# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_cncnc3 #TrackingRef 'cncnc3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C30 H20 N2 O6 Zn' _chemical_formula_sum 'C30 H20 N2 O6 Zn' _chemical_formula_weight 569.85 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M p21/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 10.1639(4) _cell_length_b 16.0423(6) _cell_length_c 16.2284(6) _cell_angle_alpha 90.00 _cell_angle_beta 102.5930(10) _cell_angle_gamma 90.00 _cell_volume 2582.42(17) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6267 _cell_measurement_theta_min 1.61 _cell_measurement_theta_max 26.02 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.466 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1168 _exptl_absorpt_coefficient_mu 0.999 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.740 _exptl_absorpt_correction_T_max 0.802 _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 16009 _diffrn_reflns_av_R_equivalents 0.0181 _diffrn_reflns_av_sigmaI/netI 0.0229 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 28.34 _reflns_number_total 6267 _reflns_number_gt 4914 _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^)+(0.0418P)^2^+0.4216P] 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 6267 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0430 _refine_ls_R_factor_gt 0.0298 _refine_ls_wR_factor_ref 0.0828 _refine_ls_wR_factor_gt 0.0770 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.127830(19) 0.054777(12) 0.312881(11) 0.04133(7) Uani 1 1 d . . . O4 O 0.22089(14) 0.05453(7) -0.17064(7) 0.0517(3) Uani 1 1 d . . . O3 O 0.34151(13) -0.23148(7) -0.20042(7) 0.0526(3) Uani 1 1 d . . . O6 O 0.05986(13) 0.09831(8) 0.18455(7) 0.0524(3) Uani 1 1 d . . . O2 O 0.70741(13) -0.45276(7) 0.08260(8) 0.0489(3) Uani 1 1 d . . . O5 O 0.21167(13) -0.00001(9) 0.21683(7) 0.0536(3) Uani 1 1 d . . . O1 O 0.74225(13) -0.33149(8) 0.14588(8) 0.0542(3) Uani 1 1 d . . . C14 C 0.20815(18) 0.05112(10) -0.08752(10) 0.0414(4) Uani 1 1 d . . . N2 N -0.02268(14) 0.10760(9) 0.36684(8) 0.0427(3) Uani 1 1 d . . . N1 N 0.02359(15) -0.05143(9) 0.33998(9) 0.0434(3) Uani 1 1 d . . . C24 C -0.1484(2) -0.10112(14) 0.40596(13) 0.0600(5) Uani 1 1 d . . . H24 H -0.2150 -0.0902 0.4358 0.072 Uiso 1 1 calc R . . C12 C 0.29867(16) -0.00612(10) -0.19864(9) 0.0394(4) Uani 1 1 d . . . C4 C 0.42595(16) -0.34871(10) -0.11989(10) 0.0415(4) Uani 1 1 d . . . H4 H 0.3731 -0.3818 -0.1613 0.050 Uiso 1 1 calc R . . C17 C 0.16849(17) 0.05231(10) 0.07619(10) 0.0401(3) Uani 1 1 d . . . C19 C 0.29871(18) 0.01087(13) -0.02442(10) 0.0515(4) Uani 1 1 d . . . H19 H 0.3732 -0.0162 -0.0365 0.062 Uiso 1 1 calc R . . C20 C 0.14531(17) 0.05007(11) 0.16399(10) 0.0433(4) Uani 1 1 d . . . C8 C 0.35823(17) -0.14664(10) -0.21558(10) 0.0417(4) Uani 1 1 d . . . C2 C 0.58579(16) -0.33636(10) 0.01336(10) 0.0388(3) Uani 1 1 d . . . C10 C 0.47262(19) -0.03824(12) -0.27093(11) 0.0508(4) Uani 1 1 d . . . H10 H 0.5364 -0.0210 -0.3006 0.061 Uiso 1 1 calc R . . C11 C 0.39565(18) 0.02037(11) -0.24066(10) 0.0449(4) Uani 1 1 d . . . H11 H 0.4089 0.0769 -0.2484 0.054 Uiso 1 1 calc R . . C25 C -0.07381(17) -0.03636(11) 0.38225(10) 0.0426(4) Uani 1 1 d . . . C27 C -0.19448(18) 0.07976(14) 0.44191(11) 0.0540(5) Uani 1 1 d . . . H27 H -0.2441 0.0415 0.4658 0.065 Uiso 1 1 calc R . . C5 C 0.42327(16) -0.26307(10) -0.12776(10) 0.0409(4) Uani 1 1 d . . . C18 C 0.27759(18) 0.01122(13) 0.05723(10) 0.0502(4) Uani 1 1 d . . . H18 H 0.3377 -0.0166 0.0998 0.060 Uiso 1 1 calc R . . C26 C -0.09899(16) 0.05262(11) 0.39854(9) 0.0412(4) Uani 1 1 d . . . C3 C 0.50789(16) -0.38480(10) -0.04982(10) 0.0413(4) Uani 1 1 d . . . H3 H 0.5109 -0.4426 -0.0449 0.050 Uiso 1 1 calc R . . C23 C -0.1228(2) -0.18136(14) 0.38496(16) 0.0729(6) Uani 1 1 d . . . H23 H -0.1722 -0.2252 0.4004 0.087 Uiso 1 1 calc R . . C16 C 0.08130(18) 0.09422(11) 0.01266(11) 0.0454(4) Uani 1 1 d . . . H16 H 0.0092 0.1236 0.0252 0.055 Uiso 1 1 calc R . . C13 C 0.27621(16) -0.08983(11) -0.18744(9) 0.0401(3) Uani 1 1 d . . . H13 H 0.2078 -0.1074 -0.1617 0.048 Uiso 1 1 calc R . . C15 C 0.09947(18) 0.09331(11) -0.06938(10) 0.0456(4) Uani 1 1 d . . . H15 H 0.0390 0.1209 -0.1119 0.055 Uiso 1 1 calc R . . C1 C 0.68304(16) -0.37547(11) 0.08597(10) 0.0423(4) Uani 1 1 d . . . C9 C 0.45579(18) -0.12227(12) -0.25757(11) 0.0498(4) Uani 1 1 d . . . H9 H 0.5094 -0.1617 -0.2766 0.060 Uiso 1 1 calc R . . C30 C -0.0429(2) 0.18924(12) 0.37511(12) 0.0526(4) Uani 1 1 d . . . H30 H 0.0103 0.2268 0.3532 0.063 Uiso 1 1 calc R . . C7 C 0.57982(18) -0.25081(11) 0.00542(11) 0.0491(4) Uani 1 1 d . . . H7 H 0.6301 -0.2177 0.0479 0.059 Uiso 1 1 calc R . . C29 C -0.1397(2) 0.21987(14) 0.41487(13) 0.0612(5) Uani 1 1 d . . . H29 H -0.1536 0.2770 0.4183 0.073 Uiso 1 1 calc R . . C6 C 0.4997(2) -0.21338(11) -0.06512(11) 0.0528(5) Uani 1 1 d . . . H6 H 0.4973 -0.1556 -0.0704 0.063 Uiso 1 1 calc R . . C21 C 0.0479(2) -0.13025(12) 0.31990(12) 0.0545(5) Uani 1 1 d . . . H21 H 0.1156 -0.1403 0.2908 0.065 Uiso 1 1 calc R . . C28 C -0.2150(2) 0.16437(14) 0.44923(13) 0.0619(5) Uani 1 1 d . . . H28 H -0.2796 0.1835 0.4774 0.074 Uiso 1 1 calc R . . C22 C -0.0240(2) -0.19682(13) 0.34096(14) 0.0674(6) Uani 1 1 d . . . H22 H -0.0061 -0.2509 0.3258 0.081 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.04440(12) 0.04797(13) 0.03245(10) -0.00526(8) 0.01017(8) -0.00817(8) O4 0.0714(9) 0.0523(7) 0.0339(6) 0.0089(5) 0.0169(6) 0.0196(6) O3 0.0635(8) 0.0412(7) 0.0434(7) 0.0047(5) -0.0094(6) 0.0007(6) O6 0.0634(8) 0.0557(8) 0.0421(6) -0.0084(6) 0.0201(6) -0.0009(6) O2 0.0516(7) 0.0459(7) 0.0485(7) 0.0121(5) 0.0093(5) 0.0124(5) O5 0.0542(7) 0.0716(9) 0.0353(6) 0.0011(6) 0.0102(5) 0.0030(6) O1 0.0546(7) 0.0605(8) 0.0428(7) 0.0022(6) 0.0004(6) 0.0103(6) C14 0.0496(9) 0.0427(9) 0.0317(7) 0.0000(6) 0.0090(7) -0.0006(7) N2 0.0452(8) 0.0489(9) 0.0343(7) -0.0023(6) 0.0092(6) -0.0093(6) N1 0.0450(8) 0.0474(8) 0.0347(7) 0.0000(6) 0.0021(6) -0.0075(6) C24 0.0538(11) 0.0623(13) 0.0634(12) 0.0211(10) 0.0113(9) -0.0082(9) C12 0.0449(9) 0.0458(9) 0.0257(7) 0.0048(6) 0.0038(6) 0.0078(7) C4 0.0429(9) 0.0379(9) 0.0420(8) -0.0022(7) 0.0056(7) 0.0009(7) C17 0.0440(9) 0.0423(9) 0.0339(8) -0.0065(6) 0.0079(7) -0.0054(7) C19 0.0431(10) 0.0748(13) 0.0358(9) -0.0032(8) 0.0070(7) 0.0126(9) C20 0.0428(9) 0.0512(10) 0.0361(8) -0.0089(7) 0.0090(7) -0.0127(8) C8 0.0479(9) 0.0415(9) 0.0308(7) 0.0062(6) -0.0024(7) 0.0025(7) C2 0.0384(8) 0.0412(9) 0.0381(8) 0.0068(6) 0.0111(6) 0.0065(7) C10 0.0447(10) 0.0660(13) 0.0436(9) 0.0095(8) 0.0139(8) 0.0003(8) C11 0.0508(10) 0.0468(9) 0.0354(8) 0.0083(7) 0.0058(7) -0.0052(8) C25 0.0384(8) 0.0530(10) 0.0329(8) 0.0087(7) 0.0000(6) -0.0060(7) C27 0.0446(10) 0.0745(13) 0.0449(10) 0.0026(9) 0.0137(8) -0.0073(9) C5 0.0434(9) 0.0395(9) 0.0376(8) 0.0047(6) 0.0043(7) 0.0040(7) C18 0.0471(10) 0.0690(12) 0.0309(8) 0.0000(8) 0.0011(7) 0.0098(9) C26 0.0390(8) 0.0542(10) 0.0274(7) 0.0031(6) 0.0011(6) -0.0078(7) C3 0.0447(9) 0.0331(8) 0.0472(9) 0.0040(7) 0.0123(7) 0.0039(7) C23 0.0718(14) 0.0567(13) 0.0875(16) 0.0240(11) 0.0119(12) -0.0148(11) C16 0.0499(10) 0.0431(9) 0.0448(9) -0.0031(7) 0.0137(8) 0.0059(8) C13 0.0406(9) 0.0488(9) 0.0300(7) 0.0078(7) 0.0055(6) -0.0007(7) C15 0.0560(10) 0.0400(9) 0.0399(9) 0.0041(7) 0.0083(7) 0.0097(8) C1 0.0397(9) 0.0507(10) 0.0392(8) 0.0118(7) 0.0142(7) 0.0088(7) C9 0.0481(10) 0.0595(12) 0.0412(9) 0.0029(8) 0.0083(8) 0.0134(8) C30 0.0579(11) 0.0489(11) 0.0525(10) -0.0071(8) 0.0153(9) -0.0106(9) C7 0.0552(10) 0.0422(10) 0.0433(9) 0.0005(7) -0.0035(8) 0.0010(8) C29 0.0593(12) 0.0577(12) 0.0681(13) -0.0169(10) 0.0169(10) -0.0032(9) C6 0.0648(12) 0.0327(9) 0.0513(10) 0.0053(7) -0.0084(9) 0.0008(8) C21 0.0591(12) 0.0511(11) 0.0499(10) -0.0005(8) 0.0044(9) -0.0020(9) C28 0.0533(11) 0.0775(15) 0.0584(12) -0.0144(10) 0.0196(9) -0.0021(10) C22 0.0777(15) 0.0459(12) 0.0725(14) 0.0087(10) 0.0028(12) -0.0027(10) _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 N2 2.0999(14) . ? Zn1 N1 2.1028(14) . ? Zn1 O2 2.1113(13) 2_655 ? Zn1 O5 2.1231(12) . ? Zn1 O6 2.1621(13) . ? Zn1 O1 2.2662(13) 2_655 ? Zn1 C20 2.4622(16) . ? Zn1 C1 2.5033(16) 2_655 ? O4 C14 1.3839(19) . ? O4 C12 1.3910(19) . ? O3 C5 1.3822(18) . ? O3 C8 1.400(2) . ? O6 C20 1.261(2) . ? O2 C1 1.268(2) . ? O2 Zn1 2.1113(13) 2_645 ? O5 C20 1.258(2) . ? O1 C1 1.245(2) . ? O1 Zn1 2.2662(13) 2_645 ? C14 C19 1.379(2) . ? C14 C15 1.381(2) . ? N2 C30 1.337(2) . ? N2 C26 1.348(2) . ? N1 C21 1.342(2) . ? N1 C25 1.344(2) . ? C24 C23 1.371(3) . ? C24 C25 1.389(2) . ? C24 H24 0.9300 . ? C12 C13 1.381(2) . ? C12 C11 1.382(2) . ? C4 C5 1.379(2) . ? C4 C3 1.382(2) . ? C4 H4 0.9300 . ? C17 C16 1.379(2) . ? C17 C18 1.381(2) . ? C17 C20 1.495(2) . ? C19 C18 1.388(2) . ? C19 H19 0.9300 . ? C8 C9 1.377(3) . ? C8 C13 1.378(2) . ? C2 C7 1.379(2) . ? C2 C3 1.389(2) . ? C2 C1 1.500(2) . ? C10 C11 1.380(3) . ? C10 C9 1.382(3) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C25 C26 1.484(2) . ? C27 C28 1.382(3) . ? C27 C26 1.387(3) . ? C27 H27 0.9300 . ? C5 C6 1.389(2) . ? C18 H18 0.9300 . ? C3 H3 0.9300 . ? C23 C22 1.376(3) . ? C23 H23 0.9300 . ? C16 C15 1.383(2) . ? C16 H16 0.9300 . ? C13 H13 0.9300 . ? C15 H15 0.9300 . ? C1 Zn1 2.5033(16) 2_645 ? C9 H9 0.9300 . ? C30 C29 1.380(3) . ? C30 H30 0.9300 . ? C7 C6 1.388(2) . ? C7 H7 0.9300 . ? C29 C28 1.369(3) . ? C29 H29 0.9300 . ? C6 H6 0.9300 . ? C21 C22 1.378(3) . ? C21 H21 0.9300 . ? C28 H28 0.9300 . ? C22 H22 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Zn1 N1 78.09(6) . . ? N2 Zn1 O2 102.15(5) . 2_655 ? N1 Zn1 O2 97.65(5) . 2_655 ? N2 Zn1 O5 156.75(5) . . ? N1 Zn1 O5 96.86(5) . . ? O2 Zn1 O5 101.02(5) 2_655 . ? N2 Zn1 O6 99.35(5) . . ? N1 Zn1 O6 113.17(5) . . ? O2 Zn1 O6 145.41(5) 2_655 . ? O5 Zn1 O6 61.42(5) . . ? N2 Zn1 O1 89.00(5) . 2_655 ? N1 Zn1 O1 151.44(5) . 2_655 ? O2 Zn1 O1 59.99(5) 2_655 2_655 ? O5 Zn1 O1 104.41(5) . 2_655 ? O6 Zn1 O1 93.88(5) . 2_655 ? N2 Zn1 C20 129.54(6) . . ? N1 Zn1 C20 109.14(5) . . ? O2 Zn1 C20 124.91(5) 2_655 . ? O5 Zn1 C20 30.73(5) . . ? O6 Zn1 C20 30.79(5) . . ? O1 Zn1 C20 98.77(5) 2_655 . ? N2 Zn1 C1 94.08(5) . 2_655 ? N1 Zn1 C1 125.09(6) . 2_655 ? O2 Zn1 C1 30.41(5) 2_655 2_655 ? O5 Zn1 C1 107.02(5) . 2_655 ? O6 Zn1 C1 121.71(5) . 2_655 ? O1 Zn1 C1 29.74(5) 2_655 2_655 ? C20 Zn1 C1 116.61(5) . 2_655 ? C14 O4 C12 118.12(12) . . ? C5 O3 C8 115.66(12) . . ? C20 O6 Zn1 87.87(10) . . ? C1 O2 Zn1 92.15(10) . 2_645 ? C20 O5 Zn1 89.70(10) . . ? C1 O1 Zn1 85.74(10) . 2_645 ? C19 C14 C15 120.43(15) . . ? C19 C14 O4 123.59(15) . . ? C15 C14 O4 115.95(14) . . ? C30 N2 C26 119.25(16) . . ? C30 N2 Zn1 125.39(12) . . ? C26 N2 Zn1 115.28(12) . . ? C21 N1 C25 119.25(16) . . ? C21 N1 Zn1 125.79(13) . . ? C25 N1 Zn1 114.96(11) . . ? C23 C24 C25 119.3(2) . . ? C23 C24 H24 120.4 . . ? C25 C24 H24 120.4 . . ? C13 C12 C11 121.34(16) . . ? C13 C12 O4 121.02(15) . . ? C11 C12 O4 117.60(15) . . ? C5 C4 C3 119.32(15) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? C16 C17 C18 118.85(15) . . ? C16 C17 C20 121.02(15) . . ? C18 C17 C20 120.13(15) . . ? C14 C19 C18 119.34(16) . . ? C14 C19 H19 120.3 . . ? C18 C19 H19 120.3 . . ? O5 C20 O6 120.61(15) . . ? O5 C20 C17 119.51(15) . . ? O6 C20 C17 119.88(16) . . ? O5 C20 Zn1 59.57(9) . . ? O6 C20 Zn1 61.34(9) . . ? C17 C20 Zn1 174.25(12) . . ? C9 C8 C13 121.95(16) . . ? C9 C8 O3 119.41(16) . . ? C13 C8 O3 118.63(15) . . ? C7 C2 C3 118.80(15) . . ? C7 C2 C1 119.86(15) . . ? C3 C2 C1 121.18(15) . . ? C11 C10 C9 120.63(17) . . ? C11 C10 H10 119.7 . . ? C9 C10 H10 119.7 . . ? C10 C11 C12 119.12(17) . . ? C10 C11 H11 120.4 . . ? C12 C11 H11 120.4 . . ? N1 C25 C24 120.96(18) . . ? N1 C25 C26 116.03(14) . . ? C24 C25 C26 122.98(17) . . ? C28 C27 C26 119.13(18) . . ? C28 C27 H27 120.4 . . ? C26 C27 H27 120.4 . . ? C4 C5 O3 116.11(14) . . ? C4 C5 C6 120.50(15) . . ? O3 C5 C6 123.39(15) . . ? C17 C18 C19 120.89(16) . . ? C17 C18 H18 119.6 . . ? C19 C18 H18 119.6 . . ? N2 C26 C27 120.83(17) . . ? N2 C26 C25 115.17(15) . . ? C27 C26 C25 123.99(16) . . ? C4 C3 C2 121.16(15) . . ? C4 C3 H3 119.4 . . ? C2 C3 H3 119.4 . . ? C24 C23 C22 119.8(2) . . ? C24 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? C17 C16 C15 121.02(16) . . ? C17 C16 H16 119.5 . . ? C15 C16 H16 119.5 . . ? C8 C13 C12 118.05(15) . . ? C8 C13 H13 121.0 . . ? C12 C13 H13 121.0 . . ? C14 C15 C16 119.43(16) . . ? C14 C15 H15 120.3 . . ? C16 C15 H15 120.3 . . ? O1 C1 O2 121.48(15) . . ? O1 C1 C2 119.98(15) . . ? O2 C1 C2 118.46(15) . . ? O1 C1 Zn1 64.53(9) . 2_645 ? O2 C1 Zn1 57.44(8) . 2_645 ? C2 C1 Zn1 169.16(11) . 2_645 ? C8 C9 C10 118.80(17) . . ? C8 C9 H9 120.6 . . ? C10 C9 H9 120.6 . . ? N2 C30 C29 122.47(18) . . ? N2 C30 H30 118.8 . . ? C29 C30 H30 118.8 . . ? C2 C7 C6 120.91(16) . . ? C2 C7 H7 119.5 . . ? C6 C7 H7 119.5 . . ? C28 C29 C30 118.5(2) . . ? C28 C29 H29 120.7 . . ? C30 C29 H29 120.7 . . ? C7 C6 C5 119.29(16) . . ? C7 C6 H6 120.4 . . ? C5 C6 H6 120.4 . . ? N1 C21 C22 122.3(2) . . ? N1 C21 H21 118.9 . . ? C22 C21 H21 118.9 . . ? C29 C28 C27 119.72(19) . . ? C29 C28 H28 120.1 . . ? C27 C28 H28 120.1 . . ? C23 C22 C21 118.4(2) . . ? C23 C22 H22 120.8 . . ? C21 C22 H22 120.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Zn1 O6 C20 -169.73(10) . . . . ? N1 Zn1 O6 C20 -88.77(10) . . . . ? O2 Zn1 O6 C20 62.35(13) 2_655 . . . ? O5 Zn1 O6 C20 -3.66(9) . . . . ? O1 Zn1 O6 C20 100.65(10) 2_655 . . . ? C1 Zn1 O6 C20 89.51(11) 2_655 . . . ? N2 Zn1 O5 C20 40.63(19) . . . . ? N1 Zn1 O5 C20 116.35(10) . . . . ? O2 Zn1 O5 C20 -144.44(10) 2_655 . . . ? O6 Zn1 O5 C20 3.66(9) . . . . ? O1 Zn1 O5 C20 -82.87(10) 2_655 . . . ? C1 Zn1 O5 C20 -113.68(10) 2_655 . . . ? C12 O4 C14 C19 22.2(3) . . . . ? C12 O4 C14 C15 -159.81(15) . . . . ? N1 Zn1 N2 C30 -177.07(15) . . . . ? O2 Zn1 N2 C30 87.55(14) 2_655 . . . ? O5 Zn1 N2 C30 -97.54(18) . . . . ? O6 Zn1 N2 C30 -65.18(15) . . . . ? O1 Zn1 N2 C30 28.59(14) 2_655 . . . ? C20 Zn1 N2 C30 -71.98(16) . . . . ? C1 Zn1 N2 C30 57.90(15) 2_655 . . . ? N1 Zn1 N2 C26 6.18(11) . . . . ? O2 Zn1 N2 C26 -89.20(11) 2_655 . . . ? O5 Zn1 N2 C26 85.71(17) . . . . ? O6 Zn1 N2 C26 118.07(11) . . . . ? O1 Zn1 N2 C26 -148.17(11) 2_655 . . . ? C20 Zn1 N2 C26 111.27(11) . . . . ? C1 Zn1 N2 C26 -118.85(11) 2_655 . . . ? N2 Zn1 N1 C21 175.72(15) . . . . ? O2 Zn1 N1 C21 -83.40(14) 2_655 . . . ? O5 Zn1 N1 C21 18.74(14) . . . . ? O6 Zn1 N1 C21 80.54(15) . . . . ? O1 Zn1 N1 C21 -119.42(15) 2_655 . . . ? C20 Zn1 N1 C21 47.74(15) . . . . ? C1 Zn1 N1 C21 -97.67(15) 2_655 . . . ? N2 Zn1 N1 C25 -5.28(11) . . . . ? O2 Zn1 N1 C25 95.60(12) 2_655 . . . ? O5 Zn1 N1 C25 -162.26(11) . . . . ? O6 Zn1 N1 C25 -100.46(11) . . . . ? O1 Zn1 N1 C25 59.58(17) 2_655 . . . ? C20 Zn1 N1 C25 -133.26(11) . . . . ? C1 Zn1 N1 C25 81.33(13) 2_655 . . . ? C14 O4 C12 C13 52.2(2) . . . . ? C14 O4 C12 C11 -130.06(16) . . . . ? C15 C14 C19 C18 1.8(3) . . . . ? O4 C14 C19 C18 179.70(17) . . . . ? Zn1 O5 C20 O6 -6.42(16) . . . . ? Zn1 O5 C20 C17 173.45(13) . . . . ? Zn1 O6 C20 O5 6.30(16) . . . . ? Zn1 O6 C20 C17 -173.56(13) . . . . ? C16 C17 C20 O5 167.61(16) . . . . ? C18 C17 C20 O5 -11.6(2) . . . . ? C16 C17 C20 O6 -12.5(2) . . . . ? C18 C17 C20 O6 168.28(16) . . . . ? C16 C17 C20 Zn1 -113.2(13) . . . . ? C18 C17 C20 Zn1 67.6(14) . . . . ? N2 Zn1 C20 O5 -160.53(9) . . . . ? N1 Zn1 C20 O5 -70.34(11) . . . . ? O2 Zn1 C20 O5 44.11(12) 2_655 . . . ? O6 Zn1 C20 O5 -173.71(16) . . . . ? O1 Zn1 C20 O5 103.48(10) 2_655 . . . ? C1 Zn1 C20 O5 78.36(11) 2_655 . . . ? N2 Zn1 C20 O6 13.18(13) . . . . ? N1 Zn1 C20 O6 103.37(10) . . . . ? O2 Zn1 C20 O6 -142.18(9) 2_655 . . . ? O5 Zn1 C20 O6 173.71(16) . . . . ? O1 Zn1 C20 O6 -82.81(10) 2_655 . . . ? C1 Zn1 C20 O6 -107.94(10) 2_655 . . . ? N2 Zn1 C20 C17 117.0(13) . . . . ? N1 Zn1 C20 C17 -152.8(13) . . . . ? O2 Zn1 C20 C17 -38.3(13) 2_655 . . . ? O5 Zn1 C20 C17 -82.4(13) . . . . ? O6 Zn1 C20 C17 103.8(13) . . . . ? O1 Zn1 C20 C17 21.0(13) 2_655 . . . ? C1 Zn1 C20 C17 -4.1(13) 2_655 . . . ? C5 O3 C8 C9 86.33(19) . . . . ? C5 O3 C8 C13 -93.39(18) . . . . ? C9 C10 C11 C12 -1.7(3) . . . . ? C13 C12 C11 C10 -0.9(2) . . . . ? O4 C12 C11 C10 -178.59(15) . . . . ? C21 N1 C25 C24 0.6(2) . . . . ? Zn1 N1 C25 C24 -178.47(13) . . . . ? C21 N1 C25 C26 -177.19(14) . . . . ? Zn1 N1 C25 C26 3.74(18) . . . . ? C23 C24 C25 N1 -0.7(3) . . . . ? C23 C24 C25 C26 176.92(18) . . . . ? C3 C4 C5 O3 178.49(15) . . . . ? C3 C4 C5 C6 -1.4(3) . . . . ? C8 O3 C5 C4 -168.51(15) . . . . ? C8 O3 C5 C6 11.4(2) . . . . ? C16 C17 C18 C19 -0.9(3) . . . . ? C20 C17 C18 C19 178.34(17) . . . . ? C14 C19 C18 C17 -1.0(3) . . . . ? C30 N2 C26 C27 -2.2(2) . . . . ? Zn1 N2 C26 C27 174.74(13) . . . . ? C30 N2 C26 C25 176.93(15) . . . . ? Zn1 N2 C26 C25 -6.11(17) . . . . ? C28 C27 C26 N2 2.8(3) . . . . ? C28 C27 C26 C25 -176.26(16) . . . . ? N1 C25 C26 N2 1.6(2) . . . . ? C24 C25 C26 N2 -176.17(16) . . . . ? N1 C25 C26 C27 -179.31(15) . . . . ? C24 C25 C26 C27 3.0(3) . . . . ? C5 C4 C3 C2 1.0(3) . . . . ? C7 C2 C3 C4 0.3(3) . . . . ? C1 C2 C3 C4 -175.04(15) . . . . ? C25 C24 C23 C22 0.1(3) . . . . ? C18 C17 C16 C15 2.0(3) . . . . ? C20 C17 C16 C15 -177.19(16) . . . . ? C9 C8 C13 C12 -3.2(2) . . . . ? O3 C8 C13 C12 176.47(13) . . . . ? C11 C12 C13 C8 3.3(2) . . . . ? O4 C12 C13 C8 -179.07(14) . . . . ? C19 C14 C15 C16 -0.6(3) . . . . ? O4 C14 C15 C16 -178.73(15) . . . . ? C17 C16 C15 C14 -1.3(3) . . . . ? Zn1 O1 C1 O2 7.84(16) 2_645 . . . ? Zn1 O1 C1 C2 -168.86(13) 2_645 . . . ? Zn1 O2 C1 O1 -8.40(17) 2_645 . . . ? Zn1 O2 C1 C2 168.34(12) 2_645 . . . ? C7 C2 C1 O1 11.6(2) . . . . ? C3 C2 C1 O1 -173.16(16) . . . . ? C7 C2 C1 O2 -165.24(16) . . . . ? C3 C2 C1 O2 10.1(2) . . . . ? C7 C2 C1 Zn1 -100.4(7) . . . 