# 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 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Jhy-Der Chen' _publ_contact_author_email jdchen@cycu.edu.tw loop_ _publ_author_name 'Jhy-Der Chen' 'Jian-Jr Cheng' 'Ya-Ting Chang' 'Chia-Jun Wu' 'Yi-Fen Hsu' 'Chai-Her Lin' D.Proserpio data_1 _database_code_depnum_ccdc_archive 'CCDC 791960' #TrackingRef '- all.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H24 N4 O7 Zn' _chemical_formula_weight 545.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.3732(4) _cell_length_b 19.2810(9) _cell_length_c 15.4445(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.890(2) _cell_angle_gamma 90.00 _cell_volume 2493.1(2) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 5343 _cell_measurement_theta_min 2.490 _cell_measurement_theta_max 23.764 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.454 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 1.036 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6251 _exptl_absorpt_correction_T_max 0.8624 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 23688 _diffrn_reflns_av_R_equivalents 0.0565 _diffrn_reflns_av_sigmaI/netI 0.0745 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 28.41 _reflns_number_total 6229 _reflns_number_gt 3503 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 (Bruker, 2008)' _computing_cell_refinement 'Bruker SAINTPLUS (Bruker, 2008)' _computing_data_reduction 'Bruker SAINTPLUS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 2008)' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0419P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6229 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0886 _refine_ls_R_factor_gt 0.0410 _refine_ls_wR_factor_ref 0.1035 _refine_ls_wR_factor_gt 0.0950 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _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 Zn Zn 0.38145(4) 0.083519(16) 0.636775(19) 0.03865(12) Uani 1 1 d . . . O1 O 1.0846(3) 0.01653(14) 0.89802(19) 0.0924(9) Uani 1 1 d . . . O2 O 1.4383(3) -0.26600(12) 1.12609(15) 0.0723(7) Uani 1 1 d . . . O3 O 0.4079(3) 0.12426(11) 0.51955(13) 0.0571(6) Uani 1 1 d . . . O4 O 0.5761(3) 0.18149(11) 0.60049(13) 0.0668(6) Uani 1 1 d . . . O5 O 0.5732(3) 0.34021(15) 0.16999(14) 0.0894(8) Uani 1 1 d . . . O6 O 0.7941(3) 0.36995(12) 0.23621(13) 0.0640(6) Uani 1 1 d . . . N1 N 0.5719(3) 0.03589(12) 0.69738(14) 0.0440(6) Uani 1 1 d . . . N2 N 0.9233(3) -0.06670(13) 0.84339(17) 0.0628(7) Uani 1 1 d . . . H2A H 0.9129 -0.1110 0.8407 0.075 Uiso 1 1 calc R . . N3 N 1.4902(3) -0.32884(12) 1.00534(15) 0.0507(6) Uani 1 1 d . . . H3A H 1.4741 -0.3295 0.9502 0.061 Uiso 1 1 calc R . . N4 N 1.7419(3) -0.50180(11) 1.09641(14) 0.0402(6) Uani 1 1 d . . . C1 C 0.5792(4) -0.03312(17) 0.7046(2) 0.0621(9) Uani 1 1 d . . . H1A H 0.5029 -0.0596 0.6752 0.075 Uiso 1 1 calc R . . C2 C 0.6922(4) -0.06651(17) 0.7527(2) 0.0689(10) Uani 1 1 d . . . H2B H 0.6906 -0.1146 0.7565 0.083 Uiso 1 1 calc R . . C3 C 0.8104(4) -0.02921(16) 0.79634(19) 0.0514(8) Uani 1 1 d . . . C4 C 0.8062(4) 0.04253(15) 0.78794(19) 0.0534(8) Uani 1 1 d . . . H4B H 0.8838 0.0700 0.8146 0.064 Uiso 1 1 calc R . . C5 C 0.6867(4) 0.07173(15) 0.74000(19) 0.0523(8) Uani 1 1 d . . . H5A H 0.6838 0.1199 0.7363 0.063 Uiso 1 1 calc R . . C6 C 1.0475(4) -0.04401(19) 0.8929(2) 0.0660(9) Uani 1 1 d . A . C7 C 1.1286(5) -0.1044(2) 0.9412(3) 0.0866(13) Uani 1 1 d . . . C8 C 1.302(2) -0.1098(9) 0.9126(11) 0.106(6) Uani 0.30 1 d P A 1 H8A H 1.3552 -0.0662 0.9250 0.127 Uiso 0.30 1 calc PR A 1 H8B H 1.3030 -0.1166 0.8503 0.127 Uiso 0.30 1 calc PR A 1 C9 C 1.4061(16) -0.1740(13) 0.9599(11) 0.134(9) Uani 0.30 1 d P A 1 H9A H 1.4800 -0.1901 0.9165 0.160 Uiso 0.30 1 calc PR A 1 H9B H 1.4709 -0.1520 1.0046 0.160 Uiso 0.30 1 calc PR A 1 C8' C 1.2814(8) -0.0899(3) 0.9770(4) 0.0727(17) Uani 0.70 1 d P A 2 H8C H 1.2750 -0.0481 1.0116 0.087 Uiso 0.70 1 calc PR A 2 H8D H 1.3547 -0.0811 0.9303 0.087 Uiso 0.70 1 calc PR A 2 C9' C 1.3476(7) -0.1474(2) 1.0326(4) 0.0769(17) Uani 0.70 1 d P A 2 H9C H 1.2806 -0.1523 1.0829 0.092 Uiso 0.70 1 calc PR A 2 H9D H 1.4532 -0.1340 1.0530 0.092 Uiso 0.70 1 calc PR A 2 C10 C 1.3600(6) -0.2185(2) 0.9881(3) 0.0864(15) Uani 1 1 d . . . C11 C 1.4323(4) -0.27184(17) 1.0477(2) 0.0584(9) Uani 1 1 d . A . C12 C 1.5710(3) -0.38554(14) 1.03922(17) 0.0405(7) Uani 1 1 d . . . C13 C 1.5839(4) -0.40195(16) 1.12674(19) 0.0573(9) Uani 1 1 d . . . H13A H 1.5362 -0.3741 1.1681 0.069 Uiso 1 1 calc R . . C14 C 1.6685(4) -0.46005(16) 1.15104(18) 