# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _publ_contact_author_email junweiye@dlut.edu.cn _publ_contact_author_name 'Junwei Ye' loop_ _publ_author_name 'Xinyi Lu' 'Junwei Ye' 'Wei Li' 'Weitao Gong' 'Lijian Yang' 'Yuan Lin' ; Guiling Ning ; # Attachment '- compounds.CIF' data_1 _database_code_depnum_ccdc_archive 'CCDC 843810' #TrackingRef '- compounds.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H13 Cd N3 O8' _chemical_formula_weight 451.66 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 8.9656(18) _cell_length_b 9.0023(18) _cell_length_c 10.242(2) _cell_angle_alpha 86.35(3) _cell_angle_beta 74.79(3) _cell_angle_gamma 81.44(3) _cell_volume 788.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7387 _cell_measurement_theta_min 2.06 _cell_measurement_theta_max 25 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.902 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 448 _exptl_absorpt_coefficient_mu 1.435 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7507 _exptl_absorpt_correction_T_max 0.8255 _exptl_absorpt_process_details 'Higashi (1995)' _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 '\f and \w scans' _diffrn_detector_area_resol_mean 'Bruker SMART CCD area' _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 2749 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0196 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2749 _reflns_number_gt 2556 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SMART (Bruker, 1997)' _computing_data_reduction 'SAINT (Bruker, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXP97 (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Bruker, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0485P)^2^+0.2695P] 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 0 _refine_ls_number_reflns 2749 _refine_ls_number_parameters 242 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0256 _refine_ls_R_factor_gt 0.0219 _refine_ls_wR_factor_ref 0.0660 _refine_ls_wR_factor_gt 0.0641 _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 Cd1 Cd 0.71727(2) 0.96736(2) -0.103837(18) 0.02901(9) Uani 1 1 d . . . O1 O 0.5552(2) 1.1079(2) 0.07666(19) 0.0333(4) Uani 1 1 d . . . O2 O 0.7706(2) 0.9914(3) 0.1179(2) 0.0473(6) Uani 1 1 d . . . O3 O 0.7863(3) 0.9525(3) 0.6146(2) 0.0448(5) Uani 1 1 d . . . O4 O 0.6310(2) 1.1244(3) 0.74969(19) 0.0412(5) Uani 1 1 d . . . O5 O 0.2724(3) 1.4933(3) 0.5958(3) 0.0542(6) Uani 1 1 d . . . O6 O 0.2386(3) 1.4903(3) 0.3966(3) 0.0651(8) Uani 1 1 d . . . O7 O 0.9503(3) 1.0554(4) -0.1819(3) 0.0551(7) Uani 1 1 d . . . O8 O 0.0280(4) 0.2339(4) 0.5928(3) 0.0610(7) Uani 1 1 d . . . N1 N 0.3047(3) 1.4419(3) 0.4828(3) 0.0386(6) Uani 1 1 d . . . N2 N 0.7782(3) 0.7196(3) -0.0802(2) 0.0338(5) Uani 1 1 d . . . N3 N 1.0000(3) 0.7055(3) -0.2565(3) 0.0549(8) Uani 1 1 d . . . H3A H 0.9840 0.8017 -0.2663 0.066 Uiso 1 1 calc R . . H3B H 1.0795 0.6545 -0.3088 0.066 Uiso 1 1 calc R . . C1 C 0.5960(3) 1.1414(3) 0.2927(3) 0.0274(5) Uani 1 1 d . . . C2 C 0.6688(3) 1.0821(3) 0.3930(3) 0.0283(5) Uani 1 1 d . . . H2 H 0.7509 1.0038 0.3729 0.034 Uiso 1 1 calc R . . C3 C 0.6203(3) 1.1385(3) 0.5223(3) 0.0278(5) Uani 1 1 d . . . C4 C 0.5004(3) 1.2574(3) 0.5514(3) 0.0301(6) Uani 1 1 d . . . H4 H 0.4678 1.2978 0.6373 0.036 Uiso 1 1 calc R . . C5 C 0.4305(3) 1.3146(3) 0.4510(3) 0.0290(6) Uani 1 1 d . . . C6 C 0.4742(3) 1.2589(3) 0.3218(3) 0.0290(6) Uani 1 1 d . . . H6 H 0.4236 1.2989 0.2564 0.035 Uiso 1 1 calc R . . C7 C 0.6444(3) 1.0761(3) 0.1542(3) 0.0299(6) Uani 1 1 d . . . C8 C 0.6874(3) 1.0659(3) 0.6352(3) 0.0311(6) Uani 1 1 d . . . C9 C 0.9000(4) 0.6344(3) -0.1586(3) 0.0372(7) Uani 1 1 d . . . C10 C 0.9252(5) 0.4790(4) -0.1395(4) 0.0499(8) Uani 1 1 d . . . H10 H 1.0097 0.4214 -0.1955 0.060 Uiso 1 1 calc R . . C11 C 0.8240(6) 0.4130(4) -0.0377(5) 0.0663(11) Uani 1 1 d . . . H11 H 0.8390 0.3093 -0.0239 0.080 Uiso 1 1 calc R . . C12 C 0.6989(5) 0.4997(5) 0.0455(5) 0.0673(11) Uani 1 1 d . . . H12 H 0.6293 0.4560 0.1158 0.081 Uiso 1 1 calc R . . C13 C 0.6808(4) 0.6519(4) 0.0212(4) 0.0508(8) Uani 1 1 d . . . H13 H 0.5976 0.7111 0.0772 0.061 Uiso 1 1 calc R . . H7A H 1.008(5) 1.038(5) -0.154(4) 0.045(12) Uiso 1 1 d . . . H8A H 0.060(5) 0.183(5) 0.532(5) 0.056(14) Uiso 1 1 d . . . H7B H 0.954(5) 1.102(5) -0.243(5) 0.065(15) Uiso 1 1 d . . . H8B H -0.028(6) 0.291(6) 0.577(5) 0.072(18) 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 Cd1 0.02828(13) 0.03575(13) 0.02071(13) -0.00420(8) -0.00612(8) 0.00409(8) O1 0.0322(10) 0.0479(12) 0.0202(9) -0.0039(8) -0.0093(8) -0.0007(8) O2 0.0368(12) 0.0702(15) 0.0326(12) -0.0213(11) -0.0125(10) 0.0156(11) O3 0.0540(13) 0.0435(13) 0.0398(12) -0.0014(10) -0.0228(11) 0.0043(11) O4 0.0447(12) 0.0585(14) 0.0191(10) -0.0004(9) -0.0099(9) -0.0003(10) O5 0.0548(15) 0.0528(14) 0.0467(15) -0.0201(11) -0.0048(12) 0.0124(11) O6 0.0720(18) 0.0635(17) 0.0579(17) -0.0117(14) -0.0326(15) 0.0299(14) O7 0.0374(14) 0.0765(19) 0.0575(18) 0.0286(15) -0.0252(13) -0.0166(13) O8 0.077(2) 0.0503(17) 0.0476(17) 0.0001(14) -0.0103(15) 0.0051(15) N1 0.0383(13) 0.0348(13) 0.0397(15) -0.0052(11) -0.0071(12) 0.0013(11) N2 0.0331(12) 0.0356(13) 0.0309(13) 0.0010(10) -0.0088(10) 0.0009(10) N3 0.0506(16) 0.0422(16) 0.0515(18) -0.0016(13) 0.0102(14) 0.0163(13) C1 0.0263(13) 0.0357(14) 0.0209(13) -0.0026(11) -0.0058(10) -0.0063(11) C2 0.0250(12) 0.0338(14) 0.0255(14) -0.0015(11) -0.0068(10) -0.0010(10) C3 0.0290(13) 0.0339(14) 0.0221(13) 0.0019(11) -0.0075(11) -0.0084(11) C4 0.0341(14) 0.0346(14) 0.0217(13) -0.0043(11) -0.0052(11) -0.0071(11) C5 0.0302(13) 0.0286(13) 0.0267(14) -0.0028(11) -0.0046(11) -0.0029(11) C6 0.0309(13) 0.0333(14) 0.0241(14) 0.0016(11) -0.0096(11) -0.0054(11) C7 0.0291(13) 0.0405(15) 0.0203(13) -0.0024(11) -0.0050(11) -0.0070(11) C8 0.0340(14) 0.0383(15) 0.0245(14) 0.0017(11) -0.0108(11) -0.0114(12) C9 0.0400(16) 0.0381(16) 0.0339(16) -0.0066(12) -0.0141(13) 0.0043(13) C10 0.063(2) 0.0376(17) 0.049(2) -0.0079(15) -0.0196(17) 0.0051(15) C11 0.088(3) 0.0372(19) 0.079(3) 0.0050(19) -0.033(2) -0.0076(19) C12 0.069(3) 0.055(2) 0.074(3) 0.024(2) -0.011(2) -0.018(2) C13 0.0446(18) 0.055(2) 0.047(2) 0.0125(16) -0.0063(15) -0.0032(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 Cd1 O4 2.204(2) 1_554 ? Cd1 N2 2.229(2) . ? Cd1 O7 2.273(3) . ? Cd1 O1 2.339(2) . ? Cd1 O2 2.469(2) . ? Cd1 O1 2.572(2) 2_675 ? O1 C7 1.260(3) . ? O1 Cd1 2.572(2) 2_675 ? O2 C7 1.249(4) . ? O3 C8 1.238(4) . ? O4 C8 1.264(3) . ? O4 Cd1 2.204(2) 1_556 ? O5 N1 1.220(3) . ? O6 N1 1.212(4) . ? O7 H7A 0.65(4) . ? O7 H7B 0.73(5) . ? O8 H8A 0.76(5) . ? O8 H8B 0.71(5) . ? N1 C5 1.470(4) . ? N2 C9 1.339(4) . ? N2 C13 1.348(4) . ? N3 C9 1.355(4) . ? N3 H3A 0.8600 . ? N3 H3B 0.8600 . ? C1 C6 1.388(4) . ? C1 C2 1.394(4) . ? C1 C7 1.501(4) . ? C2 C3 1.385(4) . ? C2 H2 0.9300 . ? C3 C4 1.385(4) . ? C3 C8 1.509(4) . ? C4 C5 1.375(4) . ? C4 H4 0.9300 . ? C5 C6 1.382(4) . ? C6 H6 0.9300 . ? C9 C10 1.393(5) . ? C10 C11 1.360(6) . ? C10 H10 0.9300 . ? C11 C12 1.384(7) . ? C11 H11 0.9300 . ? C12 C13 1.370(5) . ? C12 H12 0.9300 . ? C13 H13 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 O4 Cd1 N2 137.02(8) 1_554 . ? O4 Cd1 O7 87.19(10) 1_554 . ? N2 Cd1 O7 104.94(11) . . ? O4 Cd1 O1 90.78(8) 1_554 . ? N2 Cd1 O1 120.60(8) . . ? O7 Cd1 O1 111.42(10) . . ? O4 Cd1 O2 135.18(9) 1_554 . ? N2 Cd1 O2 87.67(9) . . ? O7 Cd1 O2 82.56(11) . . ? O1 Cd1 O2 54.00(7) . . ? O4 Cd1 O1 79.10(8) 1_554 2_675 ? N2 Cd1 O1 81.62(8) . 2_675 ? O7 Cd1 O1 165.02(9) . 2_675 ? O1 Cd1 O1 75.12(8) . 2_675 ? O2 Cd1 O1 111.47(8) . 2_675 ? C7 O1 Cd1 95.30(17) . . ? C7 O1 Cd1 128.18(17) . 2_675 ? Cd1 O1 Cd1 104.88(8) . 2_675 ? C7 O2 Cd1 89.50(16) . . ? C8 O4 Cd1 106.16(18) . 1_556 ? Cd1 O7 H7A 124(4) . . ? Cd1 O7 H7B 112(4) . . ? H7A O7 H7B 124(5) . . ? H8A O8 H8B 108(5) . . ? O6 N1 O5 123.5(3) . . ? O6 N1 C5 118.8(3) . . ? O5 N1 C5 117.7(3) . . ? C9 N2 C13 118.4(3) . . ? C9 N2 Cd1 125.7(2) . . ? C13 N2 Cd1 115.8(2) . . ? C9 N3 H3A 120.0 . . ? C9 N3 H3B 120.0 . . ? H3A N3 H3B 120.0 . . ? C6 C1 C2 119.9(2) . . ? C6 C1 C7 119.3(2) . . ? C2 C1 C7 120.7(2) . . ? C3 C2 C1 120.7(3) . . ? C3 C2 H2 119.6 . . ? C1 C2 H2 119.6 . . ? C4 C3 C2 119.6(2) . . ? C4 C3 C8 119.0(2) . . ? C2 C3 C8 121.2(3) . . ? C5 C4 C3 118.8(3) . . ? C5 C4 H4 120.6 . . ? C3 C4 H4 120.6 . . ? C4 C5 C6 123.0(3) . . ? C4 C5 N1 118.2(2) . . ? C6 C5 N1 118.8(2) . . ? C5 C6 C1 117.9(2) . . ? C5 C6 H6 121.0 . . ? C1 C6 H6 121.0 . . ? O2 C7 O1 121.2(2) . . ? O2 C7 C1 120.0(2) . . ? O1 C7 C1 118.8(2) . . ? O3 C8 O4 123.8(3) . . ? O3 C8 C3 120.5(3) . . ? O4 C8 C3 115.6(3) . . ? N2 C9 N3 117.4(3) . . ? N2 C9 C10 121.7(3) . . ? N3 C9 C10 120.9(3) . . ? C11 C10 C9 118.9(3) . . ? C11 C10 H10 120.6 . . ? C9 C10 H10 120.6 . . ? C10 C11 C12 120.2(4) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C13 C12 C11 118.0(4) . . ? C13 C12 H12 121.0 . . ? C11 C12 H12 121.0 . . ? N2 C13 C12 122.8(4) . . ? N2 C13 H13 118.6 . . ? C12 C13 H13 118.6 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O8 H8B O6 0.71(5) 2.49(5) 3.166(5) 160(5) 2_576 O7 H7B O8 0.73(5) 2.02(5) 2.722(4) 163(5) 1_664 O8 H8A O3 0.76(5) 2.07(5) 2.805(5) 161(4) 2_666 O7 H7A O2 0.65(4) 2.09(4) 2.716(4) 164(5) 2_775 N3 H3B O5 0.86 2.14 2.991(4) 167.9 1_644 N3 H3A O3 0.86 2.58 3.169(4) 126.2 1_554 N3 H3A O7 0.86 2.44 3.227(5) 152.0 . _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.394 _refine_diff_density_min -0.505 _refine_diff_density_rms 0.117 # = = = END data_2 _database_code_depnum_ccdc_archive 'CCDC 843811' #TrackingRef 'CCDC-compounds.