2_645 ? C3 C2 C1 Zn1 74.9(7) . . . 2_645 ? C13 C8 C9 C10 0.7(2) . . . . ? O3 C8 C9 C10 -178.99(15) . . . . ? C11 C10 C9 C8 1.8(3) . . . . ? C26 N2 C30 C29 -0.2(3) . . . . ? Zn1 N2 C30 C29 -176.82(14) . . . . ? C3 C2 C7 C6 -1.3(3) . . . . ? C1 C2 C7 C6 174.09(17) . . . . ? N2 C30 C29 C28 2.0(3) . . . . ? C2 C7 C6 C5 0.9(3) . . . . ? C4 C5 C6 C7 0.4(3) . . . . ? O3 C5 C6 C7 -179.47(17) . . . . ? C25 N1 C21 C22 0.1(3) . . . . ? Zn1 N1 C21 C22 179.11(14) . . . . ? C30 C29 C28 C27 -1.3(3) . . . . ? C26 C27 C28 C29 -1.0(3) . . . . ? C24 C23 C22 C21 0.6(3) . . . . ? N1 C21 C22 C23 -0.8(3) . . . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 28.34 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 0.263 _refine_diff_density_min -0.279 _refine_diff_density_rms 0.041 _database_code_depnum_ccdc_archive 'CCDC 933676' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_cncnc4 #TrackingRef 'cncnc4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C30 H28 N4 Ni O7' _chemical_formula_sum 'C30 H28 N4 Ni O7' _chemical_formula_weight 615.27 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 monoclinic _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 8.7642(6) _cell_length_b 31.696(2) _cell_length_c 10.7597(7) _cell_angle_alpha 90.00 _cell_angle_beta 110.8820(10) _cell_angle_gamma 90.00 _cell_volume 2792.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4460 _cell_measurement_theta_min 1.61 _cell_measurement_theta_max 26.02 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.463 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1280 _exptl_absorpt_coefficient_mu 0.750 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.806 _exptl_absorpt_correction_T_max 0.854 _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 7615 _diffrn_reflns_av_R_equivalents 0.0227 _diffrn_reflns_av_sigmaI/netI 0.0500 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.28 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4460 _reflns_number_gt 3875 _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^)+(0.0921P)^2^+0.8037P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.75(2) _refine_ls_number_reflns 4460 _refine_ls_number_parameters 374 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0605 _refine_ls_R_factor_gt 0.0505 _refine_ls_wR_factor_ref 0.1442 _refine_ls_wR_factor_gt 0.1347 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.33293(7) 0.419229(17) 0.50212(6) 0.03836(18) Uani 1 1 d . . . O6 O -0.2945(4) -0.03150(11) 0.3683(3) 0.0415(8) Uani 1 1 d . . . O5 O -0.1909(4) -0.02257(11) 0.5833(3) 0.0443(8) Uani 1 1 d . . . O1 O 0.2604(5) 0.36577(13) 0.3754(4) 0.0555(10) Uani 1 1 d . . . O2 O 0.1049(5) 0.39014(12) 0.4792(4) 0.0499(9) Uani 1 1 d . . . N2 N 0.7013(5) 0.46375(15) 0.3717(5) 0.0491(11) Uani 1 1 d . . . N1 N 0.5410(5) 0.43618(16) 0.4673(4) 0.0470(10) Uani 1 1 d . . . O3 O -0.3797(8) 0.16643(13) 0.4265(5) 0.0842(17) Uani 1 1 d . . . C16 C -0.3043(6) 0.06149(16) 0.5608(5) 0.0413(11) Uani 1 1 d . . . H16 H -0.2814 0.0485 0.6430 0.050 Uiso 1 1 calc R . . N4 N 0.5976(6) 0.38480(15) 0.8869(4) 0.0486(11) Uani 1 1 d . . . C20 C -0.2645(5) -0.00780(15) 0.4681(5) 0.0358(10) Uani 1 1 d . . . C15 C -0.3335(8) 0.10415(17) 0.5486(6) 0.0518(14) Uani 1 1 d . . . H15 H -0.3317 0.1200 0.6219 0.062 Uiso 1 1 calc R . . N3 N 0.4459(6) 0.38949(14) 0.6759(4) 0.0446(10) Uani 1 1 d . . . C1 C 0.1260(8) 0.36492(16) 0.3954(5) 0.0485(13) Uani 1 1 d . . . C2 C -0.0086(9) 0.33615(18) 0.3187(6) 0.0599(16) Uani 1 1 d . . . C23 C 0.5470(6) 0.45985(17) 0.3686(5) 0.0452(12) Uani 1 1 d . . . H23 H 0.4565 0.4723 0.3051 0.054 Uiso 1 1 calc R . . C14 C -0.3651(8) 0.12317(16) 0.4285(6) 0.0499(13) Uani 1 1 d . . . C17 C -0.3088(5) 0.03767(15) 0.4519(5) 0.0358(10) Uani 1 1 d . . . C19 C -0.3746(7) 0.10013(17) 0.3152(5) 0.0461(12) Uani 1 1 d . . . H19 H -0.4007 0.1133 0.2330 0.055 Uiso 1 1 calc R . . C25 C 0.8047(7) 0.4534(2) 0.1878(6) 0.0565(15) Uani 1 1 d . . . H25A H 0.8645 0.4682 0.1407 0.068 Uiso 1 1 calc R . . H25B H 0.8776 0.4328 0.2455 0.068 Uiso 1 1 calc R . . C9 C -0.3873(8) 0.21341(19) 0.2572(6) 0.0588(15) Uani 1 1 d . . . H9 H -0.2745 0.2161 0.2959 0.071 Uiso 1 1 calc R . . C28 C 0.4388(8) 0.34897(19) 0.7174(6) 0.0561(15) Uani 1 1 d . . . H28 H 0.3800 0.3270 0.6647 0.067 Uiso 1 1 calc R . . C24 C 0.7537(8) 0.4847(2) 0.2721(7) 0.0602(16) Uani 1 1 d . . . H24A H 0.8447 0.5032 0.3169 0.072 Uiso 1 1 calc R . . H24B H 0.6648 0.5018 0.2149 0.072 Uiso 1 1 calc R . . C18 C -0.3444(6) 0.05737(16) 0.3284(5) 0.0410(11) Uani 1 1 d . . . H18 H -0.3477 0.0415 0.2547 0.049 Uiso 1 1 calc R . . O4 O -0.3989(10) 0.2629(2) 0.0849(5) 0.119(3) Uani 1 1 d . . . C26 C 0.6610(8) 0.4308(2) 0.0880(6) 0.0578(15) Uani 1 1 d . . . H26A H 0.5927 0.4510 0.0248 0.069 Uiso 1 1 calc R . . H26B H 0.5958 0.4177 0.1337 0.069 Uiso 1 1 calc R . . C10 C -0.4692(9) 0.18614(17) 0.3089(6) 0.0556(15) Uani 1 1 d . . . C21 C 0.6995(8) 0.4250(2) 0.5350(6) 0.0629(18) Uani 1 1 d . . . H21 H 0.7335 0.4079 0.6103 0.076 Uiso 1 1 calc R . . C3 C -0.1521(10) 0.3367(2) 0.3406(7) 0.075(2) Uani 1 1 d . . . H3 H -0.1629 0.3543 0.4063 0.089 Uiso 1 1 calc R . . C7 C 0.0080(11) 0.3099(2) 0.2196(7) 0.074(2) Uani 1 1 d . . . H7 H 0.1057 0.3089 0.2040 0.089 Uiso 1 1 calc R . . C27 C 0.7205(8) 0.3971(2) 0.0138(6) 0.0616(16) Uani 1 1 d . . . H27A H 0.8159 0.4076 -0.0019 0.074 Uiso 1 1 calc R . . H27B H 0.7535 0.3723 0.0699 0.074 Uiso 1 1 calc R . . C8 C -0.4748(11) 0.23730(19) 0.1456(7) 0.071(2) Uani 1 1 d . . . C5 C -0.2656(13) 0.2858(3) 0.1689(7) 0.091(3) Uani 1 1 d . . . C22 C 0.7988(6) 0.4416(2) 0.4795(7) 0.0653(18) Uani 1 1 d . . . H22 H 0.9117 0.4388 0.5082 0.078 Uiso 1 1 calc R . . C11 C -0.6297(11) 0.1815(3) 0.2537(9) 0.080(2) Uani 1 1 d . . . H11 H -0.6826 0.1624 0.2903 0.096 Uiso 1 1 calc R . . C12 C -0.7171(10) 0.2038(3) 0.1457(10) 0.090(2) Uani 1 1 d . . . H12 H -0.8294 0.1998 0.1078 0.108 Uiso 1 1 calc R . . C6 C -0.1239(14) 0.2851(2) 0.1451(8) 0.092(3) Uani 1 1 d . . . H6 H -0.1147 0.2679 0.0781 0.111 Uiso 1 1 calc R . . C13 C -0.6423(11) 0.2328(2) 0.0905(8) 0.087(3) Uani 1 1 d . . . H13 H -0.7034 0.2489 0.0176 0.105 Uiso 1 1 calc R . . C29 C 0.5312(9) 0.3463(2) 0.8474(7) 0.0691(19) Uani 1 1 d . . . H29 H 0.5467 0.3224 0.9005 0.083 Uiso 1 1 calc R . . C4 C -0.2841(12) 0.3115(3) 0.2661(8) 0.088(3) Uani 1 1 d . . . H4 H -0.3818 0.3120 0.2818 0.106 Uiso 1 1 calc R . . C30 C 0.5392(9) 0.40936(19) 0.7804(6) 0.0548(14) Uani 1 1 d . . . H30 H 0.5629 0.4380 0.7808 0.066 Uiso 1 1 calc R . . O1W O 0.4194(13) 0.2869(3) 0.4039(11) 0.170(4) 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 Ni1 0.0461(3) 0.0395(3) 0.0292(3) 0.0011(3) 0.0132(2) 0.0075(3) O6 0.050(2) 0.0405(18) 0.0310(19) -0.0029(15) 0.0103(15) 0.0064(15) O5 0.056(2) 0.0451(19) 0.0306(19) 0.0017(15) 0.0135(17) 0.0098(16) O1 0.069(3) 0.050(2) 0.048(3) -0.0025(18) 0.022(2) 0.0076(19) O2 0.058(2) 0.046(2) 0.044(2) -0.0053(17) 0.0174(18) -0.0008(16) N2 0.039(2) 0.067(3) 0.042(3) -0.008(2) 0.014(2) 0.005(2) N1 0.045(2) 0.059(3) 0.037(3) 0.004(2) 0.015(2) 0.012(2) O3 0.153(5) 0.034(2) 0.046(3) -0.0019(19) 0.011(3) 0.000(3) C16 0.050(3) 0.044(3) 0.032(3) 0.000(2) 0.016(2) -0.002(2) N4 0.054(3) 0.056(3) 0.032(2) 0.003(2) 0.011(2) 0.012(2) C20 0.033(2) 0.041(2) 0.032(3) 0.003(2) 0.010(2) 0.0033(18) C15 0.077(4) 0.042(3) 0.038(3) -0.008(2) 0.022(3) 0.003(3) N3 0.054(3) 0.045(3) 0.035(2) 0.004(2) 0.018(2) 0.007(2) C1 0.072(4) 0.038(3) 0.031(3) 0.006(2) 0.013(3) 0.002(2) C2 0.093(5) 0.043(3) 0.039(3) 0.005(2) 0.017(3) -0.012(3) C23 0.039(3) 0.056(3) 0.039(3) 0.002(2) 0.011(2) 0.005(2) C14 0.070(4) 0.035(3) 0.042(3) 0.001(2) 0.016(3) -0.005(2) C17 0.034(2) 0.042(3) 0.031(3) 0.002(2) 0.0112(19) 0.0001(19) C19 0.064(3) 0.043(3) 0.032(3) 0.003(2) 0.018(2) -0.008(2) C25 0.056(3) 0.075(4) 0.048(3) -0.006(3) 0.028(3) -0.003(3) C9 0.070(4) 0.056(3) 0.042(3) -0.007(3) 0.010(3) -0.007(3) C28 0.060(4) 0.054(3) 0.047(4) 0.010(3) 0.011(3) -0.002(3) C24 0.059(4) 0.074(4) 0.055(4) -0.008(3) 0.029(3) -0.011(3) C18 0.053(3) 0.039(3) 0.032(3) -0.002(2) 0.016(2) -0.003(2) O4 0.179(6) 0.113(5) 0.042(3) 0.006(3) 0.011(3) -0.089(5) C26 0.050(3) 0.079(4) 0.043(3) -0.006(3) 0.015(3) 0.011(3) C10 0.088(5) 0.036(3) 0.043(3) 0.001(2) 0.023(3) 0.003(3) C21 0.057(4) 0.094(5) 0.039(3) 0.015(3) 0.018(3) 0.034(3) C3 0.110(6) 0.068(4) 0.051(4) -0.007(3) 0.036(4) -0.042(4) C7 0.121(6) 0.044(3) 0.054(4) -0.004(3) 0.027(4) -0.009(3) C27 0.060(4) 0.080(4) 0.036(3) 0.001(3) 0.007(3) 0.015(3) C8 0.115(6) 0.044(3) 0.040(4) -0.001(3) 0.012(4) -0.022(3) C5 0.133(8) 0.082(5) 0.043(4) 0.007(3) 0.012(4) -0.063(5) C22 0.032(4) 0.104(5) 0.054(4) -0.003(4) 0.008(3) 0.018(3) C11 0.084(5) 0.082(5) 0.071(5) 0.002(4) 0.023(4) -0.026(4) C12 0.067(5) 0.087(6) 0.103(7) 0.001(5) 0.016(5) -0.007(4) C6 0.155(9) 0.053(4) 0.049(4) -0.006(3) 0.014(5) -0.031(5) C13 0.109(6) 0.052(4) 0.058(4) 0.001(3) -0.022(4) 0.015(4) C29 0.084(5) 0.057(4) 0.054(4) 0.020(3) 0.010(3) -0.002(3) C4 0.114(7) 0.095(6) 0.050(5) 0.007(4) 0.023(5) -0.048(5) C30 0.075(4) 0.045(3) 0.040(3) 0.010(2) 0.015(3) 0.003(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N3 2.011(4) . ? Ni1 N1 2.060(5) . ? Ni1 O5 2.083(3) 3 ? Ni1 O1 2.125(4) . ? Ni1 O2 2.134(4) . ? Ni1 O6 2.148(3) 3 ? Ni1 C20 2.447(5) 3 ? Ni1 C1 2.467(6) . ? O6 C20 1.259(6) . ? O6 Ni1 2.148(3) 3_445 ? O5 C20 1.265(6) . ? O5 Ni1 2.083(3) 3_445 ? O1 C1 1.270(7) . ? O2 C1 1.267(7) . ? N2 C23 1.347(7) . ? N2 C22 1.364(8) . ? N2 C24 1.466(8) . ? N1 C23 1.316(7) . ? N1 C21 1.366(8) . ? O3 C14 1.377(7) . ? O3 C10 1.378(8) . ? C16 C15 1.374(8) . ? C16 C17 1.383(7) . ? C16 H16 0.9300 . ? N4 C30 1.329(7) . ? N4 C29 1.352(8) . ? N4 C27 1.458(7) 1_556 ? C20 C17 1.487(7) . ? C20 Ni1 2.447(5) 3_445 ? C15 C14 1.362(8) . ? C15 H15 0.9300 . ? N3 C30 1.294(8) . ? N3 C28 1.369(7) . ? C1 C2 1.487(8) . ? C2 C3 1.360(11) . ? C2 C7 1.400(10) . ? C23 H23 0.9300 . ? C14 C19 1.397(8) . ? C17 C18 1.399(7) . ? C19 C18 1.379(8) . ? C19 H19 0.9300 . ? C25 C26 1.512(9) . ? C25 C24 1.514(8) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C9 C10 1.362(9) . ? C9 C8 1.395(9) . ? C9 H9 0.9300 . ? C28 C29 1.347(9) . ? C28 H28 0.9300 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C18 H18 0.9300 . ? O4 C8 1.355(9) . ? O4 C5 1.399(9) . ? C26 C27 1.534(9) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C10 C11 1.326(11) . ? C21 C22 1.328(10) . ? C21 H21 0.9300 . ? C3 C4 1.400(10) . ? C3 H3 0.9300 . ? C7 C6 1.390(11) . ? C7 H7 0.9300 . ? C27 N4 1.458(7) 1_554 ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C8 C13 1.381(12) . ? C5 C6 1.355(14) . ? C5 C4 1.379(14) . ? C22 H22 0.9300 . ? C11 C12 1.343(12) . ? C11 H11 0.9300 . ? C12 C13 1.380(12) . ? C12 H12 0.9300 . ? C6 H6 0.9300 . ? C13 H13 0.9300 . ? C29 H29 0.9300 . ? C4 H4 0.9300 . ? C30 H30 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Ni1 N1 96.72(18) . . ? N3 Ni1 O5 96.60(16) . 3 ? N1 Ni1 O5 94.20(17) . 3 ? N3 Ni1 O1 99.11(19) . . ? N1 Ni1 O1 99.96(18) . . ? O5 Ni1 O1 157.40(15) 3 . ? N3 Ni1 O2 92.04(17) . . ? N1 Ni1 O2 160.93(16) . . ? O5 Ni1 O2 101.61(15) 3 . ? O1 Ni1 O2 61.80(15) . . ? N3 Ni1 O6 158.45(15) . 3 ? N1 Ni1 O6 88.32(16) . 3 ? O5 Ni1 O6 62.05(13) 3 3 ? O1 Ni1 O6 100.63(16) . 3 ? O2 Ni1 O6 89.71(15) . 3 ? N3 Ni1 C20 127.72(17) . 3 ? N1 Ni1 C20 90.61(17) . 3 ? O5 Ni1 C20 31.13(14) 3 3 ? O1 Ni1 C20 130.46(17) . 3 ? O2 Ni1 C20 97.39(15) . 3 ? O6 Ni1 C20 30.94(14) 3 3 ? N3 Ni1 C1 98.18(18) . . ? N1 Ni1 C1 130.5(2) . . ? O5 Ni1 C1 130.25(18) 3 . ? O1 Ni1 C1 30.99(18) . . ? O2 Ni1 C1 30.90(17) . . ? O6 Ni1 C1 94.31(16) 3 . ? C20 Ni1 C1 115.50(17) 3 . ? C20 O6 Ni1 87.8(3) . 3_445 ? C20 O5 Ni1 90.5(3) . 3_445 ? C1 O1 Ni1 89.5(3) . . ? C1 O2 Ni1 89.2(4) . . ? C23 N2 C22 107.0(5) . . ? C23 N2 C24 126.7(5) . . ? C22 N2 C24 126.1(5) . . ? C23 N1 C21 104.7(5) . . ? C23 N1 Ni1 126.0(4) . . ? C21 N1 Ni1 129.3(4) . . ? C14 O3 C10 119.0(5) . . ? C15 C16 C17 120.5(5) . . ? C15 C16 H16 119.7 . . ? C17 C16 H16 119.7 . . ? C30 N4 C29 105.5(5) . . ? C30 N4 C27 125.5(5) . 1_556 ? C29 N4 C27 128.8(5) . 1_556 ? O6 C20 O5 119.6(4) . . ? O6 C20 C17 120.8(4) . . ? O5 C20 C17 119.6(4) . . ? O6 C20 Ni1 61.3(2) . 3_445 ? O5 C20 Ni1 58.4(2) . 3_445 ? C17 C20 Ni1 175.1(3) . 3_445 ? C14 C15 C16 119.6(5) . . ? C14 C15 H15 120.2 . . ? C16 C15 H15 120.2 . . ? C30 N3 C28 105.1(5) . . ? C30 N3 Ni1 121.9(4) . . ? C28 N3 Ni1 132.7(4) . . ? O2 C1 O1 119.1(5) . . ? O2 C1 C2 119.6(6) . . ? O1 C1 C2 121.2(5) . . ? O2 C1 Ni1 59.9(3) . . ? O1 C1 Ni1 59.5(3) . . ? C2 C1 Ni1 173.0(4) . . ? C3 C2 C7 119.5(7) . . ? C3 C2 C1 119.7(6) . . ? C7 C2 C1 120.7(7) . . ? N1 C23 N2 111.2(5) . . ? N1 C23 H23 124.4 . . ? N2 C23 H23 124.4 . . ? C15 C14 O3 116.2(5) . . ? C15 C14 C19 121.7(5) . . ? O3 C14 C19 122.1(5) . . ? C16 C17 C18 119.4(5) . . ? C16 C17 C20 120.1(4) . . ? C18 C17 C20 120.3(4) . . ? C18 C19 C14 118.3(5) . . ? C18 C19 H19 120.8 . . ? C14 C19 H19 120.8 . . ? C26 C25 C24 112.7(5) . . ? C26 C25 H25A 109.1 . . ? C24 C25 H25A 109.1 . . ? C26 C25 H25B 109.1 . . ? C24 C25 H25B 109.1 . . ? H25A C25 H25B 107.8 . . ? C10 C9 C8 119.2(7) . . ? C10 C9 H9 120.4 . . ? C8 C9 H9 120.4 . . ? C29 C28 N3 108.5(6) . . ? C29 C28 H28 125.8 . . ? N3 C28 H28 125.8 . . ? N2 C24 C25 112.2(5) . . ? N2 C24 H24A 109.2 . . ? C25 C24 H24A 109.2 . . ? N2 C24 H24B 109.2 . . ? C25 C24 H24B 109.2 . . ? H24A C24 H24B 107.9 . . ? C19 C18 C17 120.4(4) . . ? C19 C18 H18 119.8 . . ? C17 C18 H18 119.8 . . ? C8 O4 C5 116.1(6) . . ? C25 C26 C27 110.4(5) . . ? C25 C26 H26A 109.6 . . ? C27 C26 H26A 109.6 . . ? C25 C26 H26B 109.6 . . ? C27 C26 H26B 109.6 . . ? H26A C26 H26B 108.1 . . ? C11 C10 C9 121.2(7) . . ? C11 C10 O3 121.7(7) . . ? C9 C10 O3 116.9(6) . . ? C22 C21 N1 111.2(6) . . ? C22 C21 H21 124.4 . . ? N1 C21 H21 124.4 . . ? C2 C3 C4 121.3(8) . . ? C2 C3 H3 119.3 . . ? C4 C3 H3 119.3 . . ? C6 C7 C2 119.0(9) . . ? C6 C7 H7 120.5 . . ? C2 C7 H7 120.5 . . ? N4 C27 C26 113.5(5) 1_554 . ? N4 C27 H27A 108.9 1_554 . ? C26 C27 H27A 108.9 . . ? N4 C27 H27B 108.9 1_554 . ? C26 C27 H27B 108.9 . . ? H27A C27 H27B 107.7 . . ? O4 C8 C13 119.0(7) . . ? O4 C8 C9 121.7(8) . . ? C13 C8 C9 119.2(7) . . ? C6 C5 C4 121.0(7) . . ? C6 C5 O4 118.7(9) . . ? C4 C5 O4 120.0(11) . . ? C21 C22 N2 106.0(5) . . ? C21 C22 H22 127.0 . . ? N2 C22 H22 127.0 . . ? C10 C11 C12 121.0(8) . . ? C10 C11 H11 119.5 . . ? C12 C11 H11 119.5 . . ? C11 C12 C13 120.8(8) . . ? C11 C12 H12 119.6 . . ? C13 C12 H12 119.6 . . ? C5 C6 C7 120.8(8) . . ? C5 C6 H6 119.6 . . ? C7 C6 H6 119.6 . . ? C12 C13 C8 118.7(7) . . ? C12 C13 H13 120.7 . . ? C8 C13 H13 120.7 . . ? C28 C29 N4 107.6(5) . . ? C28 C29 H29 126.2 . . ? N4 C29 H29 126.2 . . ? C5 C4 C3 118.4(9) . . ? C5 C4 H4 120.8 . . ? C3 C4 H4 120.8 . . ? N3 C30 N4 113.3(5) . . ? N3 C30 H30 123.4 . . ? N4 C30 H30 123.