0.0555(8) Uani 1 1 d . . . H14A H 1.6745 -0.4708 1.2097 0.067 Uiso 1 1 calc R . . C15 C 1.7264(3) -0.48608(15) 1.01254(17) 0.0441(7) Uani 1 1 d . . . H15A H 1.7752 -0.5148 0.9724 0.053 Uiso 1 1 calc R . . C16 C 1.6427(3) -0.42996(14) 0.98264(17) 0.0438(7) Uani 1 1 d . . . H16A H 1.6343 -0.4219 0.9234 0.053 Uiso 1 1 calc R . . C17 C 0.5056(3) 0.17081(14) 0.52843(17) 0.0377(6) Uani 1 1 d . . . C18 C 0.5466(3) 0.21637(14) 0.45398(17) 0.0410(7) Uani 1 1 d . . . C19 C 0.4637(4) 0.20934(16) 0.37757(19) 0.0550(8) Uani 1 1 d . . . H19A H 0.3822 0.1767 0.3733 0.066 Uiso 1 1 calc R . . C20 C 0.4990(4) 0.24997(17) 0.30641(18) 0.0582(9) Uani 1 1 d . . . H20A H 0.4400 0.2447 0.2553 0.070 Uiso 1 1 calc R . . C21 C 0.6199(3) 0.29776(14) 0.31047(17) 0.0419(7) Uani 1 1 d . . . C22 C 0.7024(3) 0.30608(16) 0.38909(18) 0.0489(8) Uani 1 1 d . . . H22A H 0.7835 0.3388 0.3938 0.059 Uiso 1 1 calc R . . C23 C 0.6642(3) 0.26615(15) 0.45934(18) 0.0477(7) Uani 1 1 d . . . H23A H 0.7189 0.2728 0.5116 0.057 Uiso 1 1 calc R . . C24 C 0.6652(3) 0.33928(14) 0.23157(17) 0.0381(6) Uani 1 1 d . . . O7 O 0.6177(4) 0.29245(12) 0.69913(16) 0.1150(12) Uani 1 1 d . . . H7C H 0.6145 0.2564 0.6674 0.138 Uiso 1 1 d R . . H7F H 0.6080 0.2801 0.7516 0.138 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 Zn 0.0475(2) 0.03656(18) 0.03201(18) -0.00164(15) 0.00358(13) -0.00021(16) O1 0.0903(19) 0.0642(18) 0.121(2) 0.0189(16) -0.0479(16) -0.0016(15) O2 0.0877(17) 0.0644(15) 0.0645(16) -0.0076(13) -0.0079(13) 0.0256(13) O3 0.0698(15) 0.0510(13) 0.0506(13) 0.0126(11) 0.0053(11) -0.0112(11) O4 0.1131(19) 0.0482(13) 0.0391(13) 0.0072(10) 0.0017(12) -0.0040(13) O5 0.110(2) 0.106(2) 0.0510(14) 0.0338(14) -0.0200(14) -0.0234(17) O6 0.0704(16) 0.0742(16) 0.0477(13) 0.0231(12) 0.0080(11) -0.0011(13) N1 0.0562(15) 0.0351(14) 0.0406(14) -0.0010(11) -0.0020(12) 0.0032(11) N2 0.082(2) 0.0443(16) 0.0618(17) 0.0049(13) -0.0214(15) 0.0131(14) N3 0.0609(16) 0.0473(16) 0.0436(14) 0.0039(12) -0.0120(12) 0.0094(13) N4 0.0481(14) 0.0414(13) 0.0312(12) 0.0018(11) 0.0050(11) 0.0057(11) C1 0.072(2) 0.045(2) 0.069(2) 0.0037(17) -0.0207(18) -0.0006(17) C2 0.089(3) 0.0369(19) 0.080(3) 0.0015(17) -0.024(2) 0.0048(18) C3 0.067(2) 0.0443(18) 0.0430(17) 0.0055(15) -0.0026(15) 0.0113(16) C4 0.065(2) 0.0423(19) 0.0528(19) 0.0004(15) -0.0153(16) 0.0020(16) C5 0.069(2) 0.0356(17) 0.0521(19) 0.0024(14) -0.0097(16) 0.0051(16) C6 0.071(2) 0.059(2) 0.068(2) 0.009(2) -0.0079(19) 0.014(2) C7 0.080(3) 0.081(3) 0.098(3) 0.021(2) -0.030(2) 0.027(2) C8 0.103(13) 0.100(13) 0.114(14) 0.064(11) 0.009(12) 0.027(10) C9 0.043(8) 0.26(3) 0.095(14) 0.069(17) -0.006(8) 0.021(13) C8' 0.080(4) 0.044(3) 0.093(5) -0.001(3) -0.024(4) 0.005(3) C9' 0.085(4) 0.044(3) 0.101(4) -0.009(3) -0.053(3) 0.024(3) C10 0.127(4) 0.057(3) 0.075(3) 0.021(2) -0.001(3) 0.038(2) C11 0.058(2) 0.051(2) 0.066(2) 0.0024(18) -0.0088(18) 0.0064(16) C12 0.0431(17) 0.0381(16) 0.0402(17) 0.0039(13) -0.0025(13) 0.0015(13) C13 0.074(2) 0.060(2) 0.0374(17) -0.0003(15) 0.0028(16) 0.0291(17) C14 0.074(2) 0.062(2) 0.0306(16) 0.0058(15) 0.0035(15) 0.0198(18) C15 0.0540(19) 0.0468(18) 0.0317(16) 0.0009(13) 0.0066(13) 0.0009(14) C16 0.0547(18) 0.0472(19) 0.0295(15) 0.0061(13) -0.0017(13) -0.0017(14) C17 0.0509(18) 0.0289(15) 0.0336(16) 0.0063(12) 0.0112(13) 0.0086(14) C18 0.0500(17) 0.0368(16) 0.0361(16) 0.0006(13) 0.0013(13) -0.0018(13) C19 0.066(2) 0.052(2) 0.0470(19) 0.0057(15) -0.0062(16) -0.0210(16) C20 0.073(2) 0.063(2) 0.0380(17) 0.0079(16) -0.0152(15) -0.0184(18) C21 0.0464(17) 0.0455(17) 0.0339(16) 0.0049(13) 0.0018(13) -0.0009(14) C22 0.0450(18) 0.0560(19) 0.0456(18) 0.0080(15) -0.0025(14) -0.0116(15) C23 0.0516(18) 0.0569(19) 0.0344(16) 0.0078(14) -0.0053(14) -0.0065(15) C24 0.0432(17) 0.0393(16) 0.0318(15) 0.0080(13) 0.0020(13) 0.0018(14) O7 0.228(4) 0.0478(15) 0.0681(18) -0.0048(13) -0.028(2) -0.0177(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 Zn O6 1.932(2) 4_566 ? Zn O3 1.9892(19) . ? Zn N4 2.053(2) 4_455 ? Zn N1 2.054(2) . ? Zn O4 2.562(2) . ? O1 C6 1.210(4) . ? O2 C11 1.217(4) . ? O3 C17 1.221(3) . ? O4 C17 1.268(3) . ? O5 C24 1.215(3) . ? O6 C24 1.232(3) . ? O6 Zn 1.932(2) 4_665 ? N1 C1 1.337(4) . ? N1 C5 1.347(3) . ? N2 C6 1.353(4) . ? N2 C3 1.387(4) . ? N2 H2A 0.8600 . ? N3 C11 1.371(4) . ? N3 C12 1.384(3) . ? N3 H3A 0.8600 . ? N4 C14 1.324(3) . ? N4 C15 1.335(3) . ? N4 Zn 2.053(2) 4_756 ? C1 C2 1.356(4) . ? C1 H1A 0.9300 . ? C2 C3 1.389(4) . ? C2 H2B 0.9300 . ? C3 C4 1.390(4) . ? C4 C5 1.358(4) . ? C4 H4B 0.9300 . ? C5 H5A 0.9300 . ? C6 C7 1.535(5) . ? C7 C8' 1.414(7) . ? C7 C8 1.527(16) . ? C8 C9 1.68(2) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.040(19) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C8' C9' 1.502(7) . ? C8' H8C 0.9700 . ? C8' H8D 0.9700 . ? C9' C10 1.537(7) . ? C9' H9C 0.9700 . ? C9' H9D 0.9700 . ? C10 C11 1.501(5) . ? C12 C16 1.369(4) . ? C12 C13 1.391(4) . ? C13 C14 1.374(4) . ? C13 H13A 0.9300 . ? C14 H14A 0.9300 . ? C15 C16 1.366(4) . ? C15 H15A 0.9300 . ? C16 H16A 0.9300 . ? C17 C18 1.491(4) . ? C18 C19 1.366(4) . ? C18 C23 1.377(4) . ? C19 C20 1.385(4) . ? C19 H19A 0.9300 . ? C20 C21 1.370(4) . ? C20 H20A 0.9300 . ? C21 C22 1.396(4) . ? C21 C24 1.511(4) . ? C22 C23 1.372(4) . ? C22 H22A 0.9300 . ? C23 H23A 0.9300 . ? O7 H7C 0.8503 . ? O7 H7F 0.8498 . ? 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 O6 Zn O3 126.08(10) 4_566 . ? O6 Zn N4 112.15(9) 4_566 4_455 ? O3 Zn N4 95.61(9) . 4_455 ? O6 Zn N1 98.41(9) 4_566 . ? O3 Zn N1 119.65(9) . . ? N4 Zn N1 103.28(9) 4_455 . ? O6 Zn O4 94.66(8) 4_566 . ? O3 Zn O4 55.22(8) . . ? N4 Zn O4 149.36(8) 4_455 . ? N1 Zn O4 86.41(8) . . ? C17 O3 Zn 105.79(18) . . ? C17 O4 Zn 77.50(16) . . ? C24 O6 Zn 121.25(18) . 4_665 ? C1 N1 C5 116.0(3) . . ? C1 N1 Zn 121.1(2) . . ? C5 N1 Zn 122.44(19) . . ? C6 N2 C3 129.7(3) . . ? C6 N2 H2A 115.1 . . ? C3 N2 H2A 115.1 . . ? C11 N3 C12 128.8(3) . . ? C11 N3 H3A 115.6 . . ? C12 N3 H3A 115.6 . . ? C14 N4 C15 116.2(2) . . ? C14 N4 Zn 122.73(18) . 4_756 ? C15 N4 Zn 121.00(18) . 4_756 ? N1 C1 C2 123.3(3) . . ? N1 C1 H1A 118.4 . . ? C2 C1 H1A 118.4 . . ? C1 C2 C3 120.4(3) . . ? C1 C2 H2B 119.8 . . ? C3 C2 H2B 119.8 . . ? N2 C3 C2 117.3(3) . . ? N2 C3 C4 125.7(3) . . ? C2 C3 C4 117.0(3) . . ? C5 C4 C3 118.7(3) . . ? C5 C4 H4B 120.6 . . ? C3 C4 H4B 120.6 . . ? N1 C5 C4 124.6(3) . . ? N1 C5 H5A 117.7 . . ? C4 C5 H5A 117.7 . . ? O1 C6 N2 122.9(3) . . ? O1 C6 C7 126.0(4) . . ? N2 C6 C7 111.1(3) . . ? C8' C7 C8 43.0(7) . . ? C8' C7 C6 115.6(4) . . ? C8 C7 C6 109.1(6) . . ? C7 C8 C9 114.5(10) . . ? C7 C8 H8A 108.6 . . ? C9 C8 H8A 108.6 . . ? C7 C8 H8B 108.6 . . ? C9 C8 H8B 108.6 . . ? H8A C8 H8B 107.6 . . ? C10 C9 C8 126.7(13) . . ? C10 C9 H9A 105.6 . . ? C8 C9 H9A 105.6 . . ? C10 C9 H9B 105.6 . . ? C8 C9 H9B 105.6 . . ? H9A C9 H9B 106.1 . . ? C7 C8' C9' 113.7(5) . . ? C7 C8' H8C 108.8 . . ? C9' C8' H8C 108.8 . . ? C7 C8' H8D 108.8 . . ? C9' C8' H8D 108.8 . . ? H8C C8' H8D 107.7 . . ? C8' C9' C10 115.4(4) . . ? C8' C9' H9C 108.4 . . ? C10 C9' H9C 108.4 . . ? C8' C9' H9D 108.4 . . ? C10 C9' H9D 108.4 . . ? H9C C9' H9D 107.5 . . ? C9 C10 C11 132.3(10) . . ? C9 C10 C9' 58.6(13) . . ? C11 C10 C9' 111.5(4) . . ? O2 C11 N3 122.6(3) . . ? O2 C11 C10 123.8(3) . . ? N3 C11 C10 113.5(3) . . ? C16 C12 N3 118.0(2) . . ? C16 C12 C13 116.7(3) . . ? N3 C12 C13 125.3(3) . . ? C14 C13 C12 118.9(3) . . ? C14 C13 H13A 120.6 . . ? C12 C13 H13A 120.6 . . ? N4 C14 C13 124.3(3) . . ? N4 C14 H14A 117.8 . . ? C13 C14 H14A 117.8 . . ? N4 C15 C16 123.3(3) . . ? N4 C15 H15A 118.3 . . ? C16 C15 H15A 118.3 . . ? C15 C16 C12 120.5(3) . . ? C15 C16 H16A 119.7 . . ? C12 C16 H16A 119.7 . . ? O3 C17 O4 121.3(2) . . ? O3 C17 C18 120.5(3) . . ? O4 C17 C18 118.1(3) . . ? C19 C18 C23 118.3(3) . . ? C19 C18 C17 119.2(3) . . ? C23 C18 C17 122.5(2) . . ? C18 C19 C20 121.2(3) . . ? C18 C19 H19A 119.4 . . ? C20 C19 H19A 119.4 . . ? C21 C20 C19 120.7(3) . . ? C21 C20 H20A 119.6 . . ? C19 C20 H20A 119.6 . . ? C20 C21 C22 118.2(3) . . ? C20 C21 C24 120.9(2) . . ? C22 C21 C24 120.9(3) . . ? C23 C22 C21 120.4(3) . . ? C23 C22 H22A 119.8 . . ? C21 C22 H22A 119.8 . . ? C22 C23 C18 121.2(3) . . ? C22 C23 H23A 119.4 . . ? C18 C23 H23A 119.4 . . ? O5 C24 O6 125.7(3) . . ? O5 C24 C21 118.4(3) . . ? O6 C24 C21 116.0(2) . . ? H7C O7 H7F 108.6 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.41 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.391 _refine_diff_density_min -0.265 _refine_diff_density_rms 0.059 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 791961' #TrackingRef '- all.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H26 Cd N4 O8' _chemical_formula_weight 610.89 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 9.0807(15) _cell_length_b 11.3600(16) _cell_length_c 13.2607(19) _cell_angle_alpha 92.714(13) _cell_angle_beta 106.281(16) _cell_angle_gamma 107.242(14) _cell_volume 1241.