu1 O1 86.28(14) . . ? O9 Cu1 O3 94.08(16) . 4_675 ? N3 Cu1 O3 88.34(15) . 4_675 ? O1 Cu1 O3 163.37(16) . 4_675 ? O9 Cu1 O4 88.74(18) . 2_355 ? N3 Cu1 O4 92.05(15) . 2_355 ? O1 Cu1 O4 105.10(14) . 2_355 ? O3 Cu1 O4 90.80(13) 4_675 2_355 ? O9 Cu2 O9 180.0(3) . 3_375 ? O9 Cu2 O2 92.34(15) . . ? O9 Cu2 O2 87.66(15) 3_375 . ? O9 Cu2 O2 87.66(15) . 3_375 ? O9 Cu2 O2 92.34(15) 3_375 3_375 ? O2 Cu2 O2 180.0(2) . 3_375 ? O9 Cu2 H1A 22(2) . . ? O9 Cu2 H1A 158(2) 3_375 . ? O2 Cu2 H1A 113(2) . . ? O2 Cu2 H1A 67(2) 3_375 . ? C7 O1 Cu1 130.5(3) . . ? C7 O2 Cu2 131.6(3) . . ? C14 O3 Cu1 126.5(3) . 4_476 ? C14 O4 Cu1 115.8(3) . 2_345 ? Cu2 O9 Cu1 134.3(2) . . ? Cu2 O9 H1A 96(5) . . ? Cu1 O9 H1A 120(6) . . ? O5 N1 O6 123.0(5) . . ? O5 N1 C2 119.0(5) . . ? O6 N1 C2 118.1(4) . . ? O8 N2 O7 122.9(4) . . ? O8 N2 C9 119.2(4) . . ? O7 N2 C9 118.0(4) . . ? C15 N3 C16 105.4(4) . . ? C15 N3 Cu1 122.8(3) . . ? C16 N3 Cu1 131.7(3) . . ? C15 N4 C17 106.9(4) . . ? C15 N4 C18 127.4(5) . . ? C17 N4 C18 125.7(5) . . ? C6 C1 C2 117.3(4) . . ? C6 C1 C8 117.0(4) . . ? C2 C1 C8 125.7(4) . . ? C3 C2 C1 122.1(4) . . ? C3 C2 N1 116.4(4) . . ? C1 C2 N1 121.5(4) . . ? C2 C3 C4 119.6(4) . . ? C2 C3 H3 120.2 . . ? C4 C3 H3 120.2 . . ? C3 C4 C5 119.1(4) . . ? C3 C4 C7 120.6(4) . . ? C5 C4 C7 120.3(4) . . ? C6 C5 C4 120.3(4) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? C1 C6 C5 121.5(4) . . ? C1 C6 H6 119.3 . . ? C5 C6 H6 119.3 . . ? O1 C7 O2 127.1(4) . . ? O1 C7 C4 117.5(4) . . ? O2 C7 C4 115.3(4) . . ? C9 C8 C13 116.4(4) . . ? C9 C8 C1 123.5(4) . . ? C13 C8 C1 119.2(4) . . ? C10 C9 C8 122.4(4) . . ? C10 C9 N2 117.0(4) . . ? C8 C9 N2 120.6(4) . . ? C11 C10 C9 120.2(4) . . ? C11 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C10 C11 C12 118.4(4) . . ? C10 C11 C14 119.7(4) . . ? C12 C11 C14 121.9(4) . . ? C13 C12 C11 120.7(5) . . ? C13 C12 H12 119.6 . . ? C11 C12 H12 119.6 . . ? C12 C13 C8 121.8(5) . . ? C12 C13 H13 119.1 . . ? C8 C13 H13 119.1 . . ? O4 C14 O3 126.0(4) . . ? O4 C14 C11 117.8(4) . . ? O3 C14 C11 116.1(4) . . ? N3 C15 N4 111.5(4) . . ? N3 C15 H15 124.3 . . ? N4 C15 H15 124.3 . . ? C17 C16 N3 110.0(4) . . ? C17 C16 H16 125.0 . . ? N3 C16 H16 125.0 . . ? C16 C17 N4 106.3(4) . . ? C16 C17 H17 126.9 . . ? N4 C17 H17 126.9 . . ? N4 C18 C19 111.9(5) . . ? N4 C18 H18A 109.2 . . ? C19 C18 H18A 109.2 . . ? N4 C18 H18B 109.2 . . ? C19 C18 H18B 109.2 . . ? H18A C18 H18B 107.9 . . ? C18 C19 C19 110.6(6) . 3_565 ? C18 C19 H19A 109.5 . . ? C19 C19 H19A 109.5 3_565 . ? C18 C19 H19B 109.5 . . ? C19 C19 H19B 109.5 3_565 . ? H19A C19 H19B 108.1 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O9 H1A O4 0.79(8) 2.15(8) 2.733(5) 132(7) 4_675 O9 H1A O2 0.79(8) 2.23(7) 2.631(5) 113(7) 3_375 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.845 _refine_diff_density_min -1.225 _refine_diff_density_rms 0.116 data_compound-5 _database_code_depnum_ccdc_archive 'CCDC 782712' #TrackingRef 'CCDC.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C38 H26 N8 O16 Zn2' _chemical_formula_sum 'C38 H26 N8 O16 Zn2' _chemical_formula_weight 981.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 19.237(4) _cell_length_b 7.5997(15) _cell_length_c 26.035(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3806.3(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4322 _cell_measurement_theta_min 2.99 _cell_measurement_theta_max 27.42 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.713 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1992 _exptl_absorpt_coefficient_mu 1.350 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method omega-scan _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 32272 _diffrn_reflns_av_R_equivalents 0.0974 _diffrn_reflns_av_sigmaI/netI 0.0571 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 27.42 _reflns_number_total 4322 _reflns_number_gt 3221 _reflns_threshold_expression >2sigma(I) _computing_data_collection Process-auto _computing_cell_refinement Process-auto _computing_data_reduction Process-auto _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^)+(0.0313P)^2^+8.7294P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4322 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0715 _refine_ls_R_factor_gt 0.0476 _refine_ls_wR_factor_ref 0.1019 _refine_ls_wR_factor_gt 0.0941 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.197420(19) 0.78752(5) 1.020060(13) 0.01220(11) Uani 1 1 d . . . O1 O 0.17458(12) 0.6346(3) 0.96139(8) 0.0151(5) Uani 1 1 d . . . O2 O 0.27779(12) 0.4978(3) 0.96414(8) 0.0157(5) Uani 1 1 d . . . O3 O 0.21156(11) 0.1695(3) 0.55344(8) 0.0162(5) Uani 1 1 d . . . O4 O 0.17359(13) -0.0992(3) 0.57640(8) 0.0188(5) Uani 1 1 d . . . O5 O 0.00369(15) 0.4524(6) 0.83706(11) 0.0679(13) Uani 1 1 d . . . O6 O 0.03651(13) 0.3873(4) 0.76082(9) 0.0323(7) Uani 1 1 d . . . O7 O 0.12056(13) -0.2188(3) 0.75416(9) 0.0218(5) Uani 1 1 d . . . O8 O 0.09784(13) -0.0057(3) 0.80688(8) 0.0237(6) Uani 1 1 d . . . N1 N 0.04855(15) 0.4131(4) 0.80584(11) 0.0270(7) Uani 1 1 d . . . N2 N 0.11905(14) -0.0619(4) 0.76545(10) 0.0165(6) Uani 1 1 d . . . N3 N 0.11506(14) 0.9286(4) 1.04429(10) 0.0154(6) Uani 1 1 d . . . N4 N 0.03943(14) 1.1437(4) 1.05441(10) 0.0177(6) Uani 1 1 d . . . C1 C 0.16936(17) 0.3021(4) 0.79594(11) 0.0140(7) Uani 1 1 d . . . C2 C 0.11994(17) 0.3907(5) 0.82528(12) 0.0168(7) Uani 1 1 d . . . C3 C 0.13492(17) 0.4590(4) 0.87344(12) 0.0165(7) Uani 1 1 d . . . H3 H 0.1007 0.5169 0.8921 0.080 Uiso 1 1 calc . . . C4 C 0.20141(17) 0.4402(4) 0.89363(11) 0.0130(6) Uani 1 1 d . . . C5 C 0.25119(17) 0.3488(4) 0.86576(11) 0.0135(6) Uani 1 1 d . . . H5 H 0.2956 0.3338 0.8792 0.080 Uiso 1 1 calc . . . C6 C 0.23501(17) 0.2794(4) 0.81770(11) 0.0152(7) Uani 1 1 d . . . H6 H 0.2687 0.2166 0.7998 0.080 Uiso 1 1 calc . . . C7 C 0.22017(17) 0.5284(4) 0.94397(11) 0.0137(7) Uani 1 1 d . . . C8 C 0.16029(16) 0.2390(4) 0.74157(11) 0.0142(7) Uani 1 1 d . . . C9 C 0.14421(16) 0.0669(4) 0.72713(11) 0.0136(7) Uani 1 1 d . . . C10 C 0.15112(16) 0.0086(4) 0.67696(12) 0.0140(7) Uani 1 1 d . . . H10 H 0.1413 -0.1078 0.6687 0.080 Uiso 1 1 calc . . . C11 C 0.17283(16) 0.1248(4) 0.63914(11) 0.0132(7) Uani 1 1 d . . . C12 C 0.18528(16) 0.3001(4) 0.65181(12) 0.0165(7) Uani 1 1 d . . . H12 H 0.1972 0.3803 0.6263 0.080 Uiso 1 1 calc . . . C13 C 0.17990(17) 0.3553(4) 0.70270(12) 0.0174(7) Uani 1 1 d . . . H13 H 0.1896 0.4719 0.7109 0.080 Uiso 1 1 calc . . . C14 C 0.18680(16) 0.0586(4) 0.58510(11) 0.0126(7) Uani 1 1 d . . . C15 C 0.09355(17) 1.0830(4) 1.02661(12) 0.0167(7) Uani 1 1 d . . . H15 H 0.1132 1.1416 0.9988 0.080 Uiso 1 1 calc . . . C16 C 0.07181(19) 0.8894(4) 1.08573(13) 0.0206(8) Uani 1 1 d . . . H16 H 0.0744 0.7884 1.1058 0.080 Uiso 1 1 calc . . . C17 C 0.02561(19) 1.0215(5) 1.09217(13) 0.0233(8) Uani 1 1 d . . . H17 H -0.0088 1.0285 1.1172 0.080 Uiso 1 1 calc . . . C18 C 0.00261(18) 1.3121(4) 1.04893(13) 0.0211(8) Uani 1 1 d . . . H18A H 0.0120 1.3836 1.0790 0.080 Uiso 1 1 calc . . . H18B H -0.0470 1.2891 1.0481 0.080 Uiso 1 1 calc . . . C19 C 0.02215(18) 1.4157(5) 1.00162(13) 0.0212(8) Uani 1 1 d . . . H19A H 0.0146 1.3444 0.9712 0.080 Uiso 1 1 calc . . . H19B H 0.0710 1.4466 1.0030 0.080 Uiso 1 1 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.01480(19) 0.01280(19) 0.00900(17) -0.00116(15) 0.00005(15) 0.00061(16) O1 0.0167(12) 0.0160(12) 0.0126(10) -0.0016(10) -0.0005(9) -0.0002(10) O2 0.0167(12) 0.0206(12) 0.0097(10) 0.0008(10) -0.0019(9) -0.0004(10) O3 0.0172(13) 0.0188(12) 0.0125(10) 0.0005(10) 0.0030(9) 0.0014(9) O4 0.0284(14) 0.0146(12) 0.0133(11) -0.0040(10) 0.0036(10) -0.0008(10) O5 0.0159(16) 0.152(4) 0.0355(17) -0.045(2) -0.0041(13) 0.019(2) O6 0.0191(14) 0.0573(19) 0.0205(13) -0.0142(13) -0.0080(10) 0.0068(13) O7 0.0260(14) 0.0161(12) 0.0232(12) 0.0024(11) -0.0011(10) -0.0003(11) O8 0.0300(14) 0.0308(14) 0.0103(11) -0.0016(10) 0.0057(10) -0.0096(12) N1 0.0156(16) 0.046(2) 0.0193(15) -0.0138(15) -0.0017(12) 0.0015(14) N2 0.0161(15) 0.0223(16) 0.0111(13) 0.0022(12) -0.0028(11) -0.0039(12) N3 0.0164(14) 0.0165(14) 0.0134(13) 0.0001(12) 0.0046(11) 0.0004(12) N4 0.0146(15) 0.0188(14) 0.0196(14) -0.0019(12) 0.0021(11) 0.0034(12) C1 