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Ni1 O1 C1 90.7(3) . . . . ? N1 Ni1 O1 C1 -170.7(3) . . . . ? O5 Ni1 O1 C1 -42.8(6) 3 . . . ? O2 Ni1 O1 C1 3.3(3) . . . . ? O6 Ni1 O1 C1 -80.6(3) 3 . . . ? C20 Ni1 O1 C1 -71.3(4) 3 . . . ? N3 Ni1 O2 C1 -102.6(3) . . . . ? N1 Ni1 O2 C1 14.9(7) . . . . ? O5 Ni1 O2 C1 160.3(3) 3 . . . ? O1 Ni1 O2 C1 -3.3(3) . . . . ? O6 Ni1 O2 C1 98.9(3) 3 . . . ? C20 Ni1 O2 C1 129.0(3) 3 . . . ? N3 Ni1 N1 C23 -174.9(5) . . . . ? O5 Ni1 N1 C23 -77.8(5) 3 . . . ? O1 Ni1 N1 C23 84.5(5) . . . . ? O2 Ni1 N1 C23 68.3(8) . . . . ? O6 Ni1 N1 C23 -16.0(5) 3 . . . ? C20 Ni1 N1 C23 -46.8(5) 3 . . . ? C1 Ni1 N1 C23 78.3(5) . . . . ? N3 Ni1 N1 C21 7.5(6) . . . . ? O5 Ni1 N1 C21 104.6(5) 3 . . . ? O1 Ni1 N1 C21 -93.0(5) . . . . ? O2 Ni1 N1 C21 -109.3(6) . . . . ? O6 Ni1 N1 C21 166.5(5) 3 . . . ? C20 Ni1 N1 C21 135.6(5) 3 . . . ? C1 Ni1 N1 C21 -99.3(5) . . . . ? Ni1 O6 C20 O5 -2.8(4) 3_445 . . . ? Ni1 O6 C20 C17 174.9(4) 3_445 . . . ? Ni1 O5 C20 O6 2.9(4) 3_445 . . . ? Ni1 O5 C20 C17 -174.8(4) 3_445 . . . ? C17 C16 C15 C14 -0.8(8) . . . . ? N1 Ni1 N3 C30 65.0(5) . . . . ? O5 Ni1 N3 C30 -30.1(5) 3 . . . ? O1 Ni1 N3 C30 166.2(5) . . . . ? O2 Ni1 N3 C30 -132.0(5) . . . . ? O6 Ni1 N3 C30 -37.6(8) 3 . . . ? C20 Ni1 N3 C30 -31.0(6) 3 . . . ? C1 Ni1 N3 C30 -162.4(5) . . . . ? N1 Ni1 N3 C28 -120.6(5) . . . . ? O5 Ni1 N3 C28 144.4(5) 3 . . . ? O1 Ni1 N3 C28 -19.3(6) . . . . ? O2 Ni1 N3 C28 42.4(5) . . . . ? O6 Ni1 N3 C28 136.8(5) 3 . . . ? C20 Ni1 N3 C28 143.4(5) 3 . . . ? C1 Ni1 N3 C28 12.0(6) . . . . ? Ni1 O2 C1 O1 5.6(5) . . . . ? Ni1 O2 C1 C2 -172.0(4) . . . . ? Ni1 O1 C1 O2 -5.7(5) . . . . ? Ni1 O1 C1 C2 171.9(5) . . . . ? N3 Ni1 C1 O2 80.2(3) . . . . ? N1 Ni1 C1 O2 -173.7(3) . . . . ? O5 Ni1 C1 O2 -25.7(4) 3 . . . ? O1 Ni1 C1 O2 174.3(5) . . . . ? O6 Ni1 C1 O2 -82.2(3) 3 . . . ? C20 Ni1 C1 O2 -58.7(3) 3 . . . ? N3 Ni1 C1 O1 -94.1(3) . . . . ? N1 Ni1 C1 O1 12.0(4) . . . . ? O5 Ni1 C1 O1 160.0(3) 3 . . . ? O2 Ni1 C1 O1 -174.3(5) . . . . ? O6 Ni1 C1 O1 103.5(3) 3 . . . ? C20 Ni1 C1 O1 127.0(3) 3 . . . ? N3 Ni1 C1 C2 168(4) . . . . ? N1 Ni1 C1 C2 -86(4) . . . . ? O5 Ni1 C1 C2 62(4) 3 . . . ? O1 Ni1 C1 C2 -98(4) . . . . ? O2 Ni1 C1 C2 88(4) . . . . ? O6 Ni1 C1 C2 5(4) 3 . . . ? C20 Ni1 C1 C2 29(4) 3 . . . ? O2 C1 C2 C3 -1.0(9) . . . . ? O1 C1 C2 C3 -178.5(6) . . . . ? Ni1 C1 C2 C3 -85(4) . . . . ? O2 C1 C2 C7 176.0(5) . . . . ? O1 C1 C2 C7 -1.6(9) . . . . ? Ni1 C1 C2 C7 92(4) . . . . ? C21 N1 C23 N2 0.2(6) . . . . ? Ni1 N1 C23 N2 -177.9(4) . . . . ? C22 N2 C23 N1 -0.7(7) . . . . ? C24 N2 C23 N1 174.5(5) . . . . ? C16 C15 C14 O3 -174.8(5) . . . . ? C16 C15 C14 C19 2.4(9) . . . . ? C10 O3 C14 C15 -155.6(6) . . . . ? C10 O3 C14 C19 27.2(10) . . . . ? C15 C16 C17 C18 -0.4(7) . . . . ? C15 C16 C17 C20 175.3(5) . . . . ? O6 C20 C17 C16 167.7(5) . . . . ? O5 C20 C17 C16 -14.7(7) . . . . ? Ni1 C20 C17 C16 -79(4) 3_445 . . . ? O6 C20 C17 C18 -16.7(7) . . . . ? O5 C20 C17 C18 160.9(5) . . . . ? Ni1 C20 C17 C18 97(4) 3_445 . . . ? C15 C14 C19 C18 -2.7(9) . . . . ? O3 C14 C19 C18 174.4(6) . . . . ? C30 N3 C28 C29 -0.5(7) . . . . ? Ni1 N3 C28 C29 -175.6(5) . . . . ? C23 N2 C24 C25 -106.3(7) . . . . ? C22 N2 C24 C25 68.1(8) . . . . ? C26 C25 C24 N2 73.7(7) . . . . ? C14 C19 C18 C17 1.4(8) . . . . ? C16 C17 C18 C19 0.1(7) . . . . ? C20 C17 C18 C19 -175.6(4) . . . . ? C24 C25 C26 C27 -175.2(5) . . . . ? C8 C9 C10 C11 1.1(10) . . . . ? C8 C9 C10 O3 -173.7(6) . . . . ? C14 O3 C10 C11 67.8(9) . . . . ? C14 O3 C10 C9 -117.4(7) . . . . ? C23 N1 C21 C22 0.4(8) . . . . ? Ni1 N1 C21 C22 178.4(5) . . . . ? C7 C2 C3 C4 0.1(11) . . . . ? C1 C2 C3 C4 177.1(6) . . . . ? C3 C2 C7 C6 0.5(10) . . . . ? C1 C2 C7 C6 -176.5(6) . . . . ? C25 C26 C27 N4 -158.9(6) . . . 1_554 ? C5 O4 C8 C13 143.7(9) . . . . ? C5 O4 C8 C9 -40.5(12) . . . . ? C10 C9 C8 O4 -175.6(7) . . . . ? C10 C9 C8 C13 0.2(10) . . . . ? C8 O4 C5 C6 130.5(9) . . . . ? C8 O4 C5 C4 -55.2(12) . . . . ? N1 C21 C22 N2 -0.8(8) . . . . ? C23 N2 C22 C21 0.9(7) . . . . ? C24 N2 C22 C21 -174.4(6) . . . . ? C9 C10 C11 C12 -0.7(12) . . . . ? O3 C10 C11 C12 173.9(8) . . . . ? C10 C11 C12 C13 -1.0(14) . . . . ? C4 C5 C6 C7 1.1(13) . . . . ? O4 C5 C6 C7 175.2(7) . . . . ? C2 C7 C6 C5 -1.1(11) . . . . ? C11 C12 C13 C8 2.2(14) . . . . ? O4 C8 C13 C12 174.1(8) . . . . ? C9 C8 C13 C12 -1.8(12) . . . . ? N3 C28 C29 N4 -0.8(8) . . . . ? C30 N4 C29 C28 1.7(8) . . . . ? C27 N4 C29 C28 -172.5(6) 1_556 . . . ? C6 C5 C4 C3 -0.4(13) . . . . ? O4 C5 C4 C3 -174.5(7) . . . . ? C2 C3 C4 C5 -0.2(12) . . . . ? C28 N3 C30 N4 1.7(7) . . . . ? Ni1 N3 C30 N4 177.4(4) . . . . ? C29 N4 C30 N3 -2.1(8) . . . . ? C27 N4 C30 N3 172.3(5) 1_556 . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.381 _refine_diff_density_min -0.296 _refine_diff_density_rms 0.110 _database_code_depnum_ccdc_archive 'CCDC 933677' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_cncnc5 #TrackingRef 'cncnc5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C33 H26 N2 Ni O6' _chemical_formula_sum 'C33 H26 N2 Ni O6' _chemical_formula_weight 605.27 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 orthorhombic _symmetry_space_group_name_H-M Fdd2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/4, y+1/4, z+1/4' 'x+1/4, -y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' '-x+1/4, y+3/4, z+3/4' 'x+1/4, -y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' '-x+3/4, y+1/4, z+3/4' 'x+3/4, -y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' '-x+3/4, y+3/4, z+1/4' 'x+3/4, -y+3/4, z+1/4' _cell_length_a 18.281(2) _cell_length_b 36.104(4) _cell_length_c 17.145(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 11316(2) _cell_formula_units_Z 16 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6234 _cell_measurement_theta_min 1.61 _cell_measurement_theta_max 26.02 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.421 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5024 _exptl_absorpt_coefficient_mu 0.735 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.816 _exptl_absorpt_correction_T_max 0.854 _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 17568 _diffrn_reflns_av_R_equivalents 0.0626 _diffrn_reflns_av_sigmaI/netI 0.0808 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 48 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 28.30 _reflns_number_total 6234 _reflns_number_gt 3888 _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^)+(0.0401P)^2^+7.0207P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.448(15) _refine_ls_number_reflns 6234 _refine_ls_number_parameters 379 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1008 _refine_ls_R_factor_gt 0.0489 _refine_ls_wR_factor_ref 0.1078 _refine_ls_wR_factor_gt 0.0911 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _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 0.45110(3) 0.216938(14) 0.07788(3) 0.03818(14) Uani 1 1 d . . . O5 O 0.50517(15) 0.19433(8) 0.98208(16) 0.0394(7) Uani 1 1 d . . . O4 O 0.46723(19) 0.06300(8) 0.73819(18) 0.0541(8) Uani 1 1 d . . . O1 O 0.48641(18) 0.17575(8) 0.15571(18) 0.0501(8) Uani 1 1 d . . . O2 O 0.39623(16) 0.21338(8) 0.18501(17) 0.0475(8) Uani 1 1 d . . . O3 O 0.4611(2) 0.14251(9) 0.51786(18) 0.0625(10) Uani 1 1 d . . . O6 O 0.39420(16) 0.17565(8) 1.01151(18) 0.0474(8) Uani 1 1 d . . . N1 N 0.39942(19) 0.25732(10) 0.0131(2) 0.0426(9) Uani 1 1 d . . . N2 N 0.52964(19) 0.25246(10) 0.1221(2) 0.0415(9) Uani 1 1 d . . . C13 C 0.4649(2) 0.10344(12) 0.6251(3) 0.0402(11) Uani 1 1 d . . . H13 H 0.4771 0.1241 0.6550 0.048 Uiso 1 1 calc R . . C8 C 0.4543(2) 0.10665(13) 0.5454(3) 0.0418(12) Uani 1 1 d . . . C1 C 0.4403(3) 0.18748(13) 0.2039(3) 0.0439(11) Uani 1 1 d . . . C14 C 0.4622(3) 0.09258(11) 0.7907(2) 0.0403(11) Uani 1 1 d . . . C17 C 0.4548(2) 0.14538(11) 0.9063(2) 0.0327(9) Uani 1 1 d . . . C12 C 0.4572(2) 0.06937(12) 0.6591(3) 0.0386(10) Uani 1 1 d . . . C23 C 0.3229(3) 0.30335(12) -0.0913(3) 0.0472(12) Uani 1 1 d . . . C5 C 0.4542(3) 0.15095(13) 0.4380(3) 0.0489(12) Uani 1 1 d . . . C31 C 0.6373(3) 0.29630(12) 0.1950(3) 0.0452(11) Uani 1 1 d . . . C3 C 0.4915(3) 0.14574(13) 0.3062(3) 0.0547(13) Uani 1 1 d . . . H3 H 0.5201 0.1346 0.2680 0.066 Uiso 1 1 calc R . . C16 C 0.3965(3) 0.12201(12) 0.8918(3) 0.0452(11) Uani 1 1 d . . . H16 H 0.3543 0.1241 0.9217 0.054 Uiso 1 1 calc R . . C11 C 0.4390(3) 0.03855(12) 0.6157(3) 0.0453(12) Uani 1 1 d . . . H11 H 0.4334 0.0155 0.6393 0.054 Uiso 1 1 calc R . . C2 C 0.4422(2) 0.17340(12) 0.2857(2) 0.0423(10) Uani 1 1 d . . . C18 C 0.5172(2) 0.14235(12) 0.8602(2) 0.0403(11) Uani 1 1 d . . . H18 H 0.5563 0.1584 0.8679 0.048 Uiso 1 1 calc R . . C9 C 0.4357(3) 0.07667(13) 0.5002(3) 0.0498(12) Uani 1 1 d . . . H9 H 0.4276 0.0792 0.4469 0.060 Uiso 1 1 calc R . . C19 C 0.5210(2) 0.11550(12) 0.8033(2) 0.0439(11) Uani 1 1 d . . . H19 H 0.5632 0.1129 0.7735 0.053 Uiso 1 1 calc R . . C10 C 0.4294(3) 0.04268(13) 0.5367(3) 0.0505(13) Uani 1 1 d . . . H10 H 0.4182 0.0219 0.5069 0.061 Uiso 1 1 calc R . . C7 C 0.3987(3) 0.18898(12) 0.3424(3) 0.0494(12) Uani 1 1 d . . . H7 H 0.3651 0.2072 0.3289 0.059 Uiso 1 1 calc R . . C20 C 0.4508(2) 0.17316(12) 0.9701(2) 0.0384(10) Uani 1 1 d . . . C33 C 0.5971(2) 0.25474(12) 0.0945(3) 0.0447(11) Uani 1 1 d . . . H33 H 0.6084 0.2414 0.0496 0.054 Uiso 1 1 calc R . . C28 C 0.1936(3) 0.31972(13) -0.2650(3) 0.0550(13) Uani 1 1 d . . . H28A H 0.1715 0.3431 -0.2504 0.066 Uiso 1 1 calc R . . H28B H 0.2328 0.3250 -0.3015 0.066 Uiso 1 1 calc R . . C15 C 0.3996(2) 0.09575(12) 0.8341(3) 0.0489(11) Uani 1 1 d . . . H15 H 0.3599 0.0803 0.8247 0.059 Uiso 1 1 calc R . . C6 C 0.4045(3) 0.17793(12) 0.4187(3) 0.0524(12) Uani 1 1 d . . . H6 H 0.3751 0.1886 0.4569 0.063 Uiso 1 1 calc R . . C32 C 0.6513(3) 0.27545(12) 0.1279(3) 0.0519(12) Uani 1 1 d . . . H32 H 0.6977 0.2757 0.1058 0.062 Uiso 1 1 calc R . . C24 C 0.2972(3) 0.29658(13) -0.0174(3) 0.0576(13) Uani 1 1 d . . . H24 H 0.2538 0.3073 -0.0006 0.069 Uiso 1 1 calc R . . C22 C 0.3887(3) 0.28715(14) -0.1113(3) 0.0574(13) Uani 1 1 d . . . H22 H 0.4088 0.2913 -0.1603 0.069 Uiso 1 1 calc R . . C26 C 0.2812(3) 0.32594(12) -0.1501(3) 0.0567(14) Uani 1 1 d . . . H26A H 0.3150 0.3367 -0.1873 0.068 Uiso 1 1 calc R . . H26B H 0.2559 0.3460 -0.1237 0.068 Uiso 1 1 calc R . . C25 C 0.3365(3) 0.27361(13) 0.0321(3) 0.0555(13) Uani 1 1 d . . . H25 H 0.3177 0.2693 0.0816 0.067 Uiso 1 1 calc R . . C4 C 0.4981(3) 0.13470(14) 0.3831(3) 0.0599(14) Uani 1 1 d . . . H4 H 0.5318 0.1166 0.3973 0.072 Uiso 1 1 calc R . . C30 C 0.5672(3) 0.29436(16) 0.2220(3) 0.0680(16) Uani 1 1 d . . . H30 H 0.5540 0.3078 0.2661 0.082 Uiso 1 1 calc R . . C21 C 0.4246(3) 0.26463(13) -0.0580(3) 0.0565(14) Uani 1 1 d . . . H21 H 0.4688 0.2540 -0.0728 0.068 Uiso 1 1 calc R . . C29 C 0.5158(3) 0.27292(15) 0.1852(3) 0.0657(16) Uani 1 1 d . . . H29 H 0.4685 0.2726 0.2054 0.079 Uiso 1 1 calc R . . C27 C 0.2257(3) 0.30187(13) -0.1931(3) 0.0595(15) Uani 1 1 d . . . H27A H 0.2493 0.2789 -0.2081 0.071 Uiso 1 1 calc R . . H27B H 0.1862 0.2957 -0.1576 0.071 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0444(3) 0.0415(3) 0.0286(2) -0.0014(3) -0.0018(3) 0.0047(3) O5 0.0400(16) 0.0447(17) 0.0334(17) -0.0037(14) -0.0054(13) -0.0025(14) O4 0.093(2) 0.0362(16) 0.0328(17) -0.0003(14) -0.0082(17) -0.0001(17) O1 0.067(2) 0.0539(19) 0.0299(17) 0.0000(15) 0.0072(16) 0.0173(17) O2 0.0529(19) 0.054(2) 0.0359(18) 0.0014(15) 0.0038(14) 0.0101(16) O3 0.111(3) 0.0468(19) 0.0296(18) 0.0021(15) -0.0025(18) -0.0112(19) O6 0.0477(18) 0.0518(19) 0.0426(19) -0.0043(15) 0.0111(15) -0.0017(15) N1 0.044(2) 0.047(2) 0.037(2) 0.0016(18) -0.0043(17) 0.0012(19) N2 0.043(2) 0.044(2) 0.037(2) -0.0054(17) -0.0028(16) 0.0037(18) C13 0.048(3) 0.035(3) 0.038(3) -0.005(2) -0.002(2) -0.006(2) C8 0.056(3) 0.037(3) 0.033(2) 0.001(2) 0.006(2) -0.003(2) C1 0.050(3) 0.049(3) 0.032(3) -0.001(2) 0.006(2) 0.001(2) C14 0.064(3) 0.032(2) 0.026(2) 0.0004(18) -0.006(2) -0.002(2) C17 0.036(2) 0.036(2) 0.026(2) -0.0004(17) -0.0017(17) -0.0019(19) C12 0.048(3) 0.039(3) 0.029(2) -0.003(2) 0.001(2) 0.002(2) C23 0.046(3) 0.042(3) 0.054(3) 0.001(2) -0.015(2) -0.003(2) C5 0.076(3) 0.047(3) 0.023(2) 0.002(2) 0.004(2) -0.012(3) C31 0.058(3) 0.037(2) 0.041(3) -0.001(2) -0.006(2) -0.002(2) C3 0.064(3) 0.059(3) 0.041(3) 0.008(2) 0.013(2) 0.013(3) C16 0.048(3) 0.048(3) 0.040(3) 0.001(2) 0.003(2) -0.006(2) C11 0.061(3) 0.030(2) 0.045(3) -0.006(2) -0.005(2) -0.002(2) C2 0.051(3) 0.048(3) 0.028(2) 0.001(2) 0.006(2) 0.001(2) C18 0.044(3) 0.041(2) 0.036(3) -0.003(2) 0.005(2) -0.009(2) C9 0.067(3) 0.050(3) 0.032(3) -0.001(2) -0.006(2) -0.004(3) C19 0.051(3) 0.047(3) 0.034(3) -0.005(2) 0.0123(19) -0.004(2) C10 0.070(3) 0.041(3) 0.040(3) -0.014(2) -0.009(2) -0.001(2) C7 0.066(3) 0.045(2) 0.037(3) 0.005(2) 0.009(2) 0.006(2) C20 0.046(3) 0.044(3) 0.025(2) 0.0031(19) -0.005(2) 0.005(2) C33 0.059(3) 0.042(2) 0.033(3) -0.007(2) 0.005(2) -0.002(2) C28 0.062(3) 0.055(3) 0.048(3) 0.008(2) -0.014(2) -0.009(3) C15 0.052(3) 0.048(3) 0.047(3) -0.001(3) -0.009(3) -0.011(2) C6 0.074(3) 0.042(3) 0.041(3) -0.001(2) 0.015(3) -0.001(3) C32 0.048(3) 0.054(3) 0.054(3) -0.005(2) 0.008(2) -0.001(2) C24 0.061(3) 0.058(3) 0.054(3) 0.000(3) -0.006(3) 0.019(3) C22 0.063(3) 0.061(3) 0.049(3) 0.019(3) -0.002(2) 0.003(3) C26 0.060(3) 0.048(3) 0.061(4) 0.006(2) -0.024(2) -0.002(2) C25 0.064(3) 0.057(3) 0.046(3) -0.004(2) -0.001(2) 0.013(3) C4 0.075(4) 0.061(3) 0.043(3) 0.012(3) 0.005(3) 0.014(3) C30 0.072(4) 0.082(4) 0.051(3) -0.041(3) 0.008(3) -0.011(3) C21 0.051(3) 0.056(3) 0.062(4) 0.018(3) 0.011(3) 0.002(2) C29 0.045(3) 0.084(4) 0.068(4) -0.038(3) 0.006(3) 0.002(3) C27 0.062(3) 0.052(3) 0.065(4) 0.017(3) -0.025(3) -0.013(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 Ni1 N1 2.062(3) . ? Ni1 N2 2.069(4) . ? Ni1 O5 2.083(3) 1_554 ? Ni1 O2 2.097(3) . ? Ni1 O1 2.100(3) . ? Ni1 O6 2.144(3) 1_554 ? Ni1 C1 2.416(5) . ? Ni1 C20 2.431(4) 1_554 ? O5 C20 1.270(5) . ? O5 Ni1 2.083(3) 1_556 ? O4 C12 1.387(5) . ? O4 C14 1.400(5) . ? O1 C1 1.254(5) . ? O2 C1 1.275(5) . ? O3 C8 1.384(5) . ? O3 C5 1.409(5) . ? O6 C20 1.258(5) . ? O6 Ni1 2.145(3) 1_556 ? N1 C21 1.329(6) . ? N1 C25 1.332(5) . ? N2 C33 1.324(5) . ? N2 C29 1.334(6) . ? C13 C12 1.369(6) . ? C13 C8 1.386(5) . ? C13 H13 0.9300 . ? C8 C9 1.374(6) . ? C1 C2 1.492(6) . ? C14 C15 1.370(6) . ? C14 C19 1.374(6) . ? C17 C16 1.382(6) . ? C17 C18 1.393(6) . ? C17 C20 1.486(6) . ? C12 C11 1.379(6) . ? C23 C24 1.374(7) . ? C23 C22 1.380(7) . ? C23 C26 1.505(6) . ? C5 C4 1.369(6) . ? C5 C6 1.372(6) . ? C31 C30 1.365(6) . ? C31 C32 1.398(6) . ? C31 C28 1.499(6) 9 ? C3 C4 1.384(6) . ? C3 C2 1.390(6) . ? C3 H3 0.9300 . ? C16 C15 1.370(6) . ? C16 H16 0.9300 . ? C11 C10 1.373(6) . ? C11 H11 0.9300 . ? C2 C7 1.376(6) . ? C18 C19 1.378(6) . ? C18 H18 0.9300 . ? C9 C10 1.383(6) . ? C9 H9 0.9300 . ? C19 H19 0.9300 . ? C10 H10 0.9300 . ? C7 C6 1.372(6) . ? C7 H7 0.9300 . ? C20 Ni1 2.431(4) 1_556 ? C33 C32 1.366(6) . ? C33 H33 0.9300 . ? C28 C31 1.499(6) 9_454 ? C28 C27 1.510(6) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C15 H15 0.9300 . ? C6 H6 0.9300 . ? C32 H32 0.9300 . ? C24 C25 1.386(6) . ? C24 H24 0.9300 . ? C22 C21 1.389(6) . ? C22 H22 0.9300 . ? C26 C27 1.526(6) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C25 H25 0.9300 . ? C4 H4 0.9300 . ? C30 C29 1.371(7) . ? C30 H30 0.9300 . ? C21 H21 0.9300 . ? C29 H29 0.9300 . ? C27 H27A 0.9700 . ? C27 H27B 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 N1 Ni1 N2 94.42(13) . . ? N1 Ni1 O5 94.03(13) . 1_554 ? N2 Ni1 O5 101.70(13) . 1_554 ? N1 Ni1 O2 107.20(14) . . ? N2 Ni1 O2 92.78(13) . . ? O5 Ni1 O2 153.31(12) 1_554 . ? N1 Ni1 O1 169.70(14) . . ? N2 Ni1 O1 89.57(14) . . ? O5 Ni1 O1 94.45(11) 1_554 . ? O2 Ni1 O1 63.06(12) . . ? N1 Ni1 O6 89.07(13) . 1_554 ? N2 Ni1 O6 164.14(13) . 1_554 ? O5 Ni1 O6 62.58(11) 1_554 1_554 ? O2 Ni1 O6 100.96(12) . 1_554 ? O1 Ni1 O6 89.66(12) . 1_554 ? N1 Ni1 C1 139.03(16) . . ? N2 Ni1 C1 90.10(15) . . ? O5 Ni1 C1 124.84(14) 1_554 . ? O2 Ni1 C1 31.84(12) . . ? O1 Ni1 C1 31.26(13) . . ? O6 Ni1 C1 97.39(14) 1_554 . ? N1 Ni1 C20 92.85(14) . 1_554 ? N2 Ni1 C20 133.08(15) . 1_554 ? O5 Ni1 C20 31.49(12) 1_554 1_554 ? O2 Ni1 C20 128.67(14) . 1_554 ? O1 Ni1 C20 91.34(13) . 1_554 ? O6 Ni1 C20 31.12(12) 1_554 1_554 ? C1 Ni1 C20 113.16(16) . 1_554 ? C20 O5 Ni1 89.5(2) . 1_556 ? C12 O4 C14 119.5(3) . . ? C1 O1 Ni1 88.4(3) . . ? C1 O2 Ni1 88.0(3) . . ? C8 O3 C5 121.7(3) . . ? C20 O6 Ni1 87.1(3) . 1_556 ? C21 N1 C25 115.7(4) . . ? C21 N1 Ni1 118.4(3) . . ? C25 N1 Ni1 125.2(3) . . ? C33 N2 C29 115.6(4) . . ? C33 N2 Ni1 123.6(3) . . ? C29 N2 Ni1 120.6(3) . . ? C12 C13 C8 118.7(4) . . ? C12 C13 H13 120.6 . . ? C8 C13 H13 120.6 . . ? C9 C8 O3 124.5(4) . . ? C9 C8 C13 121.7(5) . . ? O3 C8 C13 113.7(4) . . ? O1 C1 O2 120.3(4) . . ? O1 C1 C2 119.2(4) . . ? O2 C1 C2 120.2(4) . . ? O1 C1 Ni1 60.3(2) . . ? O2 C1 Ni1 60.1(2) . . ? C2 C1 Ni1 171.3(3) . . ? C15 C14 C19 121.2(4) . . ? C15 C14 O4 117.9(4) . . ? C19 C14 O4 120.6(4) . . ? C16 C17 C18 118.8(4) . . ? C16 C17 C20 120.5(4) . . ? C18 C17 C20 120.7(4) . . ? C13 C12 C11 121.3(4) . . ? C13 C12 O4 123.5(4) . . ? C11 C12 O4 115.2(4) . . ? C24 C23 C22 116.9(4) . . ? C24 C23 C26 122.8(5) . . ? C22 C23 C26 120.3(5) . . ? C4 C5 C6 121.8(4) . . ? C4 C5 O3 121.5(5) . . ? C6 C5 O3 116.6(4) . . ? C30 C31 C32 115.1(4) . . ? C30 C31 C28 121.3(4) . 9 ? C32 C31 C28 123.7(5) . 