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 27 _cell_measurement_theta_min 4.62 _cell_measurement_theta_max 12.40 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.634 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 620 _exptl_absorpt_coefficient_mu 0.936 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8579 _exptl_absorpt_correction_T_max 0.9998 _exptl_absorpt_process_details '(XSCANS; Siemens, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 5290 _diffrn_reflns_av_R_equivalents 0.0258 _diffrn_reflns_av_sigmaI/netI 0.0326 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4384 _reflns_number_gt 4128 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0229P)^2^+0.6370P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4384 _refine_ls_number_parameters 340 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0258 _refine_ls_R_factor_gt 0.0236 _refine_ls_wR_factor_ref 0.0612 _refine_ls_wR_factor_gt 0.0599 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _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 Cd Cd 0.044489(18) 0.198438(13) 0.672498(11) 0.02657(6) Uani 1 1 d . . . O1 O 0.4474(3) -0.19942(19) 0.98036(16) 0.0671(7) Uani 1 1 d . . . O2 O -0.6817(3) 0.1804(2) 0.23393(18) 0.0650(6) Uani 1 1 d . . . O3 O 0.0771(3) 0.26310(18) 0.84519(15) 0.0507(5) Uani 1 1 d . . . O4 O -0.0262(3) 0.37317(19) 0.73287(15) 0.0559(5) Uani 1 1 d . . . O5 O 0.3486(3) 0.3158(2) 0.69401(16) 0.0592(6) Uani 1 1 d . . . O6 O 0.1481(2) 0.2850(2) 0.54937(16) 0.0593(6) Uani 1 1 d . . . N1 N 0.1097(2) 0.02785(17) 0.72338(15) 0.0319(4) Uani 1 1 d . . . N2 N 0.2920(3) -0.26349(18) 0.80962(16) 0.0357(4) Uani 1 1 d . . . H2A H 0.2593 -0.3238 0.7585 0.043 Uiso 1 1 calc R . . N3 N -0.2085(2) 0.12832(19) 0.54885(16) 0.0350(4) Uani 1 1 d . . . N4 N -0.5985(2) 0.0121(2) 0.26807(16) 0.0377(5) Uani 1 1 d . . . H4A H -0.6204 -0.0647 0.2438 0.045 Uiso 1 1 calc R . . C1 C 0.2312(3) 0.0440(2) 0.81288(18) 0.0335(5) Uani 1 1 d . . . H1A H 0.2745 0.1219 0.8542 0.040 Uiso 1 1 calc R . . C2 C 0.2966(3) -0.0471(2) 0.84806(18) 0.0339(5) Uani 1 1 d . . . H2B H 0.3817 -0.0304 0.9109 0.041 Uiso 1 1 calc R . . C3 C 0.2328(3) -0.1646(2) 0.78762(18) 0.0297(5) Uani 1 1 d . . . C4 C 0.1051(3) -0.1827(2) 0.6950(2) 0.0374(5) Uani 1 1 d . . . H4B H 0.0576 -0.2601 0.6529 0.045 Uiso 1 1 calc R . . C5 C 0.0501(3) -0.0864(2) 0.6664(2) 0.0398(6) Uani 1 1 d . . . H5A H -0.0341 -0.1003 0.6034 0.048 Uiso 1 1 calc R . . C6 C 0.3951(3) -0.2767(2) 0.9019(2) 0.0403(6) Uani 1 1 d . . . C7 C 0.4400(4) -0.3942(2) 0.8968(2) 0.0463(6) Uani 1 1 d . . . H7A H 0.5317 -0.3791 0.8698 0.056 Uiso 1 1 calc R . . H7B H 0.3497 -0.4593 0.8475 0.056 Uiso 1 1 calc R . . C8 C 0.4829(3) -0.4387(2) 1.0041(2) 0.0414(6) Uani 1 1 d . . . H8A H 0.3939 -0.4490 1.0333 0.062 Uiso 1 1 calc R . . H8B H 0.5777 -0.3761 1.0523 0.062 Uiso 1 1 calc R . . C9 C -0.2731(3) 0.0109(2) 0.4992(2) 0.0414(6) Uani 1 1 d . . . H9A H -0.2282 -0.0479 0.5291 0.050 Uiso 1 1 calc R . . C10 C -0.4004(3) -0.0283(2) 0.4078(2) 0.0393(6) Uani 1 1 d . . . H10A H -0.4387 -0.1110 0.3764 0.047 Uiso 1 1 calc R . . C11 C -0.4721(3) 0.0567(2) 0.36229(18) 0.0327(5) Uani 1 1 d . . . C12 C -0.4112(3) 0.1789(2) 0.41439(19) 0.0371(5) Uani 1 1 d . . . H12A H -0.4574 0.2385 0.3882 0.045 Uiso 1 1 calc R . . C13 C -0.2809(3) 0.2089(2) 0.50560(19) 0.0365(5) Uani 1 1 d . . . H13A H -0.2405 0.2906 0.5394 0.044 Uiso 1 1 calc R . . C14 C -0.6933(3) 0.0736(2) 0.20820(19) 0.0382(5) Uani 1 1 d . . . C15 C -0.8130(3) -0.0089(3) 0.1085(2) 0.0438(6) Uani 1 1 d . . . H15A H -0.8720 -0.0859 0.1281 0.053 Uiso 1 1 calc R . . H15B H -0.7532 -0.0297 0.0640 0.053 Uiso 1 1 calc R . . C16 C -0.9341(3) 0.0475(2) 0.0441(2) 0.0407(6) Uani 1 1 d . . . H16A H -0.8782 0.1163 0.0137 0.061 Uiso 1 1 calc R . . H16B H -0.9831 0.0801 0.0905 0.061 Uiso 1 1 calc R . . C17 C 0.0209(3) 0.3498(2) 0.8257(2) 0.0401(6) Uani 1 1 d . . . C18 C 0.0101(3) 0.4285(2) 0.9160(2) 0.0375(5) Uani 1 1 d . . . C19 C -0.0416(4) 0.5304(3) 0.8983(2) 0.0458(6) Uani 1 1 d . . . H19A H -0.0698 0.5511 0.8301 0.069 Uiso 1 1 calc R . . C20 C 0.0516(4) 0.3979(2) 1.0174(2) 0.0463(6) Uani 1 1 d . . . H20A H 0.0863 0.3291 1.0294 0.070 Uiso 1 1 calc R . . C21 C 0.2947(3) 0.3340(2) 0.60180(19) 0.0350(5) Uani 1 1 d . . . C22 C 0.4022(3) 0.4192(2) 0.54846(19) 0.0345(5) Uani 1 1 d . . . C23 C 0.5585(4) 0.4880(4) 0.6045(3) 0.0710(11) Uani 1 1 d . . . H23A H 0.6000 0.4809 0.6756 0.107 Uiso 1 1 calc R . . C24 C 0.3451(4) 0.4319(4) 0.4443(3) 0.0714(11) Uani 1 1 d . . . H24A H 0.2391 0.3858 0.4053 0.107 Uiso 1 1 calc R . . O7 O -0.6150(3) -0.2357(2) 0.18626(19) 0.0654(6) Uani 1 1 d . . . H7E H -0.6060 -0.2320 0.1243 0.078 Uiso 1 1 d R . . H7F