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H17 Cd N5 O7' _chemical_formula_weight 527.78 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' Cd Cd -0.8075 1.2024 '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' _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 8.4601(5) _cell_length_b 10.0552(6) _cell_length_c 12.9572(7) _cell_angle_alpha 68.863(4) _cell_angle_beta 84.699(4) _cell_angle_gamma 87.698(4) _cell_volume 1023.66(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3460 _cell_measurement_theta_min 1.69 _cell_measurement_theta_max 25.01 _exptl_crystal_description block _exptl_crystal_colour colorless _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 1.712 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 528 _exptl_absorpt_coefficient_mu 1.118 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7522 _exptl_absorpt_correction_T_max 0.7910 _exptl_absorpt_process_details 'Higashi (1995)' _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 '\f and \w scans' _diffrn_detector_area_resol_mean 'Bruker SMART CCD area' _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_reflns_number 7687 _diffrn_reflns_av_R_equivalents 0.0382 _diffrn_reflns_av_sigmaI/netI 0.0473 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 25.01 _reflns_number_total 3460 _reflns_number_gt 3205 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SMART (Bruker, 1997)' _computing_data_reduction 'SAINT (Bruker, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXP97 (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Bruker, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1626P)^2^+1.1453P] 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 0 _refine_ls_number_reflns 3460 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0707 _refine_ls_R_factor_gt 0.0681 _refine_ls_wR_factor_ref 0.1920 _refine_ls_wR_factor_gt 0.1881 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.83617(5) 0.13620(4) 0.65960(3) 0.0345(2) Uani 1 1 d . . . O1 O 0.9327(6) 0.2100(5) 0.8043(4) 0.0481(11) Uani 1 1 d . . . O2 O 0.8484(7) 0.3755(6) 0.6577(5) 0.0597(15) Uani 1 1 d . . . O3 O 0.8635(6) 0.8863(5) 0.6258(4) 0.0508(12) Uani 1 1 d . . . O4 O 0.9577(6) 0.9332(5) 0.7603(4) 0.0506(12) Uani 1 1 d . . . O5 O 1.2875(6) 0.5784(6) 1.0137(4) 0.0524(12) Uani 1 1 d . . . O6 O 1.3032(7) 0.3640(6) 1.0147(5) 0.0641(15) Uani 1 1 d . . . O7 O 1.0898(8) 0.2051(7) 0.5523(5) 0.0649(15) Uani 1 1 d . . . N1 N 1.2509(6) 0.4852(6) 0.9802(4) 0.0399(12) Uani 1 1 d . . . N2 N 0.7172(6) 0.2290(6) 0.4966(4) 0.0407(12) Uani 1 1 d . . . N3 N 0.4668(9) 0.3929(9) 0.2157(6) 0.072(2) Uani 1 1 d . . . H3A H 0.4495 0.4832 0.1871 0.086 Uiso 1 1 calc R . . H3B H 0.4352 0.3371 0.1849 0.086 Uiso 1 1 calc R . . N4 N 0.5958(7) 0.0657(6) 0.7601(5) 0.0432(13) Uani 1 1 d . . . N5 N 0.1616(7) -0.0538(8) 0.9472(6) 0.0580(16) Uani 1 1 d . . . H5B H 0.0764 -0.0095 0.9214 0.070 Uiso 1 1 calc R . . H5A H 0.1570 -0.1207 1.0114 0.070 Uiso 1 1 calc R . . C1 C 0.9812(6) 0.4505(6) 0.7809(5) 0.0298(11) Uani 1 1 d . . . C2 C 0.9351(6) 0.5924(6) 0.7294(4) 0.0301(11) Uani 1 1 d . . . H2 H 0.8671 0.6163 0.6729 0.036 Uiso 1 1 calc R . . C3 C 0.9904(7) 0.6982(6) 0.7620(5) 0.0300(11) Uani 1 1 d . . . C4 C 1.0944(6) 0.6625(6) 0.8457(5) 0.0309(12) Uani 1 1 d . . . H4 H 1.1312 0.7317 0.8693 0.037 Uiso 1 1 calc R . . C5 C 1.1410(6) 0.5225(6) 0.8923(5) 0.0311(12) Uani 1 1 d . . . C6 C 1.0859(7) 0.4149(6) 0.8621(5) 0.0315(12) Uani 1 1 d . . . H6 H 1.1189 0.3210 0.8958 0.038 Uiso 1 1 calc R . . C7 C 0.9176(7) 0.3375(7) 0.7450(6) 0.0384(14) Uani 1 1 d . . . C8 C 0.9326(7) 0.8497(6) 0.7107(5) 0.0359(13) Uani 1 1 d . . . C9 C 0.6644(9) 0.1459(8) 0.4460(6) 0.0469(15) Uani 1 1 d . . . H9 H 0.6860 0.0486 0.4755 0.056 Uiso 1 1 calc R . . C10 C 0.5810(10) 0.1953(9) 0.3542(6) 0.0550(18) Uani 1 1 d . . . H10 H 0.5494 0.1326 0.3221 0.066 Uiso 1 1 calc R . . C11 C 0.5435(8) 0.3388(9) 0.3090(6) 0.0483(17) Uani 1 1 d . . . C12 C 0.5956(10) 0.4259(9) 0.3603(7) 0.060(2) Uani 1 1 d . . . H12 H 0.5739 0.5232 0.3331 0.072 Uiso 1 1 calc R . . C13 C 0.6794(11) 0.3673(8) 0.4515(6) 0.0557(19) Uani 1 1 d . . . H13 H 0.7128 0.4281 0.4848 0.067 Uiso 1 1 calc R . . C14 C 0.5841(8) -0.0408(7) 0.8586(6) 0.0429(14) Uani 1 1 d . . . H14 H 0.6772 -0.0883 0.8847 0.051 Uiso 1 1 calc R . . C15 C 0.4460(8) -0.0856(7) 0.9241(6) 0.0431(15) Uani 1 1 d . . . H15 H 0.4469 -0.1596 0.9926 0.052 Uiso 1 1 calc R . . C16 C 0.3030(8) -0.0181(8) 0.8864(6) 0.0420(14) Uani 1 1 d . . . C17 C 0.3115(9) 0.0908(8) 0.7816(6) 0.0518(17) Uani 1 1 d . . . H17 H 0.2198 0.1371 0.7518 0.062 Uiso 1 1 calc R . . C18 C 0.4565(8) 0.1282(8) 0.7234(6) 0.0496(16) Uani 1 1 d . . . H18 H 0.4596 0.2011 0.6542 0.060 Uiso 1 1 calc R . . H7B H 1.0987 0.1755 0.4984 0.060 Uiso 1 1 d R . . H7A H 1.1034 0.2954 0.5213 0.060 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0430(4) 0.0290(3) 0.0347(3) -0.0125(2) -0.0177(2) 0.0061(2) O1 0.053(3) 0.030(2) 0.067(3) -0.023(2) -0.017(2) 0.0042(18) O2 0.079(4) 0.060(3) 0.051(3) -0.026(3) -0.044(3) 0.007(3) O3 0.064(3) 0.036(2) 0.055(3) -0.015(2) -0.032(2) 0.018(2) O4 0.066(3) 0.032(2) 0.063(3) -0.023(2) -0.031(3) 0.015(2) O5 0.060(3) 0.056(3) 0.050(3) -0.026(2) -0.030(2) 0.003(2) O6 0.079(4) 0.044(3) 0.070(4) -0.014(3) -0.046(3) 0.019(3) O7 0.068(4) 0.084(4) 0.048(3) -0.029(3) -0.007(3) -0.001(3) N1 0.042(3) 0.041(3) 0.034(3) -0.008(2) -0.013(2) 0.003(2) N2 0.052(3) 0.039(3) 0.032(3) -0.012(2) -0.019(2) 0.008(2) N3 0.066(4) 0.099(6) 0.048(4) -0.017(4) -0.034(3) 0.009(4) N4 0.044(3) 0.040(3) 0.047(3) -0.016(3) -0.013(3) 0.005(2) N5 0.046(3) 0.077(5) 0.052(4) -0.025(3) -0.007(3) 0.008(3) C1 0.032(3) 0.029(3) 0.031(3) -0.013(2) -0.006(2) 0.002(2) C2 0.029(3) 0.038(3) 0.025(3) -0.012(2) -0.008(2) 0.002(2) C3 0.035(3) 0.025(3) 0.032(3) -0.011(2) -0.008(2) 0.006(2) C4 0.030(3) 0.035(3) 0.032(3) -0.016(2) -0.010(2) 0.002(2) C5 0.032(3) 0.035(3) 0.029(3) -0.013(2) -0.007(2) 0.001(2) C6 0.034(3) 0.028(3) 0.033(3) -0.010(2) -0.008(2) 0.006(2) C7 0.036(3) 0.040(4) 0.048(4) -0.026(3) -0.011(3) 0.006(2) C8 0.036(3) 0.029(3) 0.042(3) -0.010(3) -0.012(3) 0.008(2) C9 0.055(4) 0.046(4) 0.043(4) -0.017(3) -0.018(3) 0.003(3) C10 0.064(5) 0.060(5) 0.050(4) -0.026(4) -0.025(3) 0.001(3) C11 0.034(3) 0.073(5) 0.035(3) -0.015(3) -0.010(3) 0.005(3) C12 0.073(5) 0.052(4) 0.050(4) -0.011(3) -0.023(4) 0.019(4) C13 0.083(5) 0.043(4) 0.046(4) -0.018(3) -0.032(4) 0.011(3) C14 0.042(3) 0.043(4) 0.046(4) -0.017(3) -0.015(3) 0.006(3) C15 0.049(4) 0.043(4) 0.038(3) -0.014(3) -0.014(3) 0.003(3) C16 0.043(3) 0.051(4) 0.040(3) -0.025(3) -0.012(3) 0.002(3) C17 0.045(4) 0.062(5) 0.045(4) -0.015(3) -0.017(3) 0.020(3) C18 0.047(4) 0.051(4) 0.048(4) -0.013(3) -0.017(3) 0.015(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O4 2.255(4) 1_545 ? Cd1 N2 2.290(5) . ? Cd1 N4 2.301(6) . ? Cd1 O2 2.403(6) . ? Cd1 O7 2.427(6) . ? Cd1 O1 2.463(5) . ? Cd1 O3 2.700(5) 1_545 ? Cd1 C7 2.768(6) . ? Cd1 C8 2.817(6) 1_545 ? O1 C7 1.243(8) . ? O2 C7 1.250(8) . ? O3 C8 1.224(8) . ? O3 Cd1 2.700(5) 1_565 ? O4 C8 1.260(8) . ? O4 Cd1 2.255(4) 1_565 ? O5 N1 1.226(7) . ? O6 N1 1.217(7) . ? O7 H7B 0.8491 . ? O7 H7A 0.8572 . ? N1 C5 1.471(8) . ? N2 C13 1.338(9) . ? N2 C9 1.344(9) . ? N3 C11 1.349(9) . ? N3 H3A 0.8600 . ? N3 H3B 0.8600 . ? N4 C14 1.337(9) . ? N4 C18 1.355(9) . ? N5 C16 1.355(9) . ? N5 H5B 0.8600 . ? N5 H5A 0.8600 . ? C1 C6 1.376(8) . ? C1 C2 1.397(8) . ? C1 C7 1.508(8) . ? C2 C3 1.389(8) . ? C2 H2 0.9300 . ? C3 C4 1.395(8) . ? C3 C8 1.507(8) . ? C4 C5 1.374(8) . ? C4 H4 0.9300 . ? C5 C6 1.386(8) . ? C6 H6 0.9300 . ? C8 Cd1 2.817(6) 1_565 ? C9 C10 1.364(10) . ? C9 H9 0.9300 . ? C10 C11 1.384(11) . ? C10 H10 0.9300 . ? C11 C12 1.382(12) . ? C12 C13 1.366(11) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 C15 1.368(10) . ? C14 H14 0.9300 . ? C15 C16 1.402(9) . ? C15 H15 0.9300 . ? C16 C17 1.402(10) . ? C17 C18 1.370(11) . ? C17 H17 0.9300 . ? C18 H18 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 O4 Cd1 N2 139.09(18) 1_545 . ? O4 Cd1 N4 92.4(2) 1_545 . ? N2 Cd1 N4 91.7(2) . . ? O4 Cd1 O2 131.46(17) 1_545 . ? N2 Cd1 O2 87.48(18) . . ? N4 Cd1 O2 100.4(2) . . ? O4 Cd1 O7 86.8(2) 1_545 . ? N2 Cd1 O7 88.0(2) . . ? N4 Cd1 O7 178.52(18) . . ? O2 Cd1 O7 81.1(2) . . ? O4 Cd1 O1 79.85(16) 1_545 . ? N2 Cd1 O1 140.60(17) . . ? N4 Cd1 O1 92.18(19) . . ? O2 Cd1 O1 53.28(16) . . ? O7 Cd1 O1 88.94(18) . . ? O4 Cd1 O3 51.36(16) 1_545 1_545 ? N2 Cd1 O3 87.96(16) . 1_545 ? N4 Cd1 O3 90.16(19) . 1_545 ? O2 Cd1 O3 168.7(2) . 1_545 ? O7 Cd1 O3 88.4(2) . 1_545 ? O1 Cd1 O3 131.21(15) . 1_545 ? O4 Cd1 C7 105.12(18) 1_545 . ? N2 Cd1 C7 114.27(19) . . ? N4 Cd1 C7 99.4(2) . . ? O2 Cd1 C7 26.81(19) . . ? O7 Cd1 C7 82.1(2) . . ? O1 Cd1 C7 26.67(18) . . ? O3 Cd1 C7 155.28(17) 1_545 . ? O4 Cd1 C8 25.85(18) 1_545 1_545 ? N2 Cd1 C8 113.44(19) . 1_545 ? N4 Cd1 C8 90.81(19) . 1_545 ? O2 Cd1 C8 156.11(18) . 1_545 ? O7 Cd1 C8 88.0(2) . 1_545 ? O1 Cd1 C8 105.69(17) . 1_545 ? O3 Cd1 C8 25.53(17) 1_545 1_545 ? C7 Cd1 C8 130.72(19) . 1_545 ? C7 O1 Cd1 90.5(4) . . ? C7 O2 Cd1 93.1(4) . . ? C8 O3 Cd1 82.6(4) . 1_565 ? C8 O4 Cd1 102.9(4) . 1_565 ? Cd1 O7 H7B 110.7 . . ? Cd1 O7 H7A 114.6 . . ? H7B O7 H7A 103.9 . . ? O6 N1 O5 123.3(6) . . ? O6 N1 C5 118.3(5) . . ? O5 N1 C5 118.4(5) . . ? C13 N2 C9 115.0(6) . . ? C13 N2 Cd1 122.5(5) . . ? C9 N2 Cd1 122.1(4) . . ? C11 N3 H3A 120.0 . . ? C11 N3 H3B 120.0 . . ? H3A N3 H3B 120.0 . . ? C14 N4 C18 115.4(6) . . ? C14 N4 Cd1 122.0(5) . . ? C18 N4 Cd1 122.6(5) . . ? C16 N5 H5B 120.0 . . ? C16 N5 H5A 120.0 . . ? H5B N5 H5A 120.0 . . ? C6 C1 C2 120.2(5) . . ? C6 C1 C7 120.5(5) . . ? C2 C1 C7 119.3(5) . . ? C3 C2 C1 120.4(5) . . ? C3 C2 H2 119.8 . . ? C1 C2 H2 119.8 . . ? C2 C3 C4 119.7(5) . . ? C2 C3 C8 120.1(5) . . ? C4 C3 C8 120.2(5) . . ? C5 C4 C3 118.4(5) . . ? C5 C4 H4 120.8 . . ? C3 C4 H4 120.8 . . ? C4 C5 C6 122.9(6) . . ? C4 C5 N1 118.3(5) . . ? C6 C5 N1 118.8(5) . . ? C1 C6 C5 118.4(5) . . ? C1 C6 H6 120.8 . . ? C5 C6 H6 120.8 . . ? O1 C7 O2 122.2(6) . . ? O1 C7 C1 119.0(6) . . ? O2 C7 C1 118.7(6) . . ? O1 C7 Cd1 62.8(3) . . ? O2 C7 Cd1 60.1(4) . . ? C1 C7 Cd1 172.4(4) . . ? O3 C8 O4 123.1(6) . . ? O3 C8 C3 120.2(6) . . ? O4 C8 C3 116.7(6) . . ? O3 C8 Cd1 71.9(3) . 1_565 ? O4 C8 Cd1 51.3(3) . 1_565 ? C3 C8 Cd1 167.6(4) . 1_565 ? N2 C9 C10 124.1(7) . . ? N2 C9 H9 118.0 . . ? C10 C9 H9 118.0 . . ? C9 C10 C11 119.9(7) . . ? C9 C10 H10 120.1 . . ? C11 C10 H10 120.1 . . ? N3 C11 C12 121.3(8) . . ? N3 C11 C10 121.7(8) . . ? C12 C11 C10 116.9(7) . . ? C13 C12 C11 119.2(7) . . ? C13 C12 H12 120.4 . . ? C11 C12 H12 120.4 . . ? N2 C13 C12 124.9(7) . . ? N2 C13 H13 117.6 . . ? C12 C13 H13 117.6 . . ? N4 C14 C15 125.2(6) . . ? N4 C14 H14 117.4 . . ? C15 C14 H14 117.4 . . ? C14 C15 C16 118.9(6) . . ? C14 C15 H15 120.5 . . ? C16 C15 H15 120.5 . . ? N5 C16 C17 120.4(6) . . ? N5 C16 C15 122.7(7) . . ? C17 C16 C15 117.0(6) . . ? C18 C17 C16 119.3(6) . . ? C18 C17 H17 120.4 . . ? C16 C17 H17 120.4 . . ? N4 C18 C17 124.2(7) . . ? N4 C18 H18 117.9 . . ? C17 C18 H18 117.9 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3 H3A O5 0.86 2.60 3.101(8) 118.3 1_454 N3 H3B O6 0.86 2.49 3.167(9) 136.6 1_454 N5 H5B O1 0.86 2.52 3.304(8) 151.6 1_455 N5 H5B O4 0.86 2.65 3.143(8) 117.9 1_445 N5 H5A O1 0.86 2.29 3.075(9) 151.2 2_657 O7 H7B O3 0.85 1.92 2.767(8) 175.3 2_766 _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 5.158 _refine_diff_density_min -0.968 _refine_diff_density_rms 0.226 # = = = END data_3 _database_code_depnum_ccdc_archive 'CCDC 843812' #TrackingRef 'CCDC-compounds.