# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Myunghyun P. Suh' _publ_contact_author_email MPSUH@SNU.AC.KR _publ_section_title ; Stepwise and Hysteretic Sorption of N2, O2, CO2, and H2 Gases in a Porous Metal-Organic Framework [Zn2(BPnDC)2(bpy)] ; loop_ _publ_author_name 'Myunghyun P. Suh' 'Hye Jeong Park' # Attachment 'revised-CCDC_726043.cif' #============================================================================== data_1 _database_code_depnum_ccdc_archive 'CCDC 726043' #============================================================================== _audit_creation_date 2009-10-09T13:41:18-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C40 H24 N2 O10 Zn2' _chemical_formula_sum 'C40 H24 N2 O10 Zn2' _chemical_formula_weight 823.35 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.687(4) _cell_length_b 17.754(4) _cell_length_c 26.041(5) _cell_angle_alpha 90 _cell_angle_beta 103.95(3) _cell_angle_gamma 90 _cell_volume 9731(3) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_wavelength 0.79998 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.124 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3344 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.033 _exptl_absorpt_process_details 'HKL2000 Scalepack' #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.79998 _diffrn_radiation_type synchrotron _diffrn_radiation_monochromator 'Si(111) double crystal monochromator' _diffrn_radiation_source 'bending magnet 6C1 MX beamline' _diffrn_radiation_probe x-ray _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scan' _diffrn_reflns_av_R_equivalents 0.0308 _diffrn_reflns_av_unetI/netI 0.0394 _diffrn_reflns_number 13520 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 27.95 _diffrn_reflns_theta_full 24.61 _diffrn_measured_fraction_theta_full 0.976 _diffrn_measured_fraction_theta_max 0.93 _reflns_number_total 7644 _reflns_number_gt 6426 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'ADSC Quantum-210 ADX Program' _computing_cell_refinement HKL2000 _computing_data_reduction HKL2000 _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.1361P)^2^+4.5286P] 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_number_reflns 7644 _refine_ls_number_parameters 487 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.066 _refine_ls_R_factor_gt 0.0606 _refine_ls_wR_factor_ref 0.186 _refine_ls_wR_factor_gt 0.1811 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.563 _refine_diff_density_min -1.326 _refine_diff_density_rms 0.099 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' 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 0.959070(19) 0.15741(2) 0.087431(15) 0.04166(18) Uani 1 1 d . . . Zn2 Zn 0.875386(19) 0.30428(2) 0.068677(15) 