# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Hoffman, David' _publ_contact_author_email HOFFMAN@UH.EDU _publ_section_title ; Synthesis of zinc trisubstituted hydrazido complexes and ortho-metalation of 4-(dimethylamino)pyridine ; _publ_author_name D.Hoffman # Attachment '- Hoffman_Dalton.CIF' data_k1025[ZnEt(N(SiMe3)NMe2)]2 _database_code_depnum_ccdc_archive 'CCDC 784270' #TrackingRef '- Hoffman_Dalton.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_sum 'C14 H40 N4 Si2 Zn2' _chemical_formula_weight 451.42 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.0256(6) _cell_length_b 9.0317(7) _cell_length_c 9.4274(7) _cell_angle_alpha 109.784(1) _cell_angle_beta 107.771(1) _cell_angle_gamma 97.884(1) _cell_volume 589.87(8) _cell_formula_units_Z 1 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 2493 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 25.08 _exptl_crystal_description 'Prismatic block' _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.30 _exptl_crystal_density_diffrn 1.271 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 240 _exptl_absorpt_coefficient_mu 2.137 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.8543 _exptl_absorpt_correction_T_max 0.9611 _exptl_absorpt_process_details ? _publ_section_experimental ; All measurements were made with a Siemens SMART platform diffractometer equipped with a 4K CCD APEX II detector. A hemisphere of data (1271 frames at 6 cm detector distance) was collected using a narrow-frame algorithm with scan widths of 0.30\% in omega and an exposure time of 30 s/frame. The data were integrated using the Bruker-Nonius SAINT program, with the intensities corrected for Lorentz factor, polarization, air absorption, and absorption due to variation in the path length through the detector faceplate. A psi scan absorption correction was applied based on the entire data set. Redundant reflections were averaged. Final cell constants were refined using 2493 reflections having I>10\s(I), and these, along with other information pertinent to data collection and refinement, are listed in Table 1. The Laue symmetry was determined to be -1, and the space group was shown to be either P1 or P-1. The ethyl group is disordered over two slightly different positions. ; _publ_section_figure_captions ; Fig. 1 -- View of the molecule showing the atom numbering scheme. Thermal ellipsoids are 40% equiprobability envelopes, with hydrogens omitted. Only one orientation of the disordered ethyl group is shown at each site. Fig. 2 -- Packing of the molecules in the unit cell. ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX II CCD' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 4K _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 3012 _diffrn_reflns_av_R_equivalents 0.0160 _diffrn_reflns_av_sigmaI/netI 0.0145 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.48 _diffrn_reflns_theta_max 25.08 _reflns_number_total 2069 _reflns_number_gt 1889 _reflns_threshold_expression >4sigma(I) _computing_data_collection 'APEX2 v1.0-27 (Bruker-Nonius, 2005)' _computing_cell_refinement 'SAINT v7.12A (Bruker-Nonius, 2004)' _computing_data_reduction 'SAINT v7.12A (Bruker-Nonius, 2004)' _computing_structure_solution 'SHELXS v5.10 (G.M. Sheldrick, 1997)' _computing_structure_refinement 'SHELXL v5.10 (G.M. Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 4sigma(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^)+(0.0319P)^2^+0.3750P] 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 SHELXL _refine_ls_extinction_coef 0.030(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2069 _refine_ls_number_parameters 99 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0247 _refine_ls_R_factor_gt 0.0227 _refine_ls_wR_factor_ref 0.0604 _refine_ls_wR_factor_gt 0.0587 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.036 _refine_ls_shift/su_mean 0.003 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 Zn Zn 0.36598(3) 0.58783(3) 0.51395(3) 0.02859(12) Uani 1 1 d . . . Si Si 0.25497(8) 0.27030(7) 0.18454(7) 0.03119(16) Uani 1 1 d . . . N1 N 0.4258(2) 0.4509(2) 0.3228(2) 0.0277(4) Uani 1 1 d . . . N2 N 0.4569(3) 0.5177(2) 0.2047(2) 0.0334(4) Uani 1 1 d . . . C1 C 0.1748(8) 0.6994(6) 0.5273(8) 0.0396(18) Uiso 0.55 1 d PD A 1 H1A H 0.0701 0.6462 0.4237 0.048 Uiso 0.55 1 calc PR A 1 H1B H 0.1353 0.6882 0.6126 0.048 Uiso 0.55 1 calc PR A 1 C2 C 0.2385(8) 0.8857(6) 0.5652(7) 0.0541(12) Uiso 0.55 1 d PD A 1 H2A H 0.1392 0.9349 0.5706 0.081 Uiso 0.55 1 calc PR A 1 H2B H 0.2750 0.8977 0.4797 0.081 Uiso 0.55 1 calc PR A 1 H2C H 0.3405 0.9396 0.6687 0.081 Uiso 0.55 1 calc PR A 1 C1' C 0.2033(10) 0.7271(9) 0.5679(10) 0.038(2) Uiso 0.45 1 d P A 2 H1A' H 0.0882 0.6548 0.5478 0.046 Uiso 0.45 1 calc PR A 2 H1B' H 0.2583 0.7955 0.6850 0.046 Uiso 0.45 1 calc PR A 2 C2' C 0.1595(10) 0.8384(9) 0.4801(9) 0.0614(17) Uiso 0.45 1 d PD A 2 H2A' H 0.0793 0.8982 0.5184 0.092 Uiso 0.45 1 calc PR A 2 H2B' H 0.1002 0.7733 0.3640 0.092 Uiso 0.45 1 calc PR A 2 H2C' H 0.2709 0.9148 0.5019 0.092 Uiso 0.45 1 calc PR A 2 C3 C 0.3320(4) 0.1344(3) 0.0340(3) 0.0499(6) Uani 1 1 d . A . H3A H 0.3602 0.1893 -0.0316 0.075 Uiso 1 1 calc R . . H3B H 0.2362 0.0341 -0.0359 0.075 Uiso 1 1 calc R . . H3C H 0.4395 0.1091 0.0910 0.075 Uiso 1 1 calc R . . C4 C 0.2016(4) 0.1590(3) 0.3069(3) 0.0445(6) Uani 1 1 d . A . H4A H 0.1613 0.2275 0.3867 0.067 Uiso 1 1 calc R . . H4B H 0.3096 0.1330 0.3622 0.067 Uiso 1 1 calc R . . H4C H 0.1062 0.0589 0.2353 0.067 Uiso 1 1 calc R . . C5 C 0.0444(3) 0.3146(3) 0.0755(3) 0.0514(7) Uani 1 1 d . A . H5A H 0.0043 0.3850 0.1542 0.077 Uiso 1 1 calc R . . H5B H -0.0500 0.2131 0.0072 0.077 Uiso 1 1 calc R . . H5C H 0.0694 0.3688 0.0083 0.077 Uiso 1 1 calc R . . C6 C 0.4132(4) 0.6736(3) 0.2360(3) 0.0451(6) Uani 1 1 d . A . H6A H 0.4337 0.7161 0.1593 0.068 Uiso 1 1 calc R . . H6B H 0.4899 0.7501 0.3461 0.068 Uiso 1 1 calc R . . H6C H 0.2867 0.6587 0.2236 0.068 Uiso 1 1 calc R . . C7 C 0.6434(3) 0.5338(4) 0.2162(3) 0.0463(6) Uani 1 1 d . A . H7A H 0.6622 0.5768 0.1392 0.069 Uiso 1 1 calc R . . H7B H 0.6679 0.4275 0.1912 0.069 Uiso 1 1 calc R . . H7C H 0.7250 0.6077 0.3257 0.069 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 