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H16 N4 O14 Zn2' _chemical_formula_weight 679.12 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 Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.4852(19) _cell_length_b 11.060(2) _cell_length_c 11.768(2) _cell_angle_alpha 90.17(3) _cell_angle_beta 93.31(3) _cell_angle_gamma 101.11(3) _cell_volume 1209.2(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6523 _cell_measurement_theta_min 1.88 _cell_measurement_theta_max 27.47 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.865 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 684 _exptl_absorpt_coefficient_mu 2.068 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4902 _exptl_absorpt_correction_T_max 0.6143 _exptl_absorpt_process_details 'Higashi (1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 5419 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0285 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5419 _reflns_number_gt 4578 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'RAPID-AUTO (Rigaku, 1998)' _computing_cell_refinement RAPID-AUTO _computing_data_reduction RAPID-AUTO _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999) and SHELXP97' _computing_publication_material SHELXL97 _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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef 0 _refine_ls_number_reflns 5419 _refine_ls_number_parameters 370 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0487 _refine_ls_R_factor_gt 0.0373 _refine_ls_wR_factor_ref 0.1251 _refine_ls_wR_factor_gt 0.1136 _refine_ls_goodness_of_fit_ref 0.997 _refine_ls_restrained_S_all 0.997 _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 -0.56494(3) 0.11467(3) -0.21531(3) 0.02073(11) Uani 1 1 d . . . Zn2 Zn -0.65486(3) -0.01105(3) 0.04878(3) 0.02102(11) Uani 1 1 d . . . O1 O -0.3189(2) 0.20278(18) -0.0486(2) 0.0351(5) Uani 1 1 d . . . O2 O -0.4736(2) 0.28337(19) -0.1614(2) 0.0354(5) Uani 1 1 d . . . O3 O -0.4578(3) 0.7347(2) -0.1383(2) 0.0359(5) Uani 1 1 d . . . O4 O -0.3011(3) 0.84626(19) -0.0125(2) 0.0329(5) Uani 1 1 d . . . O5 O 0.0386(4) 0.6553(3) 0.2121(3) 0.0679(10) Uani 1 1 d . . . O6 O 0.0249(4) 0.4622(3) 0.2058(3) 0.0617(9) Uani 1 1 d . . . O7 O -0.5740(2) -0.0948(2) 0.33243(19) 0.0323(5) Uani 1 1 d . . . O8 O -0.7254(2) -0.0168(2) 0.21335(19) 0.0323(5) Uani 1 1 d . . . O9 O -1.2371(2) -0.1071(2) 0.2728(2) 0.0317(5) Uani 1 1 d . . . O10 O -1.3165(2) -0.2049(3) 0.4270(2) 0.0462(7) Uani 1 1 d . . . O11 O -0.9629(3) -0.1852(3) 0.7521(2) 0.0508(7) Uani 1 1 d . . . O12 O -0.7416(3) -0.1864(3) 0.7212(2) 0.0449(6) Uani 1 1 d . . . O13 O -0.5620(2) -0.01749(16) -0.10756(16) 0.0203(4) Uani 1 1 d . . . O14 O -0.8859(3) -0.0676(3) -0.0211(3) 0.0576(8) Uani 1 1 d . . . N1 N -0.0160(3) 0.5549(3) 0.1756(2) 0.0360(6) Uani 1 1 d . . . N2 N -0.8643(3) -0.1775(2) 0.6888(2) 0.0301(5) Uani 1 1 d . . . N3 N -0.3324(5) -0.5669(4) 0.3651(3) 0.0613(10) Uani 1 1 d . . . N4 N -0.5405(4) -0.7272(4) 0.3736(3) 0.0580(10) Uani 1 1 d . . . H4A H -0.5995 -0.7765 0.4130 0.070 Uiso 1 1 calc R . . H4B H -0.5518 -0.7286 0.3005 0.070 Uiso 1 1 calc R . . C1 C -0.3062(3) 0.4157(2) -0.0390(3) 0.0250(6) Uani 1 1 d . . . C2 C -0.3572(3) 0.5203(2) -0.0751(3) 0.0250(6) Uani 1 1 d . . . H2A H -0.4318 0.5130 -0.1311 0.030 Uiso 1 1 calc R . . C3 C -0.2973(3) 0.6354(2) -0.0280(3) 0.0243(6) Uani 1 1 d . . . C4 C -0.1858(3) 0.6473(3) 0.0544(3) 0.0274(6) Uani 1 1 d . . . H4C H -0.1449 0.7239 0.0865 0.033 Uiso 1 1 calc R . . C5 C -0.1365(3) 0.5426(3) 0.0883(3) 0.0276(6) Uani 1 1 d . . . C6 C -0.1944(3) 0.4277(3) 0.0447(3) 0.0280(6) Uani 1 1 d . . . H6A H -0.1596 0.3589 0.0705 0.034 Uiso 1 1 calc R . . C7 C -0.3709(3) 0.2908(2) -0.0871(3) 0.0254(6) Uani 1 1 d . . . C8 C -0.3584(3) 0.7473(2) -0.0644(2) 0.0243(6) Uani 1 1 d . . . C9 C -0.8102(3) -0.0973(2) 0.3857(2) 0.0212(5) Uani 1 1 d . . . C10 C -0.9523(3) -0.1046(2) 0.3446(2) 0.0223(5) Uani 1 1 d . . . H10A H -0.9721 -0.0844 0.2695 0.027 Uiso 1 1 calc R . . C11 C -1.0652(3) -0.1419(2) 0.4156(2) 0.0222(5) Uani 1 1 d . . . C12 C -1.0355(3) -0.1672(3) 0.5282(2) 0.0241(5) Uani 1 1 d . . . H12A H -1.1098 -0.1913 0.5764 0.029 Uiso 1 1 calc R . . C13 C -0.8935(3) -0.1560(2) 0.5683(2) 0.0227(5) Uani 1 1 d . . . C14 C -0.7795(3) -0.1232(3) 0.4990(2) 0.0237(5) Uani 1 1 d . . . H14A H -0.6851 -0.1186 0.5275 0.028 Uiso 1 1 calc R . . C15 C -0.6939(3) -0.0661(3) 0.3026(2) 0.0238(5) Uani 1 1 d . . . C16 C -1.2189(3) -0.1535(3) 0.3694(3) 0.0251(6) Uani 1 1 d . . . C17 C -0.4341(4) -0.6506(3) 0.4244(3) 0.0358(7) Uani 1 1 d . . . C18 C -0.4171(3) -0.6489(3) 0.5383(3) 0.0299(6) Uani 1 1 d . . . H18A H -0.4848 -0.7015 0.5783 0.036 Uiso 1 1 calc R . . C19 C -0.3074(5) -0.5755(4) 0.5986(3) 0.0489(9) Uani 1 1 d . . . H19A H -0.3000 -0.5806 0.6775 0.059 Uiso 1 1 calc R . . C20 C -0.2089(5) -0.4949(4) 0.5448(4) 0.0571(11) Uani 1 1 d . . . H20A H -0.1334 -0.4441 0.5858 0.069 Uiso 1 1 calc R . . C21 C -0.2222(5) -0.4895(4) 0.4276(4) 0.0571(11) Uani 1 1 d . . . H21A H -0.1561 -0.4330 0.3898 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 Zn1 0.01486(17) 0.02271(18) 0.02423(19) 0.00440(12) -0.00213(12) 0.00360(12) Zn2 0.02226(18) 0.01946(18) 0.02310(19) 0.00447(12) 0.00203(13) 0.00813(12) O1 0.0371(12) 0.0183(10) 0.0491(14) 0.0017(9) 0.0008(10) 0.0042(8) O2 0.0322(12) 0.0237(10) 0.0471(14) -0.0028(9) -0.0048(10) 0.0000(8) O3 0.0394(13) 0.0310(11) 0.0371(13) -0.0011(9) -0.0096(10) 0.0103(9) O4 0.0421(12) 0.0194(10) 0.0374(12) -0.0014(8) -0.0107(10) 0.0105(8) O5 0.076(2) 0.0427(16) 0.082(2) -0.0236(15) -0.0483(18) 0.0186(14) O6 0.069(2) 0.0447(15) 0.071(2) 0.0004(14) -0.0360(17) 0.0222(14) O7 0.0177(10) 0.0500(13) 0.0321(12) 0.0053(10) 0.0042(8) 0.0128(9) O8 0.0261(10) 0.0471(13) 0.0281(11) 0.0093(9) 0.0077(8) 0.0163(9) O9 0.0180(9) 0.0461(13) 0.0313(12) 0.0050(10) -0.0047(8) 0.0083(9) O10 0.0176(11) 0.0697(18) 0.0485(16) 0.0176(13) 0.0011(10) 0.0011(10) O11 0.0452(15) 0.078(2) 0.0267(13) 0.0119(12) 0.0069(11) 0.0055(13) O12 0.0459(14) 0.0614(16) 0.0307(13) -0.0025(11) -0.0146(11) 0.0235(12) O13 0.0220(9) 0.0173(8) 0.0217(9) 0.0024(7) -0.0003(7) 0.0046(7) O14 0.0331(14) 0.0544(17) 0.085(2) -0.0267(16) -0.0073(14) 0.0112(12) N1 0.0369(15) 0.0367(15) 0.0347(15) -0.0023(12) -0.0077(12) 0.0107(11) N2 0.0360(14) 0.0314(13) 0.0213(12) 0.0003(10) -0.0040(10) 0.0043(10) N3 0.073(3) 0.057(2) 0.055(2) 0.0132(17) 0.0214(19) 0.0094(18) N4 0.0409(18) 0.088(3) 0.0380(18) -0.0060(17) 0.0055(14) -0.0071(17) C1 0.0236(13) 0.0197(12) 0.0319(15) -0.0006(11) 0.0051(11) 0.0039(10) C2 0.0246(13) 0.0216(13) 0.0289(15) 0.0005(11) 0.0018(11) 0.0046(10) C3 0.0278(14) 0.0181(12) 0.0279(14) 0.0007(10) 0.0040(11) 0.0057(10) C4 0.0312(15) 0.0186(13) 0.0322(16) -0.0005(11) -0.0018(12) 0.0055(11) C5 0.0288(15) 0.0246(14) 0.0298(15) 0.0004(11) -0.0028(12) 0.0074(11) C6 0.0309(15) 0.0211(13) 0.0335(16) 0.0044(11) 0.0031(12) 0.0081(11) C7 0.0243(13) 0.0198(13) 0.0322(15) 0.0014(11) 0.0088(11) 0.0021(10) C8 0.0287(14) 0.0207(13) 0.0246(14) 0.0010(10) 0.0022(11) 0.0076(10) C9 0.0171(12) 0.0215(12) 0.0254(14) -0.0004(10) 0.0006(10) 0.0048(9) C10 0.0176(12) 0.0275(13) 0.0229(14) -0.0003(10) 0.0000(10) 0.0072(10) C11 0.0172(12) 0.0238(13) 0.0259(14) 0.0017(10) -0.0008(10) 0.0052(9) C12 0.0189(12) 0.0285(14) 0.0249(14) 0.0007(11) 0.0013(10) 0.0045(10) C13 0.0251(13) 0.0243(13) 0.0191(13) 0.0007(10) -0.0034(10) 0.0067(10) C14 0.0160(12) 0.0286(14) 0.0266(14) -0.0006(11) -0.0033(10) 0.0061(10) C15 0.0193(12) 0.0278(13) 0.0251(14) -0.0019(11) 0.0020(10) 0.0065(10) C16 0.0184(12) 0.0274(14) 0.0289(15) -0.0025(11) -0.0015(11) 0.0042(10) C17 0.0326(16) 0.0438(18) 0.0341(17) 0.0028(14) 0.0077(13) 0.0129(13) C18 0.0252(14) 0.0353(16) 0.0274(15) 0.0085(12) 0.0069(11) 0.0000(11) C19 0.056(2) 0.052(2) 0.035(2) 0.0059(16) -0.0018(17) 0.0028(18) C20 0.051(2) 0.052(2) 0.060(3) 0.001(2) -0.0031(19) -0.0115(18) C21 0.062(3) 0.044(2) 0.061(3) 0.0093(19) 0.021(2) -0.0063(18) _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 O13 1.9411(19) . ? Zn1 O9 1.945(2) 2_355 ? Zn1 O2 1.985(2) . ? Zn1 O7 2.001(2) 2_455 ? Zn1 Zn2 3.1566(10) 2_455 ? Zn2 O4 1.989(2) 2_465 ? Zn2 O8 2.082(2) . ? Zn2 O1 2.087(2) 2_455 ? Zn2 O13 2.092(2) . ? Zn2 O13 2.096(2) 2_455 ? Zn2 O14 2.266(3) . ? Zn2 Zn1 3.1566(10) 2_455 ? O1 C7 1.248(4) . ? O1 Zn2 2.087(2) 2_455 ? O2 C7 1.260(4) . ? O3 C8 1.233(4) . ? O4 C8 1.263(3) . ? O4 Zn2 1.989(2) 2_465 ? O5 N1 1.198(4) . ? O6 N1 1.211(4) . ? O7 C15 1.269(3) . ? O7 Zn1 2.001(2) 2_455 ? O8 C15 1.233(4) . ? O9 C16 1.265(4) . ? O9 Zn1 1.945(2) 2_355 ? O10 C16 1.229(4) . ? O11 N2 1.220(4) . ? O12 N2 1.226(3) . ? O13 Zn2 2.096(2) 2_455 ? N1 C5 1.478(4) . ? N2 C13 1.458(4) . ? N3 C21 1.389(6) . ? N3 C17 1.418(5) . ? N4 C17 1.301(5) . ? N4 H4A 0.8600 . ? N4 H4B 0.8600 . ? C1 C6 1.392(4) . ? C1 C2 1.396(4) . ? C1 C7 1.495(4) . ? C2 C3 1.390(4) . ? C2 H2A 0.9300 . ? C3 C4 1.380(4) . ? C3 C8 1.517(4) . ? C4 C5 1.381(4) . ? C4 H4C 0.9300 . ? C5 C6 1.370(4) . ? C6 H6A 0.9300 . ? C9 C14 1.391(4) . ? C9 C10 1.392(4) . ? C9 C15 1.508(4) . ? C10 C11 1.396(4) . ? C10 H10A 0.9300 . ? C11 C12 1.379(4) . ? C11 C16 1.507(4) . ? C12 C13 1.384(4) . ? C12 H12A 0.9300 . ? C13 C14 1.385(4) . ? C14 H14A 0.9300 . ? C17 C18 1.341(5) . ? C18 C19 1.353(5) . ? C18 H18A 0.9300 . ? C19 C20 1.349(6) . ? C19 H19A 0.9300 . ? C20 C21 1.380(6) . ? C20 H20A 0.9300 . ? C21 H21A 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 O13 Zn1 O9 108.23(9) . 2_355 ? O13 Zn1 O2 116.71(10) . . ? O9 Zn1 O2 111.53(10) 2_355 . ? O13 Zn1 O7 106.71(9) . 2_455 ? O9 Zn1 O7 115.59(10) 2_355 2_455 ? O2 Zn1 O7 97.97(10) . 2_455 ? O13 Zn1 Zn2 40.35(6) . 2_455 ? O9 Zn1 Zn2 148.49(7) 2_355 2_455 ? O2 Zn1 Zn2 88.43(7) . 2_455 ? O7 Zn1 Zn2 83.72(6) 2_455 2_455 ? O4 Zn2 O8 95.76(10) 2_465 . ? O4 Zn2 O1 158.12(9) 2_465 2_455 ? O8 Zn2 O1 89.19(10) . 2_455 ? O4 Zn2 O13 90.54(9) 2_465 . ? O8 Zn2 O13 172.17(8) . . ? O1 Zn2 O13 86.66(9) 2_455 . ? O4 Zn2 O13 106.90(9) 2_465 2_455 ? O8 Zn2 O13 92.56(8) . 2_455 ? O1 Zn2 O13 94.10(9) 2_455 2_455 ? O13 Zn2 O13 81.13(8) . 2_455 ? O4 Zn2 O14 80.10(10) 2_465 . ? O8 Zn2 O14 89.73(11) . . ? O1 Zn2 O14 78.63(10) 2_455 . ? O13 Zn2 O14 95.96(11) . . ? O13 Zn2 O14 172.36(9) 2_455 . ? O4 Zn2 Zn1 136.24(7) 2_465 2_455 ? O8 Zn2 Zn1 70.43(6) . 2_455 ? O1 Zn2 Zn1 65.38(7) 2_455 2_455 ? O13 Zn2 Zn1 101.78(6) . 