9 ? C4 C3 C2 120.3(4) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C15 C16 C17 121.4(4) . . ? C15 C16 H16 119.3 . . ? C17 C16 H16 119.3 . . ? C10 C11 C12 118.4(5) . . ? C10 C11 H11 120.8 . . ? C12 C11 H11 120.8 . . ? C7 C2 C3 119.3(4) . . ? C7 C2 C1 120.8(4) . . ? C3 C2 C1 119.8(4) . . ? C19 C18 C17 119.9(4) . . ? C19 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? C8 C9 C10 117.7(4) . . ? C8 C9 H9 121.2 . . ? C10 C9 H9 121.2 . . ? C14 C19 C18 119.8(4) . . ? C14 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? C11 C10 C9 122.1(5) . . ? C11 C10 H10 118.9 . . ? C9 C10 H10 118.9 . . ? C6 C7 C2 120.7(4) . . ? C6 C7 H7 119.6 . . ? C2 C7 H7 119.6 . . ? O6 C20 O5 120.6(4) . . ? O6 C20 C17 120.2(4) . . ? O5 C20 C17 119.1(4) . . ? O6 C20 Ni1 61.8(2) . 1_556 ? O5 C20 Ni1 59.0(2) . 1_556 ? C17 C20 Ni1 176.5(3) . 1_556 ? N2 C33 C32 124.0(4) . . ? N2 C33 H33 118.0 . . ? C32 C33 H33 118.0 . . ? C31 C28 C27 113.6(4) 9_454 . ? C31 C28 H28A 108.9 9_454 . ? C27 C28 H28A 108.9 . . ? C31 C28 H28B 108.9 9_454 . ? C27 C28 H28B 108.9 . . ? H28A C28 H28B 107.7 . . ? C14 C15 C16 119.0(4) . . ? C14 C15 H15 120.5 . . ? C16 C15 H15 120.5 . . ? C7 C6 C5 119.1(4) . . ? C7 C6 H6 120.4 . . ? C5 C6 H6 120.4 . . ? C33 C32 C31 120.4(4) . . ? C33 C32 H32 119.8 . . ? C31 C32 H32 119.8 . . ? C23 C24 C25 119.6(5) . . ? C23 C24 H24 120.2 . . ? C25 C24 H24 120.2 . . ? C23 C22 C21 119.7(5) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C23 C26 C27 110.6(4) . . ? C23 C26 H26A 109.5 . . ? C27 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? C27 C26 H26B 109.5 . . ? H26A C26 H26B 108.1 . . ? N1 C25 C24 124.2(5) . . ? N1 C25 H25 117.9 . . ? C24 C25 H25 117.9 . . ? C5 C4 C3 118.7(5) . . ? C5 C4 H4 120.7 . . ? C3 C4 H4 120.7 . . ? C31 C30 C29 121.1(5) . . ? C31 C30 H30 119.5 . . ? C29 C30 H30 119.5 . . ? N1 C21 C22 123.8(5) . . ? N1 C21 H21 118.1 . . ? C22 C21 H21 118.1 . . ? N2 C29 C30 123.7(5) . . ? N2 C29 H29 118.1 . . ? C30 C29 H29 118.1 . . ? C28 C27 C26 114.2(4) . . ? C28 C27 H27A 108.7 . . ? C26 C27 H27A 108.7 . . ? C28 C27 H27B 108.7 . . ? C26 C27 H27B 108.7 . . ? H27A C27 H27B 107.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Ni1 O1 C1 -22.0(9) . . . . ? N2 Ni1 O1 C1 90.9(3) . . . . ? O5 Ni1 O1 C1 -167.4(3) 1_554 . . . ? O2 Ni1 O1 C1 -2.4(3) . . . . ? O6 Ni1 O1 C1 -104.9(3) 1_554 . . . ? C20 Ni1 O1 C1 -136.0(3) 1_554 . . . ? N1 Ni1 O2 C1 178.8(2) . . . . ? N2 Ni1 O2 C1 -85.7(3) . . . . ? O5 Ni1 O2 C1 37.6(4) 1_554 . . . ? O1 Ni1 O2 C1 2.4(3) . . . . ? O6 Ni1 O2 C1 86.4(3) 1_554 . . . ? C20 Ni1 O2 C1 70.5(3) 1_554 . . . ? N2 Ni1 N1 C21 85.9(4) . . . . ? O5 Ni1 N1 C21 -16.2(4) 1_554 . . . ? O2 Ni1 N1 C21 -179.8(3) . . . . ? O1 Ni1 N1 C21 -161.6(7) . . . . ? O6 Ni1 N1 C21 -78.6(4) 1_554 . . . ? C1 Ni1 N1 C21 -178.9(3) . . . . ? C20 Ni1 N1 C21 -47.7(4) 1_554 . . . ? N2 Ni1 N1 C25 -103.6(4) . . . . ? O5 Ni1 N1 C25 154.3(4) 1_554 . . . ? O2 Ni1 N1 C25 -9.3(4) . . . . ? O1 Ni1 N1 C25 8.9(10) . . . . ? O6 Ni1 N1 C25 91.9(4) 1_554 . . . ? C1 Ni1 N1 C25 -8.4(5) . . . . ? C20 Ni1 N1 C25 122.8(4) 1_554 . . . ? N1 Ni1 N2 C33 -100.2(4) . . . . ? O5 Ni1 N2 C33 -5.2(4) 1_554 . . . ? O2 Ni1 N2 C33 152.3(4) . . . . ? O1 Ni1 N2 C33 89.3(4) . . . . ? O6 Ni1 N2 C33 2.0(7) 1_554 . . . ? C1 Ni1 N2 C33 120.5(4) . . . . ? C20 Ni1 N2 C33 -2.2(4) 1_554 . . . ? N1 Ni1 N2 C29 84.5(4) . . . . ? O5 Ni1 N2 C29 179.6(4) 1_554 . . . ? O2 Ni1 N2 C29 -23.0(4) . . . . ? O1 Ni1 N2 C29 -86.0(4) . . . . ? O6 Ni1 N2 C29 -173.2(4) 1_554 . . . ? C1 Ni1 N2 C29 -54.7(4) . . . . ? C20 Ni1 N2 C29 -177.4(4) 1_554 . . . ? C5 O3 C8 C9 -4.6(8) . . . . ? C5 O3 C8 C13 178.2(4) . . . . ? C12 C13 C8 C9 0.6(7) . . . . ? C12 C13 C8 O3 177.9(4) . . . . ? Ni1 O1 C1 O2 4.1(4) . . . . ? Ni1 O1 C1 C2 -170.0(4) . . . . ? Ni1 O2 C1 O1 -4.2(4) . . . . ? Ni1 O2 C1 C2 169.9(4) . . . . ? N1 Ni1 C1 O1 174.1(2) . . . . ? N2 Ni1 C1 O1 -89.0(3) . . . . ? O5 Ni1 C1 O1 15.4(3) 1_554 . . . ? O2 Ni1 C1 O1 175.9(4) . . . . ? O6 Ni1 C1 O1 77.0(3) 1_554 . . . ? C20 Ni1 C1 O1 49.0(3) 1_554 . . . ? N1 Ni1 C1 O2 -1.7(4) . . . . ? N2 Ni1 C1 O2 95.1(3) . . . . ? O5 Ni1 C1 O2 -160.5(2) 1_554 . . . ? O1 Ni1 C1 O2 -175.9(4) . . . . ? O6 Ni1 C1 O2 -98.9(2) 1_554 . . . ? C20 Ni1 C1 O2 -126.8(2) 1_554 . . . ? N1 Ni1 C1 C2 -96(2) . . . . ? N2 Ni1 C1 C2 0(2) . . . . ? O5 Ni1 C1 C2 105(2) 1_554 . . . ? O2 Ni1 C1 C2 -95(2) . . . . ? O1 Ni1 C1 C2 89(2) . . . . ? O6 Ni1 C1 C2 166(2) 1_554 . . . ? C20 Ni1 C1 C2 138(2) 1_554 . . . ? C12 O4 C14 C15 103.3(5) . . . . ? C12 O4 C14 C19 -82.8(5) . . . . ? C8 C13 C12 C11 -0.2(7) . . . . ? C8 C13 C12 O4 179.4(4) . . . . ? C14 O4 C12 C13 21.1(6) . . . . ? C14 O4 C12 C11 -159.4(4) . . . . ? C8 O3 C5 C4 -57.6(7) . . . . ? C8 O3 C5 C6 126.4(5) . . . . ? C18 C17 C16 C15 1.1(6) . . . . ? C20 C17 C16 C15 -178.8(4) . . . . ? C13 C12 C11 C10 0.6(7) . . . . ? O4 C12 C11 C10 -179.0(4) . . . . ? C4 C3 C2 C7 -1.7(7) . . . . ? C4 C3 C2 C1 174.4(5) . . . . ? O1 C1 C2 C7 171.7(4) . . . . ? O2 C1 C2 C7 -2.5(7) . . . . ? Ni1 C1 C2 C7 87(2) . . . . ? O1 C1 C2 C3 -4.4(7) . . . . ? O2 C1 C2 C3 -178.6(4) . . . . ? Ni1 C1 C2 C3 -89(2) . . . . ? C16 C17 C18 C19 -2.3(6) . . . . ? C20 C17 C18 C19 177.6(4) . . . . ? O3 C8 C9 C10 -178.4(5) . . . . ? C13 C8 C9 C10 -1.4(7) . . . . ? C15 C14 C19 C18 -0.3(7) . . . . ? O4 C14 C19 C18 -174.1(4) . . . . ? C17 C18 C19 C14 2.0(7) . . . . ? C12 C11 C10 C9 -1.5(8) . . . . ? C8 C9 C10 C11 1.9(8) . . . . ? C3 C2 C7 C6 1.1(7) . . . . ? C1 C2 C7 C6 -175.1(4) . . . . ? Ni1 O6 C20 O5 -3.5(4) 1_556 . . . ? Ni1 O6 C20 C17 176.6(3) 1_556 . . . ? Ni1 O5 C20 O6 3.6(4) 1_556 . . . ? Ni1 O5 C20 C17 -176.5(3) 1_556 . . . ? C16 C17 C20 O6 0.0(6) . . . . ? C18 C17 C20 O6 -179.9(4) . . . . ? C16 C17 C20 O5 -179.9(4) . . . . ? C18 C17 C20 O5 0.2(6) . . . . ? C16 C17 C20 Ni1 123(5) . . . 1_556 ? C18 C17 C20 Ni1 -57(5) . . . 1_556 ? C29 N2 C33 C32 1.9(7) . . . . ? Ni1 N2 C33 C32 -173.5(3) . . . . ? C19 C14 C15 C16 -0.9(7) . . . . ? O4 C14 C15 C16 173.0(4) . . . . ? C17 C16 C15 C14 0.5(7) . . . . ? C2 C7 C6 C5 -0.1(7) . . . . ? C4 C5 C6 C7 -0.1(7) . . . . ? O3 C5 C6 C7 175.9(4) . . . . ? N2 C33 C32 C31 -0.6(7) . . . . ? C30 C31 C32 C33 -0.8(7) . . . . ? C28 C31 C32 C33 -180.0(4) 9 . . . ? C22 C23 C24 C25 -1.6(7) . . . . ? C26 C23 C24 C25 176.0(4) . . . . ? C24 C23 C22 C21 1.3(7) . . . . ? C26 C23 C22 C21 -176.3(4) . . . . ? C24 C23 C26 C27 -84.7(6) . . . . ? C22 C23 C26 C27 92.8(6) . . . . ? C21 N1 C25 C24 0.7(7) . . . . ? Ni1 N1 C25 C24 -170.0(4) . . . . ? C23 C24 C25 N1 0.6(8) . . . . ? C6 C5 C4 C3 -0.5(8) . . . . ? O3 C5 C4 C3 -176.3(5) . . . . ? C2 C3 C4 C5 1.5(8) . . . . ? C32 C31 C30 C29 0.7(8) . . . . ? C28 C31 C30 C29 180.0(5) 9 . . . ? C25 N1 C21 C22 -1.0(7) . . . . ? Ni1 N1 C21 C22 170.4(4) . . . . ? C23 C22 C21 N1 0.0(8) . . . . ? C33 N2 C29 C30 -1.9(8) . . . . ? Ni1 N2 C29 C30 173.7(5) . . . . ? C31 C30 C29 N2 0.6(10) . . . . ? C31 C28 C27 C26 -177.9(4) 9_454 . . . ? C23 C26 C27 C28 -166.8(5) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.212 _refine_diff_density_min -0.265 _refine_diff_density_rms 0.052 _database_code_depnum_ccdc_archive 'CCDC 933678' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_cncnc6 #TrackingRef 'cncnc6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C54 H42 Cd2 N4 O14' _chemical_formula_sum 'C54 H42 Cd2 N4 O14' _chemical_formula_weight 1195.72 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 10.9446(9) _cell_length_b 15.2526(12) _cell_length_c 16.0944(13) _cell_angle_alpha 102.7930(10) _cell_angle_beta 105.4210(10) _cell_angle_gamma 99.0340(10) _cell_volume 2458.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9579 _cell_measurement_theta_min 1.61 _cell_measurement_theta_max 26.02 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.615 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1204 _exptl_absorpt_coefficient_mu 0.939 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.756 _exptl_absorpt_correction_T_max 0.808 _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 13760 _diffrn_reflns_av_R_equivalents 0.0166 _diffrn_reflns_av_sigmaI/netI 0.0409 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 26.00 _reflns_number_total 9579 _reflns_number_gt 4341 _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^)+(0.0477P)^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 9579 _refine_ls_number_parameters 667 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0740 _refine_ls_R_factor_gt 0.0283 _refine_ls_wR_factor_ref 0.0895 _refine_ls_wR_factor_gt 0.0739 _refine_ls_goodness_of_fit_ref 0.859 _refine_ls_restrained_S_all 0.859 _refine_ls_shift/su_max 0.056 _refine_ls_shift/su_mean 0.006 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd2 Cd 0.57330(5) 0.42433(3) 0.07156(3) 0.02825(13) Uani 1 1 d . . . Cd1 Cd 1.42647(5) 1.07572(3) -0.07153(3) 0.02795(13) Uani 1 1 d . . . O9 O 1.6677(5) 1.3122(3) -0.8528(3) 0.0397(13) Uani 1 1 d . . . O2 O 1.3317(5) 1.1883(3) -0.1477(3) 0.0421(14) Uani 1 1 d . . . O12 O 0.3659(5) 0.6531(3) 0.0618(3) 0.0448(14) Uani 1 1 d . . . O11 O 0.4331(5) 0.5244(3) 0.0603(3) 0.0347(12) Uani 1 1 d . . . O5 O 1.5692(5) 0.9756(3) -0.0587(3) 0.0360(12) Uani 1 1 d . . . O6 O 1.6317(5) 0.8470(3) -0.0620(3) 0.0386(13) Uani 1 1 d . . . O2W O 0.3834(4) 0.3124(3) 0.0109(3) 0.0333(12) Uani 1 1 d . . . O7 O 1.8037(5) 0.9379(3) -0.3847(3) 0.0436(14) Uani 1 1 d . . . O4 O 1.1938(5) 1.5606(4) -0.6162(3) 0.0485(15) Uani 1 1 d . . . O10 O 1.5671(5) 1.4068(4) -0.7876(3) 0.0487(15) Uani 1 1 d . . . O1W O 1.6166(4) 1.1878(3) -0.0124(3) 0.0358(12) Uani 1 1 d . . . O8 O 1.6328(5) 1.1591(4) -0.5196(4) 0.0556(17) Uani 1 1 d . . . O3 O 1.3650(5) 1.3408(4) -0.4814(3) 0.0546(17) Uani 1 1 d . . . O1 O 1.4357(5) 1.0929(4) -0.2108(3) 0.0478(14) Uani 1 1 d . . . N3 N 1.0805(6) 0.8440(4) -0.1782(4) 0.0380(16) Uani 1 1 d . . . C17 C 1.3357(6) 1.5796(5) -0.8273(4) 0.0272(16) Uani 1 1 d . . . C23 C 1.6938(7) 1.0060(5) -0.1882(5) 0.0379(19) Uani 1 1 d . . . H23 H 1.6829 1.0585 -0.1513 0.046 Uiso 1 1 calc R . . N2 N 0.9146(6) 0.6549(4) 0.1759(4) 0.0384(16) Uani 1 1 d . . . C43 C 0.8097(6) 0.5974(4) 0.1117(4) 0.0304(16) Uani 1 1 d . . . H43 H 0.7723 0.6065 0.0561 0.037 Uiso 1 1 calc R . . N1 N 0.7672(5) 0.5264(4) 0.1388(4) 0.0348(15) Uani 1 1 d . . . N4 N 1.2314(5) 0.9732(4) -0.1362(4) 0.0393(16) Uani 1 1 d . . . C54 C 1.1832(8) 0.8973(5) -0.1157(5) 0.046(2) Uani 1 1 d . . . H54 H 1.2197 0.8842 -0.0620 0.055 Uiso 1 1 calc R . . C22 C 1.6625(6) 0.9225(4) -0.1720(4) 0.0256(15) Uani 1 1 d . . . C14 C 1.2475(7) 1.5620(5) -0.6861(4) 0.0328(18) Uani 1 1 d . . . C30 C 1.7374(8) 1.1270(6) -0.4834(5) 0.042(2) Uani 1 1 d . . . C4 C 1.3380(8) 1.3370(6) -0.3388(5) 0.049(2) Uani 1 1 d . . . H4 H 1.3205 1.3954 -0.3316 0.059 Uiso 1 1 calc R . . C25 C 1.7549(7) 0.9372(5) -0.3149(5) 0.0331(17) Uani 1 1 d . . . C15 C 1.2808(7) 1.6484(5) -0.6983(4) 0.0349(18) Uani 1 1 d . . . H15 H 1.2766 1.7006 -0.6574 0.042 Uiso 1 1 calc R . . C48 C 1.0074(7) 0.7527(5) -0.0840(5) 0.042(2) Uani 1 1 d . . . C20 C 0.3835(6) 0.5872(4) 0.0940(4) 0.0227(15) Uani 1 1 d . . . C39 C 1.6621(7) 1.1613(5) -0.6628(5) 0.0405(19) Uani 1 1 d . . . H39 H 1.6793 1.1027 -0.6714 0.049 Uiso 1 1 calc R . . C8 C 1.2545(7) 1.3705(5) -0.5184(4) 0.0368(18) Uani 1 1 d . . . C28 C 1.8213(7) 1.0180(5) -0.4118(4) 0.0361(18) Uani 1 1 d . . . C26 C 1.7236(7) 0.8519(5) -0.3003(4) 0.0324(17) Uani 1 1 d . . . H26 H 1.7333 0.7995 -0.3380 0.039 Uiso 1 1 calc R . . C16 C 1.3195(7) 1.6567(4) -0.7698(4) 0.0319(17) Uani 1 1 d . . . H16 H 1.3354 1.7142 -0.7807 0.038 Uiso 1 1 calc R . . C2 C 1.3702(7) 1.2064(5) -0.2829(4) 0.0320(18) Uani 1 1 d . . . C13 C 1.2797(6) 1.4492(4) -0.5495(4) 0.0324(17) Uani 1 1 d . . . H13 H 1.3640 1.4788 -0.5432 0.039 Uiso 1 1 calc R . . C45 C 0.9939(8) 0.7481(5) 0.0862(6) 0.048(2) Uani 1 1 d . . . C3 C 1.3394(7) 1.2932(4) -0.2721(5) 0.0338(17) Uani 1 1 d . . . H3 H 1.3202 1.3208 -0.2210 0.041 Uiso 1 1 calc R . . C38 C 1.6598(7) 1.2091(5) -0.7264(5) 0.044(2) Uani 1 1 d . . . H38 H 1.6775 1.1820 -0.7784 0.052 Uiso 1 1 calc R . . C34 C 1.6379(8) 1.2041(6) -0.5857(5) 0.043(2) Uani 1 1 d . . . C50 C 1.0560(7) 0.6897(6) 0.0415(5) 0.051(2) Uani 1 1 d . . . H50 H 1.0934 0.6484 0.0688 0.061 Uiso 1 1 calc R . . C12 C 1.1727(8) 1.4801(5) -0.5899(4) 0.044(2) Uani 1 1 d . . . C27 C 1.6772(6) 0.8447(5) -0.2286(4) 0.0296(17) Uani 1 1 d . . . H27 H 1.6560 0.7872 -0.2188 0.036 Uiso 1 1 calc R . . C21 C 1.6191(7) 0.9136(5) -0.0951(5) 0.0330(18) Uani 1 1 d . . . C33 C 1.9466(9) 1.0597(6) -0.4044(6) 0.068(3) Uani 1 1 d . . . H33 H 2.0163 1.0354 -0.3804 0.082 Uiso 1 1 calc R . . C24 C 1.7418(8) 1.0144(5) -0.2590(5) 0.045(2) Uani 1 1 d . . . H24 H 1.7647 1.0721 -0.2681 0.053 Uiso 1 1 calc R . . C37 C 1.6325(6) 1.2952(5) -0.7163(4) 0.0316(17) Uani 1 1 d . . . C11 C 1.0502(7) 1.4402(7) -0.5975(6) 0.066(3) Uani 1 1 d . . . H11 H 0.9803 1.4629 -0.6243 0.079 Uiso 1 1 calc R . . C29 C 1.7182(8) 1.0534(5) -0.4508(5) 0.043(2) Uani 1 1 d . . . H29 H 1.6341 1.0259 -0.4545 0.051 Uiso 1 1 calc R . . C5 C 1.3622(7) 1.2952(5) -0.4151(5) 0.039(2) Uani 1 1 d . . . C18 C 1.3066(7) 1.4926(5) -0.8128(4) 0.0348(18) Uani 1 1 d . . . H18 H 1.3181 1.4409 -0.8505 0.042 Uiso 1 1 calc R . . C47 C 0.9428(8) 0.8101(5) -0.0416(6) 0.055(2) Uani 1 1 d . . . H47 H 0.9042 0.8507 -0.0694 0.066 Uiso 1 1 calc R . . C19 C 1.2614(7) 1.4839(4) -0.7430(4) 0.0346(18) Uani 1 1 d . . . H19 H 1.2400 1.4262 -0.7337 0.041 Uiso 1 1 calc R . . C36 C 1.6032(8) 1.3345(5) -0.6396(4) 0.042(2) Uani 1 1 d . . . H36 H 1.5784 1.3906 -0.6327 0.050 Uiso 1 1 calc R . . C7 C 1.3957(7) 1.1666(5) -0.3590(5) 0.0371(19) Uani 1 1 d . . . H7 H 1.4150 1.1087 -0.3659 0.045 Uiso 1 1 calc R . . C52 C 1.0590(7) 0.8845(5) -0.2478(5) 0.046(2) Uani 1 1 d . . . H52 H 0.9934 0.8624 -0.3028 0.055 Uiso 1 1 calc R . . C40 C 1.6206(8) 1.3395(5) -0.7907(5) 0.0376(19) Uani 1 1 d . . . C51 C 1.0125(8) 0.7548(5) -0.1745(5) 0.056(3) Uani 1 1 d . . . H51A H 1.0556 0.7076 -0.1956 0.068 Uiso 1 1 calc R . . H51B H 0.9241 0.7395 -0.2150 0.068 Uiso 1 1 calc R . . C6 C 1.3938(7) 1.2096(5) -0.4268(5) 0.0411(19) Uani 1 1 d . . . H6 H 1.4129 1.1821 -0.4781 0.049 Uiso 1 1 calc R . . C42 C 0.9406(7) 0.6163(6) 0.2461(5) 0.048(2) Uani 1 1 d . . . H42 H 1.0081 0.6408 0.2999 0.058 Uiso 1 1 calc R . . C44 C 0.9840(8) 0.7457(5) 0.1775(5) 0.052(2) Uani 1 1 d . . . H44A H 1.0709 0.7609 0.2201 0.062 Uiso 1 1 calc R . . H44B H 0.9387 0.7920 0.1974 0.062 Uiso 1 1 calc R . . C35 C 1.6117(8) 1.2885(6) -0.5729(5) 0.046(2) Uani 1 1 d . . . H35 H 1.5992 1.3165 -0.5192 0.055 Uiso 1 1 calc R . . C53 C 1.1527(7) 0.9621(5) -0.2196(5) 0.041(2) Uani 1 1 d . . . H53 H 1.1622 1.0034 -0.2535 0.049 Uiso 1 1 calc R . . C32 C 1.9669(9) 1.1380(7) -0.4333(6) 0.082(4) Uani 1 1 d . . . H32 H 2.0514 1.1688 -0.4248 0.098 Uiso 1 1 calc R . . C41 C 0.8508(8) 0.5364(6) 0.2232(5) 0.055(2) Uani 1 1 d . . . H41 H 0.8461 0.4955 0.2579 0.066 Uiso 1 1 calc R . . C1 C 1.3779(6) 1.1577(5) -0.2096(4) 0.0297(17) Uani 1 1 d . . . C31 C 1.8623(8) 1.1714(7) -0.4748(6) 0.068(3) Uani 1 1 d . . . H31 H 1.8762 1.2226 -0.4964 0.082 Uiso 1 1 calc R . . C10 C 1.0311(8) 1.3654(8) -0.5649(7) 0.088(4) Uani 1 1 d . . . H10 H 0.9469 1.3386 -0.5684 0.106 Uiso 1 1 calc R . . C46 C 0.9362(7) 0.8067(6) 0.0421(6) 0.053(2) Uani 1 1 d . . . H46 H 0.8916 0.8449 0.0697 0.064 Uiso 1 1 calc R . . C49 C 1.0632(8) 0.6917(5) -0.0417(5) 0.050(2) Uani 1 1 d . . . H49 H 1.1055 0.6521 -0.0701 0.061 Uiso 1 1 calc R . . C9 C 1.1295(8) 1.3289(6) -0.5280(6) 0.062(3) Uani 1 1 d . . . H9 H 1.1126 1.2761 -0.5094 0.074 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd2 0.0362(3) 0.0289(3) 0.0274(3) 0.0171(2) 0.0131(2) 0.0105(2) Cd1 0.0356(3) 0.0276(3) 0.0276(3) 0.0164(2) 0.0124(2) 0.0103(2) O9 0.050(3) 0.039(3) 0.036(3) 0.019(3) 0.018(3) 0.007(3) O2 0.059(4) 0.048(3) 0.027(3) 0.019(3) 0.019(3) 0.011(3) O12 0.066(4) 0.036(3) 0.050(3) 0.027(3) 0.029(3) 0.018(3) O11 0.049(3) 0.037(3) 0.035(3) 0.018(2) 0.028(2) 0.021(2) O5 0.049(3) 0.041(3) 0.031(3) 0.020(2) 0.017(2) 0.027(3) O6 0.060(4) 0.039(3) 0.043(3) 0.030(3) 0.035(3) 0.026(3) O2W 0.034(3) 0.026(3) 0.046(3) 0.025(2) 0.012(2) 0.005(2) O7 0.067(4) 0.049(3) 0.044(3) 0.029(3) 0.041(3) 0.029(3) O4 0.078(4) 0.056(4) 0.040(3) 0.034(3) 0.035(3) 0.035(3) O10 0.070(4) 0.055(4) 0.044(3) 0.038(3) 0.027(3) 0.030(3) O1W 0.043(3) 0.027(3) 0.039(3) 0.008(2) 0.016(2) 0.010(2) O8 0.054(4) 0.087(5) 0.067(4) 0.062(4) 0.040(3) 0.040(3) O3 0.068(4) 0.080(4) 0.053(4) 0.055(3) 0.038(3) 0.039(3) O1 0.060(4) 0.052(3) 0.049(4) 0.032(3) 0.023(3) 0.027(3) N3 0.028(3) 0.047(4) 0.035(3) 0.016(3) 0.007(3) -0.002(3) C17 0.025(4) 0.033(4) 0.031(4) 0.025(3) 0.008(3) 0.006(3) C23 0.055(5) 0.028(4) 0.039(5) 0.013(4) 0.024(4) 0.013(4) N2 0.038(4) 0.040(4) 