0.04233(18) Uani 1 1 d . . . O9 O 0.96222(12) 0.10254(15) 0.16005(9) 0.0456(6) Uani 1 1 d . . . O8 O 0.91830(12) 0.04214(15) 0.08620(9) 0.0477(6) Uani 1 1 d . . . O6 O 0.93550(12) 0.18474(16) 0.00946(10) 0.0465(6) Uani 1 1 d . . . O3 O 0.86070(12) 0.20021(15) 0.09201(10) 0.0463(6) Uani 1 1 d . . . O4 O 0.85791(14) 0.27423(16) 0.16012(10) 0.0508(7) Uani 1 1 d . . . O5 O 1.25462(14) 0.45692(19) 0.27673(11) 0.0641(8) Uani 1 1 d . . . O1 O 1.00414(12) 0.24847(15) 0.12488(10) 0.0490(6) Uani 1 1 d . . . O7 O 0.86552(13) 0.27985(16) -0.00679(10) 0.0504(6) Uani 1 1 d . . . O2 O 0.95475(12) 0.35674(16) 0.09695(11) 0.0495(6) Uani 1 1 d . . . N1 N 1.04333(15) 0.10620(19) 0.07845(11) 0.0467(7) Uani 1 1 d . . . N2 N 0.80441(14) 0.37709(18) 0.06442(11) 0.0419(7) Uani 1 1 d . . . C9 C 0.81744(18) 0.1500(2) 0.16185(14) 0.0428(8) Uani 1 1 d . . . C28 C 0.89975(19) -0.0658(2) 0.24925(15) 0.0526(10) Uani 1 1 d . . . H28 H 0.8993 -0.0581 0.2845 0.063 Uiso 1 1 calc R . . C37 C 0.70086(18) 0.4239(2) 0.02400(14) 0.0468(9) Uani 1 1 d . . . H37 H 0.6653 0.4228 -0.0043 0.056 Uiso 1 1 calc R . . C36 C 0.75192(18) 0.3779(2) 0.02426(14) 0.0460(9) Uani 1 1 d . . . H36 H 0.7502 0.346 -0.0044 0.055 Uiso 1 1 calc R . . C8 C 0.84828(18) 0.2124(2) 0.13836(14) 0.0441(9) Uani 1 1 d . . . C14 C 0.81435(19) 0.1543(2) 0.21445(15) 0.0461(9) Uani 1 1 d . . . H14 H 0.8325 0.1952 0.2349 0.055 Uiso 1 1 calc R . . C24 C 0.91913(18) -0.0193(2) 0.16786(14) 0.0459(9) Uani 1 1 d . . . C29 C 0.91914(18) -0.0084(2) 0.22047(14) 0.0468(9) Uani 1 1 d . . . H29 H 0.9322 0.0376 0.2366 0.056 Uiso 1 1 calc R . . C1 C 1.00165(18) 0.3195(2) 0.12266(15) 0.0459(9) Uani 1 1 d . . . C7 C 1.06828(19) 0.4354(2) 0.13798(15) 0.0504(9) Uani 1 1 d . . . H7 H 1.0376 0.4602 0.1125 0.061 Uiso 1 1 calc R . . C11 C 0.75864(18) 0.0340(2) 0.15268(15) 0.0493(9) Uani 1 1 d . . . H11 H 0.7391 -0.0057 0.1317 0.059 Uiso 1 1 calc R . . C18 C 0.9346(2) 0.1866(2) -0.10077(15) 0.0503(9) Uani 1 1 d . . . H18 H 0.9729 0.1716 -0.0784 0.06 Uiso 1 1 calc R . . C27 C 0.8809(2) -0.1352(3) 0.22524(15) 0.0607(11) Uani 1 1 d . . . C16 C 0.89700(18) 0.2281(2) -0.02103(14) 0.0446(9) Uani 1 1 d . . . O10 O 0.8171(3) 0.2408(3) -0.27364(14) 0.1166(19) Uani 1 1 d . . . C25 C 0.9024(2) -0.0890(3) 0.14448(15) 0.0615(12) Uani 1 1 d . . . H25 H 0.904 -0.0972 0.1095 0.074 Uiso 1 1 calc R . . C10 C 0.78987(17) 0.0887(2) 0.13115(14) 0.0468(9) Uani 1 1 d . . . H10 H 0.7926 0.0848 0.0962 0.056 Uiso 1 1 calc R . . C12 C 0.75620(17) 0.0379(2) 0.20573(14) 0.0466(9) Uani 1 1 d . . . C5 C 1.1687(2) 0.4375(2) 0.20232(15) 0.0515(10) Uani 1 1 d . . . C38 C 0.70286(17) 0.4719(2) 0.06630(14) 0.0442(8) Uani 1 1 d . . . C13 C 0.78521(18) 0.0996(2) 0.23641(14) 0.0476(9) Uani 1 1 d . . . H13 