H -0.5512 -0.2724 0.2198 0.078 Uiso 1 1 d R . . O8 O 0.1101(4) -0.4564(2) 0.6216(2) 0.0786(8) Uani 1 1 d . . . H8C H 0.060(5) -0.515(4) 0.663(4) 0.094 Uiso 1 1 d . . . H8D H 0.075(6) -0.491(4) 0.569(3) 0.094 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 Cd 0.03034(10) 0.02584(9) 0.02321(9) 0.00250(6) 0.00673(6) 0.01023(6) O1 0.1038(18) 0.0448(11) 0.0367(11) -0.0019(9) -0.0172(11) 0.0387(12) O2 0.0612(13) 0.0511(12) 0.0608(13) -0.0062(10) -0.0205(11) 0.0256(11) O3 0.0744(14) 0.0436(10) 0.0433(10) -0.0013(8) 0.0247(10) 0.0273(10) O4 0.0809(15) 0.0546(12) 0.0349(10) -0.0035(9) 0.0179(10) 0.0274(11) O5 0.0516(12) 0.0702(14) 0.0491(12) 0.0256(10) 0.0164(10) 0.0064(10) O6 0.0402(11) 0.0736(14) 0.0470(11) 0.0158(10) 0.0135(9) -0.0078(10) N1 0.0345(10) 0.0290(9) 0.0319(10) 0.0036(8) 0.0061(8) 0.0139(8) N2 0.0453(11) 0.0274(10) 0.0307(10) 0.0027(8) 0.0011(9) 0.0165(9) N3 0.0283(10) 0.0397(11) 0.0321(10) 0.0032(8) 0.0020(8) 0.0110(8) N4 0.0332(10) 0.0398(11) 0.0318(10) 0.0007(8) -0.0024(8) 0.0119(9) C1 0.0386(12) 0.0284(11) 0.0301(11) -0.0001(9) 0.0049(10) 0.0121(10) C2 0.0387(12) 0.0329(12) 0.0253(11) 0.0021(9) 0.0002(9) 0.0138(10) C3 0.0323(11) 0.0276(11) 0.0297(11) 0.0070(9) 0.0078(9) 0.0117(9) C4 0.0351(12) 0.0268(11) 0.0395(13) -0.0033(9) -0.0034(10) 0.0094(10) C5 0.0357(13) 0.0352(13) 0.0399(13) -0.0025(10) -0.0048(10) 0.0157(10) C6 0.0500(15) 0.0300(12) 0.0350(13) 0.0070(10) 0.0008(11) 0.0158(11) C7 0.0604(17) 0.0368(13) 0.0405(14) 0.0085(11) 0.0028(12) 0.0254(13) C8 0.0493(15) 0.0315(13) 0.0387(13) 0.0074(10) 0.0002(11) 0.0186(11) C9 0.0364(13) 0.0402(13) 0.0420(14) 0.0030(11) -0.0013(11) 0.0172(11) C10 0.0342(12) 0.0371(13) 0.0389(13) -0.0028(10) 0.0008(10) 0.0117(10) C11 0.0267(11) 0.0410(12) 0.0279(11) 0.0039(9) 0.0053(9) 0.0103(10) C12 0.0362(12) 0.0385(13) 0.0343(12) 0.0049(10) 0.0035(10) 0.0158(10) C13 0.0348(12) 0.0332(12) 0.0356(12) 0.0001(10) 0.0049(10) 0.0087(10) C14 0.0300(12) 0.0444(14) 0.0336(12) 0.0050(10) 0.0018(10) 0.0102(10) C15 0.0361(13) 0.0481(15) 0.0364(13) 0.0027(11) -0.0042(11) 0.0130(11) C16 0.0347(12) 0.0458(14) 0.0352(13) 0.0083(11) 0.0014(11) 0.0121(11) C17 0.0415(13) 0.0345(13) 0.0396(14) -0.0061(10) 0.0171(11) 0.0029(11) C18 0.0416(13) 0.0307(12) 0.0378(13) -0.0049(10) 0.0155(11) 0.0066(10) C19 0.0618(17) 0.0432(14) 0.0333(13) 0.0006(11) 0.0148(12) 0.0188(13) C20 0.0653(18) 0.0379(13) 0.0404(14) -0.0006(11) 0.0182(13) 0.0225(13) C21 0.0392(13) 0.0290(11) 0.0385(13) 0.0024(10) 0.0171(11) 0.0089(10) C22 0.0340(12) 0.0325(12) 0.0371(13) 0.0054(10) 0.0133(10) 0.0083(10) C23 0.0453(17) 0.096(3) 0.0420(16) 0.0274(17) 0.0039(13) -0.0140(17) C24 0.0377(15) 0.095(3) 0.0466(17) 0.0220(17) 0.0018(13) -0.0209(16) O7 0.0687(14) 0.0553(13) 0.0607(14) -0.0066(10) 0.0047(11) 0.0200(11) O8 0.126(2) 0.0395(12) 0.0705(17) 0.0086(11) 0.0316(17) 0.0265(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd O6 2.232(2) . ? Cd N1 2.2674(19) . ? Cd O3 2.2810(19) . ? Cd N3 2.298(2) . ? Cd O4 2.426(2) . ? Cd O5 2.613(2) . ? Cd C17 2.695(2) . ? O1 C6 1.212(3) . ? O2 C14 1.210(3) . ? O3 C17 1.244(3) . ? O4 C17 1.253(3) . ? O5 C21 1.235(3) . ? O6 C21 1.254(3) . ? N1 C1 1.336(3) . ? N1 C5 1.345(3) . ? N2 C6 1.362(3) . ? N2 C3 1.391(3) . ? N2 H2A 0.8600 . ? N3 C9 1.339(3) . ? N3 C13 1.339(3) . ? N4 C14 1.373(3) . ? N4 C11 1.388(3) . ? N4 H4A 0.8600 . ? C1 C2 1.376(3) . ? C1 H1A 0.9300 . ? C2 C3 1.393(3) . ? C2 H2B 0.9300 . ? C3 C4 1.390(3) . ? C4 C5 1.359(3) . ? C4 H4B 0.9300 . ? C5 H5A 0.9300 . ? C6 C7 1.510(3) . ? C7 C8 1.518(4) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C8 1.520(5) 2_647 ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.364(3) . ? C9 H9A 0.9300 . ? C10 C11 1.389(3) . ? C10 H10A 0.9300 . ? C11 C12 1.396(3) . ? C12 C13 1.378(3) . ? C12 H12A 0.9300 . ? C13 H13A 0.9300 . ? C14 C15 1.510(3) . ? C15 C16 1.515(3) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C16 1.515(5) 2_355 ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.503(3) . ? C18 C19 1.379(4) . ? C18 C20 1.382(4) . ? C19 C20 1.391(4) 2_567 ? C19 H19A 0.9300 . ? C20 C19 1.391(4) 2_567 ? C20 H20A 0.9300 . ? C21 C22 1.510(3) . ? C22 C24 1.363(4) . ? C22 C23 1.369(4) . ? C23 C24 1.383(4) 2_666 ? C23 H23A 0.9300 . ? C24 C23 1.383(4) 2_666 ? C24 H24A 0.9300 . ? O7 H7E 0.8501 . ? O7 H7F 0.8503 . ? O8 H8C 0.97(5) . ? O8 H8D 0.72(4) . ? 