0.0161(16) 0.0144(16) 0.0116(14) 0.0002(13) 0.0008(12) -0.0053(13) C2 0.0115(17) 0.0257(19) 0.0132(15) -0.0024(14) -0.0006(13) -0.0019(14) C3 0.0155(17) 0.0206(17) 0.0134(15) -0.0031(14) 0.0024(13) 0.0023(14) C4 0.0146(16) 0.0134(15) 0.0108(14) 0.0028(13) -0.0005(12) -0.0015(13) C5 0.0142(16) 0.0126(15) 0.0137(14) 0.0043(13) 0.0001(13) 0.0002(13) C6 0.0169(17) 0.0162(16) 0.0125(14) 0.0012(14) 0.0037(12) 0.0034(14) C7 0.0159(16) 0.0144(16) 0.0109(14) 0.0037(13) 0.0036(13) -0.0029(13) C8 0.0107(15) 0.0203(17) 0.0116(15) -0.0031(14) -0.0001(12) 0.0000(13) C9 0.0124(16) 0.0179(17) 0.0105(14) 0.0041(13) -0.0003(12) -0.0011(13) C10 0.0132(16) 0.0171(17) 0.0117(14) -0.0027(14) -0.0024(12) 0.0011(13) C11 0.0104(15) 0.0177(17) 0.0115(14) -0.0024(13) -0.0005(12) 0.0011(13) C12 0.0148(17) 0.0205(18) 0.0142(15) 0.0015(14) 0.0018(12) -0.0016(14) C13 0.0194(18) 0.0179(17) 0.0150(15) -0.0050(14) 0.0016(13) -0.0014(14) C14 0.0103(16) 0.0174(17) 0.0100(14) -0.0003(13) -0.0013(12) 0.0052(13) C15 0.0154(16) 0.0187(17) 0.0162(16) -0.0035(14) 0.0017(13) -0.0004(13) C16 0.0219(19) 0.0191(18) 0.0207(17) -0.0005(15) 0.0049(14) 0.0014(14) C17 0.024(2) 0.0271(19) 0.0190(17) 0.0016(16) 0.0073(14) -0.0005(16) C18 0.0189(18) 0.0201(18) 0.0243(18) -0.0030(15) 0.0030(14) 0.0062(14) C19 0.0190(19) 0.0189(18) 0.0258(18) -0.0012(16) 0.0017(14) 0.0032(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 Zn1 O1 1.969(2) . ? Zn1 O3 1.982(2) 2_565 ? Zn1 N3 2.014(3) . ? Zn1 O4 2.100(2) 7_566 ? Zn1 O2 2.214(2) 8_665 ? O1 C7 1.275(4) . ? O2 C7 1.248(4) . ? O2 Zn1 2.214(2) 8_655 ? O3 C14 1.272(4) . ? O3 Zn1 1.982(2) 2_564 ? O4 C14 1.246(4) . ? O4 Zn1 2.100(2) 7_565 ? O5 N1 1.223(4) . ? O6 N1 1.211(3) . ? O7 N2 1.229(3) . ? O8 N2 1.230(3) . ? N1 C2 1.474(4) . ? N2 C9 1.479(4) . ? N3 C15 1.327(4) . ? N3 C16 1.394(4) . ? N4 C15 1.349(4) . ? N4 C17 1.379(4) . ? N4 C18 1.469(4) . ? C1 C2 1.393(4) . ? C1 C6 1.395(4) . ? C1 C8 1.505(4) . ? C2 C3 1.387(4) . ? C3 C4 1.390(4) . ? C3 H3 0.9300 . ? C4 C5 1.388(4) . ? C4 C7 1.515(4) . ? C5 C6 1.393(4) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C8 C9 1.396(5) . ? C8 C13 1.396(5) . ? C9 C10 1.386(4) . ? C10 C11 1.386(4) . ? C10 H10 0.9300 . ? C11 C12 1.393(5) . ? C11 C14 1.518(4) . ? C12 C13 1.394(4) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.351(5) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.509(5) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C19 1.541(7) 5_587 ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn1 O3 129.39(9) . 2_565 ? O1 Zn1 N3 112.43(10) . . ? O3 Zn1 N3 118.03(10) 2_565 . ? O1 Zn1 O4 95.21(9) . 7_566 ? O3 Zn1 O4 89.94(9) 2_565 7_566 ? N3 Zn1 O4 88.41(10) . 7_566 ? O1 Zn1 O2 87.94(9) . 8_665 ? O3 Zn1 O2 88.80(9) 2_565 8_665 ? N3 Zn1 O2 89.50(10) . 8_665 ? O4 Zn1 O2 176.70(8) 7_566 8_665 ? C7 O1 Zn1 119.7(2) . . ? C7 O2 Zn1 127.0(2) . 8_655 ? C14 O3 Zn1 136.4(2) . 2_564 ? C14 O4 Zn1 137.6(2) . 7_565 ? O6 N1 O5 123.2(3) . . ? O6 N1 C2 119.5(3) . . ? O5 N1 C2 117.2(3) . . ? O7 N2 O8 123.7(3) . . ? O7 N2 C9 118.3(3) . . ? O8 N2 C9 118.1(3) . . ? C15 N3 C16 105.7(3) . . ? C15 N3 Zn1 127.4(2) . . ? C16 N3 Zn1 126.7(2) . . ? C15 N4 C17 107.5(3) . . ? C15 N4 C18 128.1(3) . . ? C17 N4 C18 124.3(3) . . ? C2 C1 C6 117.1(3) . . ? C2 C1 C8 126.2(3) . . ? C6 C1 C8 116.6(3) . . ? C3 C2 C1 122.3(3) . . ? C3 C2 N1 117.5(3) . . ? C1 C2 N1 120.2(3) . . ? C2 C3 C4 119.6(3) . . ? C2 C3 H3 120.2 . . ? C4 C3 H3 120.2 . . ? C5 C4 C3 119.2(3) . . ? C5 C4 C7 120.6(3) . . ? C3 C4 C7 120.1(3) . . ? C4 C5 C6 120.3(3) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C5 C6 C1 121.3(3) . . ? C5 C6 H6 119.3 . . ? C1 C6 H6 119.3 . . ? O2 C7 O1 125.3(3) . . ? O2 C7 C4 119.5(3) . . ? O1 C7 C4 115.1(3) . . ? C9 C8 C13 117.3(3) . . ? C9 C8 C1 125.3(3) . . ? C13 C8 C1 116.7(3) . . ? C10 C9 C8 122.1(3) . . ? C10 C9 N2 117.1(3) . . ? C8 C9 N2 120.7(3) . . ? C9 C10 C11 119.7(3) . . ? C9 C10 H10 120.2 . . ? C11 C10 H10 120.2 . . ? C10 C11 C12 119.5(3) . . ? C10 C11 C14 120.0(3) . . ? C12 C11 C14 120.4(3) . . ? C11 C12 C13 120.0(3) . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? C12 C13 C8 121.2(3) . . ? C12 C13 H13 119.4 . . ? C8 C13 H13 119.4 . . ? O4 C14 O3 126.6(3) . . ? O4 C14 C11 116.8(3) . . ? O3 C14 C11 116.6(3) . . ? N3 C15 N4 110.9(3) . . ? N3 C15 H15 124.5 . . ? N4 C15 H15 124.5 . . ? C17 C16 N3 109.3(3) . . ? C17 C16 H16 125.4 . . ? N3 C16 H16 125.4 . . ? C16 C17 N4 106.6(3) . . ? C16 C17 H17 126.7 . . ? N4 C17 H17 126.7 . . ? N4 C18 C19 114.4(3) . . ? N4 C18 H18A 108.7 . . ? C19 C18 H18A 108.7 . . ? N4 C18 H18B 108.7 . . ? C19 C18 H18B 108.7 . . ? H18A C18 H18B 107.6 . . ? C18 C19 C19 109.9(3) . 5_587 ? C18 C19 H19A 109.7 . . ? C19 C19 H19A 109.7 5_587 . ? C18 C19 H19B 109.7 . . ? C19 C19 H19B 109.7 5_587 . ? H19A C19 H19B 108.2 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.42 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.624 _refine_diff_density_min -0.490 _refine_diff_density_rms 0.099 data_compound-6 _database_code_depnum_ccdc_archive 'CCDC 782713' #TrackingRef 'CCDC.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C38 H28 Cd2 N8 O17' _chemical_formula_sum 'C38 H28 Cd2 N8 O17' _chemical_formula_weight 1093.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.7464(5) _cell_length_b 10.6554(8) _cell_length_c 25.6955(19) _cell_angle_alpha 88.419(4) _cell_angle_beta 88.034(4) _cell_angle_gamma 77.623(4) _cell_volume 2070.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7211 _cell_measurement_theta_min 1.59 _cell_measurement_theta_max 25.04 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.754 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1088 _exptl_absorpt_coefficient_mu 1.113 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.792 _exptl_absorpt_correction_T_max 0.818 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 9.00cm _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 11689 _diffrn_reflns_av_R_equivalents 0.0776 _diffrn_reflns_av_sigmaI/netI 0.1780 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 25.04 _reflns_number_total 7211 _reflns_number_gt 3657 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXP-97 _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0624P)^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 7211 _refine_ls_number_parameters 547 _refine_ls_number_restraints 71 _refine_ls_R_factor_all 0.1393 _refine_ls_R_factor_gt 0.0649 _refine_ls_wR_factor_ref 0.1642 _refine_ls_wR_factor_gt 0.1370 _refine_ls_goodness_of_fit_ref 0.912 _refine_ls_restrained_S_all 0.907 _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 Cd1 Cd 0.26046(9) 0.47394(7) 0.49520(3) 0.0327(2) Uani 1 1 d . . . Cd2 Cd 0.82559(9) 0.93700(7) 0.03731(3) 0.0290(2) Uani 1 1 d D . . O1 O -0.0058(9) 0.4972(8) 0.4417(3) 0.0449(19) Uani 1 1 d . . . O2 O -0.1958(10) 0.6835(8) 0.4485(3) 0.052(2) Uani 1 1 d . . . O3 O 0.5680(8) 0.8465(7) 0.0699(3) 0.0454(19) Uani 1 1 d . . . O4 O 0.7114(9) 0.9526(7) 0.1206(3) 0.049(2) Uani 1 1 d . . . O5 O 0.0007(13) 1.0430(10) 0.3544(4) 0.0920(12) Uani 1 1 d U . . O6 O 0.0528(13) 1.0091(10) 0.2727(4) 0.0920(12) Uani 1 1 d U . . O7 O 0.4558(13) 0.8368(10) 0.3411(4) 0.0920(12) Uani 1 1 d U . . O8 O 0.5998(13) 0.9590(10) 0.3051(4) 0.0920(12) Uani 1 1 d U . . O9 O 0.4688(9) 0.4803(7) 0.5632(3) 0.0438(19) Uani 1 1 d . . . O10 O 0.5955(9) 0.6469(8) 0.5693(3) 0.049(2) Uani 1 1 d . . . O11 O -0.0325(8) 0.9335(6) 0.9576(2) 0.0321(16) Uani 1 1 d . . . O12 O -0.2727(9) 0.8639(7) 0.9399(3) 0.048(2) Uani 1 1 d . . . O13 O 0.2132(13) 0.3322(11) 0.7248(4) 0.0920(12) Uani 1 1 d U . . O14 O 0.0996(13) 0.4623(10) 0.7820(4) 0.0920(12) Uani 1 1 d U . . O15 O 0.493(2) 0.5757(16) 0.8050(6) 0.0920(12) Uani 0.65 1 d PU . . O16 O 0.505(2) 0.6961(15) 0.8698(7) 0.0920(12) Uani 0.65 1 d PU . . O17 O 0.6179(8) 1.1261(6) 0.0189(3) 0.0338(16) Uani 1 1 d D . . N1 N 0.0421(15) 0.9691(11) 0.3182(4) 0.072(3) Uani 1 1 d . . . N2 N 0.4933(14) 0.8925(11) 0.3021(4) 0.063(3) Uani 1 1 d . . . N3 N 0.1843(13) 0.4403(11) 0.7416(4) 0.062(3) Uani 1 1 d . . . N4 N 0.422(2) 0.6649(17) 0.8360(7) 0.070(5) Uani 0.65 1 d P . . N5 N 0.2172(11) 0.6902(8) 0.4963(3) 0.037(2) Uani 1 1 d . . . N6 N 0.2513(13) 0.8877(9) 0.4828(4) 0.051(3) Uani 1 1 d . A . N7 N 0.9997(10) 0.7403(8) 0.0548(3) 0.039(2) Uani 1 1 d . . . N8 N 1.1684(11) 0.5483(9) 0.0404(4) 0.051(3) Uani 1 1 d . . . C1 C 0.1975(13) 0.7509(11) 0.2949(4) 0.041(3) Uani 1 1 d . . . C2 C 0.0748(13) 0.8331(10) 0.3261(4) 0.040(3) Uani 1 1 d . . . C3 C -0.0128(12) 0.7903(11) 0.3687(4) 0.040(3) Uani 1 1 d . . . H3 H -0.0919 0.8480 0.3892 0.080 Uiso 1 1 calc . . . C4 C 0.0202(13) 0.6595(11) 0.3800(4) 0.038(3) Uani 1 1 d . . . C5 C 0.1394(13) 0.5784(10) 0.3493(4) 0.037(3) Uani 1 1 d . . . H5 H 0.1635 0.4910 0.3575 0.080 Uiso 1 1 calc . . . C6 C 0.2267(13) 0.6210(10) 0.3058(4) 0.038(3) Uani 1 1 d . . . H6 H 0.3028 0.5627 0.2848 0.080 Uiso 1 1 calc . . . C7 C -0.0683(14) 0.6126(13) 0.4271(4) 0.042(3) Uani 1 1 d . . . C8 C 0.3001(13) 0.7957(11) 0.2500(4) 0.042(3) Uani 1 1 d . . . C9 C 0.4374(14) 0.8591(11) 0.2530(4) 0.041(3) Uani 1 1 d . . . C10 C 0.5290(13) 0.8936(9) 0.2091(4) 0.035(3) Uani 1 1 d . . . H10 H 0.6182 0.9385 0.2128 0.080 Uiso 1 1 calc . . . C11 C 0.4878(13) 0.8616(10) 0.1606(4) 0.042(3) Uani 1 1 d . . . C12 C 0.3501(16) 0.7957(13) 0.1563(4) 0.056(3) Uani 1 1 d . . . H12 H 0.3196 0.7738 0.1236 0.080 Uiso 1 1 calc . . . C13 C 0.2602(15) 0.7632(12) 0.1999(4) 0.054(3) Uani 1 1 d . . . H13 H 0.1706 0.7187 0.1961 0.080 Uiso 1 1 calc . . . C14 C 0.5943(14) 0.8895(10) 0.1130(4) 0.038(3) Uani 1 1 d U . . C15 C 0.2238(13) 0.6651(10) 0.7353(4) 0.036(3) Uani 1 1 d . . . C16 C 0.2397(13) 0.5450(9) 0.7131(4) 0.033(2) Uani 1 1 d . . . C17 C 0.3250(12) 0.5173(9) 0.6652(4) 0.030(2) Uani 1 1 d . . . H17 H 0.3328 0.4364 0.6514 0.080 Uiso 1 1 calc . . . C18 C 0.3987(12) 0.6067(10) 0.6374(4) 0.036(3) Uani 1 1 d . . . C19 C 0.3877(14) 0.7250(11) 0.6603(4) 0.045(3) Uani 1 1 d . . . H19 H 0.4421 0.7856 0.6437 0.080 Uiso 1 1 calc . . . C20 C 0.2974(14) 0.7539(10) 0.7070(4) 0.044(3) Uani 1 1 d . . . H20 H 0.2855 0.8360 0.7201 0.080 Uiso 1 1 calc . . . C21 C 0.4897(14) 0.5758(12) 0.5861(4) 0.039(3) Uani 1 1 d . . . C22 C 0.1294(15) 0.7094(9) 0.7860(4) 0.038(3) Uani 1 1 d . . . C23 C 0.2276(12) 0.7271(11) 0.8285(4) 0.043(3) Uani 1 1 d . . . C24 C 0.1488(13) 0.7854(11) 0.8737(4) 0.045(3) Uani 1 1 d . . . H24 H 0.2181 0.7987 0.9010 0.080 Uiso 1 1 calc . . . C25 C -0.0341(11) 0.8237(9) 0.8777(4) 0.026(2) Uani 1 1 d . . . C26 C -0.1300(12) 0.8013(11) 0.8374(4) 0.041(3) Uani 1 1 d . . . H26 H -0.2527 0.8234 0.8403 0.080 Uiso 1 1 calc . . . C27 C -0.0514(14) 0.7464(10) 0.7918(4) 0.040(3) Uani 1 1 d . . . H27 H -0.1222 0.7343 0.7647 0.080 Uiso 1 1 calc . . . C28 C -0.1194(12) 0.8802(9) 0.9281(4) 0.027(2) Uani 1 1 d . . . C29 C 0.2923(15) 0.7659(12) 0.4660(4) 0.046(3) Uani 1 1 d . . . H29 H 0.3642 0.7389 0.4370 0.080 Uiso 1 1 calc . . . C30 C 0.1274(15) 0.7672(12) 0.5356(4) 0.052(3) Uani 1 1 d . . . H30 H 0.0632 0.7394 0.5631 0.080 Uiso 1 1 calc . . . C31 C 0.1482(17) 0.8892(10) 0.5274(5) 0.059(3) Uani 1 1 d . . . H31 H 0.1020 0.9598 0.5479 0.080 Uiso 1 1 calc . . . C32 C 0.310(2) 0.9971(12) 0.4586(5) 0.071(4) Uani 1 1 d . . . C33 C 0.520(4) 0.970(3) 0.4621(14) 0.0920(12) Uani 0.50 1 d PU A 1 C33' C 0.444(4) 1.025(3) 0.4800(15) 0.0920(12) Uani 0.50 1 d PU . 2 C34 C 1.1100(15) 0.6678(11) 0.0213(4) 0.046(3) Uani 1 1 d . . . H34 H 1.1426 0.6963 -0.0113 0.080 Uiso 1 1 calc . . . C35 C 0.9873(16) 0.6607(13) 0.0972(5) 0.058(3) Uani 1 1 d . . . H35 H 0.9179 0.6824 0.1272 0.080 Uiso 1 1 calc . . . C36 C 1.0944(19) 0.5445(13) 0.0874(6) 0.072(4) Uani 1 1 d . . . H36 H 1.1126 0.4736 0.1101 0.080 Uiso 1 1 calc . . . C37 C 1.2880(16) 0.4401(13) 0.0142(6) 0.077(4) Uani 1 1 d . . . H37A H 1.3333 0.3746 0.0402 0.080 Uiso 1 1 calc . . . H37B H 1.2199 0.4026 -0.0097 0.080 Uiso 1 1 calc . . . C38 C 1.4378(17) 0.4748(12) -0.0147(7) 0.093(6) Uani 1 1 d . . . H38A H 1.5022 0.3990 -0.0324 0.080 Uiso 1 1 calc . . . H38B H 1.3912 0.5381 -0.0413 0.080 Uiso 1 1 calc . . . H1A H 0.526(5) 1.111(5) 0.045(2) 0.080 Uiso 1 1 d D . . H1B H 0.585(9) 1.102(4) -0.0156(15) 0.080 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 0.0345(5) 0.0406(5) 0.0245(4) 