2_455 ? O13 Zn2 Zn1 36.85(5) 2_455 2_455 ? O14 Zn2 Zn1 138.42(9) . 2_455 ? C7 O1 Zn2 143.9(2) . 2_455 ? C7 O2 Zn1 116.15(19) . . ? C8 O4 Zn2 124.71(19) . 2_465 ? C15 O7 Zn1 120.2(2) . 2_455 ? C15 O8 Zn2 135.0(2) . . ? C16 O9 Zn1 116.67(19) . 2_355 ? Zn1 O13 Zn2 119.91(10) . . ? Zn1 O13 Zn2 102.80(9) . 2_455 ? Zn2 O13 Zn2 98.87(8) . 2_455 ? O5 N1 O6 122.8(3) . . ? O5 N1 C5 119.1(3) . . ? O6 N1 C5 118.1(3) . . ? O11 N2 O12 123.4(3) . . ? O11 N2 C13 118.4(3) . . ? O12 N2 C13 118.2(3) . . ? C21 N3 C17 118.6(4) . . ? C17 N4 H4A 120.0 . . ? C17 N4 H4B 120.0 . . ? H4A N4 H4B 120.0 . . ? C6 C1 C2 119.4(3) . . ? C6 C1 C7 119.3(3) . . ? C2 C1 C7 121.3(3) . . ? C3 C2 C1 120.5(3) . . ? C3 C2 H2A 119.8 . . ? C1 C2 H2A 119.8 . . ? C4 C3 C2 120.1(3) . . ? C4 C3 C8 120.1(2) . . ? C2 C3 C8 119.8(3) . . ? C3 C4 C5 118.4(3) . . ? C3 C4 H4C 120.8 . . ? C5 C4 H4C 120.8 . . ? C6 C5 C4 122.9(3) . . ? C6 C5 N1 118.4(3) . . ? C4 C5 N1 118.7(3) . . ? C5 C6 C1 118.7(3) . . ? C5 C6 H6A 120.7 . . ? C1 C6 H6A 120.7 . . ? O1 C7 O2 126.0(3) . . ? O1 C7 C1 116.5(3) . . ? O2 C7 C1 117.5(3) . . ? O3 C8 O4 126.2(3) . . ? O3 C8 C3 119.0(3) . . ? O4 C8 C3 114.8(2) . . ? C14 C9 C10 120.1(3) . . ? C14 C9 C15 121.9(2) . . ? C10 C9 C15 117.9(2) . . ? C9 C10 C11 120.4(3) . . ? C9 C10 H10A 119.8 . . ? C11 C10 H10A 119.8 . . ? C12 C11 C10 119.7(2) . . ? C12 C11 C16 120.2(2) . . ? C10 C11 C16 120.0(2) . . ? C11 C12 C13 119.0(3) . . ? C11 C12 H12A 120.5 . . ? C13 C12 H12A 120.5 . . ? C12 C13 C14 122.5(3) . . ? C12 C13 N2 118.1(3) . . ? C14 C13 N2 119.3(2) . . ? C13 C14 C9 118.1(2) . . ? C13 C14 H14A 121.0 . . ? C9 C14 H14A 121.0 . . ? O8 C15 O7 127.2(3) . . ? O8 C15 C9 116.9(2) . . ? O7 C15 C9 115.9(2) . . ? O10 C16 O9 124.7(3) . . ? O10 C16 C11 119.0(3) . . ? O9 C16 C11 116.2(2) . . ? N4 C17 C18 119.7(3) . . ? N4 C17 N3 123.2(4) . . ? C18 C17 N3 117.1(3) . . ? C17 C18 C19 124.0(3) . . ? C17 C18 H18A 118.0 . . ? C19 C18 H18A 118.0 . . ? C20 C19 C18 120.3(4) . . ? C20 C19 H19A 119.9 . . ? C18 C19 H19A 119.9 . . ? C19 C20 C21 118.7(4) . . ? C19 C20 H20A 120.7 . . ? C21 C20 H20A 120.7 . . ? C20 C21 N3 121.3(4) . . ? C20 C21 H21A 119.4 . . ? N3 C21 H21A 119.4 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N4 H4A O10 0.86 2.08 2.811(4) 142.0 2_346 N4 H4B O3 0.86 1.92 2.769(4) 169.8 2_455 C18 H18A O10 0.93 1.97 2.778(4) 144.8 2_346 C18 H18A O7 0.93 2.63 3.209(4) 120.9 2_446 C20 H20A O6 0.93 2.63 3.310(6) 130.6 2_556 _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.910 _refine_diff_density_min -0.961 _refine_diff_density_rms 0.187 # = = = END data_4 _database_code_depnum_ccdc_archive 'CCDC 843813' #TrackingRef 'CCDC-compounds.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H24 N6 O28 Zn5' _chemical_formula_weight 1327.57 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 Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.2062(6) _cell_length_b 14.1995(7) _cell_length_c 15.5626(8) _cell_angle_alpha 65.057(2) _cell_angle_beta 82.427(2) _cell_angle_gamma 66.150(2) _cell_volume 2234.46(19) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7850 _cell_measurement_theta_min 2.04 _cell_measurement_theta_max 25.01 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.973 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1324 _exptl_absorpt_coefficient_mu 2.754 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5345 _exptl_absorpt_correction_T_max 0.6370 _exptl_absorpt_process_details 'Higashi (1995)' _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 '\f and \w scans' _diffrn_detector_area_resol_mean 'Bruker SMART CCD area' _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 24035 _diffrn_reflns_av_R_equivalents 0.0214 _diffrn_reflns_av_sigmaI/netI 0.0226 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 25.01 _reflns_number_total 7850 _reflns_number_gt 7015 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SMART (Bruker, 1997)' _computing_data_reduction 'SAINT (Bruker, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXP97 (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Bruker, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0324P)^2^+1.7433P] 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 0 _refine_ls_number_reflns 7850 _refine_ls_number_parameters 705 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0288 _refine_ls_R_factor_gt 0.0246 _refine_ls_wR_factor_ref 0.0644 _refine_ls_wR_factor_gt 0.0623 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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 0.80441(2) 0.06861(2) 0.13238(2) 0.02348(7) Uani 1 1 d . . . Zn2 Zn 0.63498(2) 0.16064(2) -0.098456(19) 0.02376(7) Uani 1 1 d . . . Zn3 Zn 0.07246(2) -0.04997(2) 0.098438(19) 0.02308(7) Uani 1 1 d . . . Zn4 Zn 0.57041(2) 0.44203(2) -0.399453(19) 0.02135(7) Uani 1 1 d . . . Zn5 Zn 0.53030(2) 0.29164(2) 0.47516(2) 0.02275(7) Uani 1 1 d . . . O1 O 0.85803(16) 0.10883(16) 0.22075(14) 0.0374(4) Uani 1 1 d . . . O2 O 1.04137(17) -0.01742(16) 0.22027(14) 0.0388(5) Uani 1 1 d . . . O3 O 1.33405(18) -0.15402(16) 0.46697(15) 0.0463(5) Uani 1 1 d . . . O4 O 1.3369(2) -0.04512(19) 0.5336(2) 0.0627(7) Uani 1 1 d . . . O5 O 0.92238(19) 0.23614(17) 0.53983(15) 0.0451(5) Uani 1 1 d . . . O6 O 0.81267(18) 0.32589(17) 0.40965(17) 0.0481(5) Uani 1 1 d . . . O7 O 0.80497(16) -0.08100(14) 0.20665(13) 0.0345(4) Uani 1 1 d . . . O8 O 0.98494(16) -0.16632(14) 0.15938(13) 0.0343(4) Uani 1 1 d . . . O9 O 0.61922(15) -0.29759(14) 0.46060(13) 0.0325(4) Uani 1 1 d . . . O10 O 0.70154(15) -0.48637(14) 0.52526(12) 0.0286(4) Uani 1 1 d . . . O11 O 1.10803(19) -0.67036(16) 0.43040(17) 0.0526(6) Uani 1 1 d . . . O12 O 1.18256(19) -0.57223(18) 0.31147(18) 0.0562(6) Uani 1 1 d . . . O13 O 0.53754(17) 0.26392(16) -0.03967(13) 0.0376(5) Uani 1 1 d . . . O14 O 0.64082(17) 0.17675(17) 0.09789(15) 0.0456(5) Uani 1 1 d . . . O15 O 0.50456(18) 0.32699(15) 0.34127(13) 0.0375(4) Uani 1 1 d . . . O16 O 0.41485(17) 0.51531(15) 0.28881(13) 0.0346(4) Uani 1 1 d . . . O17 O 0.1457(2) 0.68908(17) 0.00450(18) 0.0577(6) Uani 1 1 d . . . O18 O 0.1830(2) 0.6114(2) -0.09332(19) 0.0739(8) Uani 1 1 d . . . O19 O 0.43432(15) 0.38941(14) -0.32045(12) 0.0306(4) Uani 1 1 d . . . O20 O 0.54462(15) 0.21722(14) -0.21794(12) 0.0274(4) Uani 1 1 d . . . O21 O 0.34386(16) -0.00580(14) 0.01820(14) 0.0398(5) Uani 1 1 d . . . O22 O 0.15126(16) 0.07312(15) 0.04462(15) 0.0412(5) Uani 1 1 d . . . O23 O -0.0355(2) 0.4904(2) -0.0925(2) 0.0811(10) Uani 1 1 d . . . O24 O 0.03493(19) 0.58086(16) -0.21872(17) 0.0514(6) Uani 1 1 d . . . O25 O 0.91329(15) 0.07717(15) 0.02947(12) 0.0237(4) Uani 1 1 d . . . O26 O 0.77642(18) 0.1843(2) -0.15017(16) 0.0314(5) Uani 1 1 d . . . O27 O 0.71821(19) 0.29436(17) -0.34434(17) 0.0383(5) Uani 1 1 d . . . O28 O 0.56786(16) 0.40999(13) 0.48023(12) 0.0209(4) Uani 1 1 d . . . N1 N 0.8995(2) 0.24848(18) 0.46057(18) 0.0328(5) Uani 1 1 d . . . N2 N 1.10467(19) -0.58077(18) 0.36864(17) 0.0332(5) Uani 1 1 d . . . N3 N 0.2058(2) 0.61405(19) -0.02149(18) 0.0399(6) Uani 1 1 d . . . N4 N 0.0419(2) 0.49514(19) -0.14996(19) 0.0386(6) Uani 1 1 d . . . N5 N 0.4883(3) 0.0938(2) 0.3471(2) 0.0553(7) Uani 1 1 d . . . H5A H 0.5253 0.1051 0.3828 0.066 Uiso 1 1 calc R . . N6 N 0.2138(4) 0.2345(4) 0.2084(4) 0.1246(18) Uani 1 1 d . . . H6A H 0.1769 0.2236 0.1723 0.150 Uiso 1 1 calc R . . H6B H 0.1818 0.2951 0.2182 0.150 Uiso 1 1 calc R . . C1 C 1.0107(2) 0.0725(2) 0.32247(18) 0.0258(5) Uani 1 1 d . . . C2 C 1.1249(2) 0.0022(2) 0.36517(18) 0.0276(5) Uani 1 1 d . . . H2A H 1.1741 -0.0536 0.3448 0.033 Uiso 1 1 calc R . . C3 C 1.1668(2) 0.0136(2) 0.43740(18) 0.0265(5) Uani 1 1 d . . . C4 C 1.0939(2) 0.0956(2) 0.46865(18) 0.0277(5) Uani 1 1 d . . . H4A H 1.1199 0.1042 0.5174 0.033 Uiso 1 1 calc R . . C5 C 0.9804(2) 0.1646(2) 0.42499(19) 0.0270(5) Uani 1 1 d . . . C6 C 0.9373(2) 0.1558(2) 0.35250(18) 0.0280(5) Uani 1 1 d . . . H6C H 0.8611 0.2043 0.3245 0.034 Uiso 1 1 calc R . . C7 C 0.9674(2) 0.0535(2) 0.24813(18) 0.0287(6) Uani 1 1 d . . . C8 C 1.2899(2) -0.0671(2) 0.48437(19) 0.0316(6) Uani 1 1 d . . . C9 C 0.9022(2) -0.2777(2) 0.28543(17) 0.0250(5) Uani 1 1 d . . . C10 C 0.8076(2) -0.2850(2) 0.34407(17) 0.0251(5) Uani 1 1 d . . . H10A H 0.7420 -0.2193 0.3384 0.030 Uiso 1 1 calc R . . C11 C 0.8082(2) -0.38749(19) 0.41097(17) 0.0228(5) Uani 1 1 d . . . C12 C 0.9067(2) -0.4862(2) 0.42035(17) 0.0250(5) Uani 1 1 d . . . H12A H 0.9090 -0.5560 0.4647 0.030 Uiso 1 1 calc R . . C13 C 1.0009(2) -0.4772(2) 0.36158(18) 0.0260(5) Uani 1 1 d . . . C14 C 1.0015(2) -0.3759(2) 0.29444(18) 0.0273(5) Uani 1 1 d . . . H14A H 1.0664 -0.3731 0.2562 0.033 Uiso 1 1 calc R . . C15 C 0.8988(2) -0.1668(2) 0.21135(18) 0.0258(5) Uani 1 1 d . . . C16 C 0.7016(2) -0.3925(2) 0.47127(17) 0.0239(5) Uani 1 1 d . . . C17 C 0.4781(2) 0.3481(2) 0.06927(17) 0.0239(5) Uani 1 1 d . . . C18 C 0.5006(2) 0.3457(2) 0.15546(17) 0.0253(5) Uani 1 1 d . . . H18A H 0.5651 0.2858 0.1949 0.030 Uiso 1 1 calc R . . C19 C 0.4286(2) 0.4308(2) 0.18381(17) 0.0259(5) Uani 1 1 d . . . C20 C 0.3322(2) 0.5205(2) 0.12464(18) 0.0291(6) Uani 1 1 d . . . H20A H 0.2838 0.5793 0.1418 0.035 Uiso 1 1 calc R . . C21 C 0.3100(2) 0.5205(2) 0.03988(18) 0.0276(5) Uani 1 1 d . . . C22 C 0.3810(2) 0.4366(2) 0.01044(18) 0.0266(5) Uani 1 1 d . . . H22A H 0.3644 0.4391 -0.0473 0.032 Uiso 1 1 calc R . . C23 C 0.4506(2) 0.4252(2) 0.27910(18) 0.0286(6) Uani 1 1 d . . . C24 C 0.5593(2) 0.2560(2) 0.04000(18) 0.0260(5) Uani 1 1 d . . . C25 C 0.3421(2) 0.30103(19) -0.18420(17) 0.0233(5) Uani 1 1 d . . . C26 C 0.3431(2) 0.1979(2) -0.11621(17) 0.0245(5) Uani 1 1 d . . . H26B H 0.4103 0.1325 -0.1083 0.029 Uiso 1 1 calc R . . C27 C 0.2460(2) 0.1910(2) -0.06015(17) 0.0243(5) Uani 1 1 d . . . C28 C 0.1466(2) 0.2894(2) -0.06989(19) 0.0287(6) Uani 1 1 d . . . H28B H 0.0809 0.2869 -0.0326 0.034 Uiso 1 1 calc R . . C29 C 0.1487(2) 0.3908(2) -0.13673(19) 0.0279(5) Uani 1 1 d . . . C30 C 0.2433(2) 0.3994(2) -0.19513(18) 0.0259(5) Uani 1 1 d . . . H30A H 0.2406 0.4689 -0.2403 0.031 Uiso 1 1 calc R . . C31 C 0.4479(2) 0.30405(19) -0.24592(17) 0.0226(5) Uani 1 1 d . . . C32 C 0.2452(2) 0.0779(2) 0.00664(17) 0.0247(5) Uani 1 1 d . . . C33 C 0.3824(3) 0.1690(3) 0.3111(3) 0.0576(9) Uani 1 1 d . . . H33A H 0.3477 0.2308 0.3269 0.069 Uiso 1 1 calc R . . C34 C 0.3201(3) 0.1581(3) 0.2488(3) 0.0648(11) Uani 1 1 d . . . C35 C 0.3747(4) 0.0588(4) 0.2343(3) 0.0776(12) Uani 1 1 d . . . H35A H 0.3363 0.0452 0.1956 0.093 Uiso 1 1 calc R . . C36 C 0.4834(4) -0.0178(4) 0.2764(4) 