Zn 0.02913(16) 0.03125(16) 0.03004(16) 0.01458(11) 0.01289(11) 0.01245(10) Si 0.0319(3) 0.0324(3) 0.0273(3) 0.0111(3) 0.0098(2) 0.0080(2) N1 0.0302(9) 0.0332(9) 0.0245(8) 0.0156(7) 0.0116(7) 0.0096(7) N2 0.0383(10) 0.0407(11) 0.0263(9) 0.0191(8) 0.0133(8) 0.0089(8) C3 0.0585(16) 0.0438(14) 0.0416(14) 0.0065(12) 0.0247(13) 0.0103(12) C4 0.0483(14) 0.0409(13) 0.0415(13) 0.0175(11) 0.0160(11) 0.0034(11) C5 0.0387(14) 0.0511(16) 0.0504(15) 0.0187(13) 0.0017(12) 0.0093(12) C6 0.0583(16) 0.0445(14) 0.0412(13) 0.0270(12) 0.0188(12) 0.0149(12) C7 0.0434(14) 0.0643(17) 0.0387(13) 0.0269(12) 0.0207(11) 0.0099(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn C1 1.960(6) . ? Zn C1' 1.992(7) . ? Zn N1 2.0469(17) . ? Zn N1 2.0592(17) 2_666 ? Si N1 1.7596(18) . ? Si C3 1.862(3) . ? Si C5 1.865(3) . ? Si C4 1.869(2) . ? N1 N2 1.499(2) . ? N1 Zn 2.0592(17) 2_666 ? N2 C7 1.451(3) . ? N2 C6 1.453(3) . ? C1 C2 1.570(6) . ? C1' C2' 1.517(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Zn C1' 10.3(3) . . ? C1 Zn N1 132.9(2) . . ? C1' Zn N1 142.1(2) . . ? C1 Zn N1 135.6(2) . 2_666 ? C1' Zn N1 126.3(2) . 2_666 ? N1 Zn N1 91.48(6) . 2_666 ? N1 Si C3 112.22(11) . . ? N1 Si C5 111.58(11) . . ? C3 Si C5 109.65(13) . . ? N1 Si C4 106.70(10) . . ? C3 Si C4 107.78(12) . . ? C5 Si C4 108.74(13) . . ? N2 N1 Si 99.19(12) . . ? N2 N1 Zn 121.12(12) . . ? Si N1 Zn 114.24(9) . . ? N2 N1 Zn 121.85(12) . 2_666 ? Si N1 Zn 112.96(9) . 2_666 ? Zn N1 Zn 88.52(6) . 2_666 ? C7 N2 C6 111.1(2) . . ? C7 N2 N1 110.06(17) . . ? C6 N2 N1 109.92(16) . . ? C2 C1 Zn 112.8(4) . . ? C2' C1' Zn 118.6(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3 Si N1 N2 59.37(16) . . . . ? C5 Si N1 N2 -64.14(16) . . . . ? C4 Si N1 N2 177.21(13) . . . . ? C3 Si N1 Zn -170.31(11) . . . . ? C5 Si N1 Zn 66.18(13) . . . . ? C4 Si N1 Zn -52.47(13) . . . . ? C3 Si N1 Zn -71.10(13) . . . 2_666 ? C5 Si N1 Zn 165.38(11) . . . 2_666 ? C4 Si N1 Zn 46.73(13) . . . 2_666 ? C1 Zn N1 N2 55.9(3) . . . . ? C1' Zn N1 N2 48.8(4) . . . . ? N1 Zn N1 N2 -126.95(16) 2_666 . . . ? C1 Zn N1 Si -62.6(2) . . . . ? C1' Zn N1 Si -69.7(4) . . . . ? N1 Zn N1 Si 114.60(11) 2_666 . . . ? C1 Zn N1 Zn -177.2(2) . . . 2_666 ? C1' Zn N1 Zn 175.7(3) . . . 2_666 ? N1 Zn N1 Zn 0.0 2_666 . . 2_666 ? Si N1 N2 C7 -119.44(17) . . . . ? Zn N1 N2 C7 114.86(18) . . . . ? Zn N1 N2 C7 5.0(2) 2_666 . . . ? Si N1 N2 C6 117.83(16) . . . . ? Zn N1 N2 C6 -7.9(2) . . . . ? Zn N1 N2 C6 -117.72(17) 2_666 . . . ? C1' Zn C1 C2 58.4(16) . . . . ? N1 Zn C1 C2 -96.6(4) . . . . ? N1 Zn C1 C2 87.4(4) 2_666 . . . ? C1 Zn C1' C2' -68.2(16) . . . . ? N1 Zn C1' C2' -37.9(8) . . . . ? N1 Zn C1' C2' 136.8(5) 2_666 . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.08 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.454 _refine_diff_density_min -0.313 _refine_diff_density_rms 0.049 #===END data_k1012Zn3Et4(NEtNMe2)2 _database_code_depnum_ccdc_archive 'CCDC 784271' #TrackingRef '- Hoffman_Dalton.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_sum 'C16 H42 N4 Zn3' _chemical_formula_weight 486.65 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4(3)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+3/4' 'y+1/2, -x+1/2, z+1/4' '-x+1/2, y+1/2, -z+3/4' 'x+1/2, -y+1/2, -z+1/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 9.2341(4) _cell_length_b 9.2341(4) _cell_length_c 27.1810(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2317.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 5214 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 24.19 _exptl_crystal_description 'Irregular block' _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_diffrn 1.395 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1024 _exptl_absorpt_coefficient_mu 3.084 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.7380 _exptl_absorpt_correction_T_max 0.9599 _exptl_absorpt_process_details ? _publ_section_experimental ; All measurements were made with a Siemens SMART platform diffractometer equipped with a 4K CCD APEX II detector. A hemisphere of data (1271 frames at 6 cm detector distance) was collected using a narrow-frame algorithm with scan widths of 0.30\% in omega and an exposure time of 30 s/frame. The data were integrated using the Bruker-Nonius SAINT program, with the intensities corrected for Lorentz factor, polarization, air absorption, and absorption due to variation in the path length through the detector faceplate. A psi scan absorption correction was applied based on the entire data set. Redundant reflections were averaged. Final cell constants were refined using 5214 reflections having I>10\s(I), and these, along with other information pertinent to data collection and refinement, are listed in Table 1. The Laue symmetry was determined to be 4/mmm, and from the systematic absences noted the space group was shown to be either P4(1)2(1)2 or P4(3)2(1)2. The molecule is massively disordered about a two-fold axis, such that the actual connectivity is ambiguous. The model finally chosen represents the best guess at the actual atomic arrangement, however the interatomic distances and angles listed should not be considered very reliable. There are obviously several different orientations of the molecule present, and possibly different connectivities as well, which fit into roughly the same space in the crystal lattice. ; _publ_section_figure_captions ; Fig. 1 -- View of the molecule showing the atom numbering scheme, with hydrogens omitted. Due to the severe disorder involved only the Zn atoms were refined anisotropically. Only one possible orientation of the molecule is shown. Fig. 2 -- Packing of the molecules in the unit cell. ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius APEX II CCD' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 4K _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 11040 _diffrn_reflns_av_R_equivalents 0.0268 _diffrn_reflns_av_sigmaI/netI 0.0155 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 24.19 _reflns_number_total 1888 _reflns_number_gt 1551 _reflns_threshold_expression >4sigma(I) _computing_data_collection 'APEX2 v1.0-27 (Bruker-Nonius, 2005)' _computing_cell_refinement 'SAINT v7.12A (Bruker-Nonius, 2004)' _computing_data_reduction 'SAINT v7.12A (Bruker-Nonius, 2004)' _computing_structure_solution 'SHELXS v5.10 (G.M. Sheldrick, 1997)' _computing_structure_refinement 'SHELXL v5.10 (G.M. Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 4sigma(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^)+(0.0321P)^2^+0.5878P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(3) _refine_ls_number_reflns 1863 _refine_ls_number_parameters 113 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0281 _refine_ls_R_factor_gt 0.0233 _refine_ls_wR_factor_ref 0.0599 _refine_ls_wR_factor_gt 0.0571 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.193 _refine_ls_shift/su_mean 0.026 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 0.3972(4) 0.3031(3) 0.54440(16) 0.0487(9) Uani 0.50 1 d P A -1 Zn2 Zn 0.3051(5) 0.3942(5) 0.45331(19) 0.0770(16) Uani 0.50 1 d P A -1 Zn3 Zn 0.5738(5) 0.5714(6) 0.5035(6) 0.0838(12) Uani 0.50 1 d P A -1 N1 N 0.3837(9) 0.5290(9) 0.5436(3) 0.052(3) Uiso 0.50 1 d P A -1 N2 N 0.2648(10) 0.5562(10) 0.5072(3) 0.061(3) Uiso 0.50 1 d P A -1 N3 N 0.5347(11) 0.4125(10) 0.4597(4) 0.066(4) Uiso 0.50 1 d P A -1 N4 N 0.5817(10) 0.2879(10) 0.4893(3) 0.064(3) Uiso 0.50 1 d P A -1 C1 C 0.4036(10) 0.2042(10) 0.6089(3) 0.067(3) Uiso 0.50 1 d P A -1 H1A H 0.4940 0.2320 0.6253 0.081 Uiso 0.50 1 calc PR A -1 H1B H 0.3238 0.2418 0.6290 0.081 Uiso 0.50 1 calc PR A -1 C2 C 0.3947(11) 0.0493(11) 0.6092(4) 0.080(3) Uiso 0.50 1 d P A -1 H2A H 0.3990 0.0146 0.6429 0.120 Uiso 0.50 1 calc PR A -1 H2B H 0.4751 0.0094 0.5907 0.120 Uiso 0.50 1 calc PR A -1 H2C H 0.3041 0.0192 0.5943 0.120 Uiso 0.50 1 calc PR A -1 C3 C 0.1845(10) 0.4508(10) 0.3942(3) 0.063(2) Uiso 0.50 1 d P A -1 H3A H 0.2041 0.5527 0.3865 0.075 Uiso 0.50 1 calc PR A -1 H3B H 0.2168 0.3932 0.3659 0.075 Uiso 0.50 1 calc PR A -1 C4 C 0.0183(11) 0.4314(11) 0.3997(4) 0.076(3) Uiso 0.50 1 d P A -1 H4A H -0.0293 0.4610 0.3695 0.114 Uiso 0.50 1 calc PR A -1 H4B H -0.0163 0.4906 0.4267 0.114 Uiso 0.50 1 calc PR A -1 H4C H -0.0035 0.3305 0.4063 0.114 Uiso 0.50 1 calc PR A -1 C5 C 0.7230(15) 0.7222(15) 0.5162(4) 0.128(4) Uiso 0.50 1 d P A -1 H5A H 0.6743 0.8034 0.5324 0.154 Uiso 0.50 1 calc PR A -1 H5B H 0.7916 0.6818 0.5400 0.154 Uiso 0.50 1 calc PR A -1 C6 C 0.8051(13) 0.7801(13) 0.4770(4) 0.116(3) Uiso 0.50 1 d P A -1 H6A H 0.8698 0.8542 0.4895 0.175 Uiso 0.50 1 calc PR A -1 H6B H 0.7405 0.8222 0.4527 0.175 Uiso 0.50 1 calc PR A -1 H6C H 0.8615 0.7035 0.4618 0.175 Uiso 0.50 1 calc PR A -1 C7 C 0.2543(6) 0.1829(7) 0.4916(2) 0.0570(16) Uiso 0.50 1 d P A -1 H7A H 0.2555 0.1608 0.4577 0.068 Uiso 0.50 1 d P B -1 H7B H 0.3109 0.1099 0.5082 0.068 Uiso 0.50 1 d P C -1 C8 C 0.1012(8) 0.1618(8) 0.5096(3) 0.076(2) Uiso 0.50 1 d P A -1 H8A H 0.0731 0.0615 0.5052 0.091 Uiso 0.50 1 calc PR A -1 H8B H 0.0364 0.2238 0.4911 0.091 Uiso 0.50 1 calc PR A -1 H8C H 0.0958 0.1866 0.5443 0.091 Uiso 0.50 1 calc PR A -1 C9 C 0.3620(11) 0.6038(12) 0.5922(3) 0.075(3) Uiso 0.50 1 d P A -1 H9A H 0.2800 0.5604 0.6097 0.090 Uiso 0.50 1 calc PR A -1 H9B H 0.3412 0.7067 0.5869 0.090 Uiso 0.50 1 calc PR A -1 C10 C 0.4986(11) 0.5870(11) 0.6221(3) 0.086(3) Uiso 0.50 1 d P A -1 H10A H 0.4866 0.6348 0.6536 0.130 Uiso 0.50 1 calc PR A -1 H10B H 0.5791 0.6304 0.6046 0.130 Uiso 0.50 1 calc PR A -1 H10C H 0.5180 0.4849 0.6274 0.130 Uiso 0.50 1 calc PR A -1 C11 C 0.1238(9) 0.5282(11) 0.5335(3) 0.075(2) Uiso 0.50 1 d P A -1 H11A H 0.1103 0.6002 0.5591 0.113 Uiso 0.50 1 calc PR A -1 H11B H 0.1259 0.4324 0.5481 0.113 Uiso 0.50 1 calc PR A -1 H11C H 0.0445 0.5340 0.5102 0.113 Uiso 0.50 1 calc PR A -1 C12 C 0.2639(12) 0.7036(12) 0.4888(4) 0.085(3) Uiso 0.50 1 d P A -1 H12A H 0.2680 0.7707 0.5162 0.128 Uiso 0.50 1 calc PR A -1 H12B H 0.1759 0.7202 0.4701 0.128 Uiso 0.50 1 calc PR A -1 H12C H 0.3473 0.7185 0.4676 0.128 Uiso 0.50 1 calc PR A -1 C13 C 0.6104(12) 0.4127(11) 0.4116(4) 0.078(3) Uiso 0.50 1 d P A -1 H13A H 0.5769 0.3316 0.3913 0.094 Uiso 0.50 1 calc PR A -1 H13B H 0.7151 0.4029 0.4165 0.094 Uiso 0.50 1 calc PR A -1 C14 C 0.5762(11) 0.5557(10) 0.3865(4) 0.087(3) Uiso 0.50 1 d P A -1 H14A H 0.6250 0.5596 0.3549 0.130 Uiso 0.50 1 calc PR A -1 H14B H 0.6094 0.6351 0.4069 0.130 Uiso 0.50 1 calc PR A -1 H14C H 0.4725 0.5638 0.3815 0.130 Uiso 0.50 1 calc PR A -1 C15 C 0.5921(11) 0.1447(10) 0.4660(3) 0.089(3) Uiso 0.50 1 d P A -1 H15A H 0.6772 0.1415 0.4451 0.133 Uiso 0.50 1 calc PR A -1 H15B H 0.5063 0.1273 0.4463 0.133 Uiso 0.50 1 calc PR A -1 H15C H 0.5997 0.0709 0.4913 0.133 Uiso 0.50 1 calc PR A -1 C16 C 0.7259(12) 0.3147(12) 0.5122(4) 0.087(3) Uiso 0.50 1 d P A -1 H16A H 0.8002 0.3125 0.4870 0.130 Uiso 0.50 1 calc PR A -1 H16B H 0.7455 0.2401 0.5365 0.130 Uiso 0.50 1 calc PR A -1 H16C H 0.7258 0.4087 0.5281 0.130 Uiso 0.50 1 calc PR A -1 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 0.0601(18) 0.0426(14) 0.0433(15) 0.0099(11) -0.0098(12) -0.0120(13) Zn2 0.081(2) 0.098(3) 0.051(2) 0.0087(17) 0.0019(15) -0.006(2) Zn3 0.058(2) 0.091(3) 0.103(3) 0.0085(11) -0.0078(10) -0.0268(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 C1 1.978(9) . ? Zn1 N1 2.090(9) . ? Zn1 C7 2.243(7) . ? Zn1 N4 2.273(11) . ? Zn2 C3 2.025(9) . ? Zn2 N2 2.127(11) . ? Zn2 N3 2.134(11) . ? Zn2 C7 2.260(8) . ? Zn3 N3 1.923(14) . ? Zn3 C5 1.989(12) . ? Zn3 N1 2.103(13) . ? N1 N2 1.498(12) . ? N1 C9 1.505(13) . ? N2 C12 1.451(14) . ? N2 C11 1.507(12) . ? N3 N4 1.469(13) . ? N3 C13 1.484(14) . ? N4 C15 1.469(13) . ? N4 C16 1.491(14) . ? C1 C2 1.433(13) . ? C3 C4 1.553(13) . ? C5 C6 1.413(13) . ? C7 C8 1.508(8) . ? C9 C10 1.509(13) . ? C13 C14 1.520(14) . ? 