H 0.7844 0.1027 0.2719 0.057 Uiso 1 1 calc R . . C6 C 1.12418(18) 0.4724(2) 0.16324(15) 0.0497(9) Uani 1 1 d . . . H6 H 1.1313 0.5214 0.1534 0.06 Uiso 1 1 calc R . . C40 C 0.80663(19) 0.4246(2) 0.10454(15) 0.0512(10) Uani 1 1 d . . . H40 H 0.843 0.4253 0.1322 0.061 Uiso 1 1 calc R . . C34 C 1.1014(2) 0.0403(3) 0.02650(16) 0.0649(12) Uani 1 1 d . . . H34 H 1.1043 0.0253 -0.0071 0.078 Uiso 1 1 calc R . . C23 C 0.93475(17) 0.0446(2) 0.13614(14) 0.0449(9) Uani 1 1 d . . . C33 C 1.14759(18) 0.0196(2) 0.07008(14) 0.0463(9) Uani 1 1 d . . . C17 C 0.8875(2) 0.2166(2) -0.07955(15) 0.0501(9) Uani 1 1 d . . . C39 C 0.75779(18) 0.4724(2) 0.10684(14) 0.0482(9) Uani 1 1 d . . . H39 H 0.7614 0.505 0.1354 0.058 Uiso 1 1 calc R . . C2 C 1.05878(19) 0.3616(2) 0.15116(15) 0.0485(9) Uani 1 1 d . . . C3 C 1.1032(3) 0.3278(3) 0.1919(2) 0.0821(17) Uani 1 1 d . . . H3 H 1.0967 0.2786 0.2016 0.099 Uiso 1 1 calc R . . C15 C 1.22830(19) 0.4763(2) 0.23174(15) 0.0506(9) Uani 1 1 d . . . C35 C 1.0510(2) 0.0830(3) 0.03247(15) 0.0628(12) Uani 1 1 d . . . H35 H 1.0205 0.0964 0.0022 0.075 Uiso 1 1 calc R . . C22 C 0.8293(2) 0.2368(3) -0.11248(17) 0.0722(15) Uani 1 1 d . . . H22 H 0.7972 0.2562 -0.0981 0.087 Uiso 1 1 calc R . . C32 C 1.1393(2) 0.0410(3) 0.11930(16) 0.0600(11) Uani 1 1 d . . . H32 H 1.1681 0.0258 0.1501 0.072 Uiso 1 1 calc R . . C31 C 1.0878(2) 0.0849(3) 0.12191(16) 0.0608(11) Uani 1 1 d . . . H31 H 1.0835 0.1005 0.1549 0.073 Uiso 1 1 calc R . . C30 C 0.8537(3) 0.1936(3) -0.24744(18) 0.0786(16) Uani 1 1 d . . . C20 C 0.8669(3) 0.1988(3) -0.18887(17) 0.0674(13) Uani 1 1 d . . . C4 C 1.1568(2) 0.3661(3) 0.2182(2) 0.0801(17) Uani 1 1 d . . . H4 H 1.1849 0.3437 0.2467 0.096 Uiso 1 1 calc R . . C26 C 0.8836(3) -0.1458(3) 0.17282(17) 0.0756(15) Uani 1 1 d . . . H26 H 0.8724 -0.1923 0.1568 0.091 Uiso 1 1 calc R . . C19 C 0.9254(2) 0.1784(3) -0.15552(16) 0.0558(10) Uani 1 1 d . . . H19 H 0.9578 0.1597 -0.1697 0.067 Uiso 1 1 calc R . . C21 C 0.8193(3) 0.2280(4) -0.16669(19) 0.0883(19) Uani 1 1 d . . . H21 H 0.7804 0.2416 -0.1887 0.106 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 0.0352(3) 0.0533(3) 0.0333(3) -0.00028(17) 0.00209(19) 0.00482(18) Zn2 0.0332(3) 0.0529(3) 0.0370(3) -0.00162(17) 0.00082(19) 0.00371(18) O9 0.0395(14) 0.0562(15) 0.0388(13) -0.0009(12) 0.0047(11) 0.0001(12) O8 0.0458(15) 0.0610(16) 0.0323(13) 0.0003(11) 0.0018(11) 0.0043(13) O6 0.0353(14) 0.0649(16) 0.0361(13) 0.0004(12) 0.0023(11) 0.0058(13) O3 0.0366(15) 0.0582(16) 0.0410(14) -0.0001(11) 0.0033(11) 0.0023(12) O4 0.0507(17) 0.0553(16) 0.0437(14) -0.0012(13) 0.0059(12) -0.0014(13) O5 0.0579(18) 0.082(2) 0.0428(16) 0.0085(14) -0.0058(13) -0.0184(16) O1 0.0380(15) 0.0611(18) 0.0435(14) -0.0004(12) 0.0015(11) 0.0005(12) O7 