0.0993(18) Uani 1 1 d . . . H36A H 0.5184 -0.0843 0.2673 0.119 Uiso 1 1 calc R . . C37 C 0.5417(4) 0.0015(4) 0.3318(4) 0.0882(15) Uani 1 1 d . . . H37A H 0.6179 -0.0495 0.3584 0.106 Uiso 1 1 calc R . . H25 H 0.920(3) 0.126(3) 0.014(3) 0.050(12) Uiso 1 1 d . . . H26A H 0.781(4) 0.218(4) -0.148(4) 0.07(2) Uiso 1 1 d . . . H27A H 0.737(4) 0.258(4) -0.293(4) 0.095(17) Uiso 1 1 d . . . H28A H 0.623(3) 0.408(2) 0.462(2) 0.028(9) Uiso 1 1 d . . . H27B H 0.776(4) 0.288(4) -0.372(3) 0.087(17) 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 Zn1 0.02107(14) 0.02057(14) 0.02256(15) -0.00828(12) 0.00245(11) -0.00314(11) Zn2 0.02374(14) 0.02119(14) 0.02016(15) -0.00766(11) 0.00260(11) -0.00415(11) Zn3 0.01965(14) 0.02186(14) 0.02171(15) -0.00662(12) 0.00334(11) -0.00545(11) Zn4 0.02564(14) 0.01899(14) 0.01748(14) -0.00782(11) 0.00135(11) -0.00650(11) Zn5 0.02590(15) 0.01788(14) 0.02247(15) -0.00977(11) 0.00122(11) -0.00498(11) O1 0.0332(10) 0.0435(11) 0.0384(11) -0.0237(9) -0.0036(8) -0.0086(9) O2 0.0426(11) 0.0400(11) 0.0332(11) -0.0243(9) -0.0014(9) -0.0047(9) O3 0.0452(12) 0.0288(10) 0.0507(13) -0.0192(10) -0.0164(10) 0.0079(9) O4 0.0491(13) 0.0536(14) 0.0895(19) -0.0421(14) -0.0321(13) 0.0004(11) O5 0.0530(13) 0.0478(12) 0.0440(13) -0.0328(11) 0.0153(10) -0.0176(10) O6 0.0335(11) 0.0404(12) 0.0629(15) -0.0304(11) 0.0048(10) 0.0018(9) O7 0.0299(10) 0.0243(9) 0.0391(11) -0.0064(8) 0.0081(8) -0.0097(8) O8 0.0366(10) 0.0273(9) 0.0370(11) -0.0101(8) 0.0151(8) -0.0177(8) O9 0.0297(9) 0.0268(9) 0.0391(11) -0.0142(8) 0.0118(8) -0.0112(8) O10 0.0289(9) 0.0268(9) 0.0258(9) -0.0051(8) 0.0055(7) -0.0138(7) O11 0.0512(13) 0.0242(10) 0.0612(15) -0.0077(10) 0.0102(11) -0.0069(9) O12 0.0387(12) 0.0405(12) 0.0729(17) -0.0207(11) 0.0253(11) -0.0091(9) O13 0.0418(11) 0.0360(10) 0.0290(10) -0.0224(9) -0.0013(8) 0.0009(8) O14 0.0289(10) 0.0465(12) 0.0428(12) -0.0229(10) -0.0108(9) 0.0118(9) O15 0.0527(12) 0.0336(10) 0.0245(10) -0.0144(9) -0.0028(9) -0.0110(9) O16 0.0475(11) 0.0369(10) 0.0272(10) -0.0208(9) 0.0036(8) -0.0159(9) O17 0.0559(14) 0.0275(11) 0.0757(17) -0.0264(11) -0.0072(12) 0.0058(10) O18 0.0769(18) 0.0572(15) 0.0605(17) -0.0284(13) -0.0390(14) 0.0170(13) O19 0.0313(9) 0.0285(9) 0.0224(9) -0.0006(8) 0.0014(7) -0.0130(8) O20 0.0270(9) 0.0289(9) 0.0213(9) -0.0088(7) 0.0007(7) -0.0076(7) O21 0.0309(10) 0.0228(9) 0.0441(12) -0.0001(8) 0.0086(9) -0.0064(8) O22 0.0319(10) 0.0260(9) 0.0572(13) -0.0098(9) 0.0140(9) -0.0142(8) O23 0.0583(15) 0.0414(13) 0.102(2) -0.0172(14) 0.0413(16) -0.0040(11) O24 0.0490(13) 0.0242(10) 0.0588(15) -0.0055(10) -0.0026(11) -0.0035(9) O25 0.0255(9) 0.0179(9) 0.0221(9) -0.0065(7) 0.0049(7) -0.0060(7) O26 0.0245(10) 0.0265(10) 0.0344(12) -0.0082(9) 0.0015(8) -0.0060(8) O27 0.0343(11) 0.0319(11) 0.0232(11) -0.0026(9) 0.0048(9) 0.0012(8) O28 0.0207(9) 0.0206(8) 0.0215(9) -0.0105(7) 0.0054(7) -0.0073(7) N1 0.0310(12) 0.0311(12) 0.0432(15) -0.0236(11) 0.0139(11) -0.0132(10) N2 0.0288(12) 0.0280(12) 0.0425(14) -0.0169(11) 0.0033(10) -0.0084(9) N3 0.0400(13) 0.0273(12) 0.0423(15) -0.0140(11) -0.0071(11) -0.0011(10) N4 0.0313(12) 0.0278(12) 0.0515(16) -0.0157(12) 0.0020(11) -0.0069(10) N5 0.0527(17) 0.0635(18) 0.0618(19) -0.0322(16) -0.0017(14) -0.0254(15) N6 0.077(3) 0.096(3) 0.136(4) -0.018(3) -0.018(3) 0.005(2) C1 0.0289(13) 0.0243(12) 0.0253(13) -0.0111(11) 0.0028(10) -0.0106(10) C2 0.0312(13) 0.0206(12) 0.0294(14) -0.0136(11) 0.0041(11) -0.0058(10) C3 0.0285(13) 0.0205(12) 0.0293(14) -0.0099(11) 0.0009(10) -0.0085(10) C4 0.0337(14) 0.0260(12) 0.0273(14) -0.0131(11) 0.0028(11) -0.0133(11) C5 0.0288(13) 0.0215(12) 0.0332(14) -0.0157(11) 0.0082(11) -0.0093(10) C6 0.0248(12) 0.0251(12) 0.0315(14) -0.0125(11) 0.0032(10) -0.0066(10) C7 0.0357(15) 0.0255(13) 0.0230(13) -0.0076(11) 0.0023(11) -0.0126(11) C8 0.0313(14) 0.0245(13) 0.0330(15) -0.0106(11) -0.0007(11) -0.0057(11) C9 0.0266(12) 0.0248(12) 0.0239(13) -0.0081(10) 0.0025(10) -0.0126(10) C10 0.0258(12) 0.0220(12) 0.0265(13) -0.0089(10) 0.0024(10) -0.0096(10) C11 0.0240(12) 0.0232(12) 0.0232(13) -0.0097(10) 0.0019(10) -0.0111(10) C12 0.0304(13) 0.0221(12) 0.0224(13) -0.0059(10) 0.0010(10) -0.0134(10) C13 0.0234(12) 0.0234(12) 0.0288(14) -0.0105(11) -0.0005(10) -0.0064(10) C14 0.0266(13) 0.0277(13) 0.0270(13) -0.0100(11) 0.0058(10) -0.0126(10) C15 0.0289(13) 0.0258(13) 0.0244(13) -0.0080(11) 0.0011(10) -0.0145(11) C16 0.0277(13) 0.0269(13) 0.0204(12) -0.0100(11) 0.0018(10) -0.0135(10) C17 0.0230(12) 0.0265(12) 0.0237(13) -0.0132(10) 0.0041(10) -0.0086(10) C18 0.0249(12) 0.0302(13) 0.0211(13) -0.0118(11) -0.0001(10) -0.0091(10) C19 0.0329(13) 0.0286(13) 0.0204(13) -0.0125(11) 0.0045(10) -0.0143(11) C20 0.0351(14) 0.0265(13) 0.0290(14) -0.0174(11) 0.0084(11) -0.0106(11) C21 0.0274(13) 0.0207(12) 0.0291(14) -0.0091(11) -0.0013(11) -0.0044(10) C22 0.0312(13) 0.0291(13) 0.0211(13) -0.0138(11) -0.0001(10) -0.0091(10) C23 0.0328(14) 0.0362(15) 0.0238(13) -0.0173(12) 0.0066(11) -0.0164(11) C24 0.0217(12) 0.0302(13) 0.0265(14) -0.0154(11) 0.0037(10) -0.0073(10) C25 0.0266(12) 0.0228(12) 0.0210(12) -0.0066(10) -0.0009(10) -0.0118(10) C26 0.0264(12) 0.0222(12) 0.0225(13) -0.0068(10) -0.0004(10) -0.0090(10) C27 0.0257(12) 0.0247(12) 0.0223(13) -0.0068(10) -0.0011(10) -0.0118(10) C28 0.0273(13) 0.0281(13) 0.0299(14) -0.0107(11) 0.0045(11) -0.0122(10) C29 0.0261(13) 0.0213(12) 0.0331(14) -0.0104(11) -0.0031(11) -0.0055(10) C30 0.0297(13) 0.0200(12) 0.0252(13) -0.0045(10) -0.0029(10) -0.0105(10) C31 0.0276(12) 0.0233(12) 0.0189(12) -0.0066(10) -0.0024(10) -0.0127(10) C32 0.0253(13) 0.0247(12) 0.0227(13) -0.0083(10) 0.0002(10) -0.0096(10) C33 0.062(2) 0.0448(19) 0.074(3) -0.0297(18) 0.0153(19) -0.0262(17) C34 0.0387(18) 0.056(2) 0.069(3) -0.0014(19) -0.0047(17) -0.0129(16) C35 0.082(3) 0.086(3) 0.076(3) -0.049(3) -0.016(2) -0.021(2) C36 0.092(3) 0.084(3) 0.134(5) -0.080(3) -0.032(3) 0.003(3) C37 0.065(3) 0.095(3) 0.121(4) -0.081(3) -0.021(3) 0.001(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 Zn1 O14 1.9342(18) . ? Zn1 O25 1.9369(17) . ? Zn1 O7 1.9411(17) . ? Zn1 O1 1.9616(19) . ? Zn1 Zn3 3.1078(4) 1_655 ? Zn1 H25 2.24(4) . ? Zn2 O26 1.901(2) . ? Zn2 O21 1.9417(17) 2_655 ? Zn2 O13 1.9587(18) . ? Zn2 O20 1.9707(17) . ? Zn2 Zn3 3.2686(4) 2_655 ? Zn2 H26A 2.17(5) . ? Zn3 O26 1.985(2) 2_655 ? Zn3 O25 2.0651(17) 1_455 ? Zn3 O2 2.0880(19) 1_455 ? Zn3 O22 2.1433(17) . ? Zn3 O8 2.1469(16) 1_455 ? Zn3 O25 2.1551(18) 2_655 ? Zn3 Zn1 3.1078(4) 1_455 ? Zn3 Zn3 3.2034(6) 2 ? Zn3 Zn2 3.2686(4) 2_655 ? Zn4 O27 2.054(2) . ? Zn4 O28 2.0754(17) 2_665 ? Zn4 O16 2.1008(18) 2_665 ? Zn4 O28 2.1117(17) 1_554 ? Zn4 O19 2.1260(17) . ? Zn4 O10 2.1875(16) 1_564 ? Zn4 Zn5 3.1726(4) 2_665 ? Zn4 Zn4 3.2004(6) 2_664 ? Zn5 O3 1.9140(18) 2_756 ? Zn5 O28 1.9456(17) . ? Zn5 O9 1.9501(17) 2_656 ? Zn5 O15 1.9634(18) . ? Zn5 Zn4 3.1726(4) 2_665 ? O1 C7 1.265(3) . ? O2 C7 1.243(3) . ? O2 Zn3 2.0880(19) 1_655 ? O3 C8 1.262(3) . ? O3 Zn5 1.9140(18) 2_756 ? O4 C8 1.215(3) . ? O5 N1 1.225(3) . ? O6 N1 1.226(3) . ? O7 C15 1.273(3) . ? O8 C15 1.239(3) . ? O8 Zn3 2.1469(16) 1_655 ? O9 C16 1.270(3) . ? O9 Zn5 1.9501(17) 2_656 ? O10 C16 1.240(3) . ? O10 Zn4 2.1875(16) 1_546 ? O11 N2 1.217(3) . ? O12 N2 1.220(3) . ? O13 C24 1.251(3) . ? O14 C24 1.243(3) . ? O15 C23 1.266(3) . ? O16 C23 1.243(3) . ? O16 Zn4 2.1008(18) 2_665 ? O17 N3 1.221(3) . ? O18 N3 1.206(3) . ? O19 C31 1.243(3) . ? O20 C31 1.268(3) . ? O21 C32 1.270(3) . ? O21 Zn2 1.9417(17) 2_655 ? O22 C32 1.233(3) . ? O23 N4 1.214(3) . ? O24 N4 1.215(3) . ? O25 Zn3 2.0651(17) 1_655 ? O25 Zn3 2.1551(18) 2_655 ? O25 H25 0.67(3) . ? O26 Zn3 1.985(2) 2_655 ? O26 H26A 0.52(4) . ? O27 H27A 0.75(5) . ? O27 H27B 0.76(5) . ? O28 Zn4 2.0754(17) 2_665 ? O28 Zn4 2.1117(17) 1_556 ? O28 H28A 0.69(3) . ? N1 C5 1.470(3) . ? N2 C13 1.474(3) . ? N3 C21 1.476(3) . ? N4 C29 1.480(3) . ? N5 C33 1.302(4) . ? N5 C37 1.316(5) . ? N5 H5A 0.8600 . ? N6 C34 1.326(5) . ? N6 H6A 0.8600 . ? N6 H6B 0.8600 . ? C1 C6 1.385(3) . ? C1 C2 1.393(3) . ? C1 C7 1.494(4) . ? C2 C3 1.387(4) . ? C2 H2A 0.9300 . ? C3 C4 1.382(4) . ? C3 C8 1.515(3) . ? C4 C5 1.389(4) . ? C4 H4A 0.9300 . ? C5 C6 1.376(4) . ? C6 H6C 0.9300 . ? C9 C10 1.384(3) . ? C9 C14 1.395(3) . ? C9 C15 1.496(3) . ? C10 C11 1.385(3) . ? C10 H10A 0.9300 . ? C11 C12 1.393(3) . ? C11 C16 1.509(3) . ? C12 C13 1.385(3) . ? C12 H12A 0.9300 . ? C13 C14 1.378(3) . ? C14 H14A 0.9300 . ? C17 C18 1.388(3) . ? C17 C22 1.390(3) . ? C17 C24 1.495(3) . ? C18 C19 1.385(3) . ? C18 H18A 0.9300 . ? C19 C20 1.392(4) . ? C19 C23 1.505(3) . ? C20 C21 1.381(4) . ? C20 H20A 0.9300 . ? C21 C22 1.379(3) . ? C22 H22A 0.9300 . ? C25 C30 1.388(3) . ? C25 C26 1.395(3) . ? C25 C31 1.508(3) . ? C26 C27 1.388(3) . ? C26 H26B 0.9300 . ? C27 C28 1.394(3) . ? C27 C32 1.504(3) . ? C28 C29 1.383(3) . ? C28 H28B 0.9300 . ? C29 C30 1.385(4) . ? C30 H30A 0.9300 . ? C33 C34 1.399(6) . ? C33 H33A 0.9300 . ? C34 C35 1.397(6) . ? C35 C36 1.354(6) . ? C35 H35A 0.9300 . ? C36 C37 1.358(6) . ? C36 H36A 0.9300 . ? C37 H37A 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 O14 Zn1 O25 115.58(8) . . ? O14 Zn1 O7 109.48(9) . . ? O25 Zn1 O7 114.29(8) . . ? O14 Zn1 O1 103.25(8) . . ? O25 Zn1 O1 107.41(8) . . ? O7 Zn1 O1 105.73(8) . . ? O14 Zn1 Zn3 156.15(7) . 1_655 ? O25 Zn1 Zn3 40.57(5) . 1_655 ? O7 Zn1 Zn3 86.92(5) . 1_655 ? O1 Zn1 Zn3 88.06(6) . 1_655 ? O14 Zn1 H25 108.1(9) . . ? O25 Zn1 H25 16.4(9) . . ? O7 Zn1 H25 130.1(9) . . ? O1 Zn1 H25 96.3(9) . . ? Zn3 Zn1 H25 49.1(9) 1_655 . ? O26 Zn2 O21 115.97(9) . 2_655 ? O26 Zn2 O13 113.24(10) . . ? O21 Zn2 O13 111.91(8) 2_655 . ? O26 Zn2 O20 98.73(9) . . ? O21 Zn2 O20 111.57(8) 2_655 . ? O13 Zn2 O20 103.99(7) . . ? O26 Zn2 Zn3 33.54(7) . 2_655 ? O21 Zn2 Zn3 82.77(5) 2_655 2_655 ? O13 Zn2 Zn3 127.01(6) . 2_655 ? O20 Zn2 Zn3 117.59(5) . 2_655 ? O26 Zn2 H26A 12.4(13) . . ? O21 Zn2 H26A 124.3(13) 2_655 . ? O13 Zn2 H26A 100.9(13) . . ? O20 Zn2 H26A 101.9(14) . . ? Zn3 Zn2 H26A 41.9(13) 2_655 . ? O26 Zn3 O25 170.04(9) 2_655 1_455 ? O26 Zn3 O2 95.05(9) 2_655 1_455 ? O25 Zn3 O2 94.00(7) 1_455 1_455 ? O26 Zn3 O22 96.82(9) 2_655 . ? O25 Zn3 O22 87.88(7) 1_455 . ? O2 Zn3 O22 86.38(8) 1_455 . ? O26 Zn3 O8 85.58(9) 2_655 1_455 ? O25 Zn3 O8 90.37(7) 1_455 1_455 ? O2 Zn3 O8 89.44(8) 1_455 1_455 ? O22 Zn3 O8 175.35(7) . 1_455 ? O26 Zn3 O25 89.51(9) 2_655 2_655 ? O25 Zn3 O25 81.26(7) 1_455 2_655 ? O2 Zn3 O25 174.67(7) 1_455 2_655 ? O22 Zn3 O25 95.84(8) . 