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 O6 Cd N1 115.39(8) . . ? O6 Cd O3 134.17(8) . . ? N1 Cd O3 89.02(7) . . ? O6 Cd N3 89.77(8) . . ? N1 Cd N3 106.97(7) . . ? O3 Cd N3 120.95(8) . . ? O6 Cd O4 97.58(8) . . ? N1 Cd O4 143.20(7) . . ? O3 Cd O4 55.06(7) . . ? N3 Cd O4 88.10(7) . . ? O6 Cd O5 52.56(7) . . ? N1 Cd O5 89.90(7) . . ? O3 Cd O5 92.11(8) . . ? N3 Cd O5 142.25(7) . . ? O4 Cd O5 98.30(8) . . ? O6 Cd C17 118.18(9) . . ? N1 Cd C17 116.01(8) . . ? O3 Cd C17 27.36(8) . . ? N3 Cd C17 105.62(8) . . ? O4 Cd C17 27.70(8) . . ? O5 Cd C17 96.12(8) . . ? C17 O3 Cd 95.19(16) . . ? C17 O4 Cd 88.18(16) . . ? C21 O5 Cd 83.94(15) . . ? C21 O6 Cd 101.52(16) . . ? C1 N1 C5 115.9(2) . . ? C1 N1 Cd 117.48(15) . . ? C5 N1 Cd 126.19(16) . . ? C6 N2 C3 128.1(2) . . ? C6 N2 H2A 115.9 . . ? C3 N2 H2A 115.9 . . ? C9 N3 C13 115.8(2) . . ? C9 N3 Cd 121.78(16) . . ? C13 N3 Cd 120.63(16) . . ? C14 N4 C11 129.0(2) . . ? C14 N4 H4A 115.5 . . ? C11 N4 H4A 115.5 . . ? N1 C1 C2 124.4(2) . . ? N1 C1 H1A 117.8 . . ? C2 C1 H1A 117.8 . . ? C1 C2 C3 118.7(2) . . ? C1 C2 H2B 120.7 . . ? C3 C2 H2B 120.7 . . ? C4 C3 N2 117.3(2) . . ? C4 C3 C2 117.4(2) . . ? N2 C3 C2 125.2(2) . . ? C5 C4 C3 119.5(2) . . ? C5 C4 H4B 120.2 . . ? C3 C4 H4B 120.2 . . ? N1 C5 C4 124.2(2) . . ? N1 C5 H5A 117.9 . . ? C4 C5 H5A 117.9 . . ? O1 C6 N2 122.4(2) . . ? O1 C6 C7 123.4(2) . . ? N2 C6 C7 114.2(2) . . ? C6 C7 C8 112.7(2) . . ? C6 C7 H7A 109.0 . . ? C8 C7 H7A 109.0 . . ? C6 C7 H7B 109.0 . . ? C8 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? C7 C8 C8 111.8(3) . 2_647 ? C7 C8 H8A 109.2 . . ? C8 C8 H8A 109.2 2_647 . ? C7 C8 H8B 109.3 . . ? C8 C8 H8B 109.2 2_647 . ? H8A C8 H8B 107.9 . . ? N3 C9 C10 124.4(2) . . ? N3 C9 H9A 117.8 . . ? C10 C9 H9A 117.8 . . ? C9 C10 C11 119.2(2) . . ? C9 C10 H10A 120.4 . . ? C11 C10 H10A 120.4 . . ? N4 C11 C10 116.6(2) . . ? N4 C11 C12 125.7(2) . . ? C10 C11 C12 117.7(2) . . ? C13 C12 C11 118.3(2) . . ? C13 C12 H12A 120.8 . . ? C11 C12 H12A 120.8 . . ? N3 C13 C12 124.5(2) . . ? N3 C13 H13A 117.8 . . ? C12 C13 H13A 117.8 . . ? O2 C14 N4 123.4(2) . . ? O2 C14 C15 125.0(2) . . ? N4 C14 C15 111.6(2) . . ? C14 C15 C16 114.8(2) . . ? C14 C15 H15A 108.6 . . ? C16 C15 H15A 108.6 . . ? C14 C15 H15B 108.6 . . ? C16 C15 H15B 108.6 . . ? H15A C15 H15B 107.5 . . ? C15 C16 C16 111.6(3) . 2_355 ? C15 C16 H16A 109.3 . . ? C16 C16 H16A 109.3 2_355 . ? C15 C16 H16B 109.3 . . ? C16 C16 H16B 109.3 2_355 . ? H16A C16 H16B 108.0 . . ? O3 C17 O4 121.6(2) . . ? O3 C17 C18 118.9(2) . . ? O4 C17 C18 119.5(2) . . ? O3 C17 Cd 57.45(13) . . ? O4 C17 Cd 64.12(14) . . ? C18 C17 Cd 176.3(2) . . ? C19 C18 C20 119.9(2) . . ? C19 C18 C17 120.5(2) . . ? C20 C18 C17 119.6(2) . . ? C18 C19 C20 119.9(3) . 2_567 ? C18 C19 H19A 120.0 . . ? C20 C19 H19A 120.0 2_567 . ? C18 C20 C19 120.2(3) . 2_567 ? C18 C20 H20A 119.9 . . ? C19 C20 H20A 119.9 2_567 . ? O5 C21 O6 121.5(2) . . ? O5 C21 C22 121.3(2) . . ? O6 C21 C22 117.2(2) . . ? C24 C22 C23 118.3(3) . . ? C24 C22 C21 121.0(2) . . ? C23 C22 C21 120.6(2) . . ? C22 C23 C24 120.3(3) . 2_666 ? C22 C23 H23A 119.9 . . ? C24 C23 H23A 119.9 2_666 . ? C22 C24 C23 121.4(3) . 2_666 ? C22 C24 H24A 119.3 . . ? C23 C24 H24A 119.3 2_666 . ? H7E O7 H7F 108.3 . . ? H8C O8 H8D 102(5) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.333 _refine_diff_density_min -0.295 _refine_diff_density_rms 0.061 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 791962' #TrackingRef '- all.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H46 N4 O12 Zn2' _chemical_formula_weight 905.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 9.2535(2) _cell_length_b 10.2529(2) _cell_length_c 11.8897(3) _cell_angle_alpha 91.3720(10) _cell_angle_beta 111.4870(10) _cell_angle_gamma 102.4270(10) _cell_volume 1018.47(4) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 8022 _cell_measurement_theta_min 2.780 _cell_measurement_theta_max 28.049 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.476 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 470 _exptl_absorpt_coefficient_mu 1.245 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8532 _exptl_absorpt_correction_T_max 0.9525 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 18918 _diffrn_reflns_av_R_equivalents 0.0524 _diffrn_reflns_av_sigmaI/netI 0.0407 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 28.31 _reflns_number_total 5029 _reflns_number_gt 4108 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 (Bruker, 2008)' _computing_cell_refinement 'Bruker SAINTPLUS (Bruker, 2008)' _computing_data_reduction 'Bruker SAINTPLUS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 