0.0469(16) 0.0616(16) 0.0390(13) 0.0005(12) 0.0035(11) 0.0131(14) O2 0.0367(15) 0.0584(16) 0.0479(14) 0.0049(12) -0.0007(12) 0.0005(12) N1 0.0400(18) 0.0606(19) 0.0362(16) -0.0018(14) 0.0030(13) 0.0056(15) N2 0.0365(17) 0.0524(18) 0.0328(15) -0.0015(13) 0.0004(12) 0.0038(14) C9 0.035(2) 0.053(2) 0.0365(18) 0.0000(15) 0.0029(15) 0.0019(16) C28 0.049(2) 0.071(3) 0.0342(18) -0.0004(18) 0.0030(16) -0.006(2) C37 0.034(2) 0.064(2) 0.0373(18) -0.0038(17) -0.0027(15) 0.0041(18) C36 0.042(2) 0.059(2) 0.0330(17) -0.0043(16) 0.0010(15) 0.0049(18) C8 0.035(2) 0.056(2) 0.0378(19) -0.0016(17) 0.0013(15) 0.0054(17) C14 0.041(2) 0.053(2) 0.0392(19) -0.0053(16) -0.0010(16) 0.0008(17) C24 0.041(2) 0.057(2) 0.0355(18) -0.0005(16) 0.0004(15) 0.0019(17) C29 0.039(2) 0.058(2) 0.0379(19) -0.0021(16) -0.0016(15) 0.0020(18) C1 0.037(2) 0.059(2) 0.0398(19) 0.0048(17) 0.0059(16) -0.0015(18) C7 0.039(2) 0.065(2) 0.043(2) 0.0034(18) 0.0018(16) -0.0007(19) C11 0.037(2) 0.062(2) 0.043(2) -0.0052(18) -0.0011(16) -0.0013(18) C18 0.043(2) 0.065(2) 0.038(2) 0.0012(17) -0.0009(16) 0.0050(19) C27 0.065(3) 0.075(3) 0.036(2) 0.0017(19) 0.0001(19) -0.017(2) C16 0.036(2) 0.059(2) 0.0357(18) -0.0008(17) 0.0034(15) 0.0042(18) O10 0.163(5) 0.125(3) 0.0478(19) 0.002(2) -0.003(2) 0.084(3) C25 0.080(3) 0.069(3) 0.0321(19) -0.0042(19) 0.0063(19) -0.012(2) C10 0.038(2) 0.062(2) 0.0374(18) -0.0015(17) 0.0024(15) 0.0026(18) C12 0.0332(19) 0.063(2) 0.0393(19) -0.0010(17) -0.0002(15) -0.0034(18) C5 0.045(2) 0.063(2) 0.042(2) 0.0044(18) 0.0008(17) -0.0074(19) C38 0.039(2) 0.056(2) 0.0361(18) 0.0006(16) 0.0051(15) 0.0051(17) C13 0.042(2) 0.060(2) 0.0362(18) -0.0035(17) 0.0001(15) -0.0019(18) C6 0.040(2) 0.060(2) 0.047(2) 0.0002(18) 0.0050(16) -0.0059(18) C40 0.042(2) 0.065(2) 0.040(2) -0.0054(18) -0.0034(16) 0.0049(19) C34 0.059(3) 0.092(3) 0.039(2) -0.006(2) 0.0022(19) 0.026(3) C23 0.038(2) 0.059(2) 0.0353(19) 0.0017(17) 0.0029(15) 0.0078(18) C33 0.040(2) 0.058(2) 0.0374(18) -0.0039(16) 0.0020(15) 0.0059(17) C17 0.046(2) 0.062(2) 0.0370(19) -0.0019(17) 0.0001(17) 0.0093(19) C39 0.042(2) 0.061(2) 0.0375(18) -0.0106(17) 0.0018(16) 0.0043(18) C2 0.040(2) 0.058(2) 0.043(2) 0.0040(17) 0.0010(16) -0.0062(18) C3 0.067(3) 0.072(3) 0.086(4) 0.028(3) -0.024(3) -0.018(3) C15 0.041(2) 0.063(2) 0.042(2) -0.0006(18) -0.0007(17) -0.0073(19) C35 0.056(3) 0.090(3) 0.035(2) -0.004(2) -0.0025(18) 0.030(2) C22 0.064(3) 0.100(4) 0.043(2) -0.012(2) -0.006(2) 0.034(3) C32 0.047(2) 0.085(3) 0.042(2) -0.003(2) 0.0000(18) 0.011(2) C31 0.053(3) 0.083(3) 0.042(2) -0.008(2) 0.0038(18) 0.016(2) C30 0.100(4) 0.087(4) 0.039(2) 0.000(2) -0.003(2) 0.040(3) C20 0.081(3) 0.075(3) 0.038(2) -0.003(2) -0.002(2) 0.030(3) C4 0.062(3) 0.078(3) 0.077(3) 