0.043(4) 0.023(3) 0.012(3) 0.009(3) C43 0.019(3) 0.034(4) 0.027(3) 0.007(3) -0.003(2) -0.004(3) N1 0.038(3) 0.034(3) 0.041(4) 0.019(3) 0.018(3) 0.010(3) N4 0.032(3) 0.049(4) 0.032(3) 0.023(3) -0.002(3) 0.001(3) C54 0.063(5) 0.049(5) 0.049(5) 0.034(4) 0.031(4) 0.029(4) C22 0.031(4) 0.024(3) 0.025(3) 0.003(3) 0.014(3) 0.012(3) C14 0.043(5) 0.046(5) 0.020(4) 0.018(3) 0.016(3) 0.014(4) C30 0.045(4) 0.063(5) 0.029(4) 0.027(4) 0.018(3) 0.011(4) C4 0.064(6) 0.051(5) 0.055(6) 0.038(5) 0.028(5) 0.029(4) C25 0.034(4) 0.043(5) 0.032(4) 0.019(4) 0.013(3) 0.019(4) C15 0.046(4) 0.033(4) 0.030(4) 0.010(3) 0.014(3) 0.015(3) C48 0.029(4) 0.051(5) 0.047(5) 0.028(4) 0.011(4) -0.001(4) C20 0.021(3) 0.030(4) 0.029(4) 0.016(3) 0.020(3) 0.007(3) C39 0.056(5) 0.045(5) 0.045(5) 0.026(4) 0.035(4) 0.030(4) C8 0.048(4) 0.046(4) 0.031(4) 0.028(4) 0.017(3) 0.021(3) C28 0.038(4) 0.046(4) 0.030(4) 0.014(3) 0.020(3) 0.006(3) C26 0.042(4) 0.031(4) 0.028(4) 0.007(3) 0.017(3) 0.010(3) C16 0.042(4) 0.016(3) 0.040(4) 0.008(3) 0.014(3) 0.012(3) C2 0.041(4) 0.032(4) 0.017(3) 0.010(3) 0.000(3) -0.003(3) C13 0.035(4) 0.038(4) 0.032(4) 0.017(3) 0.021(3) 0.002(3) C45 0.036(5) 0.038(5) 0.068(6) 0.020(4) 0.015(4) -0.004(4) C3 0.047(4) 0.033(4) 0.042(4) 0.026(3) 0.027(3) 0.023(3) C38 0.049(5) 0.066(5) 0.023(4) 0.012(4) 0.015(3) 0.024(4) C34 0.046(5) 0.061(6) 0.037(5) 0.034(4) 0.014(4) 0.021(4) C50 0.040(5) 0.063(6) 0.060(5) 0.045(5) 0.013(4) 0.006(4) C12 0.063(5) 0.061(5) 0.030(4) 0.038(4) 0.022(4) 0.033(4) C27 0.027(4) 0.038(4) 0.034(4) 0.021(3) 0.017(3) 0.004(3) C21 0.041(4) 0.025(4) 0.030(4) 0.013(3) 0.003(3) 0.006(3) C33 0.061(6) 0.090(7) 0.072(7) 0.054(6) 0.017(5) 0.029(5) C24 0.065(6) 0.046(5) 0.043(5) 0.031(4) 0.031(4) 0.018(4) C37 0.028(4) 0.042(4) 0.039(4) 0.024(4) 0.019(3) 0.017(3) C11 0.032(4) 0.119(8) 0.069(6) 0.072(6) 0.015(4) 0.016(5) C29 0.051(5) 0.061(5) 0.034(4) 0.029(4) 0.021(4) 0.028(4) C5 0.042(5) 0.056(5) 0.040(5) 0.035(4) 0.024(4) 0.021(4) C18 0.056(5) 0.029(4) 0.034(4) 0.020(3) 0.025(4) 0.017(4) C47 0.057(6) 0.050(5) 0.079(7) 0.032(5) 0.030(5) 0.032(4) C19 0.054(5) 0.021(4) 0.040(4) 0.016(3) 0.024(4) 0.012(3) C36 0.063(5) 0.035(4) 0.028(4) 0.003(3) 0.017(4) 0.017(4) C7 0.040(4) 0.037(4) 0.043(5) 0.027(4) 0.013(4) 0.011(3) C52 0.036(4) 0.065(6) 0.037(5) 0.029(4) -0.002(4) 0.012(4) C40 0.043(5) 0.029(4) 0.035(4) 0.013(3) 0.007(4) -0.005(4) C51 0.064(6) 0.039(5) 0.054(5) 0.017(4) 0.014(4) -0.022(4) C6 0.060(5) 0.041(4) 0.032(4) 0.014(4) 0.020(4) 0.025(4) C42 0.029(4) 0.069(6) 0.044(5) 0.026(5) 0.003(4) -0.001(4) C44 0.055(5) 0.056(5) 0.049(5) 0.020(4) 0.018(4) 0.014(4) C35 0.058(5) 0.064(6) 0.022(4) 0.018(4) 0.020(4) 0.012(4) C53 0.035(4) 0.044(4) 0.049(5) 0.035(4) 0.008(3) 0.004(3) C32 0.051(6) 0.102(7) 0.085(7) 0.062(6) 0.003(5) -0.021(5) C41 0.045(5) 0.083(7) 0.043(5) 0.036(5) 0.005(4) 0.019(5) C1 0.027(4) 0.044(4) 0.021(4) 0.021(3) 0.005(3) 0.005(3) C31 0.059(6) 0.089(7) 0.069(6) 0.065(6) 0.008(5) 0.012(5) C10 0.035(5) 0.153(10) 0.111(8) 0.105(8) 0.020(5) 0.025(5) C46 0.031(4) 0.063(6) 0.077(6) 0.028(5) 0.031(4) 0.010(4) C49 0.063(6) 0.042(5) 0.055(5) 0.023(4) 0.020(4) 0.020(4) C9 0.052(5) 0.073(6) 0.070(6) 0.048(5) 0.021(4) -0.005(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd2 N1 2.257(5) . ? Cd2 O2W 2.292(4) . ? Cd2 O11 2.330(5) . ? Cd2 O10 2.357(5) 1_446 ? Cd2 O11 2.407(4) 2_665 ? Cd2 O9 2.506(5) 1_446 ? Cd2 O12 2.516(5) 2_665 ? Cd1 N4 2.266(5) . ? Cd1 O1W 2.295(4) . ? Cd1 O1 2.340(5) . ? Cd1 O5 2.353(5) . ? Cd1 O5 2.387(4) 2_875 ? Cd1 O6 2.502(5) 2_875 ? Cd1 O2 2.518(5) . ? Cd1 C1 2.756(6) . ? O9 C40 1.264(9) . ? O9 Cd2 2.506(5) 1_664 ? O2 C1 1.265(8) . ? O12 C20 1.246(7) . ? O12 Cd2 2.516(5) 2_665 ? O11 C20 1.263(7) . ? O11 Cd2 2.407(4) 2_665 ? O5 C21 1.273(8) . ? O5 Cd1 2.387(4) 2_875 ? O6 C21 1.257(7) . ? O6 Cd1 2.502(5) 2_875 ? O7 C25 1.367(8) . ? O7 C28 1.390(8) . ? O4 C12 1.390(8) . ? O4 C14 1.403(8) . ? O10 C40 1.257(9) . ? O10 Cd2 2.357(5) 1_664 ? O8 C30 1.355(9) . ? O8 C34 1.397(8) . ? O3 C8 1.390(8) . ? O3 C5 1.402(7) . ? O1 C1 1.254(9) . ? N3 C54 1.298(8) . ? N3 C52 1.380(8) . ? N3 C51 1.467(8) . ? C17 C18 1.401(8) . ? C17 C16 1.393(9) . ? C17 C20 1.512(8) 1_664 ? C23 C22 1.365(8) . ? C23 C24 1.398(9) . ? C23 H23 0.9300 . ? N2 C43 1.344(7) . ? N2 C42 1.372(8) . ? N2 C44 1.463(8) . ? C43 N1 1.319(8) . ? C43 H43 0.9300 . ? N1 C41 1.381(8) . ? N4 C54 1.341(8) . ? N4 C53 1.346(8) . ? C54 H54 0.9300 . ? C22 C27 1.387(9) . ? C22 C21 1.465(9) . ? C14 C15 1.381(9) . ? C14 C19 1.389(9) . ? C30 C29 1.352(9) . ? C30 C31 1.383(10) . ? C4 C5 1.365(11) . ? C4 C3 1.382(9) . ? C4 H4 0.9300 . ? C25 C24 1.367(10) . ? C25 C26 1.379(9) . ? C15 C16 1.353(9) . ? C15 H15 0.9300 . ? C48 C47 1.384(11) . ? C48 C49 1.394(10) . ? C48 C51 1.479(10) . ? C20 C17 1.512(8) 1_446 ? C39 C34 1.380(10) . ? C39 C38 1.380(9) . ? C39 H39 0.9300 . ? C8 C9 1.367(10) . ? C8 C13 1.416(8) . ? C28 C33 1.380(10) . ? C28 C29 1.386(10) . ? C26 C27 1.397(8) . ? C26 H26 0.9300 . ? C16 H16 0.9300 . ? C2 C7 1.362(10) . ? C2 C3 1.402(9) . ? C2 C1 1.518(8) . ? C13 C12 1.386(9) . ? C13 H13 0.9300 . ? C45 C50 1.393(11) . ? C45 C46 1.387(10) . ? C45 C44 1.510(11) . ? C3 H3 0.9300 . ? C38 C37 1.376(10) . ? C38 H38 0.9300 . ? C34 C35 1.346(11) . ? C50 C49 1.368(10) . ? C50 H50 0.9300 . ? C12 C11 1.343(10) . ? C27 H27 0.9300 . ? C33 C32 1.380(11) . ? C33 H33 0.9300 . ? C24 H24 0.9300 . ? C37 C36 1.389(9) . ? C37 C40 1.486(9) . ? C11 C10 1.368(11) . ? C11 H11 0.9300 . ? C29 H29 0.9300 . ? C5 C6 1.387(10) . ? C18 C19 1.366(9) . ? C18 H18 0.9300 . ? C47 C46 1.380(11) . ? C47 H47 0.9300 . ? C19 H19 0.9300 . ? C36 C35 1.397(9) . ? C36 H36 0.9300 . ? C7 C6 1.389(9) . ? C7 H7 0.9300 . ? C52 C53 1.339(9) . ? C52 H52 0.9300 . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C6 H6 0.9300 . ? C42 C41 1.349(10) . ? C42 H42 0.9300 . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C35 H35 0.9300 . ? C53 H53 0.9300 . ? C32 C31 1.395(12) . ? C32 H32 0.9300 . ? C41 H41 0.9300 . ? C31 H31 0.9300 . ? C10 C9 1.347(11) . ? C10 H10 0.9300 . ? C46 H46 0.9300 . ? C49 H49 0.9300 . ? C9 H9 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cd2 O2W 174.87(17) . . ? N1 Cd2 O11 100.63(19) . . ? O2W Cd2 O11 83.46(16) . . ? N1 Cd2 O10 89.76(19) . 1_446 ? O2W Cd2 O10 86.68(17) . 1_446 ? O11 Cd2 O10 96.46(17) . 1_446 ? N1 Cd2 O11 86.94(18) . 2_665 ? O2W Cd2 O11 97.35(16) . 2_665 ? O11 Cd2 O11 71.61(18) . 2_665 ? O10 Cd2 O11 166.76(19) 1_446 2_665 ? N1 Cd2 O9 88.26(18) . 1_446 ? O2W Cd2 O9 86.65(15) . 1_446 ? O11 Cd2 O9 149.07(15) . 1_446 ? O10 Cd2 O9 53.66(18) 1_446 1_446 ? O11 Cd2 O9 138.92(17) 2_665 1_446 ? N1 Cd2 O12 94.81(19) . 2_665 ? O2W Cd2 O12 85.60(17) . 2_665 ? O11 Cd2 O12 121.29(15) . 2_665 ? O10 Cd2 O12 140.17(18) 1_446 2_665 ? O11 Cd2 O12 52.99(15) 2_665 2_665 ? O9 Cd2 O12 86.89(16) 1_446 2_665 ? N4 Cd1 O1W 175.14(18) . . ? N4 Cd1 O1 91.49(19) . . ? O1W Cd1 O1 85.51(17) . . ? N4 Cd1 O5 101.0(2) . . ? O1W Cd1 O5 83.09(17) . . ? O1 Cd1 O5 96.14(18) . . ? N4 Cd1 O5 85.36(18) . 2_875 ? O1W Cd1 O5 98.44(17) . 2_875 ? O1 Cd1 O5 166.40(19) . 2_875 ? O5 Cd1 O5 71.58(19) . 2_875 ? N4 Cd1 O6 94.3(2) . 2_875 ? O1W Cd1 O6 85.70(16) . 2_875 ? O1 Cd1 O6 140.90(17) . 2_875 ? O5 Cd1 O6 120.43(15) . 2_875 ? O5 Cd1 O6 52.66(15) 2_875 2_875 ? N4 Cd1 O2 88.84(18) . . ? O1W Cd1 O2 86.30(16) . . ? O1 Cd1 O2 54.18(18) . . ? O5 Cd1 O2 149.25(16) . . ? O5 Cd1 O2 138.76(17) 2_875 . ? O6 Cd1 O2 87.27(15) 2_875 . ? N4 Cd1 C1 90.98(19) . . ? O1W Cd1 C1 84.61(17) . . ? O1 Cd1 C1 26.9(2) . . ? O5 Cd1 C1 122.55(19) . . ? O5 Cd1 C1 165.9(2) 2_875 . ? O6 Cd1 C1 114.22(19) 2_875 . ? O2 Cd1 C1 27.28(19) . . ? C40 O9 Cd2 88.7(5) . 1_664 ? C1 O2 Cd1 86.9(4) . . ? C20 O12 Cd2 89.7(4) . 2_665 ? C20 O11 Cd2 152.4(4) . . ? C20 O11 Cd2 94.3(4) . 2_665 ? Cd2 O11 Cd2 108.39(18) . 2_665 ? C21 O5 Cd1 150.1(4) . . ? C21 O5 Cd1 96.6(4) . 2_875 ? Cd1 O5 Cd1 108.42(19) . 2_875 ? C21 O6 Cd1 91.6(4) . 2_875 ? C25 O7 C28 119.3(6) . . ? C12 O4 C14 119.8(6) . . ? C40 O10 Cd2 95.8(5) . 1_664 ? C30 O8 C34 118.4(6) . . ? C8 O3 C5 117.7(6) . . ? C1 O1 Cd1 95.4(4) . . ? C54 N3 C52 106.4(6) . . ? C54 N3 C51 124.4(6) . . ? C52 N3 C51 129.0(6) . . ? C18 C17 C16 119.6(6) . . ? C18 C17 C20 118.7(6) . 1_664 ? C16 C17 C20 121.6(6) . 1_664 ? C22 C23 C24 121.4(7) . . ? C22 C23 H23 119.3 . . ? C24 C23 H23 119.3 . . ? C43 N2 C42 106.9(6) . . ? C43 N2 C44 128.4(6) . . ? C42 N2 C44 124.5(6) . . ? N1 C43 N2 110.3(6) . . ? N1 C43 H43 124.8 . . ? N2 C43 H43 124.8 . . ? C43 N1 C41 107.3(6) . . ? C43 N1 Cd2 125.5(4) . . ? C41 N1 Cd2 126.2(5) . . ? C54 N4 C53 103.1(6) . . ? C54 N4 Cd1 130.3(5) . . ? C53 N4 Cd1 124.5(4) . . ? N3 C54 N4 113.4(6) . . ? N3 C54 H54 123.3 . . ? N4 C54 H54 123.3 . . ? C23 C22 C27 118.6(6) . . ? C23 C22 C21 121.9(6) . . ? C27 C22 C21 119.4(6) . . ? C15 C14 C19 120.9(6) . . ? C15 C14 O4 114.7(7) . . ? C19 C14 O4 124.3(6) . . ? C29 C30 O8 118.5(7) . . ? C29 C30 C31 120.2(8) . . ? O8 C30 C31 121.2(7) . . ? C5 C4 C3 120.6(8) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C24 C25 O7 124.2(6) . . ? C24 C25 C26 120.2(6) . . ? O7 C25 C26 115.5(7) . . ? C16 C15 C14 119.8(7) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C47 C48 C49 119.3(7) . . ? C47 C48 C51 119.7(8) . . ? C49 C48 C51 120.9(8) . . ? O12 C20 O11 122.4(6) . . ? O12 C20 C17 118.3(6) . 1_446 ? O11 C20 C17 119.2(5) . 1_446 ? C34 C39 C38 117.2(7) . . ? C34 C39 H39 121.4 . . ? C38 C39 H39 121.4 . . ? C9 C8 O3 125.5(7) . . ? C9 C8 C13 120.3(7) . . ? O3 C8 C13 114.2(6) . . ? C33 C28 C29 119.6(7) . . ? C33 C28 O7 117.6(7) . . ? C29 C28 O7 122.6(6) . . ? C25 C26 C27 119.7(7) . . ? C25 C26 H26 120.2 . . ? C27 C26 H26 120.2 . . ? C15 C16 C17 120.3(6) . . ? C15 C16 H16 119.8 . . ? C17 C16 H16 119.8 . . ? C7 C2 C3 119.5(6) . . ? C7 C2 C1 120.0(7) . . ? C3 C2 C1 120.5(6) . . ? C12 C13 C8 116.8(6) . . ? C12 C13 H13 121.6 . . ? C8 C13 H13 121.6 . . ? C50 C45 C46 117.4(8) . . ? C50 C45 C44 121.9(8) . . ? C46 C45 C44 120.6(8) . . ? C4 C3 C2 118.9(7) . . ? C4 C3 H3 120.6 . . ? C2 C3 H3 120.6 . . ? C39 C38 C37 122.8(7) . . ? C39 C38 H38 118.6 . . ? C37 C38 H38 118.6 . . ? C35 C34 C39 121.9(6) . . ? C35 C34 O8 117.1(7) . . ? C39 C34 O8 120.9(8) . . ? C49 C50 C45 121.5(8) . . ? C49 C50 H50 119.2 . . ? C45 C50 H50 119.2 . . ? C11 C12 C13 122.7(7) . . ? C11 C12 O4 118.5(7) . . ? C13 C12 O4 118.5(7) . . ? C22 C27 C26 120.6(6) . . ? C22 C27 H27 119.7 . . ? C26 C27 H27 119.7 . . ? O6 C21 O5 118.2(6) . . ? O6 C21 C22 122.0(7) . . ? O5 C21 C22 119.8(6) . . ? C28 C33 C32 119.0(8) . . ? C28 C33 H33 120.5 . . ? C32 C33 H33 120.5 . . ? C25 C24 C23 119.5(7) . . ? C25 C24 H24 120.2 . . ? C23 C24 H24 120.2 . . ? C38 C37 C36 118.4(6) . . ? C38 C37 C40 120.0(7) . . ? C36 C37 C40 121.2(7) . . ? C12 C11 C10 118.3(8) . . ? C12 C11 H11 120.9 . . ? C10 C11 H11 120.9 . . ? C30 C29 C28 121.3(7) . . ? C30 C29 H29 119.4 . . ? C28 C29 H29 119.3 . . ? C4 C5 C6 121.5(6) . . ? C4 C5 O3 120.6(7) . . ? C6 C5 O3 117.8(7) . . ? C19 C18 C17 119.7(7) . . ? C19 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? C46 C47 C48 119.6(8) . . ? C46 C47 H47 120.2 . . ? C48 C47 H47 120.2 . . ? C18 C19 C14 119.5(6) . . ? C18 C19 H19 120.3 . . ? C14 C19 H19 120.3 . . ? C35 C36 C37 119.0(7) . . ? C35 C36 H36 120.5 . . ? C37 C36 H36 120.5 . . ? C2 C7 C6 122.2(7) . . ? C2 C7 H7 118.9 . . ? C6 C7 H7 118.9 . . ? C53 C52 N3 105.4(6) . . ? C53 C52 H52 127.3 . . ? N3 C52 H52 127.3 . . ? O9 C40 O10 121.4(7) . . ? O9 C40 C37 120.6(7) . . ? O10 C40 C37 117.9(7) . . ? N3 C51 C48 114.0(6) . . ? N3 C51 H51A 108.7 . . ? C48 C51 H51A 108.7 . . ? N3 C51 H51B 108.7 . . ? C48 C51 H51B 108.7 . . ? H51A C51 H51B 107.6 . . ? C5 C6 C7 117.3(7) . . ? C5 C6 H6 121.3 . . ? C7 C6 H6 121.3 . . ? C41 C42 N2 107.8(7) . . ? C41 C42 H42 126.1 . . ? N2 C42 H42 126.1 . . ? N2 C44 C45 111.6(6) . . ? N2 C44 H44A 109.3 . . ? C45 C44 H44A 109.3 . . ? N2 C44 H44B 109.3 . . ? C45 C44 H44B 109.3 . . ? H44A C44 H44B 108.0 . . ? C34 C35 C36 120.5(7) . . ? C34 C35 H35 119.7 . . ? C36 C35 H35 119.7 . . ? C52 C53 N4 111.7(6) . . ? C52 C53 H53 124.2 . . ? N4 C53 H53 124.2 . . ? C31 C32 C33 120.9(8) . . ? C31 C32 H32 119.5 . . ? C33 C32 H32 119.5 . . ? C42 C41 N1 107.6(7) . . ? C42 C41 H41 126.2 . . ? N1 C41 H41 126.2 . . ? O1 C1 O2 123.4(6) . . ? O1 C1 C2 118.6(7) . . ? O2 C1 C2 117.9(7) . . ? O1 C1 Cd1 57.7(3) . . ? O2 C1 Cd1 65.8(3) . . ? C2 C1 Cd1 172.6(5) . . ? C32 C31 C30 118.8(7) . . ? C32 C31 H31 120.6 . . ? C30 C31 H31 120.6 . . ? C11 C10 C9 122.6(8) . . ? C11 C10 H10 118.7 . . ? C9 C10 H10 118.7 . . ? C47 C46 C45 122.0(8) . . ? C47 C46 H46 119.0 . . ? C45 C46 H46 119.0 . . ? C50 C49 C48 120.2(8) . . ? C50 C49 H49 119.9 . . ? C48 C49 H49 119.9 . . ? C10 C9 C8 119.3(7) . . ? C10 C9 H9 120.4 . . ? C8 C9 H9 120.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 Cd1 O2 C1 -94.4(4) . . . . ? O1W Cd1 O2 C1 85.4(4) . . . . ? O1 Cd1 O2 C1 -1.7(4) . . . . ? O5 Cd1 O2 C1 15.5(6) . . . . ? O5 Cd1 O2 C1 -176.0(4) 2_875 . . . ? O6 Cd1 O2 C1 171.3(4) 2_875 . . . ? N1 Cd2 O11 C20 -60.4(9) . . . . ? O2W Cd2 O11 C20 116.4(9) . . . . ? O10 Cd2 O11 C20 30.5(9) 1_446 . . . ? O11 Cd2 O11 C20 -143.6(10) 2_665 . . . ? O9 Cd2 O11 C20 44.2(10) 1_446 . . . ? O12 Cd2 O11 C20 -162.8(8) 2_665 . . . ? N1 Cd2 O11 Cd2 83.1(2) . . . 2_665 ? O2W Cd2 O11 Cd2 -100.0(2) . . . 2_665 ? O10 Cd2 O11 Cd2 174.1(2) 1_446 . . 2_665 ? O11 Cd2 O11 Cd2 0.0 2_665 . . 2_665 ? O9 Cd2 O11 Cd2 -172.2(2) 1_446 . . 2_665 ? O12 Cd2 O11 Cd2 -19.2(3) 2_665 . . 2_665 ? N4 Cd1 O5 C21 64.0(9) . . . . ? O1W Cd1 O5 C21 -113.4(9) . . . . ? O1 Cd1 O5 C21 -28.7(9) . . . . ? O5 Cd1 O5 C21 145.3(10) 2_875 . . . ? O6 Cd1 O5 C21 165.7(9) 2_875 . . . ? O2 Cd1 O5 C21 -42.7(11) . . . . ? C1 Cd1 O5 C21 -34.3(10) . . . . ? N4 Cd1 O5 Cd1 -81.3(2) . . . 2_875 ? O1W Cd1 O5 Cd1 101.3(2) . . . 2_875 ? O1 Cd1 O5 Cd1 -174.0(2) . . . 2_875 ? O5 Cd1 O5 Cd1 0.0 2_875 . . 2_875 ? O6 Cd1 O5 Cd1 20.4(3) 2_875 . . 2_875 ? O2 Cd1 O5 Cd1 172.0(2) . . . 2_875 ? C1 Cd1 O5 Cd1 -179.62(19) . . . 2_875 ? N4 Cd1 O1 C1 89.2(4) . . . . ? O1W Cd1 O1 C1 -86.9(4) . . . . ? O5 Cd1 O1 C1 -169.5(4) . . . . ? O5 Cd1 O1 C1 165.5(7) 2_875 . . . ? O6 Cd1 O1 C1 -9.4(6) 2_875 . . . ? O2 Cd1 O1 C1 1.7(4) . . . . ? C42 N2 C43 N1 1.4(9) . . . . ? C44 N2 C43 N1 -173.4(7) . . . . ? N2 C43 N1 C41 -2.1(9) . . . . ? N2 C43 N1 Cd2 167.0(5) . . . . ? O2W Cd2 N1 C43 166(2) . . . . ? O11 Cd2 N1 C43 -51.4(6) . . . . ? O10 Cd2 N1 C43 -147.9(6) 1_446 . . . ? O11 Cd2 N1 C43 19.2(6) 2_665 . . . ? O9 Cd2 N1 C43 158.4(6) 1_446 . . . ? O12 Cd2 N1 C43 71.7(6) 2_665 . . . ? O2W Cd2 N1 C41 -27(3) . . . . ? O11 Cd2 N1 C41 115.6(7) . . . . ? O10 Cd2 N1 C41 19.1(7) 1_446 . . . ? O11 Cd2 N1 C41 -173.7(7) 2_665 . . . ? O9 Cd2 N1 C41 -34.6(7) 1_446 . . . ? O12 Cd2 N1 C41 -121.3(7) 2_665 . . . ? O1W Cd1 N4 C54 -165(2) . . . . ? O1 Cd1 N4 C54 143.4(7) . . . . ? O5 Cd1 N4 C54 46.9(7) . . . . ? O5 Cd1 N4 C54 -23.3(7) 2_875 . . . ? O6 Cd1 N4 C54 -75.3(7) 2_875 . . . ? O2 Cd1 N4 C54 -162.5(7) . . . . ? C1 Cd1 N4 C54 170.3(7) . . . . ? O1W Cd1 N4 C53 35(3) . . . . ? O1 Cd1 N4 C53 -17.1(7) . . . . ? O5 Cd1 N4 C53 -113.7(7) . . . . ? O5 Cd1 N4 C53 176.1(7) 2_875 . . . ? O6 Cd1 N4 C53 124.2(7) 2_875 . . . ? O2 Cd1 N4 C53 37.0(7) . . . . ? C1 Cd1 N4 C53 9.8(7) . . . . ? C52 N3 C54 N4 2.1(10) . . . . ? C51 N3 C54 N4 177.0(7) . . . . ? C53 N4 C54 N3 -2.2(9) . . . . ? Cd1 N4 C54 N3 -165.8(5) . . . . ? C24 C23 C22 C27 -1.1(11) . . . . ? C24 C23 C22 C21 176.5(7) . . . . ? C12 O4 C14 C15 -171.4(6) . . . . ? C12 O4 C14 C19 11.9(11) . . . . ? C34 O8 C30 C29 -152.4(8) . . . . ? C34 O8 C30 C31 31.5(12) . . . . ? C28 O7 C25 C24 -11.6(11) . . . . ? C28 O7 C25 C26 171.4(6) . . . . ? C19 C14 C15 C16 4.3(11) . . . . ? O4 C14 C15 C16 -172.5(6) . . . . ? Cd2 O12 C20 O11 8.4(7) 2_665 . . . ? Cd2 O12 C20 C17 -167.6(5) 2_665 . . 1_446 ? Cd2 O11 C20 O12 136.8(7) . . . . ? Cd2 O11 C20 O12 -8.8(7) 2_665 . . . ? Cd2 O11 C20 C17 -47.2(12) . . . 1_446 ? Cd2 O11 C20 C17 167.2(5) 2_665 . . 