0.0002(4) 0.0106(4) -0.0135(4) Cd2 0.0291(4) 0.0321(5) 0.0252(4) 0.0004(3) 0.0108(3) -0.0072(4) O1 0.049(5) 0.065(6) 0.028(4) 0.013(4) 0.003(4) -0.032(4) O2 0.046(5) 0.072(6) 0.038(5) 0.003(4) 0.026(4) -0.014(4) O3 0.040(4) 0.066(5) 0.027(4) 0.000(4) 0.012(3) -0.007(4) O4 0.051(5) 0.068(5) 0.033(4) 0.001(4) 0.020(4) -0.029(4) O5 0.0923(12) 0.0918(12) 0.0917(12) -0.0018(3) -0.0021(3) -0.0198(4) O6 0.0923(12) 0.0918(12) 0.0917(12) -0.0018(3) -0.0021(3) -0.0198(4) O7 0.0923(12) 0.0918(12) 0.0917(12) -0.0018(3) -0.0021(3) -0.0198(4) O8 0.0923(12) 0.0918(12) 0.0917(12) -0.0018(3) -0.0021(3) -0.0198(4) O9 0.052(5) 0.058(5) 0.018(4) -0.010(4) 0.010(3) -0.004(4) O10 0.049(5) 0.069(5) 0.031(4) 0.000(4) 0.016(4) -0.019(4) O11 0.030(4) 0.050(5) 0.021(4) -0.019(3) 0.005(3) -0.019(3) O12 0.029(4) 0.068(5) 0.049(5) -0.019(4) 0.015(4) -0.015(4) O13 0.0923(12) 0.0918(12) 0.0917(12) -0.0018(3) -0.0021(3) -0.0198(4) O14 0.0923(12) 0.0918(12) 0.0917(12) -0.0018(3) -0.0021(3) -0.0198(4) O15 0.0923(12) 0.0918(12) 0.0917(12) -0.0018(3) -0.0021(3) -0.0198(4) O16 0.0923(12) 0.0918(12) 0.0917(12) -0.0018(3) -0.0021(3) -0.0198(4) O17 0.029(4) 0.041(4) 0.028(4) -0.003(3) 0.003(3) 0.000(3) N1 0.097(9) 0.078(8) 0.037(6) 0.020(6) 0.030(6) -0.015(7) N2 0.079(7) 0.100(9) 0.031(6) 0.008(6) 0.001(5) -0.067(7) N3 0.077(7) 0.087(8) 0.020(5) -0.012(5) 0.034(5) -0.014(6) N4 0.057(10) 0.096(14) 0.057(11) -0.046(10) 0.017(9) -0.017(10) N5 0.038(5) 0.043(5) 0.034(5) -0.004(4) 0.006(4) -0.018(4) N6 0.069(7) 0.041(6) 0.047(6) 0.002(5) -0.005(5) -0.021(5) N7 0.034(5) 0.037(5) 0.043(6) -0.002(5) 0.001(4) -0.004(4) N8 0.039(6) 0.041(6) 0.067(7) 0.004(5) 0.011(5) -0.001(5) C1 0.029(6) 0.064(8) 0.029(6) 0.010(6) 0.007(5) -0.012(6) C2 0.038(6) 0.039(7) 0.042(7) 0.007(5) 0.013(5) -0.010(5) C3 0.031(6) 0.061(8) 0.027(6) -0.005(5) 0.015(5) -0.010(6) C4 0.036(6) 0.045(7) 0.032(6) 0.000(5) 0.005(5) -0.010(5) C5 0.044(6) 0.044(7) 0.025(6) 0.005(5) 0.004(5) -0.017(6) C6 0.043(6) 0.043(7) 0.031(6) 0.007(5) 0.008(5) -0.017(5) C7 0.037(7) 0.064(9) 0.031(7) 0.007(6) 0.003(6) -0.026(6) C8 0.037(6) 0.071(8) 0.022(6) 0.007(6) 0.004(5) -0.023(6) C9 0.048(7) 0.057(8) 0.021(6) 0.003(5) 0.010(5) -0.024(6) C10 0.052(7) 0.028(6) 0.032(6) -0.003(5) 0.001(5) -0.020(5) C11 0.028(6) 0.044(7) 0.049(8) 0.013(6) 0.021(5) -0.004(5) C12 0.067(8) 0.092(10) 0.015(6) 0.001(6) 0.005(6) -0.036(8) C13 0.054(7) 0.083(9) 0.037(7) 0.005(7) 0.010(6) -0.041(7) C14 0.038(3) 0.038(3) 0.038(3) -0.0004(10) 0.0000(10) -0.0079(11) C15 0.037(6) 0.043(7) 0.032(6) -0.014(5) 0.010(5) -0.017(5) C16 0.046(6) 0.035(6) 0.019(5) -0.004(5) 0.007(5) -0.014(5) C17 0.032(5) 0.033(6) 0.023(5) -0.008(5) 0.004(5) -0.004(5) C18 0.029(6) 0.048(7) 0.028(6) 0.009(5) 0.005(5) -0.008(5) C19 0.047(7) 0.062(8) 0.030(6) -0.012(6) 0.018(5) -0.023(6) C20 0.052(7) 0.051(7) 0.031(6) -0.014(5) 0.014(6) -0.014(6) C21 0.041(7) 0.051(7) 0.022(6) 0.001(6) 0.003(5) -0.001(6) C22 0.063(7) 0.034(6) 0.021(6) -0.013(5) 0.011(5) -0.020(6) C23 0.022(5) 0.069(8) 0.038(7) -0.027(6) 0.015(5) -0.011(5) C24 0.040(6) 0.068(8) 0.029(6) -0.024(6) 0.014(5) -0.013(6) C25 0.020(5) 0.034(6) 0.026(6) -0.002(5) 0.004(4) -0.010(4) C26 0.024(5) 0.057(8) 0.042(7) 0.006(6) 0.002(5) -0.012(5) C27 0.038(6) 0.053(7) 0.030(6) -0.004(5) -0.004(5) -0.014(6) C28 0.027(5) 0.023(5) 0.029(6) 0.007(5) 0.008(5) -0.001(5) C29 0.058(7) 0.057(8) 0.026(6) -0.005(6) 0.002(6) -0.017(7) C30 0.047(7) 0.064(9) 0.044(7) 0.000(6) 0.021(6) -0.013(7) C31 0.089(9) 0.028(7) 0.052(8) -0.005(6) 0.026(7) 0.002(6) C32 0.106(11) 0.062(9) 0.054(9) 0.022(7) 0.008(8) -0.041(9) C33 0.0923(12) 0.0918(12) 0.0917(12) -0.0018(3) -0.0021(3) -0.0198(4) C33' 0.0923(12) 0.0918(12) 0.0917(12) -0.0018(3) -0.0021(3) -0.0198(4) C34 0.047(7) 0.039(7) 0.049(8) 0.011(6) 0.003(6) -0.001(6) C35 0.054(8) 0.058(9) 0.058(9) 0.023(7) 0.006(7) -0.010(7) C36 0.081(10) 0.056(9) 0.072(11) 0.034(8) -0.020(9) -0.003(8) C37 0.035(7) 0.058(9) 0.136(14) -0.018(9) 0.005(8) -0.003(7) C38 0.054(9) 0.048(9) 0.177(18) -0.036(10) 0.013(10) -0.011(7) _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 