0.025(3) -0.030(3) -0.019(3) C26 0.108(4) 0.069(3) 0.041(2) -0.005(2) 0.001(2) -0.026(3) C19 0.053(3) 0.072(3) 0.040(2) -0.0055(19) 0.0051(18) 0.008(2) C21 0.088(4) 0.121(4) 0.044(2) -0.014(3) -0.008(2) 0.056(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O1 2.015(3) . ? Zn1 O6 2.030(3) . ? Zn1 N1 2.104(3) . ? Zn1 O9 2.114(3) . ? Zn1 O8 2.227(3) . ? Zn1 O3 2.295(3) . ? Zn1 C23 2.494(4) . ? Zn1 Zn2 3.1470(8) . ? Zn2 O2 1.939(3) . ? Zn2 O7 1.973(3) . ? Zn2 N2 1.992(3) . ? Zn2 O3 1.994(3) . ? O9 C23 1.274(5) . ? O8 C23 1.264(4) . ? O6 C16 1.265(5) . ? O3 C8 1.317(4) . ? O4 C8 1.229(5) . ? O5 C15 1.223(5) . ? O1 C1 1.264(5) . ? O7 C16 1.253(5) . ? O2 C1 1.261(5) . ? N1 C35 1.315(5) . ? N1 C31 1.352(5) . ? N2 C40 1.335(5) . ? N2 C36 1.347(5) . ? C9 C14 1.389(5) . ? C9 C10 1.396(5) . ? C9 C8 1.499(6) . ? C28 C29 1.390(6) . ? C28 C27 1.397(6) . ? C37 C36 1.375(5) . ? C37 C38 1.385(5) . ? C14 C13 1.359(6) . ? C24 C29 1.384(5) . ? C24 C25 1.389(6) . ? C24 C23 1.490(6) . ? C1 C2 1.483(6) . ? C7 C2 1.383(6) . ? C7 C6 1.396(6) . ? C11 C10 1.378(6) . ? C11 C12 1.397(5) . ? C18 C17 1.380(6) . ? C18 C19 1.399(5) . ? C27 C26 1.393(6) . ? C27 C30 1.460(7) 6_556 ? C16 C17 1.502(5) . ? O10 C30 1.239(6) . ? C25 C26 1.368(7) . ? C12 C13 1.410(5) . ? C12 C15 1.489(6) 3_445 ? C5 C6 1.370(6) . ? C5 C4 1.377(7) . ? C5 C15 1.501(5) . ? C38 C39 1.388(5) . ? C38 C33 1.490(5) 3_455 ? C40 C39 1.370(6) . ? C34 C35 1.369(6) . ? C34 C33 1.371(6) . ? C33 C32 1.390(6) . ? C33 C38 1.490(5) 3_545 ? C17 C22 1.392(6) . ? C2 C3 1.385(6) . ? C3 C4 1.378(7) . ? C15 C12 1.489(6) 3 ? C22 C21 1.384(6) . ? C32 C31 1.375(6) . ? C30 C27 1.460(7) 6 ? C30 C20 1.485(6) . ? C20 C21 1.399(7) . ? C20 C19 1.401(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn1 O6 105.56(11) . . ? O1 Zn1 N1 93.88(12) . . ? O6 Zn1 N1 90.46(11) . . ? O1 Zn1 O9 91.69(10) . . ? O6 Zn1 O9 162.05(11) . . ? N1 Zn1 O9 93.37(11) . . ? O1 Zn1 O8 152.75(10) . . ? O6 Zn1 O8 101.65(10) . . ? N1 Zn1 O8 87.34(12) . . ? O9 Zn1 O8 61.07(9) . . ? O1 Zn1 O3 93.31(10) . . ? O6 Zn1 O3 87.70(10) . . ? N1 Zn1 O3 172.81(11) . . ? O9 Zn1 O3 86.33(10) . . ? O8 Zn1 O3 86.23(10) . . ? O1 Zn1 C23 122.38(11) . . ? O6 Zn1 C23 131.88(12) . . ? N1 Zn1 C23 90.30(13) . . ? O9 Zn1 C23 30.70(11) . . ? O8 Zn1 C23 30.38(11) . . ? O3 Zn1 C23 85.77(11) . . ? O1 Zn1 Zn2 66.71(8) . . ? O6 Zn1 Zn2 69.51(8) . . ? N1 Zn1 Zn2 145.55(9) . . ? O9 Zn1 Zn2 114.44(7) . . ? O8 Zn1 Zn2 123.17(7) . . ? O3 Zn1 Zn2 39.21(7) . . ? C23 Zn1 Zn2 124.03(9) . . ? O2 Zn2 O7 110.91(12) . . ? O2 Zn2 N2 108.21(12) . . ? O7 Zn2 N2 100.97(11) . . ? O2 Zn2 O3 121.43(11) . . ? O7 Zn2 O3 96.48(11) . . ? N2 Zn2 O3 116.11(12) . . ? O2 Zn2 Zn1 85.02(9) . . ? O7 Zn2 Zn1 83.82(8) . . ? N2 Zn2 Zn1 162.75(9) . . ? O3 