1_446 ? C5 O3 C8 C9 -30.3(12) . . . . ? C5 O3 C8 C13 151.5(7) . . . . ? C25 O7 C28 C33 117.5(8) . . . . ? C25 O7 C28 C29 -66.7(9) . . . . ? C24 C25 C26 C27 0.6(11) . . . . ? O7 C25 C26 C27 177.8(6) . . . . ? C14 C15 C16 C17 -5.0(11) . . . . ? C18 C17 C16 C15 2.6(11) . . . . ? C20 C17 C16 C15 -177.8(6) 1_664 . . . ? C9 C8 C13 C12 -0.5(11) . . . . ? O3 C8 C13 C12 177.9(6) . . . . ? C5 C4 C3 C2 2.0(12) . . . . ? C7 C2 C3 C4 -1.2(11) . . . . ? C1 C2 C3 C4 177.6(6) . . . . ? C34 C39 C38 C37 -1.2(12) . . . . ? C38 C39 C34 C35 0.7(12) . . . . ? C38 C39 C34 O8 177.2(7) . . . . ? C30 O8 C34 C35 -127.0(8) . . . . ? C30 O8 C34 C39 56.4(11) . . . . ? C46 C45 C50 C49 1.8(10) . . . . ? C44 C45 C50 C49 179.3(7) . . . . ? C8 C13 C12 C11 1.9(12) . . . . ? C8 C13 C12 O4 176.0(6) . . . . ? C14 O4 C12 C11 -118.6(9) . . . . ? C14 O4 C12 C13 67.0(9) . . . . ? C23 C22 C27 C26 0.3(10) . . . . ? C21 C22 C27 C26 -177.3(6) . . . . ? C25 C26 C27 C22 -0.1(11) . . . . ? Cd1 O6 C21 O5 -9.7(6) 2_875 . . . ? Cd1 O6 C21 C22 168.9(6) 2_875 . . . ? Cd1 O5 C21 O6 -136.8(7) . . . . ? Cd1 O5 C21 O6 10.2(7) 2_875 . . . ? Cd1 O5 C21 C22 44.6(13) . . . . ? Cd1 O5 C21 C22 -168.4(5) 2_875 . . . ? C23 C22 C21 O6 -155.6(7) . . . . ? C27 C22 C21 O6 21.9(10) . . . . ? C23 C22 C21 O5 22.9(11) . . . . ? C27 C22 C21 O5 -159.5(6) . . . . ? C29 C28 C33 C32 2.3(13) . . . . ? O7 C28 C33 C32 178.2(8) . . . . ? O7 C25 C24 C23 -178.3(7) . . . . ? C26 C25 C24 C23 -1.4(12) . . . . ? C22 C23 C24 C25 1.7(12) . . . . ? C39 C38 C37 C36 -1.4(11) . . . . ? C39 C38 C37 C40 -174.8(7) . . . . ? C13 C12 C11 C10 -0.8(14) . . . . ? O4 C12 C11 C10 -174.9(8) . . . . ? O8 C30 C29 C28 -179.1(7) . . . . ? C31 C30 C29 C28 -3.0(13) . . . . ? C33 C28 C29 C30 1.3(12) . . . . ? O7 C28 C29 C30 -174.4(7) . . . . ? C3 C4 C5 C6 -2.5(13) . . . . ? C3 C4 C5 O3 -178.0(7) . . . . ? C8 O3 C5 C4 -57.3(10) . . . . ? C8 O3 C5 C6 127.1(8) . . . . ? C16 C17 C18 C19 0.7(10) . . . . ? C20 C17 C18 C19 -179.0(6) 1_664 . . . ? C49 C48 C47 C46 0.8(11) . . . . ? C51 C48 C47 C46 178.8(7) . . . . ? C17 C18 C19 C14 -1.4(11) . . . . ? C15 C14 C19 C18 -1.0(12) . . . . ? O4 C14 C19 C18 175.4(6) . . . . ? C38 C37 C36 C35 4.5(11) . . . . ? C40 C37 C36 C35 177.8(7) . . . . ? C3 C2 C7 C6 0.7(11) . . . . ? C1 C2 C7 C6 -178.0(6) . . . . ? C54 N3 C52 C53 -1.0(9) . . . . ? C51 N3 C52 C53 -175.7(8) . . . . ? Cd2 O9 C40 O10 -6.6(7) 1_664 . . . ? Cd2 O9 C40 C37 176.2(6) 1_664 . . . ? Cd2 O10 C40 O9 7.1(8) 1_664 . . . ? Cd2 O10 C40 C37 -175.7(5) 1_664 . . . ? C38 C37 C40 O9 -18.8(10) . . . . ? C36 C37 C40 O9 168.0(7) . . . . ? C38 C37 C40 O10 164.0(7) . . . . ? C36 C37 C40 O10 -9.2(10) . . . . ? C54 N3 C51 C48 37.1(12) . . . . ? C52 N3 C51 C48 -149.2(8) . . . . ? C47 C48 C51 N3 62.5(10) . . . . ? C49 C48 C51 N3 -119.5(8) . . . . ? C4 C5 C6 C7 2.0(12) . . . . ? O3 C5 C6 C7 177.6(6) . . . . ? C2 C7 C6 C5 -1.1(11) . . . . ? C43 N2 C42 C41 -0.2(9) . . . . ? C44 N2 C42 C41 174.9(7) . . . . ? C43 N2 C44 C45 -38.9(11) . . . . ? C42 N2 C44 C45 147.2(8) . . . . ? C50 C45 C44 N2 -59.8(10) . . . . ? C46 C45 C44 N2 117.6(7) . . . . ? C39 C34 C35 C36 2.5(13) . . . . ? O8 C34 C35 C36 -174.2(7) . . . . ? C37 C36 C35 C34 -5.1(12) . . . . ? N3 C52 C53 N4 -0.3(10) . . . . ? C54 N4 C53 C52 1.4(10) . . . . ? Cd1 N4 C53 C52 166.3(6) . . . . ? C28 C33 C32 C31 -4.3(15) . . . . ? N2 C42 C41 N1 -1.1(10) . . . . ? C43 N1 C41 C42 1.9(10) . . . . ? Cd2 N1 C41 C42 -167.0(6) . . . . ? Cd1 O1 C1 O2 -3.4(8) . . . . ? Cd1 O1 C1 C2 172.6(5) . . . . ? Cd1 O2 C1 O1 3.1(7) . . . . ? Cd1 O2 C1 C2 -172.8(5) . . . . ? C7 C2 C1 O1 16.1(10) . . . . ? C3 C2 C1 O1 -162.6(7) . . . . ? C7 C2 C1 O2 -167.8(7) . . . . ? C3 C2 C1 O2 13.5(10) . . . . ? C7 C2 C1 Cd1 74(4) . . . . ? C3 C2 C1 Cd1 -105(4) . . . . ? N4 Cd1 C1 O1 -91.3(4) . . . . ? O1W Cd1 C1 O1 90.7(4) . . . . ? O5 Cd1 C1 O1 12.4(5) . . . . ? O5 Cd1 C1 O1 -166.1(6) 2_875 . . . ? O6 Cd1 C1 O1 173.5(4) 2_875 . . . ? O2 Cd1 C1 O1 -176.9(7) . . . . ? N4 Cd1 C1 O2 85.6(4) . . . . ? O1W Cd1 C1 O2 -92.4(4) . . . . ? O1 Cd1 C1 O2 176.9(7) . . . . ? O5 Cd1 C1 O2 -170.6(4) . . . . ? O5 Cd1 C1 O2 10.8(10) 2_875 . . . ? O6 Cd1 C1 O2 -9.6(4) 2_875 . . . ? N4 Cd1 C1 C2 -153(4) . . . . ? O1W Cd1 C1 C2 29(4) . . . . ? O1 Cd1 C1 C2 -62(4) . . . . ? O5 Cd1 C1 C2 -49(4) . . . . ? O5 Cd1 C1 C2 132(4) 2_875 . . . ? O6 Cd1 C1 C2 112(4) 2_875 . . . ? O2 Cd1 C1 C2 121(4) . . . . ? C33 C32 C31 C30 2.7(16) . . . . ? C29 C30 C31 C32 0.9(14) . . . . ? O8 C30 C31 C32 177.0(9) . . . . ? C12 C11 C10 C9 -2.0(17) . . . . ? C48 C47 C46 C45 0.9(11) . . . . ? C50 C45 C46 C47 -2.1(10) . . . . ? C44 C45 C46 C47 -179.6(7) . . . . ? C45 C50 C49 C48 -0.3(11) . . . . ? C47 C48 C49 C50 -1.1(10) . . . . ? C51 C48 C49 C50 -179.0(7) . . . . ? C11 C10 C9 C8 3.3(17) . . . . ? O3 C8 C9 C10 179.8(9) . . . . ? C13 C8 C9 C10 -2.0(14) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.525 _refine_diff_density_min -0.408 _refine_diff_density_rms 0.121 _database_code_depnum_ccdc_archive 'CCDC 933679' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_cncnc7 #TrackingRef 'cncnc7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C84 H54 Mn3 N4 O19' _chemical_formula_sum 'C84 H54 Mn3 N4 O19' _chemical_formula_weight 1588.13 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 triclinic _symmetry_space_group_name_H-M p-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.0578(5) _cell_length_b 11.4735(5) _cell_length_c 28.3323(12) _cell_angle_alpha 94.6960(10) _cell_angle_beta 90.3450(10) _cell_angle_gamma 95.7970(10) _cell_volume 3563.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 13868 _cell_measurement_theta_min 1.61 _cell_measurement_theta_max 26.02 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.480 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1626 _exptl_absorpt_coefficient_mu 0.604 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.828 _exptl_absorpt_correction_T_max 0.870 _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 19737 _diffrn_reflns_av_R_equivalents 0.0187 _diffrn_reflns_av_sigmaI/netI 0.0413 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 26.00 _reflns_number_total 13868 _reflns_number_gt 10358 _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^)+(0.0601P)^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 13868 _refine_ls_number_parameters 989 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0629 _refine_ls_R_factor_gt 0.0398 _refine_ls_wR_factor_ref 0.1098 _refine_ls_wR_factor_gt 0.0991 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.4306(3) 0.3528(3) 0.47326(11) 0.0534(8) Uani 1 1 d . . . H1 H -0.3722 0.4096 0.4635 0.064 Uiso 1 1 calc R . . C2 C -0.5491(3) 0.3511(3) 0.45602(12) 0.0641(9) Uani 1 1 d . . . H2 H -0.5690 0.4065 0.4359 0.077 Uiso 1 1 calc R . . C3 C -0.6349(3) 0.2677(3) 0.46906(11) 0.0568(8) Uani 1 1 d . . . H3 H -0.7140 0.2644 0.4573 0.068 Uiso 1 1 calc R . . C4 C -0.6043(2) 0.1862(2) 0.50028(9) 0.0397(6) Uani 1 1 d . . . C5 C -0.6894(2) 0.0976(3) 0.51653(10) 0.0470(7) Uani 1 1 d . . . H5 H -0.7687 0.0890 0.5047 0.056 Uiso 1 1 calc R . . C6 C -0.6578(2) 0.0258(2) 0.54869(11) 0.0468(7) Uani 1 1 d . . . H6 H -0.7157 -0.0308 0.5590 0.056 Uiso 1 1 calc R . . C7 C -0.5364(2) 0.0353(2) 0.56735(9) 0.0390(6) Uani 1 1 d . . . C8 C -0.5002(3) -0.0349(2) 0.60194(11) 0.0527(8) Uani 1 1 d . . . H8 H -0.5561 -0.0898 0.6144 0.063 Uiso 1 1 calc R . . C9 C -0.3819(3) -0.0220(3) 0.61716(11) 0.0539(8) Uani 1 1 d . . . H9 H -0.3567 -0.0679 0.6402 0.065 Uiso 1 1 calc R . . C10 C -0.2991(2) 0.0605(2) 0.59798(9) 0.0428(6) Uani 1 1 d . . . H10 H -0.2183 0.0668 0.6081 0.051 Uiso 1 1 calc R . . C11 C -0.4488(2) 0.1189(2) 0.55080(8) 0.0304(5) Uani 1 1 d . . . C12 C -0.4829(2) 0.1963(2) 0.51696(8) 0.0326(5) Uani 1 1 d . . . C13 C 0.7917(3) -0.3540(3) 1.06172(11) 0.0544(8) Uani 1 1 d . . . H13 H 0.8698 -0.3182 1.0578 0.065 Uiso 1 1 calc R . . C14 C 0.7757(4) -0.4493(3) 1.09006(12) 0.0651(9) Uani 1 1 d . . . H14 H 0.8420 -0.4750 1.1051 0.078 Uiso 1 1 calc R . . C15 C 0.6624(4) -0.5031(3) 1.09517(11) 0.0619(9) Uani 1 1 d . . . H15 H 0.6508 -0.5671 1.1133 0.074 Uiso 1 1 calc R . . C16 C 0.5637(3) -0.4635(2) 1.07355(9) 0.0477(7) Uani 1 1 d . . . C17 C 0.4400(3) -0.5168(3) 1.07593(10) 0.0588(9) Uani 1 1 d . . . H17 H 0.4238 -0.5827 1.0928 0.071 Uiso 1 1 calc R . . C18 C 0.3485(3) -0.4740(3) 1.05454(11) 0.0600(9) Uani 1 1 d . . . H18 H 0.2699 -0.5099 1.0573 0.072 Uiso 1 1 calc R . . C19 C 0.3685(3) -0.3741(3) 1.02751(9) 0.0473(7) Uani 1 1 d . . . C20 C 0.2752(3) -0.3252(3) 1.00441(10) 0.0560(8) Uani 1 1 d . . . H20 H 0.1952 -0.3583 1.0062 0.067 Uiso 1 1 calc R . . C21 C 0.3015(3) -0.2299(3) 0.97946(10) 0.0544(8) Uani 1 1 d . . . H21 H 0.2399 -0.1960 0.9648 0.065 Uiso 1 1 calc R . . C22 C 0.4230(2) -0.1836(3) 0.97627(9) 0.0447(7) Uani 1 1 d . . . H22 H 0.4404 -0.1187 0.9589 0.054 Uiso 1 1 calc R . . C23 C 0.4873(2) -0.3213(2) 1.02285(8) 0.0374(6) Uani 1 1 d . . . C24 C 0.5864(2) -0.3659(2) 1.04600(8) 0.0389(6) Uani 1 1 d . . . C25 C 0.7867(2) -0.0591(2) 1.07947(8) 0.0359(6) Uani 1 1 d . . . C26 C 0.8327(2) -0.0587(2) 1.12914(8) 0.0344(5) Uani 1 1 d . . . C27 C 0.7515(3) -0.0929(3) 1.16370(9) 0.0460(7) Uani 1 1 d . . . H27 H 0.6686 -0.1037 1.1569 0.055 Uiso 1 1 calc R . . C28 C 0.7939(3) -0.1109(3) 1.20835(9) 0.0521(7) Uani 1 1 d . . . H28 H 0.7398 -0.1348 1.2315 0.062 Uiso 1 1 calc R . . C29 C 0.9157(3) -0.0934(2) 1.21817(9) 0.0460(7) Uani 1 1 d . . . C30 C 0.9964(3) -0.0524(3) 1.18535(10) 0.0537(8) Uani 1 1 d . . . H30 H 1.0784 -0.0355 1.1932 0.064 Uiso 1 1 calc R . . C31 C 0.9549(3) -0.0364(3) 1.14040(9) 0.0468(7) Uani 1 1 d . . . H31 H 1.0095 -0.0106 1.1177 0.056 Uiso 1 1 calc R . . C32 C 0.9889(3) -0.2264(2) 1.26891(8) 0.0427(6) Uani 1 1 d . . . C33 C 1.0702(3) -0.2352(3) 1.30522(9) 0.0487(7) Uani 1 1 d . . . H33 H 1.1078 -0.1676 1.3217 0.058 Uiso 1 1 calc R . . C34 C 1.0957(3) -0.3440(3) 1.31693(10) 0.0584(8) Uani 1 1 d . . . H34 H 1.1497 -0.3499 1.3417 0.070 Uiso 1 1 calc R . . C35 C 1.0415(3) -0.4453(3) 1.29212(10) 0.0555(8) Uani 1 1 d . . . H35 H 1.0576 -0.5191 1.3003 0.067 Uiso 1 1 calc R . . C36 C 0.9634(2) -0.4342(2) 1.25523(9) 0.0419(6) Uani 1 1 d . . . C37 C 0.9361(2) -0.3254(2) 1.24279(8) 0.0418(6) Uani 1 1 d . . . H37 H 0.8835 -0.3194 1.2175 0.050 Uiso 1 1 calc R . . C38 C 1.0731(2) -0.5677(2) 1.18098(9) 0.0399(6) Uani 1 1 d . . . H38 H 1.1255 -0.5141 1.1997 0.048 Uiso 1 1 calc R . . C39 C 1.1150(2) -0.6270(2) 1.14051(9) 0.0405(6) Uani 1 1 d . . . H39 H 1.1960 -0.6122 1.1322 0.049 Uiso 1 1 calc R . . C40 C 1.0385(2) -0.7079(2) 1.11226(8) 0.0338(5) Uani 1 1 d . . . C41 C 0.9181(2) -0.7301(2) 1.12645(9) 0.0428(6) Uani 1 1 d . . . H41 H 0.8656 -0.7857 1.1087 0.051 Uiso 1 1 calc R . . C42 C 0.8760(2) -0.6713(2) 1.16610(10) 0.0441(6) Uani 1 1 d . . . H42 H 0.7955 -0.6868 1.1749 0.053 Uiso 1 1 calc R . . C43 C 0.9530(2) -0.5892(2) 1.19299(8) 0.0350(6) Uani 1 1 d . . . C44 C 0.9182(2) -0.2282(2) 0.93183(9) 0.0373(6) Uani 1 1 d . . . C45 C -0.1896(2) 0.2652(2) 0.38399(8) 0.0311(5) Uani 1 1 d . . . C46 C -0.1705(2) 0.1575(2) 0.36127(9) 0.0386(6) Uani 1 1 d . . . H46 H -0.1323 0.1040 0.3776 0.046 Uiso 1 1 calc R . . C47 C -0.2068(2) 0.1281(2) 0.31498(9) 0.0422(6) Uani 1 1 d . . . H47 H -0.1903 0.0565 0.2999 0.051 Uiso 1 1 calc R . . C48 C -0.2673(2) 0.2043(2) 0.29106(9) 0.0429(6) Uani 1 1 d . . . C49 C -0.2860(3) 0.3119(3) 0.31228(10) 0.0594(9) Uani 1 1 d . . . H49 H -0.3256 0.3642 0.2959 0.071 Uiso 1 1 calc R . . C50 C -0.2457(3) 0.3429(2) 0.35862(10) 0.0516(7) Uani 1 1 d . . . H50 H -0.2565 0.4171 0.3727 0.062 Uiso 1 1 calc R . . C51 C -0.4140(3) 0.1778(2) 0.22644(9) 0.0429(6) Uani 1 1 d . . . C52 C -0.5156(3) 0.1850(3) 0.25387(10) 0.0517(7) Uani 1 1 d . . . H52 H -0.5095 0.1888 0.2867 0.062 Uiso 1 1 calc R . . C53 C -0.6264(3) 0.1864(3) 0.23165(10) 0.0541(8) Uani 1 1 d . . . C54 C -0.6375(3) 0.1809(3) 0.18319(11) 0.0607(8) Uani 1 1 d . . . H54 H -0.7128 0.1835 0.1688 0.073 Uiso 1 1 calc R . . C55 C -0.5356(3) 0.1714(3) 0.15652(10) 0.0572(8) Uani 1 1 d . . . H55 H -0.5425 0.1662 0.1237 0.069 Uiso 1 1 calc R . . C56 C -0.4239(3) 0.1695(2) 0.17734(9) 0.0481(7) Uani 1 1 d . . . H56 H -0.3554 0.1627 0.1588 0.058 Uiso 1 1 calc R . . C57 C -0.1576(2) 0.2945(2) 0.43570(8) 0.0316(5) Uani 1 1 d . . . C58 C -0.2566(3) 0.7405(3) 0.70300(10) 0.0517(7) Uani 1 1 d . . . C59 C -0.1713(3) 0.7780(3) 0.67075(11) 0.0532(8) Uani 1 1 d . . . H59 H -0.1272 0.8514 0.6760 0.064 Uiso 1 1 calc R . . C60 C -0.1522(2) 0.7059(2) 0.63068(10) 0.0426(6) Uani 1 1 d . . . H60 H -0.0963 0.7319 0.6084 0.051 Uiso 1 1 calc R . . C61 C -0.2154(2) 0.5946(2) 0.62315(8) 0.0308(5) Uani 1 1 d . . . C62 C -0.2995(2) 0.5578(2) 0.65647(9) 0.0390(6) Uani 1 1 d . . . H62 H -0.3420 0.4834 0.6519 0.047 Uiso 1 1 calc R . . C63 C -0.3208(3) 0.6305(3) 0.69629(9) 0.0475(7) Uani 1 1 d . . . H63 H -0.3778 0.6057 0.7183 0.057 Uiso 1 1 calc R . . C64 C -0.1907(2) 0.5157(2) 0.58028(8) 0.0337(5) Uani 1 1 d . . . C65 C 0.0245(2) 0.26664(19) 0.56380(8) 0.0276(5) Uani 1 1 d . . . C66 C 0.1431(2) 0.2660(2) 0.58857(8) 0.0286(5) Uani 1 1 d . . . C67 C 0.1573(2) 0.1848(2) 0.62167(8) 0.0352(6) Uani 1 1 d . . . H67 H 0.0935 0.1285 0.6272 0.042 Uiso 1 1 calc R . . C68 C 0.2657(3) 0.1879(3) 0.64611(9) 0.0455(7) Uani 1 1 d . . . H68 H 0.2751 0.1350 0.6687 0.055 Uiso 1 1 calc R . . C69 C 0.3600(2) 0.2702(3) 0.63686(10) 0.0443(7) Uani 1 1 d . . . C70 C 0.3496(2) 0.3494(2) 0.60367(10) 0.0457(7) Uani 1 1 d . . . H70 H 0.4147 0.4035 0.5975 0.055 Uiso 1 1 calc R . . C71 C 0.2399(2) 0.3471(2) 0.57966(9) 0.0372(6) Uani 1 1 d . . . H71 H 0.2312 0.4006 0.5573 0.045 Uiso 1 1 calc R . . C72 C 0.4773(2) 0.3264(2) 0.70639(9) 0.0419(6) Uani 1 1 d . . . C73 C 0.3907(2) 0.3941(2) 0.72526(9) 0.0447(7) Uani 1 1 d . . . H73 H 0.3208 0.4023 0.7080 0.054 Uiso 1 1 calc R . . C74 C 0.4092(3) 0.4496(3) 0.77022(10) 0.0627(9) Uani 1 1 d . . . H74 H 0.3507 0.4949 0.7833 0.075 Uiso 1 1 calc R . . C75 C 0.5128(3) 0.4391(3) 0.79594(11) 0.0669(9) Uani 1 1 d . . . H75 H 0.5258 0.4785 0.8258 0.080 Uiso 1 1 calc R . . C76 C 0.5967(3) 0.3690(3) 0.77654(10) 0.0517(8) Uani 1 1 d . . . C77 C 0.5813(2) 0.3127(2) 0.73216(10) 0.0476(7) Uani 1 1 d . . . H77 H 0.6392 0.2661 0.7195 0.057 Uiso 1 1 calc R . . C78 C 0.7068(2) 0.2825(2) 0.83512(9) 0.0440(7) Uani 1 1 d . . . C79 C 0.8173(2) 0.2845(2) 0.85849(9) 0.0448(7) Uani 1 1 d . . . H79 H 0.8827 0.3372 0.8513 0.054 Uiso 1 1 calc R . . C80 C 0.8288(2) 0.2073(2) 0.89253(9) 0.0417(6) Uani 1 1 d . . . H80 H 0.9028 0.2086 0.9084 0.050 Uiso 1 1 calc R . . C81 C 0.7328(2) 0.1277(2) 0.90369(8) 0.0332(5) Uani 1 1 d . . . C82 C 0.6221(2) 0.1297(2) 0.88097(9) 0.0429(6) Uani 1 1 d . . . H82 H 0.5558 0.0787 0.8888 0.052 Uiso 1 1 calc R . . C83 C 0.6089(2) 0.2070(3) 0.84668(10) 0.0511(8) Uani 1 1 d . . . H83 H 0.5341 0.2078 0.8315 0.061 Uiso 1 1 calc R . . C84 C 0.7509(2) 0.0422(2) 0.93954(8) 0.0356(6) Uani 1 1 d . . . N1 N -0.39649(18) 0.27819(18) 0.50272(7) 0.0367(5) Uani 1 1 d . . . N2 N -0.33028(17) 0.13025(17) 0.56600(7) 0.0317(4) Uani 1 1 d . . . N3 N 0.51441(19) -0.22735(18) 0.99669(7) 0.0358(5) Uani 1 1 d . . . N4 N 0.7000(2) -0.31333(19) 1.04047(7) 0.0408(5) Uani 1 1 d . . . O1 O 0.86146(16) -0.08140(16) 1.04601(6) 0.0430(4) Uani 1 1 d . . . O2 O 0.67893(18) -0.04996(18) 1.07074(7) 0.0530(5) Uani 1 1 d . . . O1W O -0.9491(2) 0.0689(2) 0.44639(9) 0.0854(7) Uiso 1 1 d . . . O3 O 0.9610(2) -0.11350(17) 1.26265(6) 0.0618(6) Uani 1 1 d . . . O4 O 0.90048(17) -0.53368(16) 1.23142(7) 0.0490(5) Uani 1 1 d . . . O5 O 0.99642(17) -0.16182(16) 0.95621(7) 0.0501(5) Uani 1 1 d . . . O6 O 0.80699(17) -0.24608(16) 0.94163(6) 0.0476(5) Uani 1 1 d . . . O7 O -0.14577(16) 0.39971(14) 0.45215(6) 0.0439(4) Uani 1 1 d . . . O8 O -0.15314(15) 0.20959(14) 0.46120(6) 0.0359(4) Uani 1 1 d . . . O9 O -0.29853(18) 0.1708(2) 0.24392(6) 0.0590(6) Uani 1 1 d . . . O10 O -0.7335(2) 0.1831(2) 0.25751(8) 0.0843(8) Uani 1 1 d . . . O11 O -0.13028(17) 0.56058(16) 0.54781(6) 0.0468(5) Uani 1 1 d . . . O12 O -0.23339(16) 0.40954(16) 0.57956(6) 0.0423(4) Uani 1 1 d . . . O13 O 0.00723(16) 0.34960(14) 0.53893(6) 0.0388(4) Uani 1 1 d . . . O14 O -0.05870(15) 0.18540(15) 0.56842(6) 0.0391(4) Uani 1 1 d . . . O15 O 0.47080(18) 0.2716(2) 0.66128(8) 0.0650(6) Uani 1 1 d . . . O16 O 0.70503(18) 0.3614(2) 0.80107(8) 0.0694(7) Uani 1 1 d . . . O17 O 0.85518(17) 0.04614(18) 0.95761(6) 0.0499(5) Uani 1 1 d . . . O18 O 0.66255(17) -0.02889(16) 0.94956(6) 0.0449(4) Uani 1 1 d . . . Mn1 Mn -0.20481(3) 0.26612(3) 0.532262(12) 0.02888(9) Uani 1 1 d . . . Mn2 Mn 0.0000 0.5000 0.5000 0.02483(11) Uani 1 2 d S . . Mn3 Mn 0.71095(3) -0.15389(3) 0.994849(12) 0.03209(10) Uani 1 1 d . . . Mn4 Mn 1.0000 0.0000 1.0000 0.02779(12) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0388(16) 0.0646(19) 0.0618(19) 0.0271(16) -0.0003(14) 0.0112(14) C2 0.0403(17) 0.085(2) 0.075(2) 0.0325(19) -0.0065(15) 0.0209(17) C3 0.0342(16) 0.078(2) 0.0603(19) 0.0058(17) -0.0115(14) 0.0187(16) C4 0.0263(13) 0.0523(16) 0.0396(14) -0.0080(12) -0.0036(11) 0.0090(12) C5 0.0241(13) 0.0572(18) 0.0557(17) -0.0191(14) -0.0025(12) 0.0034(13) C6 0.0297(14) 0.0433(15) 0.0625(18) -0.0120(14) 0.0088(13) -0.0081(12) C7 0.0331(14) 0.0338(13) 0.0474(15) -0.0069(12) 0.0071(11) -0.0023(11) C8 0.0519(18) 0.0418(16) 0.0644(19) 0.0152(14) 0.0144(15) -0.0043(14) C9 0.0521(19) 0.0554(18) 0.0573(18) 0.0245(15) 