2_655 ? O8 Zn3 O25 88.15(7) 1_455 2_655 ? O26 Zn3 Zn1 146.01(7) 2_655 1_455 ? O25 Zn3 Zn1 37.59(5) 1_455 1_455 ? O2 Zn3 Zn1 64.86(5) 1_455 1_455 ? O22 Zn3 Zn1 108.21(5) . 1_455 ? O8 Zn3 Zn1 68.04(5) 1_455 1_455 ? O25 Zn3 Zn1 109.82(5) 2_655 1_455 ? O26 Zn3 Zn3 128.99(8) 2_655 2 ? O25 Zn3 Zn3 41.68(5) 1_455 2 ? O2 Zn3 Zn3 135.63(5) 1_455 2 ? O22 Zn3 Zn3 92.55(6) . 2 ? O8 Zn3 Zn3 89.00(5) 1_455 2 ? O25 Zn3 Zn3 39.58(5) 2_655 2 ? Zn1 Zn3 Zn3 73.574(11) 1_455 2 ? O26 Zn3 Zn2 31.96(7) 2_655 2_655 ? O25 Zn3 Zn2 148.05(5) 1_455 2_655 ? O2 Zn3 Zn2 103.01(5) 1_455 2_655 ? O22 Zn3 Zn2 66.78(5) . 2_655 ? O8 Zn3 Zn2 116.28(5) 1_455 2_655 ? O25 Zn3 Zn2 82.32(5) 2_655 2_655 ? Zn1 Zn3 Zn2 167.593(13) 1_455 2_655 ? Zn3 Zn3 Zn2 117.199(14) 2 2_655 ? O27 Zn4 O28 168.90(8) . 2_665 ? O27 Zn4 O16 90.71(9) . 2_665 ? O28 Zn4 O16 98.76(7) 2_665 2_665 ? O27 Zn4 O28 89.62(8) . 1_554 ? O28 Zn4 O28 80.30(7) 2_665 1_554 ? O16 Zn4 O28 173.30(7) 2_665 1_554 ? O27 Zn4 O19 100.09(8) . . ? O28 Zn4 O19 86.44(7) 2_665 . ? O16 Zn4 O19 85.79(7) 2_665 . ? O28 Zn4 O19 100.74(7) 1_554 . ? O27 Zn4 O10 84.36(8) . 1_564 ? O28 Zn4 O10 90.10(7) 2_665 1_564 ? O16 Zn4 O10 88.42(7) 2_665 1_564 ? O28 Zn4 O10 84.96(7) 1_554 1_564 ? O19 Zn4 O10 172.72(7) . 1_564 ? O27 Zn4 Zn5 145.44(7) . 2_665 ? O28 Zn4 Zn5 36.49(5) 2_665 2_665 ? O16 Zn4 Zn5 71.15(5) 2_665 2_665 ? O28 Zn4 Zn5 105.14(4) 1_554 2_665 ? O19 Zn4 Zn5 107.34(5) . 2_665 ? O10 Zn4 Zn5 66.50(5) 1_564 2_665 ? O27 Zn4 Zn4 129.19(7) . 2_664 ? O28 Zn4 Zn4 40.57(5) 2_665 2_664 ? O16 Zn4 Zn4 138.95(5) 2_665 2_664 ? O28 Zn4 Zn4 39.73(4) 1_554 2_664 ? O19 Zn4 Zn4 94.74(5) . 2_664 ? O10 Zn4 Zn4 86.74(5) 1_564 2_664 ? Zn5 Zn4 Zn4 69.572(10) 2_665 2_664 ? O3 Zn5 O28 106.31(8) 2_756 . ? O3 Zn5 O9 115.01(9) 2_756 2_656 ? O28 Zn5 O9 106.66(8) . 2_656 ? O3 Zn5 O15 111.51(9) 2_756 . ? O28 Zn5 O15 107.91(8) . . ? O9 Zn5 O15 109.08(8) 2_656 . ? O3 Zn5 Zn4 145.08(7) 2_756 2_665 ? O28 Zn5 Zn4 39.37(5) . 2_665 ? O9 Zn5 Zn4 87.90(5) 2_656 2_665 ? O15 Zn5 Zn4 82.40(5) . 2_665 ? C7 O1 Zn1 114.69(17) . . ? C7 O2 Zn3 138.64(18) . 1_655 ? C8 O3 Zn5 130.46(19) . 2_756 ? C15 O7 Zn1 119.29(15) . . ? C15 O8 Zn3 132.45(16) . 1_655 ? C16 O9 Zn5 119.59(15) . 2_656 ? C16 O10 Zn4 137.69(16) . 1_546 ? C24 O13 Zn2 125.59(16) . . ? C24 O14 Zn1 153.0(2) . . ? C23 O15 Zn5 124.36(17) . . ? C23 O16 Zn4 134.04(18) . 2_665 ? C31 O19 Zn4 127.25(15) . . ? C31 O20 Zn2 124.26(16) . . ? C32 O21 Zn2 123.62(16) . 2_655 ? C32 O22 Zn3 135.74(17) . . ? Zn1 O25 Zn3 101.84(8) . 1_655 ? Zn1 O25 Zn3 134.91(10) . 2_655 ? Zn3 O25 Zn3 98.74(7) 1_655 2_655 ? Zn1 O25 H25 109(3) . . ? Zn3 O25 H25 108(3) 1_655 . ? Zn3 O25 H25 102(3) 2_655 . ? Zn2 O26 Zn3 114.50(12) . 2_655 ? Zn2 O26 H26A 115(6) . . ? Zn3 O26 H26A 108(6) 2_655 . ? Zn4 O27 H27A 127(4) . . ? Zn4 O27 H27B 119(3) . . ? H27A O27 H27B 107(5) . . ? Zn5 O28 Zn4 104.14(8) . 2_665 ? Zn5 O28 Zn4 127.27(9) . 1_556 ? Zn4 O28 Zn4 99.70(7) 2_665 1_556 ? Zn5 O28 H28A 111(3) . . ? Zn4 O28 H28A 112(2) 2_665 . ? Zn4 O28 H28A 102(3) 1_556 . ? O5 N1 O6 123.9(2) . . ? O5 N1 C5 117.9(2) . . ? O6 N1 C5 118.2(2) . . ? O11 N2 O12 123.3(2) . . ? O11 N2 C13 118.6(2) . . ? O12 N2 C13 118.1(2) . . ? O18 N3 O17 123.5(2) . . ? O18 N3 C21 118.6(2) . . ? O17 N3 C21 117.9(2) . . ? O23 N4 O24 123.2(2) . . ? O23 N4 C29 118.4(2) . . ? O24 N4 C29 118.4(2) . . ? C33 N5 C37 123.6(3) . . ? C33 N5 H5A 118.2 . . ? C37 N5 H5A 118.2 . . ? C34 N6 H6A 120.0 . . ? C34 N6 H6B 120.0 . . ? H6A N6 H6B 120.0 . . ? C6 C1 C2 119.5(2) . . ? C6 C1 C7 121.0(2) . . ? C2 C1 C7 119.4(2) . . ? C3 C2 C1 121.4(2) . . ? C3 C2 H2A 119.3 . . ? C1 C2 H2A 119.3 . . ? C4 C3 C2 119.6(2) . . ? C4 C3 C8 120.5(2) . . ? C2 C3 C8 119.8(2) . . ? C3 C4 C5 117.9(2) . . ? C3 C4 H4A 121.1 . . ? C5 C4 H4A 121.1 . . ? C6 C5 C4 123.6(2) . . ? C6 C5 N1 117.8(2) . . ? C4 C5 N1 118.5(2) . . ? C5 C6 C1 118.0(2) . . ? C5 C6 H6C 121.0 . . ? C1 C6 H6C 121.0 . . ? O2 C7 O1 125.7(3) . . ? O2 C7 C1 117.1(2) . . ? O1 C7 C1 117.2(2) . . ? O4 C8 O3 126.0(3) . . ? O4 C8 C3 120.0(2) . . ? O3 C8 C3 113.9(2) . . ? C10 C9 C14 119.3(2) . . ? C10 C9 C15 121.2(2) . . ? C14 C9 C15 119.4(2) . . ? C9 C10 C11 121.7(2) . . ? C9 C10 H10A 119.1 . . ? C11 C10 H10A 119.1 . . ? C10 C11 C12 119.5(2) . . ? C10 C11 C16 120.2(2) . . ? C12 C11 C16 120.3(2) . . ? C13 C12 C11 118.0(2) . . ? C13 C12 H12A 121.0 . . ? C11 C12 H12A 121.0 . . ? C14 C13 C12 123.3(2) . . ? C14 C13 N2 117.8(2) . . ? C12 C13 N2 118.9(2) . . ? C13 C14 C9 118.2(2) . . ? C13 C14 H14A 120.9 . . ? C9 C14 H14A 120.9 . . ? O8 C15 O7 125.9(2) . . ? O8 C15 C9 118.1(2) . . ? O7 C15 C9 116.0(2) . . ? O10 C16 O9 126.4(2) . . ? O10 C16 C11 118.3(2) . . ? O9 C16 C11 115.3(2) . . ? C18 C17 C22 119.8(2) . . ? C18 C17 C24 119.7(2) . . ? C22 C17 C24 120.5(2) . . ? C19 C18 C17 121.1(2) . . ? C19 C18 H18A 119.4 . . ? C17 C18 H18A 119.4 . . ? C18 C19 C20 119.3(2) . . ? C18 C19 C23 120.8(2) . . ? C20 C19 C23 119.8(2) . . ? C21 C20 C19 118.7(2) . . ? C21 C20 H20A 120.7 . . ? C19 C20 H20A 120.7 . . ? C22 C21 C20 122.7(2) . . ? C22 C21 N3 118.7(2) . . ? C20 C21 N3 118.6(2) . . ? C21 C22 C17 118.3(2) . . ? C21 C22 H22A 120.8 . . ? C17 C22 H22A 120.8 . . ? O16 C23 O15 127.1(2) . . ? O16 C23 C19 117.8(2) . . ? O15 C23 C19 115.1(2) . . ? O14 C24 O13 125.6(2) . . ? O14 C24 C17 117.1(2) . . ? O13 C24 C17 117.2(2) . . ? C30 C25 C26 119.7(2) . . ? C30 C25 C31 120.8(2) . . ? C26 C25 C31 119.5(2) . . ? C27 C26 C25 121.4(2) . . ? C27 C26 H26B 119.3 . . ? C25 C26 H26B 119.3 . . ? C26 C27 C28 119.4(2) . . ? C26 C27 C32 120.1(2) . . ? C28 C27 C32 120.3(2) . . ? C29 C28 C27 118.1(2) . . ? C29 C28 H28B 121.0 . . ? C27 C28 H28B 121.0 . . ? C28 C29 C30 123.5(2) . . ? C28 C29 N4 118.4(2) . . ? C30 C29 N4 118.0(2) . . ? C29 C30 C25 118.0(2) . . ? C29 C30 H30A 121.0 . . ? C25 C30 H30A 121.0 . . ? O19 C31 O20 124.7(2) . . ? O19 C31 C25 118.5(2) . . ? O20 C31 C25 116.8(2) . . ? O22 C32 O21 125.6(2) . . ? O22 C32 C27 118.7(2) . . ? O21 C32 C27 115.7(2) . . ? N5 C33 C34 120.9(3) . . ? N5 C33 H33A 119.6 . . ? C34 C33 H33A 119.6 . . ? N6 C34 C35 121.5(5) . . ? N6 C34 C33 122.7(5) . . ? C35 C34 C33 115.8(3) . . ? C36 C35 C34 120.3(4) . . ? C36 C35 H35A 119.9 . . ? C34 C35 H35A 119.9 . . ? C35 C36 C37 120.6(4) . . ? C35 C36 H36A 119.7 . . ? C37 C36 H36A 119.7 . . ? N5 C37 C36 118.7(4) . . ? N5 C37 H37A 120.7 . . ? C36 C37 H37A 120.7 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O28 H28A O6 0.69(3) 2.34(3) 2.986(3) 155(3) . O27 H27A O26 0.75(5) 2.04(5) 2.786(3) 170(5) . O25 H25 O17 0.67(3) 2.31(4) 2.916(3) 152(4) 2_665 O27 H27B O5 0.76(5) 2.19(5) 2.924(3) 162(5) 1_554 N6 H6B O24 0.86 2.52 3.147(5) 130.8 2_565 N5 H5A O4 0.86 1.93 2.692(4) 146.8 2_756 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.520 _refine_diff_density_min -0.496 _refine_diff_density_rms 0.063 # = = = END data_5 _database_code_depnum_ccdc_archive 'CCDC 843814' #TrackingRef 'CCDC-compounds.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H26 N6 O29 Zn5' _chemical_formula_weight 1345.59 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 12.608(4) _cell_length_b 14.324(5) _cell_length_c 15.693(5) _cell_angle_alpha 63.256(4) _cell_angle_beta 81.245(4) _cell_angle_gamma 64.466(3) _cell_volume 2280.7(13) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7853 _cell_measurement_theta_min 1.92 _cell_measurement_theta_max 25.01 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.959 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1344 _exptl_absorpt_coefficient_mu 2.701 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5184 _exptl_absorpt_correction_T_max 0.5879 _exptl_absorpt_process_details 'Higashi (1995)' _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 '\f and \w scans' _diffrn_detector_area_resol_mean 'Bruker SMART CCD area' _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 11377 _diffrn_reflns_av_R_equivalents 0.0227 _diffrn_reflns_av_sigmaI/netI 0.0470 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 25.01 _reflns_number_total 7853 _reflns_number_gt 6240 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SMART (Bruker, 1997)' _computing_data_reduction 'SAINT (Bruker, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXP97 (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Bruker, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0691P)^2^+1.1711P] 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 0 _refine_ls_number_reflns 7853 _refine_ls_number_parameters 694 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0560 _refine_ls_R_factor_gt 0.0413 _refine_ls_wR_factor_ref 0.1201 _refine_ls_wR_factor_gt 0.1091 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.038 _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 0.57349(4) -0.05937(4) 0.59861(3) 0.02302(14) Uani 1 1 d . . . Zn2 Zn 0.63873(5) -0.33079(4) 0.90661(4) 0.02469(14) Uani 1 1 d . . . Zn3 Zn 0.19027(4) 0.42782(4) 0.86862(4) 0.02499(14) Uani 1 1 d . . . Zn4 Zn 0.07379(4) -0.55116(4) 1.09720(4) 0.02413(14) Uani 1 1 d . . . Zn5 Zn 0.46990(5) 0.21038(4) 0.52052(4) 0.02455(14) Uani 1 1 d . . . O1 O 0.4450(3) -0.1149(3) 0.6803(2) 0.0328(8) Uani 1 1 d . . . O2 O 0.5514(3) -0.2883(3) 0.7912(2) 0.0288(7) Uani 1 1 d . . . O3 O 0.3389(3) -0.5127(3) 1.0067(3) 0.0405(9) Uani 1 1 d . . . O4 O 0.1496(3) -0.4276(3) 1.0310(3) 0.0392(9) Uani 1 1 d . . . O5 O -0.0288(4) -0.0055(4) 0.8904(4) 0.093(2) Uani 1 1 d . . . O6 O 0.0444(4) 0.0867(3) 0.7688(3) 0.0594(12) Uani 1 1 d . . . O7 O 0.4619(3) 0.2289(3) 1.0353(2) 0.0392(9) Uani 1 1 d . . . O8 O 0.3478(3) 0.3091(3) 0.9052(3) 0.0495(11) Uani 1 1 d . . . O9 O 0.4960(3) 0.1698(3) 0.6556(2) 0.0381(9) Uani 1 1 d . . . O10 O 0.5922(3) -0.0217(3) 0.7099(2) 0.0366(8) Uani 1 1 d . . . O11 O 0.8697(3) -0.1856(3) 0.9860(3) 0.0508(10) Uani 1 1 d . . . O12 O 0.8272(4) -0.1042(4) 1.0807(4) 0.0808(16) Uani 1 1 d . . . O13 O 0.1350(3) 0.3912(3) 0.7824(3) 0.0419(9) Uani 1 1 d . . . O14 O -0.0487(3) 0.5130(3) 0.7855(2) 0.0420(9) Uani 1 1 d . . . O15 O -0.3364(3) 0.6479(3) 0.5438(3) 0.0470(10) Uani 1 1 d . . . O16 O -0.3206(4) 0.5528(4) 0.4610(4) 0.0748(15) Uani 1 1 d . . . O17 O 0.0849(3) 0.2659(3) 0.4640(3) 0.0442(9) Uani 1 1 d . . . O18 O 0.1968(3) 0.1776(3) 0.5924(3) 0.0495(10) Uani 1 1 d . . . O19 O 0.9897(3) 0.3327(3) 0.1695(2) 0.0362(8) Uani 1 1 d . . . O20 O 0.8089(3) 0.4218(3) 0.2090(2) 0.0358(8) Uani 1 1 d . . . O21 O 0.6162(3) 0.2021(3) 0.4558(2) 0.0341(8) Uani 1 1 d . . . O22 O 0.6989(3) 0.0096(3) 0.5204(2) 0.0298(7) Uani 1 1 d . . . O23 O 1.1051(4) -0.1794(3) 0.4411(3) 0.0616(12) Uani 1 1 d . . . O24 O 1.1870(4) -0.0801(4) 0.3320(4) 