Zn2 Zn1 46.65(8) . . ? C23 O9 Zn1 91.4(2) . . ? C23 O8 Zn1 86.6(2) . . ? C16 O6 Zn1 137.9(2) . . ? C8 O3 Zn2 102.1(2) . . ? C8 O3 Zn1 120.0(2) . . ? Zn2 O3 Zn1 94.14(11) . . ? C1 O1 Zn1 140.2(3) . . ? C16 O7 Zn2 121.3(2) . . ? C1 O2 Zn2 118.6(3) . . ? C35 N1 C31 116.9(3) . . ? C35 N1 Zn1 122.8(3) . . ? C31 N1 Zn1 119.5(3) . . ? C40 N2 C36 117.7(3) . . ? C40 N2 Zn2 119.0(2) . . ? C36 N2 Zn2 123.1(3) . . ? C14 C9 C10 119.4(4) . . ? C14 C9 C8 119.6(3) . . ? C10 C9 C8 120.9(3) . . ? C29 C28 C27 120.0(4) . . ? C36 C37 C38 119.4(3) . . ? N2 C36 C37 122.6(3) . . ? O4 C8 O3 121.4(4) . . ? O4 C8 C9 121.0(3) . . ? O3 C8 C9 117.5(3) . . ? C13 C14 C9 120.9(4) . . ? C29 C24 C25 119.8(4) . . ? C29 C24 C23 119.8(4) . . ? C25 C24 C23 120.4(3) . . ? C24 C29 C28 120.2(4) . . ? O2 C1 O1 124.6(4) . . ? O2 C1 C2 118.1(4) . . ? O1 C1 C2 117.3(4) . . ? C2 C7 C6 119.6(4) . . ? C10 C11 C12 120.5(4) . . ? C17 C18 C19 120.7(4) . . ? C26 C27 C28 118.7(4) . . ? C26 C27 C30 119.9(4) . 6_556 ? C28 C27 C30 121.1(4) . 6_556 ? O7 C16 O6 125.8(3) . . ? O7 C16 C17 116.6(3) . . ? O6 C16 C17 117.6(3) . . ? C26 C25 C24 120.0(4) . . ? C11 C10 C9 120.0(4) . . ? C11 C12 C13 118.7(4) . . ? C11 C12 C15 122.0(4) . 3_445 ? C13 C12 C15 119.1(3) . 3_445 ? C6 C5 C4 119.2(4) . . ? C6 C5 C15 122.5(4) . . ? C4 C5 C15 118.1(4) . . ? C37 C38 C39 117.7(3) . . ? C37 C38 C33 122.0(3) . 3_455 ? C39 C38 C33 120.2(3) . 3_455 ? C14 C13 C12 120.4(3) . . ? C5 C6 C7 120.9(4) . . ? N2 C40 C39 122.9(3) . . ? C35 C34 C33 119.9(4) . . ? O8 C23 O9 120.9(4) . . ? O8 C23 C24 119.9(4) . . ? O9 C23 C24 119.1(3) . . ? O8 C23 Zn1 63.0(2) . . ? O9 C23 Zn1 57.89(19) . . ? C24 C23 Zn1 176.2(3) . . ? C34 C33 C32 117.3(4) . . ? C34 C33 C38 122.5(3) . 3_545 ? C32 C33 C38 120.1(3) . 3_545 ? C18 C17 C22 120.2(4) . . ? C18 C17 C16 121.7(3) . . ? C22 C17 C16 118.2(4) . . ? C40 C39 C38 119.6(3) . . ? C7 C2 C3 118.9(4) . . ? C7 C2 C1 120.6(4) . . ? C3 C2 C1 120.5(4) . . ? C4 C3 C2 120.9(5) . . ? O5 C15 C12 119.7(3) . 3 ? O5 C15 C5 120.3(4) . . ? C12 C15 C5 119.9(3) 3 . ? N1 C35 C34 123.9(4) . . ? C21 C22 C17 119.6(4) . . ? C31 C32 C33 119.2(4) . . ? N1 C31 C32 122.7(4) . . ? O10 C30 C27 119.5(4) . 6 ? O10 C30 C20 117.6(4) . . ? C27 C30 C20 122.9(4) 6 . ? C21 C20 C19 119.2(4) . . ? C21 C20 C30 117.9(4) . . ? C19 C20 C30 122.8(4) . . ? C5 C4 C3 120.2(4) . . ? C25 C26 C27 121.2(4) . . ? C18 C19 C20 119.4(4) . . ? C22 C21 C20 120.9(5) . . ? #=============================================================================# # End of CIF #=============================================================================# # Attachment 'revised-CCDC_726044.cif' #============================================================================== data_1m _database_code_depnum_ccdc_archive 