O10 2.242(7) 2_666 ? Cd1 N5 2.257(8) . ? Cd1 O2 2.310(7) 2_566 ? Cd1 O9 2.430(7) . ? Cd1 O1 2.482(7) . ? Cd1 O1 2.482(7) 2_566 ? Cd1 C7 2.708(11) 2_566 ? Cd2 N7 2.278(8) . ? Cd2 O4 2.283(7) . ? Cd2 O11 2.289(6) 1_654 ? Cd2 O11 2.338(6) 2_676 ? Cd2 O17 2.341(6) . ? Cd2 O3 2.506(7) . ? Cd2 C14 2.710(11) . ? O1 C7 1.273(12) . ? O1 Cd1 2.482(7) 2_566 ? O2 C7 1.230(13) . ? O2 Cd1 2.310(7) 2_566 ? O3 C14 1.250(12) . ? O4 C14 1.263(12) . ? O5 N1 1.225(13) . ? O6 N1 1.239(12) . ? O7 N2 1.210(12) . ? O8 N2 1.203(12) . ? O9 C21 1.233(12) . ? O10 C21 1.286(12) . ? O10 Cd1 2.242(7) 2_666 ? O11 C28 1.253(11) . ? O11 Cd2 2.289(6) 1_456 ? O11 Cd2 2.338(6) 2_676 ? O12 C28 1.262(11) . ? O13 N3 1.212(13) . ? O14 N3 1.212(12) . ? O15 N4 1.28(2) . ? O16 N4 1.196(18) . ? O17 H1A 0.99(2) . ? O17 H1B 0.98(2) . ? N1 C2 1.427(14) . ? N2 C9 1.425(13) . ? N3 C16 1.450(13) . ? N4 C23 1.524(18) . ? N5 C29 1.315(13) . ? N5 C30 1.388(13) . ? N6 C29 1.348(14) . ? N6 C31 1.374(14) . ? N6 C32 1.455(14) . ? N7 C34 1.331(13) . ? N7 C35 1.375(13) . ? N8 C36 1.321(16) . ? N8 C34 1.342(13) . ? N8 C37 1.479(15) . ? C1 C6 1.376(14) . ? C1 C2 1.393(14) . ? C1 C8 1.504(13) . ? C2 C3 1.386(13) . ? C3 C4 1.387(14) . ? C3 H3 0.9300 . ? C4 C5 1.367(14) . ? C4 C7 1.496(14) . ? C5 C6 1.400(13) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 Cd1 2.708(11) 2_566 ? C8 C9 1.382(13) . ? C8 C13 1.403(14) . ? C9 C10 1.395(13) . ? C10 C11 1.367(14) . ? C10 H10 0.9300 . ? C11 C12 1.406(15) . ? C11 C14 1.510(14) . ? C12 C13 1.375(14) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C15 C20 1.384(14) . ? C15 C16 1.395(13) . ? C15 C22 1.507(13) . ? C16 C17 1.385(13) . ? C17 C18 1.383(13) . ? C17 H17 0.9300 . ? C18 C19 1.390(15) . ? C18 C21 1.485(14) . ? C19 C20 1.378(14) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C22 C27 1.376(14) . ? C22 C23 1.392(14) . ? C23 C24 1.390(13) . ? C24 C25 1.389(13) . ? C24 H24 0.9300 . ? C25 C26 1.350(13) . ? C25 C28 1.515(13) . ? C26 C27 1.386(14) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C29 H29 0.9300 . ? C30 C31 1.353(15) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 C33' 1.29(3) . ? C32 C33 1.59(4) . ? C33' C33' 1.38(7) 2_676 ? C34 H34 0.9300 . ? C35 C36 1.359(17) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C37 C38 1.465(19) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 C38 1.44(3) 2_865 ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O10 Cd1 N5 124.0(3) 2_666 . ? O10 Cd1 O2 100.6(3) 2_666 2_566 ? N5 Cd1 O2 135.4(3) . 2_566 ? O10 Cd1 O9 108.2(2) 2_666 . ? N5 Cd1 O9 84.3(3) . . ? O2 Cd1 O9 79.9(3) 2_566 . ? O10 Cd1 O1 86.0(3) 2_666 . ? N5 Cd1 O1 88.8(3) . . ? O2 Cd1 O1 96.6(2) 2_566 . ? O9 Cd1 O1 165.8(2) . . ? O10 Cd1 O1 145.1(3) 2_666 2_566 ? N5 Cd1 O1 84.9(3) . 2_566 ? O2 Cd1 O1 54.8(3) 2_566 2_566 ? O9 Cd1 O1 92.5(2) . 2_566 ? O1 Cd1 O1 74.4(2) . 2_566 ? O10 Cd1 C7 124.7(3) 2_666 2_566 ? N5 Cd1 C7 110.5(4) . 2_566 ? O2 Cd1 C7 26.9(3) 2_566 2_566 ? O9 Cd1 C7 84.3(3) . 2_566 ? O1 Cd1 C7 86.5(3) . 2_566 ? O1 Cd1 C7 28.0(3) 2_566 2_566 ? N7 Cd2 O4 91.9(3) . . ? N7 Cd2 O11 88.1(3) . 1_654 ? O4 Cd2 O11 172.7(2) . 1_654 ? N7 Cd2 O11 100.3(3) . 2_676 ? O4 Cd2 O11 99.9(2) . 2_676 ? O11 Cd2 O11 73.0(2) 1_654 2_676 ? N7 Cd2 O17 173.0(3) . . ? O4 Cd2 O17 86.6(2) . . ? O11 Cd2 O17 94.3(2) 1_654 . ? O11 Cd2 O17 86.7(2) 2_676 . ? N7 Cd2 O3 87.3(3) . . ? O4 Cd2 O3 55.0(2) . . ? O11 Cd2 O3 132.3(2) 1_654 . ? O11 Cd2 O3 154.2(2) 2_676 . ? O17 Cd2 O3 86.2(2) . . ? N7 Cd2 C14 88.9(3) . . ? O4 Cd2 C14 27.6(3) . . ? O11 Cd2 C14 159.6(3) 1_654 . ? O11 Cd2 C14 127.4(3) 2_676 . ? O17 Cd2 C14 86.6(3) . . ? O3 Cd2 C14 27.4(3) . . ? C7 O1 Cd1 113.3(6) . . ? C7 O1 Cd1 86.0(6) . 2_566 ? Cd1 O1 Cd1 105.6(2) . 2_566 ? C7 O2 Cd1 94.9(7) . 2_566 ? C14 O3 Cd2 85.5(6) . . ? C14 O4 Cd2 95.4(7) . . ? C21 O9 Cd1 127.1(7) . . ? C21 O10 Cd1 100.5(7) . 2_666 ? C28 O11 Cd2 105.3(6) . 1_456 ? C28 O11 Cd2 146.1(6) . 