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 C1 Zn1 N1 118.2(4) . . ? C1 Zn1 C7 110.9(3) . . ? N1 Zn1 C7 116.9(3) . . ? C1 Zn1 N4 122.2(4) . . ? N1 Zn1 N4 95.7(4) . . ? C7 Zn1 N4 89.4(3) . . ? C3 Zn2 N2 105.6(4) . . ? C3 Zn2 N3 126.2(4) . . ? N2 Zn2 N3 93.5(4) . . ? C3 Zn2 C7 118.3(3) . . ? N2 Zn2 C7 104.7(3) . . ? N3 Zn2 C7 103.7(4) . . ? N3 Zn3 C5 140.5(7) . . ? N3 Zn3 N1 91.22(18) . . ? C5 Zn3 N1 128.3(8) . . ? N2 N1 C9 113.9(8) . . ? N2 N1 Zn1 102.6(6) . . ? C9 N1 Zn1 117.1(7) . . ? N2 N1 Zn3 103.8(7) . . ? C9 N1 Zn3 118.7(7) . . ? Zn1 N1 Zn3 98.1(4) . . ? C12 N2 N1 112.9(8) . . ? C12 N2 C11 108.7(8) . . ? N1 N2 C11 107.0(7) . . ? C12 N2 Zn2 115.0(7) . . ? N1 N2 Zn2 102.0(6) . . ? C11 N2 Zn2 110.9(6) . . ? N4 N3 C13 110.1(8) . . ? N4 N3 Zn3 101.8(8) . . ? C13 N3 Zn3 117.1(8) . . ? N4 N3 Zn2 106.0(7) . . ? C13 N3 Zn2 113.4(7) . . ? Zn3 N3 Zn2 107.3(5) . . ? N3 N4 C15 119.3(8) . . ? N3 N4 C16 111.3(9) . . ? C15 N4 C16 105.7(9) . . ? N3 N4 Zn1 95.2(6) . . ? C15 N4 Zn1 112.9(7) . . ? C16 N4 Zn1 112.6(6) . . ? C2 C1 Zn1 117.7(7) . . ? C4 C3 Zn2 115.9(6) . . ? C6 C5 Zn3 120.4(8) . . ? C8 C7 Zn1 114.0(4) . . ? C8 C7 Zn2 117.1(4) . . ? Zn1 C7 Zn2 75.3(2) . . ? N1 C9 C10 108.4(8) . . ? N3 C13 C14 107.4(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 C1 Zn1 N1 N2 -132.5(6) . . . . ? C7 Zn1 N1 N2 3.9(7) . . . . ? N4 Zn1 N1 N2 96.1(6) . . . . ? C1 Zn1 N1 C9 -6.9(9) . . . . ? C7 Zn1 N1 C9 129.4(7) . . . . ? N4 Zn1 N1 C9 -138.4(7) . . . . ? C1 Zn1 N1 Zn3 121.3(6) . . . . ? C7 Zn1 N1 Zn3 -102.3(5) . . . . ? N4 Zn1 N1 Zn3 -10.1(6) . . . . ? N3 Zn3 N1 N2 -64.2(8) . . . . ? C5 Zn3 N1 N2 117.9(10) . . . . ? N3 Zn3 N1 C9 168.2(6) . . . . ? C5 Zn3 N1 C9 -9.7(13) . . . . ? N3 Zn3 N1 Zn1 41.0(7) . . . . ? C5 Zn3 N1 Zn1 -136.9(9) . . . . ? C9 N1 N2 C12 70.2(11) . . . . ? Zn1 N1 N2 C12 -162.2(7) . . . . ? Zn3 N1 N2 C12 -60.4(9) . . . . ? C9 N1 N2 C11 -49.3(11) . . . . ? Zn1 N1 N2 C11 78.4(7) . . . . ? Zn3 N1 N2 C11 -179.8(6) . . . . ? C9 N1 N2 Zn2 -165.8(7) . . . . ? Zn1 N1 N2 Zn2 -38.2(6) . . . . ? Zn3 N1 N2 Zn2 63.6(5) . . . . ? C3 Zn2 N2 C12 -43.4(8) . . . . ? N3 Zn2 N2 C12 85.8(8) . . . . ? C7 Zn2 N2 C12 -169.1(7) . . . . ? C3 Zn2 N2 N1 -166.0(6) . . . . ? N3 Zn2 N2 N1 -36.8(6) . . . . ? C7 Zn2 N2 N1 68.4(6) . . . . ? C3 Zn2 N2 C11 80.4(7) . . . . ? N3 Zn2 N2 C11 -150.4(7) . . . . ? C7 Zn2 N2 C11 -45.3(7) . . . . ? C5 Zn3 N3 N4 98.4(14) . . . . ? N1 Zn3 N3 N4 -79.0(8) . . . . ? C5 Zn3 N3 C13 -21.7(17) . . . . ? N1 Zn3 N3 C13 160.9(6) . . . . ? C5 Zn3 N3 Zn2 -150.4(11) . . . . ? N1 Zn3 N3 Zn2 32.1(8) . . . . ? C3 Zn2 N3 N4 -145.1(7) . . . . ? N2 Zn2 N3 N4 102.6(7) . . . . ? C7 Zn2 N3 N4 -3.5(7) . . . . ? C3 Zn2 N3 C13 -24.2(10) . . . . ? N2 Zn2 N3 C13 -136.5(7) . . . . ? C7 Zn2 N3 C13 117.4(7) . . . . ? C3 Zn2 N3 Zn3 106.7(7) . . . . ? N2 Zn2 N3 Zn3 -5.6(7) . . . . ? C7 Zn2 N3 Zn3 -111.6(6) . . . . ? C13 N3 N4 C15 -45.2(13) . . . . ? Zn3 N3 N4 C15 -170.1(8) . . . . ? Zn2 N3 N4 C15 77.8(10) . . . . ? C13 N3 N4 C16 78.3(10) . . . . ? Zn3 N3 N4 C16 -46.6(9) . . . . ? Zn2 N3 N4 C16 -158.7(7) . . . . ? C13 N3 N4 Zn1 -165.0(7) . . . . ? Zn3 N3 N4 Zn1 70.1(6) . . . . ? Zn2 N3 N4 Zn1 -42.0(6) . . . . ? C1 Zn1 N4 N3 -163.4(6) . . . . ? N1 Zn1 N4 N3 -34.7(6) . . . . ? C7 Zn1 N4 N3 82.2(6) . . . . ? C1 Zn1 N4 C15 71.8(8) . . . . ? N1 Zn1 N4 C15 -159.6(7) . . . . ? C7 Zn1 N4 C15 -42.6(7) . . . . ? C1 Zn1 N4 C16 -47.7(9) . . . . ? N1 Zn1 N4 C16 80.9(8) . . . . ? C7 Zn1 N4 C16 -162.2(7) . . . . ? N1 Zn1 C1 C2 172.4(7) . . . . ? C7 Zn1 C1 C2 33.6(9) . . . . ? N4 Zn1 C1 C2 -69.5(9) . . . . ? N2 Zn2 C3 C4 -71.4(8) . . . . ? N3 Zn2 C3 C4 -177.9(7) . . . . ? C7 Zn2 C3 C4 45.3(8) . . . . ? N3 Zn3 C5 C6 31.7(18) . . . . ? N1 Zn3 C5 C6 -151.6(10) . . . . ? C1 Zn1 C7 C8 57.0(6) . . . . ? N1 Zn1 C7 C8 -82.4(6) . . . . ? N4 Zn1 C7 C8 -178.5(5) . . . . ? C1 Zn1 C7 Zn2 170.5(3) . . . . ? N1 Zn1 C7 Zn2 31.1(4) . . . . ? N4 Zn1 C7 Zn2 -65.0(3) . . . . ? C3 Zn2 C7 C8 -55.8(6) . . . . ? N2 Zn2 C7 C8 61.4(6) . . . . ? N3 Zn2 C7 C8 158.8(5) . . . . ? C3 Zn2 C7 Zn1 -165.6(4) . . . . ? N2 Zn2 C7 Zn1 -48.4(3) . . . . ? N3 Zn2 C7 Zn1 49.1(4) . . . . ? N2 N1 C9 C10 -171.3(8) . . . . ? Zn1 N1 C9 C10 69.0(10) . . . . ? Zn3 N1 C9 C10 -48.5(10) . . . . ? N4 N3 C13 C14 -170.9(8) . . . . ? Zn3 N3 C13 C14 -55.4(11) . . . . ? Zn2 N3 C13 C14 70.5(9) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.19 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.180 _refine_diff_density_min -0.195 _refine_diff_density_rms 0.039 #===END data_k1047[ZnEt2(iPrNNMe2)2(dmap)2 _database_code_depnum_ccdc_archive 'CCDC 784272' #TrackingRef '- Hoffman_Dalton.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H54 N8 Zn3, C4 H10 O' _chemical_formula_sum 'C32 H64 N8 O Zn3' _chemical_formula_weight 773.02 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 I2/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' _cell_length_a 24.5861(11) _cell_length_b 12.0656(4) _cell_length_c 27.1240(10) _cell_angle_alpha 90.00 _cell_angle_beta 106.337(1) _cell_angle_gamma 90.00 _cell_volume 7721.3(5) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 8163 _cell_measurement_theta_min 1.73 _cell_measurement_theta_max 25.04 _exptl_crystal_description 'Diamond plate' _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 1.330 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3280 _exptl_absorpt_coefficient_mu 1.883 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.6676 _exptl_absorpt_correction_T_max 0.9678 _exptl_absorpt_process_details ? _publ_section_experimental ; All measurements were made with a Siemens SMART platform diffractometer equipped with a 4K CCD APEX II detector. A hemisphere of data (1271 frames at 6 cm detector distance) was collected using a narrow-frame algorithm with scan widths of 0.30\% in omega and an exposure time of 25 s/frame. The data were integrated using the Bruker-Nonius SAINT program, with the intensities corrected for Lorentz factor, polarization, air absorption, and absorption due to variation in the path length through the detector faceplate. A psi scan absorption correction was applied based on the entire data set. Redundant reflections were averaged. Final cell constants were refined using 8163 reflections having I>10\s(I), and these, along with other information pertinent to data collection and refinement, are listed in Table 1. The Laue symmetry was determined to be 2/m, and from the systematic absences noted the space group was shown to be either Ia or I2/a. The asymmetric unit consists of one molcule in a general postion, and two half-molecules of diethyl ether solvent disordered about a two fold axis. Both of the ethyl groups attached to Zn were found to be massively disordered, and were refined using distant constraints with occupancy factors estimated based on comparison of isotropic displacement parameters. ; _publ_section_figure_captions ; Fig. 1 -- View of the molecule showing the atom numbering scheme for the core atoms. Thermal ellipsoids are 40% equiprobability envelopes, with hydrogens omitted. Only one orientation of each disordered group is shown. Fig. 2 -- Isotropic view of the molecule. Fig. 3 -- Packing of the molecules in the unit cell. ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius APEX II CCD' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 4K _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 19494 _diffrn_reflns_av_R_equivalents 0.0220 _diffrn_reflns_av_sigmaI/netI 0.0166 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 25.04 _reflns_number_total 7176 _reflns_number_gt 5374 _reflns_threshold_expression >4sigma(I) _computing_data_collection 'APEX2 v1.0-27 (Bruker-Nonius, 2005)' _computing_cell_refinement 'SAINT v7.12A (Bruker-Nonius, 2004)' _computing_data_reduction 'SAINT v7.12A (Bruker-Nonius, 2004)' _computing_structure_solution 'SHELXS v5.10 (G.M. Sheldrick, 1997)' _computing_structure_refinement 'SHELXL v5.10 (G.M. Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 4sigma(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^)+(0.0385P)^2^+7.6584P] 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_number_reflns 6824 _refine_ls_number_parameters 416 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.0309 _refine_ls_R_factor_gt 0.0244 _refine_ls_wR_factor_ref 0.0687 _refine_ls_wR_factor_gt 0.0657 _refine_ls_goodness_of_fit_ref 0.966 _refine_ls_restrained_S_all 0.973 _refine_ls_shift/su_max 0.101 _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 Zn1 Zn 0.579058(11) 0.38718(2) 0.708913(9) 0.03696(8) Uani 1 1 d D . . Zn2 Zn 0.548035(10) 0.20290(2) 0.589865(9) 0.03470(8) Uani 1 1 d D . . Zn3 Zn 0.631286(10) 0.39034(2) 0.621543(8) 0.03118(7) Uani 1 1 d . . . N1 N 0.55005(7) 0.43507(14) 0.63353(6) 0.0323(4) Uani 1 1 d . A . N2 N 0.50686(7) 0.35852(15) 0.60238(7) 0.0357(4) Uani 1 1 d . A . N3 N 0.65497(7) 0.47523(15) 0.72159(6) 0.0372(4) Uani 1 1 d . A . N4 N 0.81193(9) 0.63135(18) 0.74553(8) 0.0519(5) Uani 1 1 d . . . N5 N 0.62349(7) 0.22070(14) 0.64653(6) 0.0326(4) Uani 1 1 d . A . N6 N 0.61518(8) 0.22516(15) 0.69857(6) 0.0363(4) Uani 1 1 d . A . N7 N 0.58113(7) 0.26623(14) 0.53298(6) 0.0337(4) Uani 1 1 d . A . N8 N 0.64851(9) 0.40354(18) 0.42137(7) 0.0507(5) Uani 1 1 d . . . C1 C 0.5534(3) 0.3956(7) 0.7726(2) 0.0466(17) Uiso 0.45 1 d PD A 1 H1A H 0.5744 0.3401 0.7970 0.056 Uiso 0.45 1 calc PR A 1 H1B H 0.5637 0.4687 0.7883 0.056 Uiso 0.45 1 calc PR A 1 C2 C 0.4903(3) 0.3776(6) 0.7651(3) 0.0634(17) Uiso 0.45 1 d PD A 1 H2A H 0.4836 0.3636 0.7981 0.095 Uiso 0.45 1 calc PR A 1 H2B H 0.4775 0.3145 0.7427 0.095 Uiso 0.45 1 calc PR A 1 H2C H 0.4695 0.4433 0.7498 0.095 Uiso 0.45 1 calc PR A 1 C1' C 0.5329(4) 0.3695(8) 0.7601(3) 0.040(2) Uiso 0.30 1 d PD A 2 H1'A H 0.4937 0.3911 0.7429 0.048 Uiso 0.30 1 calc PR A 2 H1'B H 0.5324 0.2906 0.7687 0.048 Uiso 0.30 1 calc PR A 2 C2' C 0.5524(5) 0.4345(9) 0.8104(4) 0.070(3) Uiso 0.30 1 d PD A 2 H2'A H 0.5271 0.4192 0.8314 0.105 Uiso 0.30 1 calc PR A 2 H2'B H 0.5518 0.5132 0.8030 0.105 Uiso 0.30 1 calc PR A 2 H2'C H 0.5906 0.4123 0.8288 0.105 Uiso 0.30 1 calc PR A 2 C1" C 0.5531(5) 0.3517(9) 0.7720(4) 0.033(2) Uiso 0.25 1 d PD A 3 H1"A H 0.5332 0.2805 0.7662 0.039 Uiso 0.25 1 calc PR A 3 H1"B H 0.5868 0.3424 0.8013 0.039 Uiso 0.25 1 calc PR A 3 C2" C 0.5147(5) 0.4362(9) 0.7866(5) 0.062(3) Uiso 0.25 1 d PD A 3 H2"A H 0.5047 0.4108 0.8168 0.094 Uiso 0.25 1 calc PR A 3 H2"B H 0.4806 0.4453 0.7584 0.094 Uiso 0.25 1 calc PR A 3 H2"C H 0.5344 0.5067 0.7939 0.094 Uiso 0.25 1 calc PR A 3 C3 C 0.53073(9) 0.55356(18) 0.62738(8) 0.0390(5) Uani 1 1 d . . . H3 H 0.4914 0.5535 0.6046 0.047 Uiso 1 1 calc R A . C4 C 0.56600(11) 0.6228(2) 0.60098(10) 0.0512(6) Uani 1 1 d . A . H4A H 0.5660 0.5882 0.5687 0.077 Uiso 1 1 calc R . . H4B H 0.6046 0.6277 0.6229 0.077 Uiso 1 1 calc R . . H4C H 0.5499 0.6966 0.5945 0.077 Uiso 1 1 calc R . . C5 C 0.52911(12) 0.6089(2) 0.67743(10) 0.0537(7) Uani 1 1 d . A . H5A H 0.5048 0.5667 0.6931 0.081 Uiso 1 1 calc R . . H5B H 0.5144 0.6836 0.6704 0.081 Uiso 1 1 calc R . . H5C H 0.5671 0.6118 0.7007 0.081 Uiso 1 1 calc R . . C6 C 0.48111(10) 0.3974(2) 0.54895(9) 0.0448(6) Uani 1 1 d . . . H6A H 0.4547 0.4571 0.5491 0.067 Uiso 1 1 calc R B . H6B H 0.4611 0.3365 0.5282 0.067 Uiso 1 1 calc R . . H6C H 0.5107 0.4241 0.5347 0.067 Uiso 1 1 calc R . . C7 C 0.46050(10) 0.3399(2) 0.62621(10) 0.0496(6) Uani 1 1 d . . . H7A H 0.4420 0.4099 0.6287 0.074 Uiso 1 1 calc R B . H7B H 0.4759 0.3090 0.6603 0.074 Uiso 1 1 calc R . . H7C H 0.4332 0.2887 0.6053 0.074 Uiso 1 1 calc R . . C8 C 0.68042(9) 0.47567(17) 0.68249(7) 0.0331(5) Uani 1 1 d . A . C9 C 0.73243(9) 0.52751(17) 0.69086(8) 0.0351(5) Uani 1 1 d . . . H9 H 0.7498 0.5278 0.6641 0.042 Uiso 1 1 calc R A . C10 C 0.76067(9) 0.57999(18) 0.73755(8) 0.0380(5) Uani 1 1 d . A . C11 C 0.73312(10) 0.57607(19) 0.77630(8) 0.0418(5) Uani 1 1 d . . . H11 H 0.7497 0.6084 0.8086 0.050 Uiso 1 1 calc R A . C12 C 0.68165(10) 0.52428(19) 0.76631(8) 0.0424(5) Uani 1 1 d . A . H12 H 0.6637 0.5229 0.7926 0.051 Uiso 1 1 calc R . . C13 C 0.83756(12) 0.6451(3) 0.70411(11) 0.0654(8) Uani 1 1 d . . . H13A H 0.8095 0.6727 0.6739 0.098 Uiso 1 1 calc R . . H13B H 0.8518 0.5742 0.6962 0.098 Uiso 1 1 calc R . . H13C H 0.8686 0.6974 0.7143 0.098 Uiso 1 1 calc R . . C14 C 0.84078(11) 0.6810(2) 0.79496(10) 0.0567(7) Uani 1 1 d . . . H14A H 0.8418 0.6283 0.8222 0.085 Uiso 1 1 calc R . . H14B H 0.8206 0.7471 0.8001 0.085 Uiso 1 1 calc R . . H14C H 0.8792 0.7006 0.7955 0.085 Uiso 1 1 calc R . . C15 C 0.4871(2) 0.0887(4) 0.5694(3) 0.0443(17) Uiso 0.60 1 d PD B 1 H15A H 0.5057 0.0181 0.5666 0.053 Uiso 0.60 1 calc PR B 1 H15B H 0.4705 0.0811 0.5981 0.053 Uiso 0.60 1 calc PR B 1 C16 C 0.43924(19) 0.1010(4) 0.52189(18) 0.0576(12) Uiso 0.60 1 d PD B 1 H16A H 0.4146 0.0368 0.5180 0.086 Uiso 0.60 1 calc PR B 1 H16B H 0.4540 0.1068 0.4924 0.086 Uiso 0.60 1 calc PR B 1 H16C H 0.4179 0.1673 0.5244 0.086 Uiso 0.60 1 calc PR B 1 C15' C 0.4959(7) 0.0727(13) 0.5619(6) 0.031(4) Uiso 0.20 1 d PD B 2 H15C H 0.4678 0.0963 0.5303 