'CCDC 726044' #============================================================================== _audit_creation_date 2009-10-09T14:05:40-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C40 H24 N2 O10 Zn2' _chemical_formula_sum 'C40 H24 N2 O10 Zn2' _chemical_formula_weight 823.35 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.536(4) _cell_length_b 18.048(4) _cell_length_c 26.298(5) _cell_angle_alpha 90 _cell_angle_beta 104.55(3) _cell_angle_gamma 90 _cell_volume 9894(3) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_wavelength 0.82655 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.106 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3344 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.016 _exptl_absorpt_process_details 'HKL2000 Scalepack' #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.82655 _diffrn_radiation_type synchrotron _diffrn_radiation_monochromator 'Si(111) double crystal monochromator' _diffrn_radiation_source 'bending magnet 6C1 MX beamline' _diffrn_radiation_probe x-ray _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scan' _diffrn_reflns_av_R_equivalents 0.0222 _diffrn_reflns_av_unetI/netI 0.0257 _diffrn_reflns_number 11988 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.1 _diffrn_reflns_theta_max 26.09 _diffrn_reflns_theta_full 22.5 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.986 _reflns_number_total 6139 _reflns_number_gt 5783 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'ADSC Quantum-210 ADX Program' _computing_cell_refinement HKL2000 _computing_data_reduction HKL2000 _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0955P)^2^+28.1400P] 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_number_reflns 6139 _refine_ls_number_parameters 487 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0484 _refine_ls_R_factor_gt 0.047 _refine_ls_wR_factor_ref 0.1405 _refine_ls_wR_factor_gt 0.139 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.515 _refine_diff_density_min -0.944 _refine_diff_density_rms 0.092 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.00503(17) 0.3087(2) 0.11924(14) 0.0269(9) Uani 1 1 d . . . C2 C 1.06362(17) 0.3521(2) 0.14669(15) 0.0290(9) Uani 1 1 d . . . C3 C 1.10954(19) 0.3192(2) 0.18573(18) 0.0437(11) Uani 1 1 d . . . H3 H 1.1046 0.27 0.1945 0.052 Uiso 1 1 calc R . . C4 C 1.1632(2) 0.3582(2) 0.21231(18) 0.0440(11) Uani 1 1 d . . . H4 H 1.1933 0.3359 0.2397 0.053 Uiso 1 1 calc R . . C5 C 1.17201(17) 0.4307(2) 0.19801(15) 0.0304(9) Uani 1 1 d . . . C6 C 1.12530(18) 0.4637(2) 0.15803(16) 0.0365(10) Uani 1 1 d . . . H6 H 1.1309 0.5121 0.148 0.044 Uiso 1 1 calc R . . C7 C 1.07049(17) 0.4248(2) 0.13300(15) 0.0328(9) Uani 1 1 d . . . H7 H 1.0387 0.4476 0.1072 