2008)' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0802P)^2^+0.0012P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5029 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0492 _refine_ls_R_factor_gt 0.0399 _refine_ls_wR_factor_ref 0.1287 _refine_ls_wR_factor_gt 0.1245 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.085 _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 Zn Zn 0.31072(3) 0.45801(2) 0.38533(2) 0.03060(12) Uani 1 1 d . . . O1 O -0.4004(3) -0.0542(2) 0.1532(3) 0.0876(10) Uani 1 1 d . . . O2 O 0.3843(2) 0.5199(2) 0.25978(18) 0.0464(5) Uani 1 1 d . . . O3 O 0.3740(3) 0.3068(2) 0.2186(2) 0.0516(5) Uani 1 1 d . . . O4 O 0.3423(2) 0.63609(16) 0.47116(17) 0.0380(4) Uani 1 1 d . . . O5 O 0.6036(2) 0.67620(16) 0.51230(17) 0.0375(4) Uani 1 1 d . . . N1 N 0.0795(2) 0.3646(2) 0.3286(2) 0.0352(5) Uani 1 1 d . . . N2 N -0.3995(2) 0.1569(2) 0.2136(2) 0.0410(5) Uani 1 1 d . . . H2A H -0.4618 0.2055 0.2200 0.049 Uiso 1 1 calc R . . C1 C -0.0343(3) 0.4217(3) 0.3385(3) 0.0406(6) Uani 1 1 d . . . H1A H -0.0045 0.5107 0.3725 0.049 Uiso 1 1 calc R . . C2 C -0.1920(3) 0.3543(3) 0.3008(3) 0.0432(6) Uani 1 1 d . . . H2B H -0.2666 0.3975 0.3095 0.052 Uiso 1 1 calc R . . C3 C -0.2397(3) 0.2221(3) 0.2497(2) 0.0375(6) Uani 1 1 d . . . C4 C -0.1233(3) 0.1628(3) 0.2373(3) 0.0466(7) Uani 1 1 d . . . H4A H -0.1506 0.0745 0.2019 0.056 Uiso 1 1 calc R . . C5 C 0.0308(3) 0.2362(3) 0.2778(3) 0.0438(6) Uani 1 1 d . . . H5A H 0.1074 0.1950 0.2699 0.053 Uiso 1 1 calc R . . C6 C -0.4705(3) 0.0259(3) 0.1694(3) 0.0509(7) Uani 1 1 d . . . C7 C -0.6503(4) -0.0089(3) 0.1395(4) 0.0619(9) Uani 1 1 d . . . H7A H -0.6707 0.0338 0.2039 0.074 Uiso 1 1 calc R . . H7B H -0.7030 0.0272 0.0647 0.074 Uiso 1 1 calc R . . C8 C -0.7213(3) -0.1572(3) 0.1249(3) 0.0506(7) Uani 1 1 d . . . H8A H -0.6641 -0.1949 0.1974 0.061 Uiso 1 1 calc R . . H8B H -0.7084 -0.1995 0.0565 0.061 Uiso 1 1 calc R . . C9 C -0.8988(3) -0.1884(3) 0.1041(3) 0.0566(8) Uani 1 1 d . . . H9A H -0.9131 -0.1380 0.1678 0.068 Uiso 1 1 calc R . . H9B H -0.9579 -0.1601 0.0268 0.068 Uiso 1 1 calc R . . C10 C -0.9654(4) -0.3380(3) 0.1039(3) 0.0538(8) Uani 1 1 d . . . H10A H -0.9020 -0.3664 0.1797 0.065 Uiso 1 1 calc R . . H10B H -1.0740 -0.3518 0.1006 0.065 Uiso 1 1 calc R . . C11 C -0.9665(4) -0.4250(3) 0.0000(3) 0.0490(7) Uani 1 1 d . . . H11A H -0.8580 -0.4112 0.0032 0.059 Uiso 1 1 calc R . . H11B H -1.0299 -0.3966 -0.0759 0.059 Uiso 1 1 calc R . . C12 C 0.3985(3) 0.4266(3) 0.1959(2) 0.0325(5) Uani 1 1 d . . . C13 C 0.4510(3) 0.4645(3) 0.0943(2) 0.0357(5) Uani 1 1 d . . . C14 C 0.5140(3) 0.5978(3) 0.0888(2) 0.0386(6) Uani 1 1 d . . . H14A H 0.5229 0.6635 0.1479 0.046 Uiso 1 1 calc R . . C15 C 0.4358(3) 0.3665(3) 0.0053(3) 0.0391(6) Uani 1 1 d . . . H15A H 0.3920 0.2768 0.0087 0.047 Uiso 1 1 calc R . . C16 C 0.4768(3) 0.7141(2) 0.4941(2) 0.0299(5) Uani 1 1 d . . . C17 C 0.4881(3) 0.8623(2) 0.4972(2) 0.0319(5) Uani 1 1 d . . . C18 C 0.6332(3) 0.9513(2) 0.5150(3) 0.0418(6) Uani 1 1 d . . . H18A H 0.7232 0.9188 0.5255 0.050 Uiso 1 1 calc R . . C19 C 0.3561(3) 0.9123(2) 0.4831(3) 0.0412(6) Uani 1 1 d . . . H19A H 0.2591 0.8535 0.4722 0.049 Uiso 1 1 calc R . . O6 O 0.8457(12) 0.7085(12) 0.3773(9) 0.325(5) Uiso 1 1 d . . . H6A H 0.7870 0.7009 0.4155 0.390 Uiso 1 1 calc R . . C20 C 0.8986(14) 0.8407(12) 0.3684(11) 0.251(5) Uiso 1 1 d . . . H20A H 0.9276 0.8491 0.2987 0.302 Uiso 1 1 calc R . . H20B H 0.9903 0.8801 0.4405 0.302 Uiso 1 1 calc R . . H20C H 0.8153 0.8862 0.3596 0.302 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn 0.02744(16) 0.02025(16) 0.0428(2) 0.00333(12) 0.01291(13) 0.00398(11) O1 0.0441(13) 0.0391(13) 0.172(3) -0.0216(15) 0.0418(16) -0.0026(10) O2 0.0583(12) 0.0414(11) 0.0489(11) 0.0028(9) 0.0311(10) 0.0120(9) O3 0.0622(13) 0.0436(12) 0.0635(13) 0.0089(10) 0.0406(11) 0.0121(10) O4 0.0427(10) 0.0197(8) 0.0554(11) -0.0007(7) 0.0258(9) 0.0029(7) O5 0.0404(10) 0.0229(8) 0.0509(11) 0.0097(8) 0.0171(8) 0.0110(7) N1 0.0289(10) 0.0284(10) 0.0452(12) 0.0041(9) 0.0127(9) 0.0029(8) N2 0.0271(10) 0.0329(11) 0.0595(14) -0.0022(10) 0.0159(10) 0.0018(9) C1 0.0327(13) 0.0286(12) 0.0558(17) -0.0035(11) 0.0156(12) 0.0009(10) C2 0.0312(13) 0.0368(14) 0.0617(18) -0.0042(13) 0.0199(12) 0.0055(11) C3 0.0299(12) 0.0333(13) 0.0454(15) 0.0020(11) 0.0133(11) 0.0018(10) C4 0.0356(14) 0.0293(13) 0.071(2) -0.0037(13) 0.0198(14) 0.0023(11) C5 0.0291(12) 0.0330(13) 0.0670(19) -0.0020(13) 0.0175(12) 0.0055(11) C6 0.0339(14) 0.0354(14) 0.077(2) -0.0050(14) 0.0200(14) -0.0014(12) C7 0.0348(15) 0.0385(16) 0.104(3) -0.0074(17) 0.0261(17) -0.0056(12) C8 