0.037 Uiso 0.20 1 calc PR B 2 H15D H 0.5185 0.0134 0.5526 0.037 Uiso 0.20 1 calc PR B 2 C16' C 0.4644(8) 0.0246(15) 0.5989(6) 0.089 Uiso 0.20 1 d PD B 2 H16D H 0.4437 -0.0413 0.5838 0.133 Uiso 0.20 1 calc PR B 2 H16E H 0.4380 0.0794 0.6048 0.133 Uiso 0.20 1 calc PR B 2 H16F H 0.4915 0.0057 0.6313 0.133 Uiso 0.20 1 calc PR B 2 C15" C 0.5001(6) 0.0641(10) 0.5780(8) 0.041(4) Uiso 0.20 1 d PD B 3 H15E H 0.5172 0.0108 0.5595 0.050 Uiso 0.20 1 calc PR B 3 H15F H 0.5021 0.0315 0.6116 0.050 Uiso 0.20 1 calc PR B 3 C16" C 0.4379(6) 0.0776(18) 0.5485(8) 0.095 Uiso 0.20 1 d PD B 3 H16G H 0.4186 0.0071 0.5472 0.143 Uiso 0.20 1 calc PR B 3 H16H H 0.4349 0.1023 0.5138 0.143 Uiso 0.20 1 calc PR B 3 H16I H 0.4205 0.1320 0.5656 0.143 Uiso 0.20 1 calc PR B 3 C17 C 0.66757(10) 0.13705(19) 0.64328(9) 0.0413(5) Uani 1 1 d . . . H17 H 0.6779 0.0959 0.6762 0.050 Uiso 1 1 calc R A . C18 C 0.72145(10) 0.1922(2) 0.63824(10) 0.0542(7) Uani 1 1 d . A . H18A H 0.7351 0.2446 0.6661 0.081 Uiso 1 1 calc R . . H18B H 0.7134 0.2310 0.6056 0.081 Uiso 1 1 calc R . . H18C H 0.7502 0.1363 0.6398 0.081 Uiso 1 1 calc R . . C19 C 0.64687(12) 0.0516(2) 0.60057(10) 0.0573(7) Uani 1 1 d . A . H19A H 0.6139 0.0135 0.6052 0.086 Uiso 1 1 calc R . . H19B H 0.6768 -0.0017 0.6018 0.086 Uiso 1 1 calc R . . H19C H 0.6368 0.0887 0.5675 0.086 Uiso 1 1 calc R . . C20 C 0.66890(10) 0.2256(2) 0.74090(8) 0.0450(6) Uani 1 1 d . . . H20A H 0.6848 0.1515 0.7454 0.067 Uiso 1 1 calc R A . H20B H 0.6613 0.2496 0.7725 0.067 Uiso 1 1 calc R . . H20C H 0.6957 0.2760 0.7324 0.067 Uiso 1 1 calc R . . C21 C 0.58078(11) 0.1315(2) 0.70727(9) 0.0508(6) Uani 1 1 d . . . H21A H 0.5999 0.0625 0.7045 0.076 Uiso 1 1 calc R A . H21B H 0.5441 0.1330 0.6818 0.076 Uiso 1 1 calc R . . H21C H 0.5756 0.1373 0.7413 0.076 Uiso 1 1 calc R . . C22 C 0.61843(8) 0.35286(17) 0.54644(7) 0.0313(4) Uani 1 1 d . A . C23 C 0.64056(9) 0.39788(18) 0.50906(8) 0.0341(5) Uani 1 1 d . . . H23 H 0.6661 0.4574 0.5181 0.041 Uiso 1 1 calc R A . C24 C 0.62642(9) 0.35834(18) 0.45817(8) 0.0358(5) Uani 1 1 d . A . C25 C 0.58786(9) 0.27027(18) 0.44654(8) 0.0381(5) Uani 1 1 d . . . H25 H 0.5764 0.2405 0.4132 0.046 Uiso 1 1 calc R A . C26 C 0.56709(9) 0.22820(18) 0.48443(8) 0.0378(5) Uani 1 1 d . A . H26 H 0.5414 0.1689 0.4760 0.045 Uiso 1 1 calc R . . C27 C 0.68939(13) 0.4913(3) 0.43365(10) 0.0791(10) Uani 1 1 d . . . H27A H 0.6779 0.5454 0.4552 0.119 Uiso 1 1 calc R . . H27B H 0.6918 0.5267 0.4022 0.119 Uiso 1 1 calc R . . H27C H 0.7261 0.4612 0.4518 0.119 Uiso 1 1 calc R . . C28 C 0.63900(12) 0.3515(3) 0.37162(9) 0.0590(7) Uani 1 1 d . . . H28A H 0.5991 0.3561 0.3531 0.088 Uiso 1 1 calc R . . H28B H 0.6504 0.2743 0.3762 0.088 Uiso 1 1 calc R . . H28C H 0.6612 0.3892 0.3523 0.088 Uiso 1 1 calc R . . O1 O 0.7560(3) 0.7217(3) 0.5077(2) 0.0762(12) Uiso 0.50 1 d PD C -1 C29 C 0.8011(3) 0.7761(7) 0.4928(3) 0.100(2) Uiso 0.50 1 d PD C -1 H29A H 0.8350 0.7776 0.5223 0.120 Uiso 0.50 1 calc PR C -1 H29B H 0.7901 0.8529 0.4833 0.120 Uiso 0.50 1 calc PR C -1 C30 C 0.8150(5) 0.7214(11) 0.4496(4) 0.098(4) Uiso 0.50 1 d PD C -1 H30A H 0.8455 0.7613 0.4412 0.147 Uiso 0.50 1 calc PR C -1 H30B H 0.7818 0.7211 0.4200 0.147 Uiso 0.50 1 calc PR C -1 H30C H 0.8268 0.6458 0.4589 0.147 Uiso 0.50 1 calc PR C -1 C31 C 0.7416(3) 0.7798(6) 0.5494(3) 0.097(2) Uiso 0.50 1 d PD C -1 H31A H 0.7278 0.8544 0.5382 0.116 Uiso 0.50 1 calc PR C -1 H31B H 0.7753 0.7867 0.5789 0.116 Uiso 0.50 1 calc PR C -1 C32 C 0.6977(4) 0.7176(10) 0.5643(4) 0.085(3) Uiso 0.50 1 d PD C -1 H32A H 0.6884 0.7553 0.5925 0.128 Uiso 0.50 1 calc PR C -1 H32B H 0.7115 0.6436 0.5751 0.128 Uiso 0.50 1 calc PR C -1 H32C H 0.6641 0.7126 0.5353 0.128 Uiso 0.50 1 calc PR C -1 O2 O 0.71883(17) 1.0140(3) 0.45659(16) 0.0735(11) Uiso 0.50 1 d PD D -1 C33 C 0.6674(3) 1.0016(5) 0.4168(2) 0.0734(17) Uiso 0.50 1 d PD D -1 H33A H 0.6658 1.0558 0.3895 0.088 Uiso 0.50 1 calc PR D -1 H33B H 0.6350 1.0145 0.4303 0.088 Uiso 0.50 1 calc PR D -1 C34 C 0.6650(3) 0.8879(5) 0.3959(3) 0.0786(18) Uiso 0.50 1 d PD D -1 H34A H 0.6302 0.8785 0.3685 0.118 Uiso 0.50 1 calc PR D -1 H34B H 0.6660 0.8348 0.4230 0.118 Uiso 0.50 1 calc PR D -1 H34C H 0.6972 0.8757 0.3826 0.118 Uiso 0.50 1 calc PR D -1 C35 C 0.7280(3) 1.1212(6) 0.4858(3) 0.068(2) Uiso 0.50 1 d PD D -1 H35A H 0.6973 1.1337 0.5017 0.082 Uiso 0.50 1 calc PR D -1 H35B H 0.7286 1.1831 0.4626 0.082 Uiso 0.50 1 calc PR D -1 C36 C 0.7840(4) 1.1134(7) 0.5267(3) 0.079(3) Uiso 0.50 1 d PD D -1 H36A H 0.7911 1.1820 0.5461 0.118 Uiso 0.50 1 calc PR D -1 H36B H 0.8141 1.1008 0.5106 0.118 Uiso 0.50 1 calc PR D -1 H36C H 0.7828 1.0523 0.5496 0.118 Uiso 0.50 1 calc PR D -1 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 0.03772(15) 0.04633(16) 0.02854(14) 0.00218(11) 0.01214(11) 0.00444(11) Zn2 0.03535(14) 0.03590(14) 0.03198(14) 0.00161(10) 0.00806(10) -0.00268(11) Zn3 0.03123(13) 0.03775(14) 0.02317(13) -0.00092(10) 0.00538(10) -0.00015(10) N1 0.0294(9) 0.0346(9) 0.0309(9) -0.0008(7) 0.0050(7) 0.0024(8) N2 0.0290(9) 0.0405(10) 0.0352(10) 0.0003(8) 0.0052(7) 0.0000(8) N3 0.0381(10) 0.0446(11) 0.0267(9) -0.0014(8) 0.0053(8) 0.0038(8) N4 0.0492(12) 0.0550(13) 0.0465(12) -0.0138(10) 0.0053(10) -0.0134(10) N5 0.0351(9) 0.0368(10) 0.0253(9) 0.0046(7) 0.0077(7) 0.0064(8) N6 0.0409(10) 0.0419(10) 0.0260(9) 0.0059(8) 0.0090(8) 0.0048(8) N7 0.0349(9) 0.0369(10) 0.0279(9) 0.0010(7) 0.0064(7) -0.0008(8) N8 0.0615(13) 0.0644(14) 0.0303(10) -0.0037(9) 0.0195(9) -0.0149(11) C3 0.0348(11) 0.0379(12) 0.0412(12) 0.0024(10) 0.0053(10) 0.0058(10) C4 0.0564(15) 0.0414(14) 0.0529(15) 0.0109(11) 0.0106(12) 0.0058(12) C5 0.0626(17) 0.0432(14) 0.0558(16) -0.0038(12) 0.0175(13) 0.0127(12) C6 0.0391(13) 0.0486(14) 0.0382(13) -0.0013(10) -0.0029(10) 0.0087(11) C7 0.0373(13) 0.0560(15) 0.0571(16) -0.0059(12) 0.0160(11) -0.0046(11) C8 0.0342(11) 0.0349(11) 0.0275(10) 0.0000(9) 0.0042(9) 0.0066(9) C9 0.0386(12) 0.0340(11) 0.0306(11) -0.0019(9) 0.0064(9) 0.0042(9) C10 0.0403(12) 0.0314(11) 0.0374(12) -0.0016(9) 0.0028(10) 0.0050(10) C11 0.0487(14) 0.0417(13) 0.0283(11) -0.0064(10) -0.0002(10) 0.0042(11) C12 0.0490(14) 0.0490(14) 0.0276(11) -0.0028(10) 0.0084(10) 0.0079(11) C13 0.0550(17) 0.0733(19) 0.0675(19) -0.0160(15) 