0.0034(14) 0.0038(15) C10 0.0376(15) 0.0490(16) 0.0433(15) 0.0153(13) -0.0041(12) 0.0029(12) C11 0.0244(12) 0.0320(12) 0.0339(13) -0.0038(10) 0.0023(10) 0.0038(10) C12 0.0256(12) 0.0366(13) 0.0347(13) -0.0047(10) 0.0005(10) 0.0052(10) C13 0.0541(19) 0.0522(18) 0.0593(19) 0.0103(15) -0.0062(15) 0.0124(15) C14 0.082(3) 0.056(2) 0.064(2) 0.0190(17) -0.0088(18) 0.0249(19) C15 0.102(3) 0.0388(17) 0.0485(18) 0.0132(14) 0.0085(18) 0.0151(18) C16 0.074(2) 0.0347(14) 0.0346(14) 0.0021(12) 0.0134(14) 0.0053(14) C17 0.091(3) 0.0391(16) 0.0417(17) -0.0003(13) 0.0252(17) -0.0132(17) C18 0.068(2) 0.0585(19) 0.0461(17) -0.0042(15) 0.0206(16) -0.0237(17) C19 0.0466(17) 0.0532(17) 0.0371(14) -0.0123(13) 0.0137(13) -0.0073(14) C20 0.0351(16) 0.076(2) 0.0508(18) -0.0157(16) 0.0041(13) -0.0077(15) C21 0.0357(16) 0.078(2) 0.0467(17) -0.0144(16) -0.0061(13) 0.0096(15) C22 0.0387(15) 0.0577(17) 0.0381(14) -0.0024(13) -0.0020(12) 0.0118(13) C23 0.0403(15) 0.0405(14) 0.0291(13) -0.0046(11) 0.0078(11) -0.0015(12) C24 0.0506(16) 0.0361(14) 0.0298(13) 0.0022(11) 0.0095(12) 0.0026(12) C25 0.0441(15) 0.0348(14) 0.0287(13) 0.0062(10) -0.0025(11) 0.0006(11) C26 0.0415(14) 0.0365(13) 0.0264(12) 0.0049(10) -0.0008(10) 0.0086(11) C27 0.0418(16) 0.0618(18) 0.0348(14) 0.0069(13) 0.0033(12) 0.0049(14) C28 0.062(2) 0.0651(19) 0.0303(14) 0.0094(13) 0.0075(13) 0.0066(16) C29 0.072(2) 0.0422(15) 0.0252(13) 0.0027(11) -0.0079(13) 0.0153(14) C30 0.0451(17) 0.071(2) 0.0456(17) 0.0048(15) -0.0115(13) 0.0095(15) C31 0.0421(16) 0.0639(19) 0.0350(14) 0.0098(13) -0.0006(12) 0.0036(14) C32 0.0557(17) 0.0516(16) 0.0224(12) 0.0012(11) -0.0003(11) 0.0146(14) C33 0.0542(18) 0.0602(18) 0.0316(14) -0.0065(13) -0.0104(12) 0.0148(15) C34 0.066(2) 0.074(2) 0.0375(16) -0.0032(15) -0.0169(14) 0.0279(18) C35 0.066(2) 0.0587(19) 0.0461(17) 0.0042(14) -0.0043(15) 0.0283(16) C36 0.0443(15) 0.0511(16) 0.0306(13) -0.0035(12) 0.0070(11) 0.0113(13) C37 0.0480(16) 0.0531(17) 0.0254(13) 0.0019(12) -0.0026(11) 0.0118(13) C38 0.0362(14) 0.0419(15) 0.0376(14) -0.0052(11) 0.0024(11) -0.0085(11) C39 0.0328(14) 0.0443(15) 0.0423(15) 0.0012(12) 0.0071(11) -0.0044(12) C40 0.0369(14) 0.0306(13) 0.0341(13) 0.0045(10) 0.0010(10) 0.0035(11) C41 0.0344(14) 0.0434(15) 0.0476(16) -0.0059(12) -0.0071(12) -0.0023(12) C42 0.0304(14) 0.0489(16) 0.0519(16) 0.0001(13) 0.0042(12) 0.0009(12) C43 0.0381(14) 0.0342(13) 0.0342(13) 0.0054(11) 0.0032(11) 0.0083(11) C44 0.0442(16) 0.0341(14) 0.0335(13) 0.0034(11) 0.0010(11) 0.0032(12) C45 0.0297(12) 0.0295(12) 0.0334(13) 0.0034(10) 0.0000(10) -0.0007(10) C46 0.0444(15) 0.0352(14) 0.0370(14) 0.0039(11) -0.0014(11) 0.0070(12) C47 0.0473(16) 0.0400(15) 0.0384(14) -0.0052(12) 0.0014(12) 0.0061(12) C48 0.0442(16) 0.0538(17) 0.0305(13) -0.0006(12) -0.0003(11) 0.0068(13) C49 0.090(2) 0.0519(18) 0.0398(16) 0.0035(14) -0.0173(16) 0.0281(17) C50 0.076(2) 0.0378(15) 0.0424(16) -0.0019(12) -0.0105(14) 0.0164(15) C51 0.0526(17) 0.0449(15) 0.0308(13) -0.0044(11) -0.0046(12) 0.0087(13) C52 0.0597(19) 0.0618(19) 0.0316(14) -0.0088(13) 0.0039(13) 0.0066(15) C53 0.0478(17) 0.0616(19) 0.0488(17) -0.0205(14) 0.0026(14) 0.0060(15) C54 0.060(2) 0.070(2) 0.0499(18) -0.0146(16) -0.0135(16) 0.0126(17) C55 0.068(2) 0.069(2) 0.0326(15) -0.0014(14) -0.0085(14) 0.0008(17) C56 0.0570(18) 0.0546(17) 0.0299(14) -0.0035(12) 0.0031(13) -0.0023(14) C57 0.0231(12) 0.0353(13) 0.0350(13) -0.0017(11) -0.0022(10) 0.0003(10) C58 0.0416(16) 0.0643(19) 0.0465(16) -0.0167(14) 0.0019(13) 0.0088(14) C59 0.0407(16) 0.0460(16) 0.069(2) -0.0129(15) 0.0029(14) 0.0002(13) C60 0.0337(14) 0.0468(16) 0.0480(16) 0.0055(13) 0.0054(12) 0.0063(12) C61 0.0268(12) 0.0361(13) 0.0318(12) 0.0069(10) 0.0008(10) 0.0106(10) C62 0.0389(14) 0.0380(14) 0.0411(14) 0.0056(11) 0.0037(11) 0.0069(12) C63 0.0474(17) 0.0601(18) 0.0355(14) 0.0036(13) 0.0086(12) 0.0086(14) C64 0.0285(13) 0.0412(15) 0.0344(13) 0.0082(11) 0.0012(10) 0.0135(11) C65 0.0278(12) 0.0289(12) 0.0265(11) 0.0033(9) -0.0011(9) 0.0043(10) C66 0.0275(12) 0.0303(12) 0.0290(12) 0.0021(10) -0.0008(9) 0.0078(10) C67 0.0321(13) 0.0394(14) 0.0355(13) 0.0089(11) -0.0002(10) 0.0055(11) C68 0.0499(17) 0.0540(17) 0.0359(14) 0.0084(13) -0.0081(12) 0.0191(14) C69 0.0306(14) 0.0574(17) 0.0443(15) -0.0131(13) -0.0123(12) 0.0155(13) C70 0.0318(14) 0.0409(15) 0.0624(18) -0.0036(14) -0.0034(13) 0.0001(12) C71 0.0334(14) 0.0324(13) 0.0466(15) 0.0075(11) -0.0019(11) 0.0040(11) C72 0.0361(14) 0.0447(15) 0.0448(15) 0.0050(12) -0.0128(12) 0.0034(12) C73 0.0394(15) 0.0553(17) 0.0407(15) 0.0060(13) -0.0104(12) 0.0103(13) C74 0.060(2) 0.088(2) 0.0408(17) -0.0022(16) -0.0026(15) 0.0146(18) C75 0.068(2) 0.094(3) 0.0355(16) 0.0029(17) -0.0141(15) -0.004(2) C76 0.0444(17) 0.0625(19) 0.0484(17) 0.0335(15) -0.0222(14) -0.0152(15) C77 0.0364(15) 0.0456(16) 0.0621(19) 0.0162(14) -0.0153(13) 0.0025(12) C78 0.0413(15) 0.0546(17) 0.0363(14) 0.0210(13) -0.0138(12) -0.0075(13) C79 0.0305(14) 0.0600(18) 0.0434(15) 0.0189(13) -0.0099(11) -0.0093(12) C80 0.0302(13) 0.0535(16) 0.0421(15) 0.0117(13) -0.0099(11) 0.0020(12) C81 0.0316(13) 0.0414(14) 0.0274(12) 0.0060(10) -0.0050(10) 0.0055(11) C82 0.0342(14) 0.0501(16) 0.0442(15) 0.0186(13) -0.0105(12) -0.0087(12) C83 0.0332(15) 0.0651(19) 0.0561(18) 0.0285(15) -0.0233(13) -0.0076(13) C84 0.0365(14) 0.0455(15) 0.0267(12) 0.0054(11) -0.0022(11) 0.0113(12) N1 0.0270(11) 0.0423(12) 0.0429(12) 0.0115(10) -0.0015(9) 0.0071(9) N2 0.0275(10) 0.0356(11) 0.0321(11) 0.0053(9) -0.0016(8) 0.0016(9) N3 0.0361(12) 0.0404(12) 0.0313(11) 0.0042(9) 0.0033(9) 0.0040(10) N4 0.0421(13) 0.0412(12) 0.0407(12) 0.0096(10) 0.0009(10) 0.0078(10) O1 0.0469(11) 0.0540(11) 0.0259(9) 0.0058(8) 0.0030(8) -0.0077(9) O2 0.0447(12) 0.0738(14) 0.0428(11) 0.0094(10) -0.0103(9) 0.0144(10) O3 0.1086(18) 0.0467(12) 0.0313(10) -0.0003(9) -0.0220(11) 0.0183(12) O4 0.0445(11) 0.0519(11) 0.0494(11) -0.0047(9) 0.0145(9) 0.0050(9) O5 0.0509(12) 0.0477(11) 0.0489(11) -0.0147(9) -0.0064(9) 0.0075(9) O6 0.0480(12) 0.0473(11) 0.0450(11) -0.0055(9) 0.0124(9) -0.0003(9) O7 0.0465(11) 0.0348(10) 0.0485(11) -0.0080(8) -0.0198(9) 0.0059(8) O8 0.0385(10) 0.0353(9) 0.0337(9) 0.0049(8) -0.0040(7) 0.0009(8) O9 0.0545(13) 0.0913(16) 0.0311(10) -0.0120(10) -0.0045(9) 0.0219(12) O10 0.0523(14) 0.1095(19) 0.0781(16) -0.0536(15) 0.0146(12) -0.0070(13) O11 0.0565(12) 0.0477(11) 0.0414(10) 0.0138(9) 0.0210(9) 0.0208(9) O12 0.0399(10) 0.0431(11) 0.0429(10) -0.0011(8) 0.0052(8) 0.0027(8) O13 0.0438(10) 0.0328(9) 0.0418(10) 0.0147(8) -0.0089(8) 0.0054(8) O14 0.0291(9) 0.0390(10) 0.0498(11) 0.0153(8) -0.0070(8) -0.0022(8) O15 0.0392(11) 0.0890(16) 0.0653(14) -0.0269(12) -0.0233(10) 0.0280(11) O16 0.0467(12) 0.0918(16) 0.0700(14) 0.0546(13) -0.0319(11) -0.0282(11) O17 0.0406(11) 0.0686(13) 0.0449(11) 0.0185(10) -0.0107(9) 0.0168(10) O18 0.0437(11) 0.0521(11) 0.0415(10) 0.0205(9) -0.0027(8) 0.0050(9) Mn1 0.02381(18) 0.03183(19) 0.03143(19) 0.00657(15) -0.00247(14) 0.00188(15) Mn2 0.0256(3) 0.0244(2) 0.0248(2) 0.00508(19) 0.00062(19) 0.0017(2) Mn3 0.0301(2) 0.0381(2) 0.02835(19) 0.00691(15) -0.00082(15) 0.00143(16) Mn4 0.0252(3) 0.0341(3) 0.0241(2) 0.0037(2) -0.00346(19) 0.0020(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.323(3) . ? C1 C2 1.394(4) . ? C1 H1 0.9300 . ? C2 C3 1.353(4) . ? C2 H2 0.9300 . ? C3 C4 1.403(4) . ? C3 H3 0.9300 . ? C4 C12 1.411(3) . ? C4 C5 1.421(4) . ? C5 C6 1.344(4) . ? C5 H5 0.9300 . ? C6 C7 1.430(4) . ? C6 H6 0.9300 . ? C7 C8 1.400(4) . ? C7 C11 1.404(3) . ? C8 C9 1.365(4) . ? C8 H8 0.9300 . ? C9 C10 1.395(4) . ? C9 H9 0.9300 . ? C10 N2 1.323(3) . ? C10 H10 0.9300 . ? C11 N2 1.367(3) . ? C11 C12 1.433(3) . ? C12 N1 1.358(3) . ? C13 N4 1.319(3) . ? C13 C14 1.407(4) . ? C13 H13 0.9300 . ? C14 C15 1.354(5) . ? C14 H14 0.9300 . ? C15 C16 1.382(4) . ? C15 H15 0.9300 . ? C16 C24 1.419(4) . ? C16 C17 1.445(4) . ? C17 C18 1.331(4) . ? C17 H17 0.9300 . ? C18 C19 1.430(4) . ? C18 H18 0.9300 . ? C19 C23 1.401(4) . ? C19 C20 1.405(4) . ? C20 C21 1.358(4) . ? C20 H20 0.9300 . ? C21 C22 1.401(4) . ? C21 H21 0.9300 . ? C22 N3 1.323(3) . ? C22 H22 0.9300 . ? C23 N3 1.368(3) . ? C23 C24 1.433(4) . ? C24 N4 1.354(3) . ? C25 O2 1.233(3) . ? C25 O1 1.288(3) . ? C25 C26 1.493(3) . ? C26 C31 1.381(4) . ? C26 C27 1.386(3) . ? C27 C28 1.385(4) . ? C27 H27 0.9300 . ? C28 C29 1.365(4) . ? C28 H28 0.9300 . ? C29 C30 1.371(4) . ? C29 O3 1.398(3) . ? C30 C31 1.384(4) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 C33 1.379(4) . ? C32 C37 1.380(4) . ? C32 O3 1.386(3) . ? C33 C34 1.373(4) . ? C33 H33 0.9300 . ? C34 C35 1.387(4) . ? C34 H34 0.9300 . ? C35 C36 1.374(4) . ? C35 H35 0.9300 . ? C36 C37 1.386(4) . ? C36 O4 1.396(3) . ? C37 H37 0.9300 . ? C38 C43 1.376(3) . ? C38 C39 1.391(3) . ? C38 H38 0.9300 . ? C39 C40 1.389(3) . ? C39 H39 0.9300 . ? C40 C41 1.398(4) . ? C40 C44 1.502(3) 2_747 ? C41 C42 1.370(4) . ? C41 H41 0.9300 . ? C42 C43 1.380(4) . ? C42 H42 0.9300 . ? C43 O4 1.377(3) . ? C44 O5 1.257(3) . ? C44 O6 1.262(3) . ? C44 C40 1.502(3) 2_747 ? C45 C50 1.381(3) . ? C45 C46 1.382(3) . ? C45 C57 1.508(3) . ? C46 C47 1.374(3) . ? C46 H46 0.9300 . ? C47 C48 1.371(4) . ? C47 H47 0.9300 . ? C48 C49 1.364(4) . ? C48 O9 1.391(3) . ? C49 C50 1.391(4) . ? C49 H49 0.9300 . ? C50 H50 0.9300 . ? C51 C52 1.376(4) . ? C51 O9 1.379(3) . ? C51 C56 1.389(3) . ? C52 C53 1.377(4) . ? C52 H52 0.9300 . ? C53 C54 1.374(4) . ? C53 O10 1.395(4) . ? C54 C55 1.368(4) . ? C54 H54 0.9300 . ? C55 C56 1.369(4) . ? C55 H55 0.9300 . ? C56 H56 0.9300 . ? C57 O7 1.252(3) . ? C57 O8 1.264(3) . ? C58 O10 1.376(3) 2_466 ? C58 C59 1.379(4) . ? C58 C63 1.382(4) . ? C59 C60 1.380(4) . ? C59 H59 0.9300 . ? C60 C61 1.392(4) . ? C60 H60 0.9300 . ? C61 C62 1.390(3) . ? C61 C64 1.498(3) . ? C62 C63 1.384(4) . ? C62 H62 0.9300 . ? C63 H63 0.9300 . ? C64 O11 1.254(3) . ? C64 O12 1.260(3) . ? C65 O14 1.257(3) . ? C65 O13 1.258(3) . ? C65 C66 1.485(3) . ? C66 C71 1.384(3) . ? C66 C67 1.394(3) . ? C67 C68 1.377(4) . ? C67 H67 0.9300 . ? C68 C69 1.375(4) . ? C68 H68 0.9300 . ? C69 C70 1.373(4) . ? C69 O15 1.401(3) . ? C70 C71 1.383(4) . ? C70 H70 0.9300 . ? C71 H71 0.9300 . ? C72 O15 1.376(3) . ? C72 C73 1.376(4) . ? C72 C77 1.387(3) . ? C73 C74 1.381(4) . ? C73 H73 0.9300 . ? C74 C75 1.375(4) . ? C74 H74 0.9300 . ? C75 C76 1.377(5) . ? C75 H75 0.9300 . ? C76 C77 1.367(4) . ? C76 O16 1.395(3) . ? C77 H77 0.9300 . ? C78 C83 1.376(4) . ? C78 O16 1.377(3) . ? C78 C79 1.383(3) . ? C79 C80 1.375(3) . ? C79 H79 0.9300 . ? C80 C81 1.385(3) . ? C80 H80 0.9300 . ? C81 C82 1.383(3) . ? C81 C84 1.495(3) . ? C82 C83 1.384(3) . ? C82 H82 0.9300 . ? C83 H83 0.9300 . ? C84 O17 1.254(3) . ? C84 O18 1.257(3) . ? N1 Mn1 2.296(2) . ? N2 Mn1 2.2566(19) . ? N3 Mn3 2.253(2) . ? N4 Mn3 2.319(2) . ? O1 Mn4 2.2028(16) . ? O1 Mn3 2.2486(18) . ? O2 Mn3 2.418(2) . ? O5 Mn4 2.1436(17) . ? O6 Mn3 2.1225(17) . ? O7 Mn2 2.2591(16) . ? O8 Mn1 2.1623(16) . ? O10 C58 1.376(3) 2_466 ? O11 Mn2 2.1131(16) . ? O12 Mn1 2.0863(17) . ? O13 Mn2 2.1305(15) . ? O13 Mn1 2.4416(18) . ? O14 Mn1 2.2260(16) . ? O17 Mn4 2.1305(17) . ? O18 Mn3 2.1067(17) . ? Mn2 O11 2.1131(16) 2_566 ? Mn2 O13 2.1305(15) 2_566 ? Mn2 O7 2.2591(16) 2_566 ? Mn4 O17 2.1305(17) 2_757 ? Mn4 O5 2.1436(17) 2_757 ? Mn4 O1 2.2028(17) 2_757 ? 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 N1 C1 C2 123.7(3) . . ? N1 C1 H1 118.2 . . ? C2 C1 H1 118.2 . . ? C3 C2 C1 119.0(3) . . ? C3 C2 H2 120.5 . . ? C1 C2 H2 120.5 . . ? C2 C3 C4 119.9(3) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C3 C4 C12 117.2(3) . . ? C3 C4 C5 123.4(2) . . ? C12 C4 C5 119.3(2) . . ? C6 C5 C4 121.4(2) . . ? C6 C5 H5 119.3 . . ? C4 C5 H5 119.3 . . ? C5 C6 C7 120.9(3) . . ? C5 C6 H6 119.5 . . ? C7 C6 H6 119.5 . . ? C8 C7 C11 117.8(2) . . ? C8 C7 C6 123.0(3) . . ? C11 C7 C6 119.2(3) . . ? C9 C8 C7 119.3(3) . . ? C9 C8 H8 120.3 . . ? C7 C8 H8 120.3 . . ? C8 C9 C10 119.6(3) . . ? C8 C9 H9 120.2 . . ? C10 C9 H9 120.2 . . ? N2 C10 C9 122.9(3) . . ? N2 C10 H10 118.6 . . ? C9 C10 H10 118.6 . . ? N2 C11 C7 122.3(2) . . ? N2 C11 C12 117.9(2) . . ? C7 C11 C12 119.8(2) . . ? N1 C12 C4 122.6(2) . . ? N1 C12 C11 118.2(2) . . ? C4 C12 C11 119.3(2) . . ? N4 C13 C14 122.5(3) . . ? N4 C13 H13 118.7 . . ? C14 C13 H13 118.7 . . ? C15 C14 C13 119.0(3) . . ? C15 C14 H14 120.5 . . ? C13 C14 H14 120.5 . . ? C14 C15 C16 120.4(3) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C15 C16 C24 117.5(3) . . ? C15 C16 C17 124.5(3) . . ? C24 C16 C17 118.0(3) . . ? C18 C17 C16 121.7(3) . . ? C18 C17 H17 119.2 . . ? C16 C17 H17 119.2 . . ? C17 C18 C19 121.5(3) . . ? C17 C18 H18 119.3 . . ? C19 C18 H18 119.3 . . ? C23 C19 C20 117.1(3) . . ? C23 C19 C18 119.1(3) . . ? C20 C19 C18 123.8(3) . . ? C21 C20 C19 120.2(3) . . ? C21 C20 H20 119.9 . . ? C19 C20 H20 119.9 . . ? C20 C21 C22 118.8(3) . . ? C20 C21 H21 120.6 . . ? C22 C21 H21 120.6 . . ? N3 C22 C21 123.4(3) . . ? N3 C22 H22 118.3 . . ? C21 C22 H22 118.3 . . ? N3 C23 C19 122.8(3) . . ? N3 C23 C24 117.3(2) . . ? C19 C23 C24 120.0(2) . . ? N4 C24 C16 121.9(3) . . ? N4 C24 C23 118.3(2) . . ? C16 C24 C23 119.8(3) . . ? O2 C25 O1 121.1(2) . . ? O2 C25 C26 121.4(2) . . ? O1 C25 C26 117.1(2) . . ? C31 C26 C27 119.4(2) . . ? C31 C26 C25 121.7(2) . . ? C27 C26 C25 118.6(2) . . ? C28 C27 C26 120.0(3) . . ? C28 C27 H27 120.0 . . ? C26 C27 H27 120.0 . . ? C29 C28 C27 119.6(3) . . ? C29 C28 H28 120.2 . . ? C27 C28 H28 120.2 . . ? C28 C29 C30 121.1(2) . . ? C28 C29 O3 120.7(3) . . ? C30 C29 O3 118.2(3) . . ? C29 C30 C31 119.5(3) . . ? C29 C30 H30 120.3 . . ? C31 C30 H30 120.3 . . ? C26 C31 C30 120.2(3) . . ? C26 C31 H31 119.9 . . ? C30 C31 H31 119.9 . . ? C33 C32 C37 120.9(3) . . ? C33 C32 O3 115.4(3) . . ? C37 C32 O3 123.7(2) . . ? C34 C33 C32 119.8(3) . . ? C34 C33 H33 120.1 . . ? C32 C33 H33 120.1 . . ? C33 C34 C35 120.6(3) . . ? C33 C34 H34 119.7 . . ? C35 C34 H34 119.7 . . ? C36 C35 C34 118.6(3) . . ? C36 C35 H35 120.7 . . ? C34 C35 H35 120.7 . . ? C35 C36 C37 122.0(3) . . ? C35 C36 O4 120.4(3) . . ? C37 C36 O4 117.4(2) . . ? C32 C37 C36 118.1(2) . . ? C32 C37 H37 120.9 . . ? C36 C37 H37 120.9 . . ? C43 C38 C39 119.1(2) . . ? C43 C38 H38 120.4 . . ? C39 C38 H38 120.4 . . ? C40 C39 C38 121.4(2) . . ? C40 C39 H39 119.3 . . ? C38 C39 H39 119.3 . . ? C39 C40 C41 117.7(2) . . ? C39 C40 C44 122.2(2) . 2_747 ? C41 C40 C44 120.1(2) . 2_747 ? C42 C41 C40 121.1(2) . . ? C42 C41 H41 119.5 . . ? C40 C41 H41 119.5 . . ? C41 C42 C43 120.1(2) . . ? C41 C42 H42 119.9 . . ? C43 C42 H42 119.9 . . ? C38 C43 O4 124.4(2) . . ? C38 C43 C42 120.5(2) . . ? O4 C43 C42 115.2(2) . . ? O5 C44 O6 125.3(2) . . ? O5 C44 C40 117.0(2) . 2_747 ? O6 C44 C40 117.7(2) . 