0.0361(14) 0.0367(15) 0.069(2) -0.0014(14) 0.0158(14) -0.0035(12) C9 0.0374(15) 0.0415(16) 0.083(2) -0.0060(16) 0.0225(16) -0.0043(13) C10 0.0362(15) 0.0433(16) 0.072(2) 0.0040(15) 0.0194(15) -0.0072(13) C11 0.0397(15) 0.0427(16) 0.0524(18) 0.0074(14) 0.0122(13) -0.0053(13) C12 0.0227(11) 0.0381(13) 0.0368(13) -0.0010(10) 0.0125(10) 0.0060(10) C13 0.0309(12) 0.0377(13) 0.0405(14) 0.0026(11) 0.0160(11) 0.0081(10) C14 0.0423(14) 0.0333(13) 0.0423(15) -0.0022(11) 0.0200(12) 0.0074(11) C15 0.0413(14) 0.0294(12) 0.0481(15) 0.0003(11) 0.0225(12) 0.0020(11) C16 0.0366(12) 0.0217(11) 0.0320(12) 0.0033(9) 0.0136(10) 0.0073(9) C17 0.0347(12) 0.0201(10) 0.0383(13) 0.0015(9) 0.0116(10) 0.0058(9) C18 0.0314(12) 0.0246(12) 0.0685(19) 0.0041(12) 0.0170(12) 0.0089(10) C19 0.0310(12) 0.0219(11) 0.0669(18) 0.0032(11) 0.0166(12) 0.0027(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn O2 1.9231(19) . ? Zn O5 1.9611(16) 2_666 ? Zn O4 1.9807(16) . ? Zn N1 1.995(2) . ? O1 C6 1.202(3) . ? O2 C12 1.265(3) . ? O3 C12 1.255(3) . ? O4 C16 1.255(3) . ? O5 C16 1.261(3) . ? O5 Zn 1.9611(16) 2_666 ? N1 C5 1.345(3) . ? N1 C1 1.348(3) . ? N2 C6 1.358(3) . ? N2 C3 1.384(3) . ? N2 H2A 0.8600 . ? C1 C2 1.371(4) . ? C1 H1A 0.9300 . ? C2 C3 1.381(4) . ? C2 H2B 0.9300 . ? C3 C4 1.395(3) . ? C4 C5 1.360(4) . ? C4 H4A 0.9300 . ? C5 H5A 0.9300 . ? C6 C7 1.526(4) . ? C7 C8 1.499(4) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.527(4) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.524(4) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.502(5) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C11 1.530(6) 2_345 ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.489(3) . ? C13 C14 1.379(4) . ? C13 C15 1.389(4) . ? C14 C15 1.389(4) 2_665 ? C14 H14A 0.9300 . ? C15 C14 1.389(4) 2_665 ? C15 H15A 0.9300 . ? C16 C17 1.499(3) . ? C17 C19 1.381(3) . ? C17 C18 1.391(3) . ? C18 C19 1.379(3) 2_676 ? C18 H18A 0.9300 . ? C19 C18 1.379(3) 2_676 ? C19 H19A 0.9300 . ? O6 C20 1.359(11) . ? O6 H6A 0.8200 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Zn O5 121.93(8) . 2_666 ? O2 Zn O4 97.82(8) . . ? O5 Zn O4 116.11(8) 2_666 . ? O2 Zn N1 115.49(9) . . ? O5 Zn N1 97.54(8) 2_666 . ? O4 Zn N1 108.23(8) . . ? C12 O2 Zn 113.70(17) . . ? C16 O4 Zn 114.69(14) . . ? C16 O5 Zn 129.55(16) . 2_666 ? C5 N1 C1 116.5(2) . . ? C5 N1 Zn 119.30(16) . . ? C1 N1 Zn 124.17(17) . . ? C6 N2 C3 128.2(2) . . ? C6 N2 H2A 115.9 . . ? C3 N2 H2A 115.9 . . ? N1 C1 C2 123.0(2) . . ? N1 C1 H1A 118.5 . . ? C2 C1 H1A 118.5 . . ? C1 C2 C3 119.7(2) . . ? C1 C2 H2B 120.1 . . ? C3 C2 H2B 120.1 . . ? C2 C3 N2 118.2(2) . . ? C2 C3 C4 117.8(2) . . ? N2 C3 C4 124.1(2) . . ? C5 C4 C3 118.8(2) . . ? C5 C4 H4A 120.6 . . ? C3 C4 H4A 120.6 . . ? N1 C5 C4 124.2(2) . . ? N1 C5 H5A 117.9 . . ? C4 C5 H5A 117.9 . . ? O1 C6 N2 123.9(3) . . ? O1 C6 C7 123.1(3) . . ? N2 C6 C7 112.9(2) . . ? C8 C7 C6 113.1(3) . . ? C8 C7 H7A 109.0 . . ? C6 C7 H7A 109.0 . . ? C8 C7 H7B 109.0 . . ? C6 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? C7 C8 C9 111.9(2) . . ? C7 C8 H8A 109.2 . . ? C9 C8 H8A 109.2 . . ? C7 C8 H8B 109.2 . . ? C9 C8 H8B 109.2 . . ? H8A C8 H8B 107.9 . . ? C10 C9 C8 111.5(3) . . ? C10 C9 H9A 109.3 . . ? C8 C9 H9A 109.3 . . ? C10 C9 H9B 109.3 . . ? C8 C9 H9B 109.3 . . ? H9A C9 H9B 108.0 . . ? C11 C10 C9 114.0(3) . . ? C11 C10 H10A 108.7 . . ? C9 C10 H10A 108.7 . . ? C11 C10 H10B 108.7 . . ? C9 C10 H10B 108.7 . . ? H10A C10 H10B 107.6 . . ? C10 C11 C11 113.9(3) . 2_345 ? C10 C11 H11A 108.8 . . ? C11 C11 H11A 108.8 2_345 . ? C10 C11 H11B 108.8 . . ? C11 C11 H11B 108.8 2_345 . ? H11A C11 H11B 107.7 . . ? O3 C12 O2 121.8(2) . . ? O3 C12 C13 120.6(2) . . ? O2 C12 C13 117.6(2) . . ? C14 C13 C15 120.2(2) . . ? C14 C13 C12 119.5(2) . . ? C15 C13 C12 120.3(2) . . ? C13 C14 C15 119.7(2) . 2_665 ? C13 C14 H14A 120.2 . . ? C15 C14 H14A 120.2 2_665 . ? C13 C15 C14 120.1(2) . 2_665 ? C13 C15 H15A 119.9 . . ? C14 C15 H15A 119.9 2_665 . ? O4 C16 O5 124.3(2) . . ? O4 C16 C17 118.36(19) . . ? O5 C16 C17 117.3(2) . . ? C19 C17 C18 119.2(2) . . ? C19 C17 C16 120.8(2) . . ? C18 C17 C16 119.9(2) . . ? C19 C18 C17 120.1(2) 2_676 . ? C19 C18 H18A 119.9 2_676 . ? C17 C18 H18A 119.9 . . ? C18 C19 C17 120.6(2) 2_676 . ? C18 C19 H19A 119.7 2_676 . ? C17 C19 H19A 119.7 . . ? C20 O6 H6A 109.5 . . ? O6 C20 H20A 109.5 . . ? O6 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? O6 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.961 _refine_diff_density_min -0.643 _refine_diff_density_rms 0.105 #===END