0.0166(14) -0.0236(15) C14 0.0541(15) 0.0488(15) 0.0541(16) -0.0107(12) -0.0062(12) -0.0068(12) C17 0.0443(13) 0.0437(13) 0.0345(12) 0.0052(10) 0.0088(10) 0.0133(11) C18 0.0420(14) 0.0627(17) 0.0589(16) 0.0047(13) 0.0156(12) 0.0143(12) C19 0.0663(17) 0.0496(15) 0.0520(15) -0.0055(12) 0.0102(13) 0.0210(13) C20 0.0496(14) 0.0524(14) 0.0286(11) 0.0067(10) 0.0041(10) 0.0129(11) C21 0.0632(17) 0.0499(15) 0.0430(14) 0.0115(11) 0.0207(12) -0.0014(12) C22 0.0307(11) 0.0343(11) 0.0270(10) 0.0006(9) 0.0049(8) 0.0042(9) C23 0.0322(11) 0.0394(12) 0.0294(11) 0.0001(9) 0.0067(9) 0.0008(9) C24 0.0364(12) 0.0433(12) 0.0277(11) 0.0027(9) 0.0092(9) 0.0073(10) C25 0.0426(12) 0.0429(13) 0.0269(11) -0.0053(9) 0.0066(9) 0.0035(10) C26 0.0399(12) 0.0371(12) 0.0332(12) -0.0020(9) 0.0049(9) -0.0009(10) C27 0.074(2) 0.125(3) 0.0425(15) -0.0011(17) 0.0220(14) -0.044(2) C28 0.0701(18) 0.0775(19) 0.0355(14) -0.0030(13) 0.0250(13) -0.0013(15) _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 C1 2.001(5) . ? Zn1 C1" 2.033(7) . ? Zn1 C1' 2.038(7) . ? Zn1 N1 2.0502(17) . ? Zn1 N3 2.0902(19) . ? Zn1 N6 2.1974(18) . ? Zn2 C15 1.995(4) . ? Zn2 C15" 2.021(9) . ? Zn2 C15' 2.035(8) . ? Zn2 N5 2.0607(17) . ? Zn2 N7 2.0816(17) . ? Zn2 N2 2.2042(18) . ? Zn3 C22 2.023(2) . ? Zn3 C8 2.032(2) . ? Zn3 N1 2.1798(17) . ? Zn3 N5 2.1814(17) . ? N1 N2 1.480(2) . ? N1 C3 1.501(3) . ? N2 C7 1.477(3) . ? N2 C6 1.485(3) . ? N3 C12 1.343(3) . ? N3 C8 1.375(3) . ? N4 C10 1.366(3) . ? N4 C13 1.444(3) . ? N4 C14 1.457(3) . ? N5 N6 1.483(2) . ? N5 C17 1.502(3) . ? N6 C21 1.469(3) . ? N6 C20 1.487(3) . ? N7 C26 1.345(3) . ? N7 C22 1.371(3) . ? N8 C24 1.376(3) . ? N8 C27 1.434(3) . ? N8 C28 1.446(3) . ? C1 C2 1.524(7) . ? C1' C2' 1.529(9) . ? C1" C2" 1.515(9) . ? C3 C4 1.521(3) . ? C3 C5 1.524(3) . ? C8 C9 1.384(3) . ? C9 C10 1.411(3) . ? C10 C11 1.402(3) . ? C11 C12 1.368(3) . ? C15 C16 1.488(7) . ? C15' C16' 1.543(11) . ? C15" C16" 1.524(11) . ? C17 C18 1.523(3) . ? C17 C19 1.527(3) . ? C22 C23 1.389(3) . ? C23 C24 1.408(3) . ? C24 C25 1.400(3) . ? C25 C26 1.367(3) . ? O1 C29 1.442(7) . ? O1 C31 1.456(7) . ? C29 C30 1.466(8) . ? C31 C32 1.462(8) . ? O2 C33 1.421(6) . ? O2 C35 1.500(7) . ? C33 C34 1.479(6) . ? C35 C36 1.508(7) . ? 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 C1 Zn1 C1" 15.1(3) . . ? C1 Zn1 C1' 17.4(3) . . ? C1" Zn1 C1' 15.6(3) . . ? C1 Zn1 N1 137.8(2) . . ? C1" Zn1 N1 142.7(3) . . ? C1' Zn1 N1 127.2(3) . . ? C1 Zn1 N3 108.4(2) . . ? C1" Zn1 N3 116.5(4) . . ? C1' Zn1 N3 125.7(3) . . ? N1 Zn1 N3 93.72(7) . . ? C1 Zn1 N6 113.1(2) . . ? C1" Zn1 N6 98.9(3) . . ? C1' Zn1 N6 108.5(3) . . ? N1 Zn1 N6 99.39(6) . . ? N3 Zn1 N6 95.68(7) . . ? C15 Zn2 C15" 12.9(4) . . ? C15 Zn2 C15' 11.0(4) . . ? C15" Zn2 C15' 12.3(5) . . ? C15 Zn2 N5 136.7(2) . . ? C15" Zn2 N5 124.6(4) . . ? C15' Zn2 N5 134.4(6) . . ? C15 Zn2 N7 117.8(2) . . ? C15" Zn2 N7 121.2(6) . . ? C15' Zn2 N7 110.1(4) . . ? N5 Zn2 N7 93.27(7) . . ? C15 Zn2 N2 106.84(18) . . ? C15" Zn2 N2 117.3(5) . . ? C15' Zn2 N2 116.6(6) . . ? N5 Zn2 N2 98.77(7) . . ? N7 Zn2 N2 95.37(7) . . ? C22 Zn3 C8 145.22(8) . . ? C22 Zn3 N1 108.38(7) . . ? C8 Zn3 N1 96.50(7) . . ? C22 Zn3 N5 95.78(7) . . ? C8 Zn3 N5 107.86(7) . . ? N1 Zn3 N5 91.24(6) . . ? N2 N1 C3 112.17(15) . . ? N2 N1 Zn1 112.71(12) . . ? C3 N1 Zn1 112.93(13) . . ? N2 N1 Zn3 107.50(11) . . ? C3 N1 Zn3 119.59(13) . . ? Zn1 N1 Zn3 90.15(6) . . ? C7 N2 N1 111.29(17) . . ? C7 N2 C6 107.78(17) . . ? N1 N2 C6 113.60(16) . . ? C7 N2 Zn2 112.48(14) . . ? N1 N2 Zn2 109.44(11) . . ? C6 N2 Zn2 101.96(13) . . ? C12 N3 C8 118.83(19) . . ? C12 N3 Zn1 124.00(15) . . ? C8 N3 Zn1 117.02(13) . . ? C10 N4 C13 120.9(2) . . ? C10 N4 C14 121.4(2) . . ? C13 N4 C14 117.6(2) . . ? N6 N5 C17 112.05(15) . . ? N6 N5 Zn2 112.18(12) . . ? C17 N5 Zn2 113.54(13) . . ? N6 N5 Zn3 108.02(11) . . ? C17 N5 Zn3 118.97(13) . . ? Zn2 N5 Zn3 90.31(6) . . ? C21 N6 N5 111.39(16) . . ? C21 N6 C20 107.77(18) . . ? N5 N6 C20 113.87(16) . . ? C21 N6 Zn1 113.07(14) . . ? N5 N6 Zn1 108.82(11) . . ? C20 N6 Zn1 101.62(13) . . ? C26 N7 C22 119.30(18) . . ? C26 N7 Zn2 123.68(14) . . ? C22 N7 Zn2 117.01(13) . . ? C24 N8 C27 121.2(2) . . ? C24 N8 C28 120.8(2) . . ? C27 N8 C28 117.2(2) . . ? C2 C1 Zn1 115.7(5) . . ? C2' C1' Zn1 117.3(7) . . ? C2" C1" Zn1 116.4(7) . . ? N1 C3 C4 111.78(18) . . ? N1 C3 C5 113.91(18) . . ? C4 C3 C5 109.9(2) . . ? N3 C8 C9 118.39(18) . . ? N3 C8 Zn3 109.28(14) . . ? C9 C8 Zn3 132.31(16) . . ? C8 C9 C10 123.3(2) . . ? N4 C10 C11 121.0(2) . . ? N4 C10 C9 123.0(2) . . ? C11 C10 C9 116.0(2) . . ? C12 C11 C10 118.8(2) . . ? N3 C12 C11 124.7(2) . . ? C16 C15 Zn2 121.4(4) . . ? C16' C15' Zn2 115.2(10) . . ? C16" C15" Zn2 116.7(11) . . ? N5 C17 C18 111.83(19) . . ? N5 C17 C19 113.97(18) . . ? C18 C17 C19 109.9(2) . . ? N7 C22 C23 118.29(18) . . ? N7 C22 Zn3 110.01(14) . . ? C23 C22 Zn3 131.70(16) . . ? C22 C23 C24 122.9(2) . . ? N8 C24 C25 121.18(19) . . ? N8 C24 C23 122.5(2) . . ? C25 C24 C23 116.30(19) . . ? C26 C25 C24 119.0(2) . . ? N7 C26 C25 124.2(2) . . ? C29 O1 C31 111.9(5) . . ? O1 C29 C30 113.0(8) . . ? O1 C31 C32 109.1(7) . . ? C33 O2 C35 117.5(5) . . ? O2 C33 C34 108.7(5) . . ? O2 C35 C36 107.8(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Zn1 N1 N2 -79.7(3) . . . . ? C1" Zn1 N1 N2 -57.3(5) . . . . ? C1' Zn1 N1 N2 -60.9(4) . . . . ? N3 Zn1 N1 N2 157.46(12) . . . . ? N6 Zn1 N1 N2 61.07(13) . . . . ? C1 Zn1 N1 C3 48.7(4) . . . . ? C1" Zn1 N1 C3 71.1(5) . . . . ? C1' Zn1 N1 C3 67.5(4) . . . . ? N3 Zn1 N1 C3 -74.14(14) . . . . ? N6 Zn1 N1 C3 -170.53(13) . . . . ? C1 Zn1 N1 Zn3 171.2(3) . . . . ? C1" Zn1 N1 Zn3 -166.4(5) . . . . ? C1' Zn1 N1 Zn3 -169.9(3) . . . . ? N3 Zn1 N1 Zn3 48.36(7) . . . . ? N6 Zn1 N1 Zn3 -48.03(7) . . . . ? C22 Zn3 N1 N2 40.02(13) . . . . ? C8 Zn3 N1 N2 -164.62(12) . . . . ? N5 Zn3 N1 N2 -56.49(12) . . . . ? C22 Zn3 N1 C3 -89.33(15) . . . . ? C8 Zn3 N1 C3 66.03(15) . . . . ? N5 Zn3 N1 C3 174.16(15) . . . . ? C22 Zn3 N1 Zn1 153.95(7) . . . . ? C8 Zn3 N1 Zn1 -50.69(8) . . . . ? N5 Zn3 N1 Zn1 57.44(7) . . . . ? C3 N1 N2 C7 -76.4(2) . . . . ? Zn1 N1 N2 C7 52.40(19) . . . . ? Zn3 N1 N2 C7 150.15(15) . . . . ? C3 N1 N2 C6 45.5(2) . . . . ? Zn1 N1 N2 C6 174.25(14) . . . . ? Zn3 N1 N2 C6 -87.99(16) . . . . ? C3 N1 N2 Zn2 158.66(13) . . . . ? Zn1 N1 N2 Zn2 -72.54(12) . . . . ? Zn3 N1 N2 Zn2 25.21(13) . . . . ? C15 Zn2 N2 C7 37.1(3) . . . . ? C15" Zn2 N2 C7 29.0(6) . . . . ? C15' Zn2 N2 C7 42.7(5) . . . . ? N5 Zn2 N2 C7 -107.51(15) . . . . ? N7 Zn2 N2 C7 158.33(15) . . . . ? C15 Zn2 N2 N1 161.4(3) . . . . ? C15" Zn2 N2 N1 153.2(6) . . . . ? C15' Zn2 N2 N1 166.9(5) . . . . ? N5 Zn2 N2 N1 16.73(13) . . . . ? N7 Zn2 N2 N1 -77.43(12) . . . . ? C15 Zn2 N2 C6 -78.0(3) . . . . ? C15" Zn2 N2 C6 -86.2(6) . . . . ? C15' Zn2 N2 C6 -72.5(5) . . . . ? N5 Zn2 N2 C6 137.31(13) . . . . ? N7 Zn2 N2 C6 43.15(14) . . . . ? C1 Zn1 N3 C12 2.3(3) . . . . ? C1" Zn1 N3 C12 -11.4(4) . . . . ? C1' Zn1 N3 C12 3.3(4) . . . . ? N1 Zn1 N3 C12 145.86(18) . . . . ? N6 Zn1 N3 C12 -114.31(18) . . . . ? C1 Zn1 N3 C8 177.8(3) . . . . ? C1" Zn1 N3 C8 164.0(3) . . . . ? C1' Zn1 N3 C8 178.7(4) . . . . ? N1 Zn1 N3 C8 -38.70(15) . . . . ? N6 Zn1 N3 C8 61.13(15) . . . . ? C15 Zn2 N5 N6 -64.0(3) . . . . ? C15" Zn2 N5 N6 -69.8(8) . . . . ? C15' Zn2 N5 N6 -79.4(6) . . . . ? N7 Zn2 N5 N6 158.12(12) . . . . ? N2 Zn2 N5 N6 62.17(13) . . . . ? C15 Zn2 N5 C17 64.3(3) . . . . ? C15" Zn2 N5 C17 58.5(8) . . . . ? C15' Zn2 N5 C17 48.9(6) . . . . ? N7 Zn2 N5 C17 -73.58(14) . . . . ? N2 Zn2 N5 C17 -169.53(14) . . . . ? C15 Zn2 N5 Zn3 -173.7(3) . . . . ? C15" Zn2 N5 Zn3 -179.5(8) . . . . ? C15' Zn2 N5 Zn3 170.9(5) . . . . ? N7 Zn2 N5 Zn3 48.47(7) . . . . ? N2 Zn2 N5 Zn3 -47.48(7) . . . . ? C22 Zn3 N5 N6 -164.36(12) . . . . ? C8 Zn3 N5 N6 41.49(13) . . . . ? N1 Zn3 N5 N6 -55.75(12) . . . . ? C22 Zn3 N5 C17 66.48(15) . . . . ? C8 Zn3 N5 C17 -87.66(15) . . . . ? N1 Zn3 N5 C17 175.09(15) . . . . ? C22 Zn3 N5 Zn2 -50.87(8) . . . . ? C8 Zn3 N5 Zn2 154.99(7) . . . . ? N1 Zn3 N5 Zn2 57.75(6) . . . . ? C17 N5 N6 C21 -77.5(2) . . . . ? Zn2 N5 N6 C21 51.56(19) . . . . ? Zn3 N5 N6 C21 149.53(15) . . . . ? C17 N5 N6 C20 44.6(2) . . . . ? Zn2 N5 N6 C20 173.69(14) . . . . ? Zn3 N5 N6 C20 -88.34(17) . . . . ? C17 N5 N6 Zn1 157.17(13) . . . . ? Zn2 N5 N6 Zn1 -73.75(12) . . . . ? Zn3 N5 N6 Zn1 24.22(13) . . . . ? C1 Zn1 N6 C21 46.0(3) . . . . ? C1" Zn1 N6 C21 40.8(4) . . . . ? C1' Zn1 N6 C21 28.0(3) . . . . ? N1 Zn1 N6 C21 -106.54(15) . . . . ? N3 Zn1 N6 C21 158.73(15) . . . . ? C1 Zn1 N6 N5 170.3(2) . . . . ? C1" Zn1 N6 N5 165.1(4) . . . . ? C1' Zn1 N6 N5 152.4(3) . . . . ? N1 Zn1 N6 N5 17.79(13) . . . . ? N3 Zn1 N6 N5 -76.95(12) . . . . ? C1 Zn1 N6 C20 -69.3(2) . . . . ? C1" Zn1 N6 C20 -74.5(4) . . . . ? C1' Zn1 N6 C20 -87.2(3) . . . . ? N1 Zn1 N6 C20 138.22(13) . . . . ? N3 Zn1 N6 C20 43.49(13) . . . . ? C15 Zn2 N7 C26 -5.6(3) . . . . ? C15" Zn2 N7 C26 8.7(5) . . . . ? C15' Zn2 N7 C26 3.0(7) . . . . ? N5 Zn2 N7 C26 143.01(17) . . . . ? N2 Zn2 N7 C26 -117.85(17) . . . . ? C15 Zn2 N7 C22 173.1(2) . . . . ? C15" Zn2 N7 C22 -172.6(5) . . . . ? C15' Zn2 N7 C22 -178.3(7) . . . . ? N5 Zn2 N7 C22 -38.24(15) . . . . ? N2 Zn2 N7 C22 60.90(15) . . . . ? C1" Zn1 C1 C2 -78.1(16) . . . . ? C1' Zn1 C1 C2 -20.4(13) . . . . ? N1 Zn1 C1 C2 39.0(7) . . . . ? N3 Zn1 C1 C2 156.9(5) . . . . ? N6 Zn1 C1 C2 -98.3(5) . . . . ? C1 Zn1 C1' C2' 8.9(11) . . . . ? C1" Zn1 C1' C2' 63.6(16) . . . . ? N1 Zn1 C1' C2' -124.6(7) . . . . ? N3 Zn1 C1' C2' 5.8(10) . . . . ? N6 Zn1 C1' C2' 117.4(8) . . . . ? C1 Zn1 C1" C2" 30.3(12) . . . . ? C1' Zn1 C1" C2" -39.2(14) . . . . ? N1 Zn1 C1" C2" -49.9(13) . . . . ? N3 Zn1 C1" C2" 90.7(10) . . . . ? N6 Zn1 C1" C2" -168.4(9) . . . . ? N2 N1 C3 C4 -113.8(2) . . . . ? Zn1 N1 C3 C4 117.54(17) . . . . ? Zn3 N1 C3 C4 13.4(2) . . . . ? N2 N1 C3 C5 120.9(2) . . . . ? Zn1 N1 C3 C5 -7.7(2) . . . . ? Zn3 N1 C3 C5 -111.85(19) . . . . ? C12 N3 C8 C9 -0.4(3) . . . . ? Zn1 N3 C8 C9 -176.13(15) . . . . ? C12 N3 C8 Zn3 177.78(16) . . . . ? Zn1 N3 C8 Zn3 2.10(18) . . . . ? C22 Zn3 C8 N3 169.08(13) . . . . ? N1 Zn3 C8 N3 33.00(15) . . . . ? N5 Zn3 C8 N3 -60.43(15) . . . . ? C22 Zn3 C8 C9 -13.0(3) . . . . ? N1 Zn3 C8 C9 -149.1(2) . . . . ? N5 Zn3 C8 C9 117.5(2) . . . . ? N3 C8 C9 C10 0.0(3) . . . . ? Zn3 C8 C9 C10 -177.74(16) . . . . ? C13 N4 C10 C11 -173.7(2) . . . . ? C14 N4 C10 C11 1.9(3) . . . . ? C13 N4 C10 C9 6.7(4) . . . . ? C14 N4 C10 C9 -177.6(2) . . . . ? C8 C9 C10 N4 -179.8(2) . . . . ? C8 C9 C10 C11 0.7(3) . . . . ? N4 C10 C11 C12 179.6(2) . . . . ? C9 C10 C11 C12 -0.9(3) . . . . ? C8 N3 C12 C11 0.2(3) . . . . ? Zn1 N3 C12 C11 175.58(18) . . . . ? C10 C11 C12 N3 0.5(4) . . . . ? C15" Zn2 C15 C16 -153(4) . . . . ? C15' Zn2 C15 C16 -91(4) . . . . ? N5 Zn2 C15 C16 -174.8(3) . . . . ? N7 Zn2 C15 C16 -44.1(5) . . . . ? N2 Zn2 C15 C16 61.6(5) . . . . ? C15 Zn2 C15' C16' -39(3) . . . . ? C15" Zn2 C15' C16' 29(3) . . . . ? N5 Zn2 C15' C16' 69.0(16) . . . . ? N7 Zn2 C15' C16' -174.8(13) . . . . ? N2 Zn2 C15' C16' -67.7(16) . . . . ? C15 Zn2 C15" C16" -3(2) . . . . ? C15' Zn2 C15" C16" -55(4) . . . . ? N5 Zn2 C15" C16" 159.0(13) . . . . ? N7 Zn2 C15" C16" -81.1(17) . . . . ? N2 Zn2 C15" C16" 34.7(18) . . . . ? N6 N5 C17 C18 -109.4(2) . . . . ? Zn2 N5 C17 C18 122.20(17) . . . . ? Zn3 N5 C17 C18 17.9(2) . . . . ? N6 N5 C17 C19 125.2(2) . . . . ? Zn2 N5 C17 C19 -3.2(2) . . . . ? Zn3 N5 C17 C19 -107.5(2) . . . . ? C26 N7 C22 C23 -0.3(3) . . . . ? Zn2 N7 C22 C23 -179.08(14) . . . . ? C26 N7 C22 Zn3 -179.72(15) . . . . ? Zn2 N7 C22 Zn3 1.47(18) . . . . ? C8 Zn3 C22 N7 167.00(13) . . . . ? N1 Zn3 C22 N7 -59.56(15) . . . . ? N5 Zn3 C22 N7 33.68(14) . . . . ? C8 Zn3 C22 C23 -12.3(3) . . . . ? N1 Zn3 C22 C23 121.1(2) . . . . ? N5 Zn3 C22 C23 -145.7(2) . . . . ? N7 C22 C23 C24 -0.1(3) . . . . ? Zn3 C22 C23 C24 179.22(16) . . . . ? C27 N8 C24 C25 -178.0(3) . . . . ? C28 N8 C24 C25 -9.0(3) . . . . ? C27 N8 C24 C23 2.7(4) . . . . ? C28 N8 C24 C23 171.6(2) . . . . ? C22 C23 C24 N8 179.9(2) . . . . ? C22 C23 C24 C25 0.5(3) . . . . ? N8 C24 C25 C26 -180.0(2) . . . . ? C23 C24 C25 C26 -0.6(3) . . . . ? C22 N7 C26 C25 0.2(3) . . . . ? Zn2 N7 C26 C25 178.92(17) . . . . ? C24 C25 C26 N7 0.2(3) . . . . ? C31 O1 C29 C30 -177.9(8) . . . . ? C29 O1 C31 C32 -177.2(8) . . . . ? C35 O2 C33 C34 -175.6(6) . . . . ? C33 O2 C35 C36 178.3(5) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.420 _refine_diff_density_min -0.330 _refine_diff_density_rms 0.048