2_676 ? Cd2 O11 Cd2 107.0(2) 1_456 2_676 ? Cd2 O17 H1A 96.8(15) . . ? Cd2 O17 H1B 97.4(16) . . ? H1A O17 H1B 108(3) . . ? O5 N1 O6 121.5(12) . . ? O5 N1 C2 121.7(10) . . ? O6 N1 C2 116.8(12) . . ? O8 N2 O7 118.1(11) . . ? O8 N2 C9 121.6(10) . . ? O7 N2 C9 119.2(10) . . ? O14 N3 O13 118.9(12) . . ? O14 N3 C16 119.2(11) . . ? O13 N3 C16 121.9(10) . . ? O16 N4 O15 120.6(17) . . ? O16 N4 C23 122.2(15) . . ? O15 N4 C23 117.2(15) . . ? C29 N5 C30 105.9(9) . . ? C29 N5 Cd1 128.1(8) . . ? C30 N5 Cd1 125.2(7) . . ? C29 N6 C31 107.6(9) . . ? C29 N6 C32 126.0(11) . . ? C31 N6 C32 126.3(10) . . ? C34 N7 C35 104.9(9) . . ? C34 N7 Cd2 126.2(7) . . ? C35 N7 Cd2 127.6(8) . . ? C36 N8 C34 106.5(10) . . ? C36 N8 C37 126.1(11) . . ? C34 N8 C37 127.4(11) . . ? C6 C1 C2 118.2(9) . . ? C6 C1 C8 118.0(10) . . ? C2 C1 C8 123.8(11) . . ? C3 C2 C1 122.9(10) . . ? C3 C2 N1 115.6(10) . . ? C1 C2 N1 121.3(10) . . ? C2 C3 C4 118.5(10) . . ? C2 C3 H3 120.8 . . ? C4 C3 H3 120.8 . . ? C5 C4 C3 118.7(9) . . ? C5 C4 C7 122.3(10) . . ? C3 C4 C7 118.9(10) . . ? C4 C5 C6 123.0(10) . . ? C4 C5 H5 118.5 . . ? C6 C5 H5 118.5 . . ? C1 C6 C5 118.6(10) . . ? C1 C6 H6 120.7 . . ? C5 C6 H6 120.7 . . ? O2 C7 O1 124.0(10) . . ? O2 C7 C4 120.1(11) . . ? O1 C7 C4 115.8(10) . . ? O2 C7 Cd1 58.2(6) . 2_566 ? O1 C7 Cd1 66.1(5) . 2_566 ? C4 C7 Cd1 173.1(7) . 2_566 ? C9 C8 C13 116.3(9) . . ? C9 C8 C1 126.7(9) . . ? C13 C8 C1 117.0(9) . . ? C8 C9 C10 122.7(9) . . ? C8 C9 N2 121.0(9) . . ? C10 C9 N2 116.3(9) . . ? C11 C10 C9 120.1(9) . . ? C11 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C10 C11 C12 118.5(9) . . ? C10 C11 C14 120.9(10) . . ? C12 C11 C14 120.6(10) . . ? C13 C12 C11 120.7(10) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C12 C13 C8 121.7(10) . . ? C12 C13 H13 119.2 . . ? C8 C13 H13 119.2 . . ? O3 C14 O4 124.1(10) . . ? O3 C14 C11 119.9(10) . . ? O4 C14 C11 115.9(10) . . ? O3 C14 Cd2 67.2(6) . . ? O4 C14 Cd2 57.0(5) . . ? C11 C14 Cd2 171.5(8) . . ? C20 C15 C16 116.5(9) . . ? C20 C15 C22 116.7(9) . . ? C16 C15 C22 126.7(9) . . ? C17 C16 C15 121.2(9) . . ? C17 C16 N3 117.2(9) . . ? C15 C16 N3 121.3(9) . . ? C18 C17 C16 121.7(9) . . ? C18 C17 H17 119.1 . . ? C16 C17 H17 119.1 . . ? C17 C18 C19 117.0(10) . . ? C17 C18 C21 121.2(10) . . ? C19 C18 C21 121.8(10) . . ? C20 C19 C18 121.1(10) . . ? C20 C19 H19 119.4 . . ? C18 C19 H19 119.4 . . ? C19 C20 C15 122.3(10) . . ? C19 C20 H20 118.9 . . ? C15 C20 H20 118.9 . . ? O9 C21 O10 123.2(10) . . ? O9 C21 C18 119.1(10) . . ? O10 C21 C18 117.5(10) . . ? C27 C22 C23 116.5(9) . . ? C27 C22 C15 123.7(9) . . ? C23 C22 C15 119.4(10) . . ? C24 C23 C22 122.2(9) . . ? C24 C23 N4 111.7(10) . . ? C22 C23 N4 125.2(11) . . ? C25 C24 C23 119.5(9) . . ? C25 C24 H24 120.3 . . ? C23 C24 H24 120.3 . . ? C26 C25 C24 118.4(9) . . ? C26 C25 C28 122.3(8) . . ? C24 C25 C28 119.1(8) . . ? C25 C26 C27 122.1(9) . . ? C25 C26 H26 119.0 . . ? C27 C26 H26 119.0 . . ? C22 C27 C26 121.2(9) . . ? C22 C27 H27 119.4 . . ? C26 C27 H27 119.4 . . ? O11 C28 O12 123.0(9) . . ? O11 C28 C25 119.3(8) . . ? O12 C28 C25 117.5(9) . . ? N5 C29 N6 111.0(10) . . ? N5 C29 H29 124.5 . . ? N6 C29 H29 124.5 . . ? C31 C30 N5 109.3(10) . . ? C31 C30 H30 125.3 . . ? N5 C30 H30 125.3 . . ? C30 C31 N6 106.1(10) . . ? C30 C31 H31 126.9 . . ? N6 C31 H31 126.9 . . ? C33' C32 N6 114.0(18) . . ? C33' C32 C33 33(2) . . ? N6 C32 C33 107.3(15) . . ? C32 C33' C33' 137(4) . 2_676 ? N7 C34 N8 111.7(10) . . ? N7 C34 H34 124.1 . . ? N8 C34 H34 124.1 . . ? C36 C35 N7 107.8(12) . . ? C36 C35 H35 126.1 . . ? N7 C35 H35 126.1 . . ? N8 C36 C35 109.0(10) . . ? N8 C36 H36 125.5 . . ? C35 C36 H36 125.5 . . ? C38 C37 N8 114.6(11) . . ? C38 C37 H37A 108.6 . . ? N8 C37 H37A 108.6 . . ? C38 C37 H37B 108.6 . . ? N8 C37 H37B 108.6 . . ? H37A C37 H37B 107.6 . . ? C38 C38 C37 117(2) 2_865 . ? C38 C38 H38A 108.0 2_865 . ? C37 C38 H38A 108.0 . . ? C38 C38 H38B 108.0 2_865 . ? C37 C38 H38B 108.0 . . ? H38A C38 H38B 107.2 . . ? 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 O17 H1A O12 0.99(2) 1.95(4) 2.823(9) 145(4) 2_576 O17 H1B O3 0.98(2) 1.86(2) 2.716(9) 144(2) 2_675 _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.624 _refine_diff_density_min -0.883 _refine_diff_density_rms 0.146