0.0682(14) Uani 1 1 d . . . O25 O 0.7184(3) -0.2146(3) 0.6557(2) 0.0377(9) Uani 1 1 d . . . H25A H 0.7479 -0.2003 0.6143 0.045 Uiso 1 1 d R . . H25B H 0.7255 -0.2402 0.7064 0.045 Uiso 1 1 d R . . O26 O 0.7763(3) -0.3115(3) 0.8498(2) 0.0313(8) Uani 1 1 d . . . H26A H 0.7781 -0.2801 0.8689 0.038 Uiso 1 1 d R . . O27 O 0.0838(3) 0.4206(2) 0.9726(2) 0.0243(7) Uani 1 1 d . . . H27A H 0.0846 0.3702 0.9855 0.029 Uiso 1 1 d R . . O28 O 0.4350(3) 0.0905(2) 0.5197(2) 0.0225(7) Uani 1 1 d . . . H28 H 0.3830 0.0938 0.5413 0.027 Uiso 1 1 d R . . N1 N 0.0490(4) -0.0009(4) 0.8345(3) 0.0417(11) Uani 1 1 d . . . N2 N 0.8049(4) -0.1105(4) 1.0115(3) 0.0426(11) Uani 1 1 d . . . N3 N 0.1087(4) 0.2541(4) 0.5425(3) 0.0359(10) Uani 1 1 d . . . N4 N 1.1052(4) -0.0883(4) 0.3815(3) 0.0380(10) Uani 1 1 d . . . C1 C 0.3484(4) -0.2027(4) 0.8122(3) 0.0244(10) Uani 1 1 d . . . C2 C 0.3465(4) -0.3073(4) 0.8793(3) 0.0272(10) Uani 1 1 d . . . H2A H 0.4137 -0.3746 0.8912 0.033 Uiso 1 1 calc R . . C3 C 0.2468(4) -0.3127(4) 0.9283(3) 0.0259(10) Uani 1 1 d . . . C4 C 0.1483(4) -0.2110(4) 0.9138(3) 0.0319(11) Uani 1 1 d . . . H4A H 0.0808 -0.2125 0.9469 0.038 Uiso 1 1 calc R . . C5 C 0.1524(4) -0.1069(4) 0.8489(3) 0.0307(11) Uani 1 1 d . . . C6 C 0.2493(4) -0.1010(4) 0.7968(3) 0.0290(11) Uani 1 1 d . . . H6C H 0.2489 -0.0307 0.7522 0.035 Uiso 1 1 calc R . . C7 C 0.4566(4) -0.2006(4) 0.7567(3) 0.0259(10) Uani 1 1 d . . . C8 C 0.2429(4) -0.4254(4) 0.9935(3) 0.0276(11) Uani 1 1 d . . . C9 C 0.5216(4) 0.1464(4) 0.9268(3) 0.0264(10) Uani 1 1 d . . . C10 C 0.4997(4) 0.1482(4) 0.8412(3) 0.0284(11) Uani 1 1 d . . . H10A H 0.4329 0.2064 0.8028 0.034 Uiso 1 1 calc R . . C11 C 0.5761(4) 0.0644(4) 0.8129(3) 0.0283(11) Uani 1 1 d . . . C12 C 0.6759(4) -0.0224(4) 0.8690(3) 0.0316(11) Uani 1 1 d . . . H12A H 0.7270 -0.0798 0.8512 0.038 Uiso 1 1 calc R . . C13 C 0.6984(4) -0.0219(4) 0.9532(3) 0.0284(11) Uani 1 1 d . . . C14 C 0.6220(4) 0.0609(4) 0.9830(3) 0.0316(11) Uani 1 1 d . . . H14A H 0.6381 0.0588 1.0399 0.038 Uiso 1 1 calc R . . C15 C 0.4364(4) 0.2351(4) 0.9582(3) 0.0266(10) Uani 1 1 d . . . C16 C 0.5534(4) 0.0706(4) 0.7180(3) 0.0287(11) Uani 1 1 d . . . C17 C -0.0114(4) 0.4278(4) 0.6798(3) 0.0264(10) Uani 1 1 d . . . C18 C -0.1231(4) 0.4974(4) 0.6385(3) 0.0282(11) Uani 1 1 d . . . H18A H -0.1736 0.5522 0.6594 0.034 Uiso 1 1 calc R . . C19 C -0.1621(4) 0.4876(4) 0.5658(3) 0.0299(11) Uani 1 1 d . . . C20 C -0.0855(4) 0.4049(4) 0.5351(3) 0.0275(10) Uani 1 1 d . . . H20A H -0.1091 0.3963 0.4867 0.033 Uiso 1 1 calc R . . C21 C 0.0252(4) 0.3371(4) 0.5780(3) 0.0280(11) Uani 1 1 d . . . C22 C 0.0654(4) 0.3456(4) 0.6502(3) 0.0291(11) Uani 1 1 d . . . H22A H 0.1411 0.2978 0.6779 0.035 Uiso 1 1 calc R . . C23 C 0.0286(4) 0.4452(4) 0.7561(3) 0.0319(11) Uani 1 1 d . . . C24 C -0.2824(5) 0.5681(4) 0.5181(4) 0.0363(12) Uani 1 1 d . . . C25 C 0.9037(4) 0.2202(4) 0.2906(3) 0.0262(10) Uani 1 1 d . . . C26 C 0.8064(4) 0.2142(4) 0.3448(3) 0.0256(10) Uani 1 1 d . . . H26B H 0.7405 0.2815 0.3364 0.031 Uiso 1 1 calc R . . C27 C 0.8058(4) 0.1098(4) 0.4110(3) 0.0254(10) Uani 1 1 d . . . C28 C 0.9044(4) 0.0093(4) 0.4233(3) 0.0283(11) Uani 1 1 d . . . H28B H 0.9059 -0.0617 0.4671 0.034 Uiso 1 1 calc R . . C29 C 0.9997(4) 0.0168(4) 0.3695(3) 0.0287(11) Uani 1 1 d . . . C30 C 1.0021(4) 0.1204(4) 0.3033(3) 0.0286(11) Uani 1 1 d . . . H30A H 1.0682 0.1226 0.2683 0.034 Uiso 1 1 calc R . . C31 C 0.9019(4) 0.3330(4) 0.2176(3) 0.0289(11) Uani 1 1 d . . . C32 C 0.6990(4) 0.1044(4) 0.4678(3) 0.0265(10) Uani 1 1 d . . . N5 N 0.4995(6) 0.5999(6) 0.3534(5) 0.0824(19) Uani 1 1 d . . . H5A H 0.5386 0.6100 0.3865 0.099 Uiso 1 1 d R . . N6 N 0.3216(6) 0.5536(7) 0.1969(5) 0.098(2) Uani 1 1 d . . . H6A H 0.3520 0.4981 0.1804 0.117 Uiso 1 1 d R . . H6B H 0.2497 0.6022 0.1798 0.117 Uiso 1 1 d R . . C33 C 0.5517(11) 0.5148(9) 0.3284(8) 0.125(4) Uani 1 1 d U . . H33A H 0.6307 0.4667 0.3463 0.150 Uiso 1 1 calc R . . C34 C 0.4940(9) 0.4965(10) 0.2787(8) 0.123(4) Uani 1 1 d . . . H34A H 0.5328 0.4336 0.2647 0.148 Uiso 1 1 calc R . . C35 C 0.3838(8) 0.5634(9) 0.2479(6) 0.088(3) Uani 1 1 d . . . C36 C 0.3224(7) 0.6652(7) 0.2716(5) 0.073(2) Uani 1 1 d . . . H36A H 0.2457 0.7187 0.2496 0.088 Uiso 1 1 calc R . . C37 C 0.3847(7) 0.6715(7) 0.3243(6) 0.075(2) Uani 1 1 d . . . H37A H 0.3487 0.7296 0.3444 0.090 Uiso 1 1 calc R . . O29 O 0.1012(7) 0.7447(6) 0.1346(5) 0.143(3) Uani 1 1 d . . . H29A H 0.1495 0.7689 0.1350 0.171 Uiso 1 1 d R . . H29B H 0.0877 0.7021 0.1200 0.171 Uiso 1 1 d 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 0.0259(3) 0.0208(3) 0.0216(3) -0.0102(2) 0.0028(2) -0.0083(2) Zn2 0.0248(3) 0.0217(3) 0.0234(3) -0.0111(2) 0.0035(2) -0.0052(2) Zn3 0.0214(3) 0.0217(3) 0.0260(3) -0.0108(2) 0.0027(2) -0.0036(2) Zn4 0.0205(3) 0.0231(3) 0.0242(3) -0.0098(2) 0.0035(2) -0.0061(2) Zn5 0.0249(3) 0.0192(3) 0.0276(3) -0.0123(2) 0.0014(2) -0.0051(2) O1 0.0304(19) 0.028(2) 0.0290(18) -0.0026(15) 0.0017(14) -0.0131(16) O2 0.0273(18) 0.0279(19) 0.0258(17) -0.0099(15) -0.0031(14) -0.0071(16) O3 0.033(2) 0.026(2) 0.045(2) -0.0065(17) 0.0120(16) -0.0090(17) O4 0.033(2) 0.025(2) 0.053(2) -0.0126(17) 0.0117(17) -0.0139(16) O5 0.062(3) 0.034(3) 0.131(5) -0.022(3) 0.051(3) -0.004(2) O6 0.056(3) 0.024(2) 0.068(3) -0.007(2) 0.010(2) -0.007(2) O7 0.039(2) 0.039(2) 0.035(2) -0.0278(17) -0.0002(16) -0.0003(17) O8 0.026(2) 0.051(3) 0.053(2) -0.033(2) -0.0115(18) 0.0141(18) O9 0.052(2) 0.033(2) 0.0286(18) -0.0166(17) -0.0044(17) -0.0118(18) O10 0.050(2) 0.033(2) 0.0296(18) -0.0190(16) 0.0009(16) -0.0136(18) O11 0.040(2) 0.029(2) 0.073(3) -0.025(2) 0.000(2) -0.0005(18) O12 0.064(3) 0.078(4) 0.073(3) -0.044(3) -0.036(3) 0.020(3) O13 0.034(2) 0.050(2) 0.046(2) -0.0305(19) -0.0019(17) -0.0100(19) O14 0.041(2) 0.046(2) 0.038(2) -0.0304(19) 0.0004(17) -0.0043(18) O15 0.043(2) 0.029(2) 0.049(2) -0.0212(19) -0.0104(18) 0.0105(18) O16 0.056(3) 0.062(3) 0.110(4) -0.056(3) -0.043(3) 0.008(2) O17 0.054(2) 0.048(2) 0.045(2) -0.035(2) 0.0170(19) -0.022(2) O18 0.032(2) 0.044(2) 0.061(3) -0.030(2) 0.007(2) 0.001(2) O19 0.036(2) 0.029(2) 0.039(2) -0.0103(16) 0.0148(16) -0.0175(17) O20 0.0312(19) 0.0230(19) 0.041(2) -0.0072(16) 0.0085(16) -0.0100(16) O21 0.0261(18) 0.027(2) 0.045(2) -0.0149(17) 0.0110(15) -0.0116(16) O22 0.0302(19) 0.0255(19) 0.0295(17) -0.0069(15) 0.0043(14) -0.0141(16) O23 0.052(3) 0.025(2) 0.083(3) -0.012(2) 0.009(2) -0.007(2) O24 0.038(2) 0.043(3) 0.097(4) -0.026(2) 0.034(2) -0.008(2) O25 0.037(2) 0.032(2) 0.0195(16) -0.0039(15) 0.0056(15) -0.0023(17) O26 0.0238(17) 0.0269(19) 0.0366(19) -0.0121(15) 0.0008(14) -0.0062(15) O27 0.0277(17) 0.0153(16) 0.0263(16) -0.0093(13) 0.0033(13) -0.0061(14) O28 0.0221(16) 0.0207(17) 0.0255(16) -0.0141(14) 0.0054(13) -0.0063(14) N1 0.038(3) 0.026(3) 0.056(3) -0.017(2) 0.008(2) -0.011(2) N2 0.035(3) 0.032(3) 0.048(3) -0.018(2) -0.005(2) 0.002(2) N3 0.035(3) 0.031(3) 0.045(3) -0.025(2) 0.017(2) -0.013(2) N4 0.032(2) 0.025(3) 0.051(3) -0.019(2) 0.005(2) -0.005(2) C1 0.027(2) 0.023(3) 0.021(2) -0.007(2) 0.0017(19) -0.012(2) C2 0.028(3) 0.030(3) 0.023(2) -0.009(2) 0.0019(19) -0.014(2) C3 0.029(3) 0.022(3) 0.028(2) -0.012(2) -0.002(2) -0.009(2) C4 0.032(3) 0.034(3) 0.031(3) -0.014(2) 0.011(2) -0.018(2) C5 0.030(3) 0.022(3) 0.035(3) -0.012(2) 0.000(2) -0.005(2) C6 0.034(3) 0.022(3) 0.030(2) -0.008(2) 0.001(2) -0.014(2) C7 0.031(3) 0.028(3) 0.026(2) -0.011(2) -0.002(2) -0.018(2) C8 0.034(3) 0.026(3) 0.022(2) -0.010(2) 0.003(2) -0.014(2) C9 0.024(2) 0.024(3) 0.029(2) -0.014(2) 0.003(2) -0.006(2) C10 0.029(3) 0.028(3) 0.027(2) -0.014(2) -0.003(2) -0.007(2) C11 0.036(3) 0.031(3) 0.024(2) -0.017(2) 0.008(2) -0.016(2) C12 0.033(3) 0.029(3) 0.035(3) -0.021(2) 0.008(2) -0.008(2) C13 0.026(3) 0.021(3) 0.032(3) -0.012(2) 0.001(2) -0.003(2) C14 0.034(3) 0.032(3) 0.033(3) -0.023(2) 0.002(2) -0.009(2) C15 0.024(2) 0.027(3) 0.028(2) -0.015(2) 0.006(2) -0.008(2) C16 0.036(3) 0.034(3) 0.026(2) -0.019(2) 0.008(2) -0.019(2) C17 0.035(3) 0.021(3) 0.026(2) -0.015(2) 0.005(2) -0.010(2) C18 0.028(3) 0.022(3) 0.035(3) -0.016(2) 0.005(2) -0.008(2) C19 0.034(3) 0.023(3) 0.031(3) -0.011(2) 0.003(2) -0.012(2) C20 0.031(3) 0.023(3) 0.032(3) -0.016(2) 0.003(2) -0.011(2) C21 0.029(3) 0.024(3) 0.034(3) -0.019(2) 0.011(2) -0.010(2) C22 0.024(2) 0.023(3) 0.032(3) -0.011(2) 0.001(2) -0.003(2) C23 0.036(3) 0.031(3) 0.026(3) -0.011(2) 0.002(2) -0.013(2) C24 0.035(3) 0.031(3) 0.039(3) -0.015(2) 0.003(2) -0.010(2) C25 0.029(3) 0.024(3) 0.025(2) -0.010(2) 0.002(2) -0.012(2) C26 0.027(2) 0.020(2) 0.024(2) -0.009(2) 0.0027(19) -0.006(2) C27 0.028(3) 0.021(3) 0.025(2) -0.008(2) -0.0006(19) -0.009(2) C28 0.036(3) 0.019(3) 0.029(2) -0.009(2) 0.001(2) -0.013(2) C29 0.027(3) 0.020(3) 0.035(3) -0.012(2) 0.001(2) -0.005(2) C30 0.025(3) 0.030(3) 0.031(3) -0.015(2) 0.009(2) -0.012(2) C31 0.031(3) 0.030(3) 0.026(2) -0.009(2) 0.001(2) -0.016(2) C32 0.025(3) 0.030(3) 0.022(2) -0.008(2) -0.0006(19) -0.012(2) N5 0.086(5) 0.078(5) 0.097(5) -0.051(4) 0.005(4) -0.031(4) N6 0.082(5) 0.131(7) 0.102(5) -0.079(5) -0.007(4) -0.028(5) C33 0.171(8) 0.112(7) 0.132(7) -0.099(6) 0.005(6) -0.043(6) C34 0.111(8) 0.131(10) 0.129(9) -0.068(8) -0.044(7) -0.022(7) C35 0.089(6) 0.141(9) 0.074(5) -0.061(6) 0.010(5) -0.067(6) C36 0.076(5) 0.085(6) 0.076(5) -0.043(5) 0.023(4) -0.045(5) C37 0.057(5) 0.068(5) 0.090(6) -0.033(4) 0.010(4) -0.022(4) O29 0.198(8) 0.148(7) 0.111(6) -0.065(5) 0.027(5) -0.092(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O28 2.055(3) . ? Zn1 O25 2.071(3) . ? Zn1 O1 2.113(3) . ? Zn1 O10 2.117(3) . ? Zn1 O28 2.123(3) 2_656 ? Zn1 O22 2.156(3) . ? Zn1 Zn5 3.1643(14) . ? Zn1 Zn1 3.1933(13) 2_656 ? Zn1 H25A 2.2052 . ? Zn2 O26 1.897(3) . ? Zn2 O3 1.945(3) 2_647 ? Zn2 O7 1.954(3) 2_657 ? Zn2 O2 1.976(3) . ? Zn2 Zn4 3.2775(12) 2_647 ? Zn2 H26A 2.0881 . ? Zn3 O8 1.930(3) . ? Zn3 O27 1.943(3) . ? Zn3 O20 1.944(3) 2_666 ? Zn3 O13 1.959(3) . ? Zn3 Zn4 3.1195(11) 2_557 ? Zn3 H27A 2.1586 . ? Zn4 O26 1.984(3) 2_647 ? Zn4 O27 2.064(3) 2_557 ? Zn4 O14 2.089(3) 2_557 ? Zn4 O27 2.145(3) 1_545 ? Zn4 O4 2.151(3) . ? Zn4 O19 2.154(3) 1_446 ? Zn4 Zn3 3.1195(11) 2_557 ? Zn4 Zn4 3.2046(14) 2_547 ? Zn4 Zn2 3.2775(12) 2_647 ? Zn5 O15 1.924(3) 2_566 ? Zn5 O21 1.949(3) . ? Zn5 O28 1.953(3) . ? Zn5 O9 1.969(3) . ? Zn5 H28 2.2516 . ? O1 C7 1.240(5) . ? O2 C7 1.261(5) . ? O3 C8 1.269(6) . ? O3 Zn2 1.945(3) 2_647 ? O4 C8 1.239(6) . ? O5 N1 1.216(6) . ? O6 N1 1.196(6) . ? O7 C15 1.254(5) . ? O7 Zn2 1.954(3) 2_657 ? O8 C15 1.238(6) . ? O9 C16 1.257(6) . ? O10 