2_747 ? C50 C45 C46 117.9(2) . . ? C50 C45 C57 120.7(2) . . ? C46 C45 C57 121.3(2) . . ? C47 C46 C45 121.2(2) . . ? C47 C46 H46 119.4 . . ? C45 C46 H46 119.4 . . ? C48 C47 C46 120.0(2) . . ? C48 C47 H47 120.0 . . ? C46 C47 H47 120.0 . . ? C49 C48 C47 120.1(2) . . ? C49 C48 O9 122.5(3) . . ? C47 C48 O9 117.2(2) . . ? C48 C49 C50 119.6(3) . . ? C48 C49 H49 120.2 . . ? C50 C49 H49 120.2 . . ? C45 C50 C49 121.0(3) . . ? C45 C50 H50 119.5 . . ? C49 C50 H50 119.5 . . ? C52 C51 O9 124.6(2) . . ? C52 C51 C56 120.5(3) . . ? O9 C51 C56 114.9(2) . . ? C51 C52 C53 118.6(3) . . ? C51 C52 H52 120.7 . . ? C53 C52 H52 120.7 . . ? C54 C53 C52 121.7(3) . . ? C54 C53 O10 117.2(3) . . ? C52 C53 O10 120.9(3) . . ? C55 C54 C53 118.8(3) . . ? C55 C54 H54 120.6 . . ? C53 C54 H54 120.6 . . ? C54 C55 C56 121.2(3) . . ? C54 C55 H55 119.4 . . ? C56 C55 H55 119.4 . . ? C55 C56 C51 119.3(3) . . ? C55 C56 H56 120.4 . . ? C51 C56 H56 120.4 . . ? O7 C57 O8 122.9(2) . . ? O7 C57 C45 119.5(2) . . ? O8 C57 C45 117.4(2) . . ? O10 C58 C59 115.2(3) 2_466 . ? O10 C58 C63 123.8(3) 2_466 . ? C59 C58 C63 120.9(3) . . ? C58 C59 C60 119.5(3) . . ? C58 C59 H59 120.3 . . ? C60 C59 H59 120.3 . . ? C59 C60 C61 120.8(3) . . ? C59 C60 H60 119.6 . . ? C61 C60 H60 119.6 . . ? C62 C61 C60 118.8(2) . . ? C62 C61 C64 121.0(2) . . ? C60 C61 C64 120.2(2) . . ? C63 C62 C61 120.7(3) . . ? C63 C62 H62 119.7 . . ? C61 C62 H62 119.7 . . ? C58 C63 C62 119.3(3) . . ? C58 C63 H63 120.3 . . ? C62 C63 H63 120.3 . . ? O11 C64 O12 125.2(2) . . ? O11 C64 C61 117.6(2) . . ? O12 C64 C61 117.2(2) . . ? O14 C65 O13 120.4(2) . . ? O14 C65 C66 119.8(2) . . ? O13 C65 C66 119.7(2) . . ? C71 C66 C67 119.4(2) . . ? C71 C66 C65 120.5(2) . . ? C67 C66 C65 120.1(2) . . ? C68 C67 C66 119.9(2) . . ? C68 C67 H67 120.0 . . ? C66 C67 H67 120.0 . . ? C69 C68 C67 119.4(2) . . ? C69 C68 H68 120.3 . . ? C67 C68 H68 120.3 . . ? C70 C69 C68 121.8(2) . . ? C70 C69 O15 119.0(3) . . ? C68 C69 O15 119.1(3) . . ? C69 C70 C71 118.6(3) . . ? C69 C70 H70 120.7 . . ? C71 C70 H70 120.7 . . ? C70 C71 C66 120.8(2) . . ? C70 C71 H71 119.6 . . ? C66 C71 H71 119.6 . . ? O15 C72 C73 123.9(2) . . ? O15 C72 C77 115.3(2) . . ? C73 C72 C77 120.8(3) . . ? C72 C73 C74 119.1(3) . . ? C72 C73 H73 120.5 . . ? C74 C73 H73 120.5 . . ? C75 C74 C73 121.0(3) . . ? C75 C74 H74 119.5 . . ? C73 C74 H74 119.5 . . ? C74 C75 C76 118.6(3) . . ? C74 C75 H75 120.7 . . ? C76 C75 H75 120.7 . . ? C77 C76 C75 121.8(3) . . ? C77 C76 O16 118.5(3) . . ? C75 C76 O16 119.5(3) . . ? C76 C77 C72 118.6(3) . . ? C76 C77 H77 120.7 . . ? C72 C77 H77 120.7 . . ? C83 C78 O16 124.8(2) . . ? C83 C78 C79 120.6(2) . . ? O16 C78 C79 114.6(2) . . ? C80 C79 C78 119.0(2) . . ? C80 C79 H79 120.5 . . ? C78 C79 H79 120.5 . . ? C79 C80 C81 121.5(2) . . ? C79 C80 H80 119.2 . . ? C81 C80 H80 119.2 . . ? C82 C81 C80 118.5(2) . . ? C82 C81 C84 121.8(2) . . ? C80 C81 C84 119.7(2) . . ? C81 C82 C83 120.6(2) . . ? C81 C82 H82 119.7 . . ? C83 C82 H82 119.7 . . ? C78 C83 C82 119.7(2) . . ? C78 C83 H83 120.2 . . ? C82 C83 H83 120.2 . . ? O17 C84 O18 124.1(2) . . ? O17 C84 C81 116.9(2) . . ? O18 C84 C81 118.9(2) . . ? C1 N1 C12 117.5(2) . . ? C1 N1 Mn1 127.77(18) . . ? C12 N1 Mn1 114.68(15) . . ? C10 N2 C11 118.1(2) . . ? C10 N2 Mn1 126.12(17) . . ? C11 N2 Mn1 115.81(15) . . ? C22 N3 C23 117.6(2) . . ? C22 N3 Mn3 125.18(18) . . ? C23 N3 Mn3 117.09(17) . . ? C13 N4 C24 118.6(2) . . ? C13 N4 Mn3 126.5(2) . . ? C24 N4 Mn3 114.80(17) . . ? C25 O1 Mn4 143.61(17) . . ? C25 O1 Mn3 92.79(15) . . ? Mn4 O1 Mn3 103.18(6) . . ? C25 O2 Mn3 86.47(15) . . ? C32 O3 C29 117.1(2) . . ? C43 O4 C36 119.3(2) . . ? C44 O5 Mn4 136.42(18) . . ? C44 O6 Mn3 127.52(17) . . ? C57 O7 Mn2 130.53(15) . . ? C57 O8 Mn1 108.32(14) . . ? C51 O9 C48 121.7(2) . . ? C58 O10 C53 120.7(2) 2_466 . ? C64 O11 Mn2 133.99(16) . . ? C64 O12 Mn1 130.38(16) . . ? C65 O13 Mn2 172.75(16) . . ? C65 O13 Mn1 86.73(14) . . ? Mn2 O13 Mn1 100.32(6) . . ? C65 O14 Mn1 96.77(13) . . ? C72 O15 C69 116.4(2) . . ? C78 O16 C76 119.1(2) . . ? C84 O17 Mn4 159.12(19) . . ? C84 O18 Mn3 113.11(15) . . ? O12 Mn1 O8 145.72(7) . . ? O12 Mn1 O14 102.53(7) . . ? O8 Mn1 O14 95.50(6) . . ? O12 Mn1 N2 97.44(7) . . ? O8 Mn1 N2 113.34(7) . . ? O14 Mn1 N2 84.19(6) . . ? O12 Mn1 N1 87.06(7) . . ? O8 Mn1 N1 87.77(7) . . ? O14 Mn1 N1 156.47(7) . . ? N2 Mn1 N1 73.19(7) . . ? O12 Mn1 O13 83.46(6) . . ? O8 Mn1 O13 83.13(6) . . ? O14 Mn1 O13 55.54(6) . . ? N2 Mn1 O13 138.47(6) . . ? N1 Mn1 O13 147.85(6) . . ? O11 Mn2 O11 180.00(7) 2_566 . ? O11 Mn2 O13 90.77(7) 2_566 . ? O11 Mn2 O13 89.23(7) . . ? O11 Mn2 O13 89.23(7) 2_566 2_566 ? O11 Mn2 O13 90.77(7) . 2_566 ? O13 Mn2 O13 180.00(7) . 2_566 ? O11 Mn2 O7 91.95(7) 2_566 2_566 ? O11 Mn2 O7 88.05(7) . 2_566 ? O13 Mn2 O7 90.16(6) . 2_566 ? O13 Mn2 O7 89.84(6) 2_566 2_566 ? O11 Mn2 O7 88.05(7) 2_566 . ? O11 Mn2 O7 91.95(7) . . ? O13 Mn2 O7 89.84(6) . . ? O13 Mn2 O7 90.16(6) 2_566 . ? O7 Mn2 O7 180.0 2_566 . ? O18 Mn3 O6 93.75(7) . . ? O18 Mn3 O1 112.58(7) . . ? O6 Mn3 O1 101.78(7) . . ? O18 Mn3 N3 89.45(7) . . ? O6 Mn3 N3 111.56(7) . . ? O1 Mn3 N3 138.66(7) . . ? O18 Mn3 N4 161.77(8) . . ? O6 Mn3 N4 90.96(7) . . ? O1 Mn3 N4 83.55(7) . . ? N3 Mn3 N4 72.46(8) . . ? O18 Mn3 O2 99.80(7) . . ? O6 Mn3 O2 157.14(7) . . ? O1 Mn3 O2 55.98(6) . . ? N3 Mn3 O2 87.05(7) . . ? N4 Mn3 O2 81.89(7) . . ? O17 Mn4 O17 180.000(1) 2_757 . ? O17 Mn4 O5 91.65(7) 2_757 . ? O17 Mn4 O5 88.35(8) . . ? O17 Mn4 O5 88.35(8) 2_757 2_757 ? O17 Mn4 O5 91.65(7) . 2_757 ? O5 Mn4 O5 180.000(1) . 2_757 ? O17 Mn4 O1 92.17(7) 2_757 . ? O17 Mn4 O1 87.83(7) . . ? O5 Mn4 O1 90.26(7) . . ? O5 Mn4 O1 89.74(7) 2_757 . ? O17 Mn4 O1 87.83(7) 2_757 2_757 ? O17 Mn4 O1 92.17(7) . 2_757 ? O5 Mn4 O1 89.74(7) . 2_757 ? O5 Mn4 O1 90.26(7) 2_757 2_757 ? O1 Mn4 O1 180.0 . 2_757 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 -1.3(5) . . . . ? C1 C2 C3 C4 1.3(5) . . . . ? C2 C3 C4 C12 0.3(4) . . . . ? C2 C3 C4 C5 178.6(3) . . . . ? C3 C4 C5 C6 -175.9(3) . . . . ? C12 C4 C5 C6 2.3(4) . . . . ? C4 C5 C6 C7 -0.7(4) . . . . ? C5 C6 C7 C8 178.0(2) . . . . ? C5 C6 C7 C11 -1.6(4) . . . . ? C11 C7 C8 C9 -1.8(4) . . . . ? C6 C7 C8 C9 178.6(3) . . . . ? C7 C8 C9 C10 -0.2(5) . . . . ? C8 C9 C10 N2 1.7(5) . . . . ? C8 C7 C11 N2 2.5(3) . . . . ? C6 C7 C11 N2 -177.9(2) . . . . ? C8 C7 C11 C12 -177.2(2) . . . . ? C6 C7 C11 C12 2.4(3) . . . . ? C3 C4 C12 N1 -2.2(4) . . . . ? C5 C4 C12 N1 179.5(2) . . . . ? C3 C4 C12 C11 176.8(2) . . . . ? C5 C4 C12 C11 -1.5(3) . . . . ? N2 C11 C12 N1 -1.5(3) . . . . ? C7 C11 C12 N1 178.2(2) . . . . ? N2 C11 C12 C4 179.4(2) . . . . ? C7 C11 C12 C4 -0.8(3) . . . . ? N4 C13 C14 C15 1.2(5) . . . . ? C13 C14 C15 C16 -1.2(5) . . . . ? C14 C15 C16 C24 0.3(4) . . . . ? C14 C15 C16 C17 178.4(3) . . . . ? C15 C16 C17 C18 179.5(3) . . . . ? C24 C16 C17 C18 -2.4(4) . . . . ? C16 C17 C18 C19 1.0(4) . . . . ? C17 C18 C19 C23 1.0(4) . . . . ? C17 C18 C19 C20 -179.8(3) . . . . ? C23 C19 C20 C21 -1.0(4) . . . . ? C18 C19 C20 C21 179.8(3) . . . . ? C19 C20 C21 C22 1.7(4) . . . . ? C20 C21 C22 N3 -0.6(4) . . . . ? C20 C19 C23 N3 -0.9(4) . . . . ? C18 C19 C23 N3 178.4(2) . . . . ? C20 C19 C23 C24 179.2(2) . . . . ? C18 C19 C23 C24 -1.5(4) . . . . ? C15 C16 C24 N4 0.5(4) . . . . ? C17 C16 C24 N4 -177.6(2) . . . . ? C15 C16 C24 C23 -180.0(2) . . . . ? C17 C16 C24 C23 1.9(4) . . . . ? N3 C23 C24 N4 -0.3(3) . . . . ? C19 C23 C24 N4 179.6(2) . . . . ? N3 C23 C24 C16 -179.9(2) . . . . ? C19 C23 C24 C16 0.0(3) . . . . ? O2 C25 C26 C31 -161.9(3) . . . . ? O1 C25 C26 C31 25.1(4) . . . . ? O2 C25 C26 C27 24.5(4) . . . . ? O1 C25 C26 C27 -148.6(2) . . . . ? C31 C26 C27 C28 -3.7(4) . . . . ? C25 C26 C27 C28 170.1(3) . . . . ? C26 C27 C28 C29 0.8(4) . . . . ? C27 C28 C29 C30 3.4(5) . . . . ? C27 C28 C29 O3 -178.6(2) . . . . ? C28 C29 C30 C31 -4.7(5) . . . . ? O3 C29 C30 C31 177.3(3) . . . . ? C27 C26 C31 C30 2.4(4) . . . . ? C25 C26 C31 C30 -171.1(3) . . . . ? C29 C30 C31 C26 1.7(4) . . . . ? C37 C32 C33 C34 -2.6(4) . . . . ? O3 C32 C33 C34 174.4(3) . . . . ? C32 C33 C34 C35 0.9(5) . . . . ? C33 C34 C35 C36 1.0(5) . . . . ? C34 C35 C36 C37 -1.1(4) . . . . ? C34 C35 C36 O4 -175.6(3) . . . . ? C33 C32 C37 C36 2.4(4) . . . . ? O3 C32 C37 C36 -174.3(2) . . . . ? C35 C36 C37 C32 -0.5(4) . . . . ? O4 C36 C37 C32 174.1(2) . . . . ? C43 C38 C39 C40 -0.4(4) . . . . ? C38 C39 C40 C41 -1.6(4) . . . . ? C38 C39 C40 C44 179.3(2) . . . 2_747 ? C39 C40 C41 C42 2.0(4) . . . . ? C44 C40 C41 C42 -178.8(2) 2_747 . . . ? C40 C41 C42 C43 -0.4(4) . . . . ? C39 C38 C43 O4 -178.2(2) . . . . ? C39 C38 C43 C42 2.1(4) . . . . ? C41 C42 C43 C38 -1.6(4) . . . . ? C41 C42 C43 O4 178.6(2) . . . . ? C50 C45 C46 C47 -0.5(4) . . . . ? C57 C45 C46 C47 175.8(2) . . . . ? C45 C46 C47 C48 -2.5(4) . . . . ? C46 C47 C48 C49 3.4(4) . . . . ? C46 C47 C48 O9 178.3(2) . . . . ? C47 C48 C49 C50 -1.3(5) . . . . ? O9 C48 C49 C50 -175.9(3) . . . . ? C46 C45 C50 C49 2.6(4) . . . . ? C57 C45 C50 C49 -173.7(3) . . . . ? C48 C49 C50 C45 -1.7(5) . . . . ? O9 C51 C52 C53 -177.2(3) . . . . ? C56 C51 C52 C53 -1.4(4) . . . . ? C51 C52 C53 C54 0.0(5) . . . . ? C51 C52 C53 O10 174.3(3) . . . . ? C52 C53 C54 C55 1.3(5) . . . . ? O10 C53 C54 C55 -173.2(3) . . . . ? C53 C54 C55 C56 -1.1(5) . . . . ? C54 C55 C56 C51 -0.3(5) . . . . ? C52 C51 C56 C55 1.5(4) . . . . ? O9 C51 C56 C55 177.8(3) . . . . ? C50 C45 C57 O7 -22.3(3) . . . . ? C46 C45 C57 O7 161.5(2) . . . . ? C50 C45 C57 O8 152.5(2) . . . . ? C46 C45 C57 O8 -23.8(3) . . . . ? O10 C58 C59 C60 178.0(3) 2_466 . . . ? C63 C58 C59 C60 1.6(5) . . . . ? C58 C59 C60 C61 -1.8(4) . . . . ? C59 C60 C61 C62 0.8(4) . . . . ? C59 C60 C61 C64 -178.0(2) . . . . ? C60 C61 C62 C63 0.4(4) . . . . ? C64 C61 C62 C63 179.2(2) . . . . ? O10 C58 C63 C62 -176.5(3) 2_466 . . . ? C59 C58 C63 C62 -0.4(4) . . . . ? C61 C62 C63 C58 -0.6(4) . . . . ? C62 C61 C64 O11 168.0(2) . . . . ? C60 C61 C64 O11 -13.3(3) . . . . ? C62 C61 C64 O12 -11.4(3) . . . . ? C60 C61 C64 O12 167.4(2) . . . . ? O14 C65 C66 C71 172.6(2) . . . . ? O13 C65 C66 C71 -8.5(3) . . . . ? O14 C65 C66 C67 -8.5(3) . . . . ? O13 C65 C66 C67 170.4(2) . . . . ? C71 C66 C67 C68 1.9(4) . . . . ? C65 C66 C67 C68 -177.1(2) . . . . ? C66 C67 C68 C69 -1.3(4) . . . . ? C67 C68 C69 C70 -0.2(4) . . . . ? C67 C68 C69 O15 -178.9(2) . . . . ? C68 C69 C70 C71 1.1(4) . . . . ? O15 C69 C70 C71 179.8(2) . . . . ? C69 C70 C71 C66 -0.5(4) . . . . ? C67 C66 C71 C70 -1.0(4) . . . . ? C65 C66 C71 C70 178.0(2) . . . . ? O15 C72 C73 C74 -177.0(3) . . . . ? C77 C72 C73 C74 0.7(4) . . . . ? C72 C73 C74 C75 0.6(5) . . . . ? C73 C74 C75 C76 -1.9(5) . . . . ? C74 C75 C76 C77 1.8(5) . . . . ? C74 C75 C76 O16 177.0(3) . . . . ? C75 C76 C77 C72 -0.5(4) . . . . ? O16 C76 C77 C72 -175.7(2) . . . . ? O15 C72 C77 C76 177.1(3) . . . . ? C73 C72 C77 C76 -0.8(4) . . . . ? C83 C78 C79 C80 1.9(4) . . . . ? O16 C78 C79 C80 -178.8(3) . . . . ? C78 C79 C80 C81 0.3(4) . . . . ? C79 C80 C81 C82 -2.3(4) . . . . ? C79 C80 C81 C84 177.5(2) . . . . ? C80 C81 C82 C83 2.1(4) . . . . ? C84 C81 C82 C83 -177.7(3) . . . . ? O16 C78 C83 C82 178.7(3) . . . . ? C79 C78 C83 C82 -2.1(5) . . . . ? C81 C82 C83 C78 0.0(5) . . . . ? C82 C81 C84 O17 178.9(2) . . . . ? C80 C81 C84 O17 -0.9(3) . . . . ? C82 C81 C84 O18 -0.7(4) . . . . ? C80 C81 C84 O18 179.4(2) . . . . ? C2 C1 N1 C12 -0.5(4) . . . . ? C2 C1 N1 Mn1 177.9(2) . . . . ? C4 C12 N1 C1 2.3(4) . . . . ? C11 C12 N1 C1 -176.7(2) . . . . ? C4 C12 N1 Mn1 -176.35(18) . . . . ? C11 C12 N1 Mn1 4.6(3) . . . . ? C9 C10 N2 C11 -1.0(4) . . . . ? C9 C10 N2 Mn1 -179.7(2) . . . . ? C7 C11 N2 C10 -1.1(3) . . . . ? C12 C11 N2 C10 178.6(2) . . . . ? C7 C11 N2 Mn1 177.74(17) . . . . ? C12 C11 N2 Mn1 -2.5(3) . . . . ? C21 C22 N3 C23 -1.2(4) . . . . ? C21 C22 N3 Mn3 -178.01(19) . . . . ? C19 C23 N3 C22 1.9(3) . . . . ? C24 C23 N3 C22 -178.2(2) . . . . ? C19 C23 N3 Mn3 178.99(18) . . . . ? C24 C23 N3 Mn3 -1.1(3) . . . . ? C14 C13 N4 C24 -0.4(4) . . . . ? C14 C13 N4 Mn3 177.9(2) . . . . ? C16 C24 N4 C13 -0.5(4) . . . . ? C23 C24 N4 C13 180.0(2) . . . . ? C16 C24 N4 Mn3 -178.95(18) . . . . ? C23 C24 N4 Mn3 1.5(3) . . . . ? O2 C25 O1 Mn4 96.6(3) . . . . ? C26 C25 O1 Mn4 -90.3(3) . . . . ? O2 C25 O1 Mn3 -20.2(3) . . . . ? C26 C25 O1 Mn3 152.90(19) . . . . ? O1 C25 O2 Mn3 18.7(2) . . . . ? C26 C25 O2 Mn3 -154.1(2) . . . . ? C33 C32 O3 C29 158.2(3) . . . . ? C37 C32 O3 C29 -24.9(4) . . . . ? C28 C29 O3 C32 88.4(3) . . . . ? C30 C29 O3 C32 -93.6(3) . . . . ? C38 C43 O4 C36 12.6(4) . . . . ? C42 C43 O4 C36 -167.7(2) . . . . ? C35 C36 O4 C43 -89.2(3) . . . . ? C37 C36 O4 C43 96.2(3) . . . . ? O6 C44 O5 Mn4 -33.5(4) . . . . ? C40 C44 O5 Mn4 147.06(19) 2_747 . . . ? O5 C44 O6 Mn3 10.0(4) . . . . ? C40 C44 O6 Mn3 -170.61(15) 2_747 . . . ? O8 C57 O7 Mn2 51.5(3) . . . . ? C45 C57 O7 Mn2 -134.02(19) . . . . ? O7 C57 O8 Mn1 25.5(3) . . . . ? C45 C57 O8 Mn1 -149.09(16) . . . . ? C52 C51 O9 C48 -19.1(4) . . . . ? C56 C51 O9 C48 164.8(3) . . . . ? C49 C48 O9 C51 -53.3(4) . . . . ? C47 C48 O9 C51 132.0(3) . . . . ? C54 C53 O10 C58 -135.1(3) . . . 2_466 ? C52 C53 O10 C58 50.4(5) . . . 2_466 ? O12 C64 O11 Mn2 -36.2(4) . . . . ? C61 C64 O11 Mn2 144.55(19) . . . . ? O11 C64 O12 Mn1 9.2(4) . . . . ? C61 C64 O12 Mn1 -171.53(15) . . . . ? O14 C65 O13 Mn2 173.4(11) . . . . ? C66 C65 O13 Mn2 -5.4(14) . . . . ? O14 C65 O13 Mn1 6.9(2) . . . . ? C66 C65 O13 Mn1 -171.92(19) . . . . ? O13 C65 O14 Mn1 -7.7(2) . . . . ? C66 C65 O14 Mn1 171.21(17) . . . . ? C73 C72 O15 C69 -10.7(4) . . . . ? C77 C72 O15 C69 171.5(3) . . . . ? C70 C69 O15 C72 100.7(3) . . . . ? C68 C69 O15 C72 -80.6(3) . . . . ? C83 C78 O16 C76 1.3(5) . . . . ? C79 C78 O16 C76 -177.9(3) . . . . ? C77 C76 O16 C78 -100.0(3) . . . . ? C75 C76 O16 C78 84.7(4) . . . . ? O18 C84 O17 Mn4 2.9(7) . . . . ? C81 C84 O17 Mn4 -176.7(4) . . . . ? O17 C84 O18 Mn3 -6.0(3) . . . . ? C81 C84 O18 Mn3 173.59(16) . . . . ? C64 O12 Mn1 O8 -24.3(3) . . . . ? C64 O12 Mn1 O14 95.7(2) . . . . ? C64 O12 Mn1 N2 -178.6(2) . . . . ? C64 O12 Mn1 N1 -106.0(2) . . . . ? C64 O12 Mn1 O13 43.3(2) . . . . ? C57 O8 Mn1 O12 -14.7(2) . . . . ? C57 O8 Mn1 O14 -136.56(15) . . . . ? C57 O8 Mn1 N2 137.41(15) . . . . ? C57 O8 Mn1 N1 66.80(15) . . . . ? C57 O8 Mn1 O13 -82.30(15) . . . . ? C65 O14 Mn1 O12 -68.79(15) . . . . ? C65 O14 Mn1 O8 81.88(14) . . . . ? C65 O14 Mn1 N2 -165.15(15) . . . . ? C65 O14 Mn1 N1 178.97(17) . . . . ? C65 O14 Mn1 O13 4.12(12) . . . . ? C10 N2 Mn1 O12 -93.1(2) . . . . ? C11 N2 Mn1 O12 88.20(16) . . . . ? C10 N2 Mn1 O8 102.4(2) . . . . ? C11 N2 Mn1 O8 -76.38(17) . . . . ? C10 N2 Mn1 O14 8.9(2) . . . . ? C11 N2 Mn1 O14 -169.88(16) . . . . ? C10 N2 Mn1 N1 -177.7(2) . . . . ? C11 N2 Mn1 N1 3.56(15) . . . . ? C10 N2 Mn1 O13 -4.5(2) . . . . ? C11 N2 Mn1 O13 176.72(13) . . . . ? C1 N1 Mn1 O12 78.5(2) . . . . ? C12 N1 Mn1 O12 -102.99(17) . . . . ? C1 N1 Mn1 O8 -67.6(2) . . . . ? C12 N1 Mn1 O8 110.91(17) . . . . ? C1 N1 Mn1 O14 -166.3(2) . . . . ? C12 N1 Mn1 O14 12.2(3) . . . . ? C1 N1 Mn1 N2 177.2(2) . . . . ? C12 N1 Mn1 N2 -4.30(16) . . . . ? C1 N1 Mn1 O13 5.8(3) . . . . ? C12 N1 Mn1 O13 -175.77(14) . . . . ? C65 O13 Mn1 O12 106.00(13) . . . . ? Mn2 O13 Mn1 O12 -72.28(7) . . . . ? C65 O13 Mn1 O8 -105.62(13) . . . . ? Mn2 O13 Mn1 O8 76.10(7) . . . . ? C65 O13 Mn1 O14 -4.09(12) . . . . ? Mn2 O13 Mn1 O14 177.63(10) . . . . ? C65 O13 Mn1 N2 12.15(17) . . . . ? Mn2 O13 Mn1 N2 -166.14(8) . . . . ? C65 O13 Mn1 N1 179.77(14) . . . . ? Mn2 O13 Mn1 N1 1.49(16) . . . . ? C64 O11 Mn2 O11 108(100) . . . 2_566 ? C64 O11 Mn2 O13 -10.0(3) . . . . ? C64 O11 Mn2 O13 170.0(3) . . . 2_566 ? C64 O11 Mn2 O7 -100.2(3) . . . 2_566 ? C64 O11 Mn2 O7 79.8(3) . . . . ? C65 O13 Mn2 O11 72.8(13) . . . 2_566 ? Mn1 O13 Mn2 O11 -120.86(8) . . . 2_566 ? C65 O13 Mn2 O11 -107.2(13) . . . . ? Mn1 O13 Mn2 O11 59.14(8) . . . . ? C65 O13 Mn2 O13 -160(100) . . . 2_566 ? Mn1 O13 Mn2 O13 6(100) . . . 2_566 ? C65 O13 Mn2 O7 -19.1(13) . . . 2_566 ? Mn1 O13 Mn2 O7 147.19(7) . . . 2_566 ? C65 O13 Mn2 O7 160.9(13) . . . . ? Mn1 O13 Mn2 O7 -32.81(7) . . . . ? C57 O7 Mn2 O11 52.2(2) . . . 2_566 ? C57 O7 Mn2 O11 -127.8(2) . . . . ? C57 O7 Mn2 O13 -38.6(2) . . . . ? C57 O7 Mn2 O13 141.4(2) . . . 2_566 ? C57 O7 Mn2 O7 -138(100) . . . 2_566 ? C84 O18 Mn3 O6 -71.56(17) . . . . ? C84 O18 Mn3 O1 32.86(19) . . . . ? C84 O18 Mn3 N3 176.88(17) . . . . ? C84 O18 Mn3 N4 -176.2(2) . . . . ? C84 O18 Mn3 O2 89.96(17) . . . . ? C44 O6 Mn3 O18 90.2(2) . . . . ? C44 O6 Mn3 O1 -23.8(2) . . . . ? C44 O6 Mn3 N3 -178.9(2) . . . . ? C44 O6 Mn3 N4 -107.4(2) . . . . ? C44 O6 Mn3 O2 -36.3(3) . . . . ? C25 O1 Mn3 O18 97.13(15) . . . . ? Mn4 O1 Mn3 O18 -49.92(9) . . . . ? C25 O1 Mn3 O6 -163.72(14) . . . . ? Mn4 O1 Mn3 O6 49.23(9) . . . . ? C25 O1 Mn3 N3 -20.08(19) . . . . ? Mn4 O1 Mn3 N3 -167.13(8) . . . . ? C25 O1 Mn3 N4 -74.08(15) . . . . ? Mn4 O1 Mn3 N4 138.87(8) . . . . ? C25 O1 Mn3 O2 10.47(14) . . . . ? Mn4 O1 Mn3 O2 -136.58(10) . . . . ? C22 N3 Mn3 O18 -4.1(2) . . . . ? C23 N3 Mn3 O18 179.11(17) . . . . ? C22 N3 Mn3 O6 -97.9(2) . . . . ? C23 N3 Mn3 O6 85.29(17) . . . . ? C22 N3 Mn3 O1 120.72(19) . . . . ? C23 N3 Mn3 O1 -56.1(2) . . . . ? C22 N3 Mn3 N4 178.2(2) . . . . ? C23 N3 Mn3 N4 1.38(16) . . . . ? C22 N3 Mn3 O2 95.8(2) . . . . ? C23 N3 Mn3 O2 -81.05(17) . . . . ? C13 N4 Mn3 O18 172.9(2) . . . . ? C24 N4 Mn3 O18 -8.8(4) . . . . ? C13 N4 Mn3 O6 67.8(2) . . . . ? C24 N4 Mn3 O6 -113.85(18) . . . . ? C13 N4 Mn3 O1 -33.9(2) . . . . ? C24 N4 Mn3 O1 144.40(18) . . . . ? C13 N4 Mn3 N3 -179.8(2) . . . . ? C24 N4 Mn3 N3 -1.52(16) . . . . ? C13 N4 Mn3 O2 -90.4(2) . . . . ? C24 N4 Mn3 O2 87.94(17) . . . . ? C25 O2 Mn3 O18 -121.67(16) . . . . ? C25 O2 Mn3 O6 3.8(3) . . . . ? C25 O2 Mn3 O1 -10.96(14) . . . . ? C25 O2 Mn3 N3 149.40(16) . . . . ? C25 O2 Mn3 N4 76.71(16) . . . . ? C84 O17 Mn4 O17 -78(100) . . . 2_757 ? C84 O17 Mn4 O5 66.3(5) . . . . ? C84 O17 Mn4 O5 -113.7(5) . . . 2_757 ? C84 O17 Mn4 O1 -24.0(5) . . . . ? C84 O17 Mn4 O1 156.0(5) . . . 2_757 ? C44 O5 Mn4 O17 151.5(3) . . . 2_757 ? C44 O5 Mn4 O17 -28.5(3) . . . . ? C44 O5 Mn4 O5 -21(100) . . . 2_757 ? C44 O5 Mn4 O1 59.3(3) . . . . ? C44 O5 Mn4 O1 -120.7(3) . . . 2_757 ? C25 O1 Mn4 O17 101.0(3) . . . 2_757 ? Mn3 O1 Mn4 O17 -145.33(8) . . . 2_757 ? C25 O1 Mn4 O17 -79.0(3) . . . . ? Mn3 O1 Mn4 O17 34.67(8) . . . . ? C25 O1 Mn4 O5 -167.4(3) . . . . ? Mn3 O1 Mn4 O5 -53.68(8) . . . . ? C25 O1 Mn4 O5 12.6(3) . . . 2_757 ? Mn3 O1 Mn4 O5 126.32(8) . . . 2_757 ? C25 O1 Mn4 O1 28(100) . . . 2_757 ? Mn3 O1 Mn4 O1 142(100) . . . 2_757 ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.898 _refine_diff_density_min -0.538 _refine_diff_density_rms 0.103 _database_code_depnum_ccdc_archive 'CCDC 933680'