C16 1.256(5) . ? O11 N2 1.231(5) . ? O12 N2 1.212(6) . ? O13 C23 1.247(6) . ? O14 C23 1.248(6) . ? O14 Zn4 2.089(3) 2_557 ? O15 C24 1.262(6) . ? O15 Zn5 1.924(3) 2_566 ? O16 C24 1.216(6) . ? O17 N3 1.232(5) . ? O18 N3 1.221(5) . ? O19 C31 1.240(5) . ? O19 Zn4 2.154(3) 1_664 ? O20 C31 1.272(6) . ? O20 Zn3 1.944(3) 2_666 ? O21 C32 1.283(6) . ? O22 C32 1.232(6) . ? O23 N4 1.217(6) . ? O24 N4 1.208(6) . ? O25 H25A 0.6888 . ? O25 H25B 0.7115 . ? O26 Zn4 1.984(3) 2_647 ? O26 H26A 0.6517 . ? O27 Zn4 2.064(3) 2_557 ? O27 Zn4 2.145(3) 1_565 ? O27 H27A 0.6508 . ? O28 Zn1 2.123(3) 2_656 ? O28 H28 0.6834 . ? N1 C5 1.460(6) . ? N2 C13 1.453(6) . ? N3 C21 1.473(6) . ? N4 C29 1.472(6) . ? C1 C6 1.395(6) . ? C1 C2 1.399(6) . ? C1 C7 1.506(6) . ? C2 C3 1.383(6) . ? C2 H2A 0.9300 . ? C3 C4 1.395(7) . ? C3 C8 1.491(6) . ? C4 C5 1.396(7) . ? C4 H4A 0.9300 . ? C5 C6 1.375(7) . ? C6 H6C 0.9300 . ? C9 C14 1.382(6) . ? C9 C10 1.399(6) . ? C9 C15 1.495(6) . ? C10 C11 1.385(6) . ? C10 H10A 0.9300 . ? C11 C12 1.382(7) . ? C11 C16 1.514(6) . ? C12 C13 1.396(7) . ? C12 H12A 0.9300 . ? C13 C14 1.389(6) . ? C14 H14A 0.9300 . ? C17 C18 1.372(6) . ? C17 C22 1.382(6) . ? C17 C23 1.520(6) . ? C18 C19 1.392(7) . ? C18 H18A 0.9300 . ? C19 C20 1.397(6) . ? C19 C24 1.501(7) . ? C20 C21 1.370(7) . ? C20 H20A 0.9300 . ? C21 C22 1.381(6) . ? C22 H22A 0.9300 . ? C25 C30 1.383(6) . ? C25 C26 1.394(6) . ? C25 C31 1.495(6) . ? C26 C27 1.387(6) . ? C26 H26B 0.9300 . ? C27 C28 1.392(6) . ? C27 C32 1.508(6) . ? C28 C29 1.374(6) . ? C28 H28B 0.9300 . ? C29 C30 1.387(7) . ? C30 H30A 0.9300 . ? N5 C33 1.316(9) . ? N5 C37 1.362(9) . ? N5 H5A 0.8598 . ? N6 C35 1.290(9) . ? N6 H6A 0.8601 . ? N6 H6B 0.8600 . ? C33 C34 1.316(12) . ? C33 H33A 0.9300 . ? C34 C35 1.311(12) . ? C34 H34A 0.9300 . ? C35 C36 1.513(11) . ? C36 C37 1.279(10) . ? C36 H36A 0.9300 . ? C37 H37A 0.9300 . ? O29 H29A 0.8235 . ? O29 H29B 0.8251 . ? 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 O28 Zn1 O25 169.61(12) . . ? O28 Zn1 O1 86.33(12) . . ? O25 Zn1 O1 97.68(13) . . ? O28 Zn1 O10 99.59(12) . . ? O25 Zn1 O10 90.25(13) . . ? O1 Zn1 O10 86.53(13) . . ? O28 Zn1 O28 80.32(12) . 2_656 ? O25 Zn1 O28 89.58(12) . 2_656 ? O1 Zn1 O28 98.45(12) . 2_656 ? O10 Zn1 O28 175.00(12) . 2_656 ? O28 Zn1 O22 91.39(12) . . ? O25 Zn1 O22 85.41(13) . . ? O1 Zn1 O22 174.53(12) . . ? O10 Zn1 O22 88.95(13) . . ? O28 Zn1 O22 86.05(12) 2_656 . ? O28 Zn1 Zn5 36.74(8) . . ? O25 Zn1 Zn5 147.33(10) . . ? O1 Zn1 Zn5 107.99(9) . . ? O10 Zn1 Zn5 71.96(10) . . ? O28 Zn1 Zn5 105.80(8) 2_656 . ? O22 Zn1 Zn5 67.58(9) . . ? O28 Zn1 Zn1 40.94(8) . 2_656 ? O25 Zn1 Zn1 128.92(10) . 2_656 ? O1 Zn1 Zn1 93.23(9) . 2_656 ? O10 Zn1 Zn1 140.31(10) . 2_656 ? O28 Zn1 Zn1 39.38(8) 2_656 2_656 ? O22 Zn1 Zn1 88.27(9) . 2_656 ? Zn5 Zn1 Zn1 70.44(2) . 2_656 ? O28 Zn1 H25A 153.1 . . ? O25 Zn1 H25A 18.2 . . ? O1 Zn1 H25A 113.7 . . ? O10 Zn1 H25A 99.5 . . ? O28 Zn1 H25A 79.0 2_656 . ? O22 Zn1 H25A 70.1 . . ? Zn5 Zn1 H25A 136.9 . . ? Zn1 Zn1 H25A 116.6 2_656 . ? O26 Zn2 O3 115.65(14) . 2_647 ? O26 Zn2 O7 117.78(15) . 2_657 ? O3 Zn2 O7 108.96(15) 2_647 2_657 ? O26 Zn2 O2 99.23(14) . . ? O3 Zn2 O2 106.75(15) 2_647 . ? O7 Zn2 O2 107.10(14) 2_657 . ? O26 Zn2 Zn4 33.22(10) . 2_647 ? O3 Zn2 Zn4 82.82(10) 2_647 2_647 ? O7 Zn2 Zn4 130.20(11) 2_657 2_647 ? O2 Zn2 Zn4 115.48(9) . 2_647 ? O26 Zn2 H26A 18.0 . . ? O3 Zn2 H26A 122.3 2_647 . ? O7 Zn2 H26A 100.3 2_657 . ? O2 Zn2 H26A 110.5 . . ? Zn4 Zn2 H26A 41.6 2_647 . ? O8 Zn3 O27 114.56(15) . . ? O8 Zn3 O20 111.65(17) . 2_666 ? O27 Zn3 O20 114.76(13) . 2_666 ? O8 Zn3 O13 101.83(15) . . ? O27 Zn3 O13 106.82(14) . . ? O20 Zn3 O13 105.82(16) 2_666 . ? O8 Zn3 Zn4 154.65(13) . 2_557 ? O27 Zn3 Zn4 40.29(9) . 2_557 ? O20 Zn3 Zn4 88.07(10) 2_666 2_557 ? O13 Zn3 Zn4 87.04(11) . 2_557 ? O8 Zn3 H27A 105.3 . . ? O27 Zn3 H27A 17.2 . . ? O20 Zn3 H27A 131.6 2_666 . ? O13 Zn3 H27A 95.7 . . ? Zn4 Zn3 H27A 49.7 2_557 . ? O26 Zn4 O27 170.17(13) 2_647 2_557 ? O26 Zn4 O14 95.04(14) 2_647 2_557 ? O27 Zn4 O14 94.14(13) 2_557 2_557 ? O26 Zn4 O27 89.93(12) 2_647 1_545 ? O27 Zn4 O27 80.83(12) 2_557 1_545 ? O14 Zn4 O27 174.92(12) 2_557 1_545 ? O26 Zn4 O4 96.78(13) 2_647 . ? O27 Zn4 O4 87.26(13) 2_557 . ? O14 Zn4 O4 86.64(15) 2_557 . ? O27 Zn4 O4 93.81(13) 1_545 . ? O26 Zn4 O19 85.68(13) 2_647 1_446 ? O27 Zn4 O19 90.89(13) 2_557 1_446 ? O14 Zn4 O19 89.49(14) 2_557 1_446 ? O27 Zn4 O19 89.85(12) 1_545 1_446 ? O4 Zn4 O19 175.58(13) . 1_446 ? O26 Zn4 Zn3 146.17(9) 2_647 2_557 ? O27 Zn4 Zn3 37.50(8) 2_557 2_557 ? O14 Zn4 Zn3 66.33(10) 2_557 2_557 ? O27 Zn4 Zn3 108.82(8) 1_545 2_557 ? O4 Zn4 Zn3 109.32(9) . 2_557 ? O19 Zn4 Zn3 67.06(9) 1_446 2_557 ? O26 Zn4 Zn4 129.33(10) 2_647 2_547 ? O27 Zn4 Zn4 41.35(8) 2_557 2_547 ? O14 Zn4 Zn4 135.49(10) 2_557 2_547 ? O27 Zn4 Zn4 39.48(8) 1_545 2_547 ? O4 Zn4 Zn4 90.79(10) . 2_547 ? O19 Zn4 Zn4 90.48(10) 1_446 2_547 ? Zn3 Zn4 Zn4 72.84(3) 2_557 2_547 ? O26 Zn4 Zn2 31.59(9) 2_647 2_647 ? O27 Zn4 Zn2 147.91(8) 2_557 2_647 ? O14 Zn4 Zn2 102.59(10) 2_557 2_647 ? O27 Zn4 Zn2 82.20(8) 1_545 2_647 ? O4 Zn4 Zn2 66.91(9) . 2_647 ? O19 Zn4 Zn2 116.12(9) 1_446 2_647 ? Zn3 Zn4 Zn2 168.80(2) 2_557 2_647 ? Zn4 Zn4 Zn2 117.06(3) 2_547 2_647 ? O15 Zn5 O21 113.88(16) 2_566 . ? O15 Zn5 O28 105.97(15) 2_566 . ? O21 Zn5 O28 106.60(13) . . ? O15 Zn5 O9 114.26(15) 2_566 . ? O21 Zn5 O9 109.15(15) . . ? O28 Zn5 O9 106.37(13) . . ? O15 Zn5 Zn1 144.80(13) 2_566 . ? O21 Zn5 Zn1 86.97(10) . . ? O28 Zn5 Zn1 39.02(9) . . ? O9 Zn5 Zn1 81.93(10) . . ? O15 Zn5 H28 96.4 2_566 . ? O21 Zn5 H28 123.5 . . ? O28 Zn5 H28 16.9 . . ? O9 Zn5 H28 98.8 . . ? Zn1 Zn5 H28 49.0 . . ? C7 O1 Zn1 129.8(3) . . ? C7 O2 Zn2 124.1(3) . . ? C8 O3 Zn2 124.3(3) . 2_647 ? C8 O4 Zn4 137.0(3) . . ? C15 O7 Zn2 124.5(3) . 2_657 ? C15 O8 Zn3 157.8(3) . . ? C16 O9 Zn5 125.3(3) . . ? C16 O10 Zn1 132.2(3) . . ? C23 O13 Zn3 116.9(3) . . ? C23 O14 Zn4 138.4(3) . 2_557 ? C24 O15 Zn5 127.7(4) . 2_566 ? C31 O19 Zn4 136.5(3) . 1_664 ? C31 O20 Zn3 119.0(3) . 2_666 ? C32 O21 Zn5 120.1(3) . . ? C32 O22 Zn1 137.8(3) . . ? Zn1 O25 H25A 92.0 . . ? Zn1 O25 H25B 114.3 . . ? H25A O25 H25B 143.3 . . ? Zn2 O26 Zn4 115.19(16) . 2_647 ? Zn2 O26 H26A 97.8 . . ? Zn4 O26 H26A 101.3 2_647 . ? Zn3 O27 Zn4 102.21(13) . 2_557 ? Zn3 O27 Zn4 133.42(16) . 1_565 ? Zn4 O27 Zn4 99.17(12) 2_557 1_565 ? Zn3 O27 H27A 100.5 . . ? Zn4 O27 H27A 112.0 2_557 . ? Zn4 O27 H27A 109.0 1_565 . ? Zn5 O28 Zn1 104.24(13) . . ? Zn5 O28 Zn1 128.19(15) . 2_656 ? Zn1 O28 Zn1 99.68(12) . 2_656 ? Zn5 O28 H28 107.2 . . ? Zn1 O28 H28 111.7 . . ? Zn1 O28 H28 105.4 2_656 . ? O6 N1 O5 122.8(5) . . ? O6 N1 C5 118.9(5) . . ? O5 N1 C5 118.3(4) . . ? O12 N2 O11 123.6(5) . . ? O12 N2 C13 118.2(4) . . ? O11 N2 C13 118.2(4) . . ? O18 N3 O17 123.8(4) . . ? O18 N3 C21 118.4(4) . . ? O17 N3 C21 117.8(4) . . ? O24 N4 O23 123.4(4) . . ? O24 N4 C29 118.8(4) . . ? O23 N4 C29 117.9(4) . . ? C6 C1 C2 119.5(4) . . ? C6 C1 C7 120.5(4) . . ? C2 C1 C7 120.0(4) . . ? C3 C2 C1 121.4(4) . . ? C3 C2 H2A 119.3 . . ? C1 C2 H2A 119.3 . . ? C2 C3 C4 119.0(4) . . ? C2 C3 C8 120.8(4) . . ? C4 C3 C8 120.2(4) . . ? C3 C4 C5 119.0(4) . . ? C3 C4 H4A 120.5 . . ? C5 C4 H4A 120.5 . . ? C6 C5 C4 122.3(4) . . ? C6 C5 N1 119.1(4) . . ? C4 C5 N1 118.6(4) . . ? C5 C6 C1 118.7(4) . . ? C5 C6 H6C 120.7 . . ? C1 C6 H6C 120.7 . . ? O1 C7 O2 125.4(4) . . ? O1 C7 C1 117.9(4) . . ? O2 C7 C1 116.6(4) . . ? O4 C8 O3 125.3(4) . . ? O4 C8 C3 119.2(4) . . ? O3 C8 C3 115.5(4) . . ? C14 C9 C10 119.4(4) . . ? C14 C9 C15 120.2(4) . . ? C10 C9 C15 120.4(4) . . ? C11 C10 C9 121.0(4) . . ? C11 C10 H10A 119.5 . . ? C9 C10 H10A 119.5 . . ? C12 C11 C10 120.1(4) . . ? C12 C11 C16 119.7(4) . . ? C10 C11 C16 120.1(4) . . ? C11 C12 C13 118.5(4) . . ? C11 C12 H12A 120.8 . . ? C13 C12 H12A 120.8 . . ? C14 C13 C12 122.0(4) . . ? C14 C13 N2 118.9(4) . . ? C12 C13 N2 119.1(4) . . ? C9 C14 C13 119.0(4) . . ? C9 C14 H14A 120.5 . . ? C13 C14 H14A 120.5 . . ? O8 C15 O7 125.7(4) . . ? O8 C15 C9 117.2(4) . . ? O7 C15 C9 117.1(4) . . ? O10 C16 O9 127.1(4) . . ? O10 C16 C11 117.8(4) . . ? O9 C16 C11 115.0(4) . . ? C18 C17 C22 120.6(4) . . ? C18 C17 C23 119.1(4) . . ? C22 C17 C23 120.2(4) . . ? C17 C18 C19 121.1(4) . . ? C17 C18 H18A 119.4 . . ? C19 C18 H18A 119.4 . . ? C18 C19 C20 118.9(4) . . ? C18 C19 C24 120.5(4) . . ? C20 C19 C24 120.5(4) . . ? C21 C20 C19 118.2(4) . . ? C21 C20 H20A 120.9 . . ? C19 C20 H20A 120.9 . . ? C20 C21 C22 123.6(4) . . ? C20 C21 N3 118.6(4) . . ? C22 C21 N3 117.7(4) . . ? C21 C22 C17 117.4(4) . . ? C21 C22 H22A 121.3 . . ? C17 C22 H22A 121.3 . . ? O13 C23 O14 126.6(5) . . ? O13 C23 C17 116.9(4) . . ? O14 C23 C17 116.4(4) . . ? O16 C24 O15 125.6(5) . . ? O16 C24 C19 120.4(5) . . ? O15 C24 C19 114.0(5) . . ? C30 C25 C26 119.6(4) . . ? C30 C25 C31 119.7(4) . . ? C26 C25 C31 120.8(4) . . ? C27 C26 C25 121.3(4) . . ? C27 C26 H26B 119.3 . . ? C25 C26 H26B 119.3 . . ? C26 C27 C28 119.1(4) . . ? C26 C27 C32 120.8(4) . . ? C28 C27 C32 120.1(4) . . ? C29 C28 C27 118.8(4) . . ? C29 C28 H28B 120.6 . . ? C27 C28 H28B 120.6 . . ? C28 C29 C30 122.9(4) . . ? C28 C29 N4 119.7(4) . . ? C30 C29 N4 117.4(4) . . ? C25 C30 C29 118.3(4) . . ? C25 C30 H30A 120.8 . . ? C29 C30 H30A 120.8 . . ? O19 C31 O20 125.3(4) . . ? O19 C31 C25 117.8(4) . . ? O20 C31 C25 116.8(4) . . ? O22 C32 O21 126.6(4) . . ? O22 C32 C27 118.5(4) . . ? O21 C32 C27 114.9(4) . . ? C33 N5 C37 118.8(8) . . ? C33 N5 H5A 119.7 . . ? C37 N5 H5A 121.6 . . ? C35 N6 H6A 119.8 . . ? C35 N6 H6B 120.2 . . ? H6A N6 H6B 120.0 . . ? N5 C33 C34 121.1(11) . . ? N5 C33 H33A 119.5 . . ? C34 C33 H33A 119.5 . . ? C35 C34 C33 122.7(11) . . ? C35 C34 H34A 118.7 . . ? C33 C34 H34A 118.7 . . ? N6 C35 C34 126.8(10) . . ? N6 C35 C36 115.4(8) . . ? C34 C35 C36 117.8(8) . . ? C37 C36 C35 114.4(8) . . ? C37 C36 H36A 122.8 . . ? C35 C36 H36A 122.8 . . ? C36 C37 N5 125.2(8) . . ? C36 C37 H37A 117.4 . . ? N5 C37 H37A 117.4 . . ? H29A O29 H29B 145.7 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O25 H25A O17 0.69 2.32 2.910(5) 145.0 2_656 O25 H25A O22 0.69 2.51 2.867(5) 115.1 . O25 H25B O26 0.71 2.08 2.782(5) 169.0 . O25 H25B O2 0.71 2.58 2.933(5) 113.2 . O27 H27A O11 0.65 2.29 2.923(5) 166.1 2_657 O28 H28 O18 0.68 2.34 2.982(5) 158.0 . N5 H5A O16 0.86 1.93 2.697(8) 148.6 1_655 N6 H6A O2 0.86 2.55 3.354(8) 155.4 2_656 N6 H6B O29 0.86 2.00 2.834(10) 164.5 . O29 H29A N6 0.82 2.71 2.834(10) 90.2 . _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 1.414 _refine_diff_density_min -0.633 _refine_diff_density_rms 0.101 # = = = END