0.039 Uiso 1 1 calc R . . C8 C 0.84768(16) 0.2075(2) 0.13764(15) 0.0260(9) Uani 1 1 d . . . C9 C 0.81664(16) 0.1462(2) 0.16022(14) 0.0254(8) Uani 1 1 d . . . C10 C 0.78926(16) 0.0859(2) 0.12963(14) 0.0276(8) Uani 1 1 d . . . H10 H 0.7916 0.0825 0.0949 0.033 Uiso 1 1 calc R . . C11 C 0.75868(16) 0.0311(2) 0.15083(14) 0.0293(9) Uani 1 1 d . . . H11 H 0.7398 -0.0085 0.13 0.035 Uiso 1 1 calc R . . C12 C 0.75599(16) 0.0347(2) 0.20298(14) 0.0272(8) Uani 1 1 d . . . C13 C 0.78389(16) 0.0950(2) 0.23391(14) 0.0288(9) Uani 1 1 d . . . H13 H 0.7825 0.098 0.2689 0.035 Uiso 1 1 calc R . . C14 C 0.81325(17) 0.1497(2) 0.21229(15) 0.0271(9) Uani 1 1 d . . . H14 H 0.8313 0.19 0.2328 0.032 Uiso 1 1 calc R . . C15 C 1.22875(17) 0.4725(2) 0.22824(15) 0.0308(9) Uani 1 1 d . . . C16 C 0.89486(16) 0.2185(2) -0.02115(14) 0.0241(8) Uani 1 1 d . . . C17 C 0.88491(17) 0.20747(19) -0.07902(14) 0.0260(8) Uani 1 1 d . . . C18 C 0.93268(17) 0.1778(2) -0.09983(14) 0.0296(9) Uani 1 1 d . . . H18 H 0.9712 0.1626 -0.0775 0.036 Uiso 1 1 calc R . . C19 C 0.92334(18) 0.1707(2) -0.15345(15) 0.0320(9) Uani 1 1 d . . . H19 H 0.9559 0.1516 -0.1671 0.038 Uiso 1 1 calc R . . C20 C 0.8650(2) 0.1923(2) -0.18743(15) 0.0354(10) Uani 1 1 d . . . C21 C 0.8173(2) 0.2211(2) -0.16601(16) 0.0396(10) Uani 1 1 d . . . H21 H 0.7781 0.2348 -0.1881 0.048 Uiso 1 1 calc R . . C22 C 0.82724(18) 0.2297(2) -0.11265(14) 0.0330(9) Uani 1 1 d . . . H22 H 0.7953 0.2504 -0.099 0.04 Uiso 1 1 calc R . . C23 C 0.93514(16) 0.0429(2) 0.13713(14) 0.0257(8) Uani 1 1 d . . . C24 C 0.91973(16) -0.0196(2) 0.16918(14) 0.0267(8) Uani 1 1 d . . . C25 C 0.90156(19) -0.0886(2) 0.14611(15) 0.0334(9) Uani 1 1 d . . . H25 H 0.9029 -0.0973 0.1115 0.04 Uiso 1 1 calc R . . C26 C 0.8817(2) -0.1435(2) 0.17464(15) 0.0383(10) Uani 1 1 d . . . H26 H 0.8692 -0.1891 0.159 0.046 Uiso 1 1 calc R . . C27 C 0.88019(18) -0.1317(2) 0.22662(15) 0.0328(9) Uani 1 1 d . . . C28 C 0.89955(17) -0.0631(2) 0.24987(14) 0.0309(9) Uani 1 1 d . . . H28 H 0.899 -0.0547 0.2847 0.037 Uiso 1 1 calc R . . C29 C 0.91947(17) -0.0078(2) 0.22135(14) 0.0270(8) Uani 1 1 d . . . H29 H 0.9328 0.0376 0.2371 0.032 Uiso 1 1 calc R . . C30 C 0.8527(2) 0.1896(2) -0.24536(16) 0.0399(10) Uani 1 1 d . . . C31 C 1.08892(18) 0.0767(2) 0.12161(16) 0.0383(10) Uani 1 1 d . . . H31 H 1.084 0.0906 0.1545 0.046 Uiso 1 1 calc R . . C32 C 1.14081(18) 0.0339(2) 0.11919(16) 0.0397(10) Uani 1 1 d . . . H32 H 1.1696 0.0182 0.1499 0.048 Uiso 1 1 calc R . . C33 C 1.15005(17) 0.0141(2) 0.07053(14) 0.0265(8) Uani 1 1 d . . . C34 C 1.1043(2) 0.0370(2) 0.02674(15) 0.0420(11) Uani 1 1 d . . . H34 H 1.1082 0.0245 -0.0067 0.05 Uiso 1 1 calc R . . C35 C 1.05285(19) 0.0783(3) 0.03259(15) 0.0421(11) Uani 1 1 d . . . H35 H 1.022 0.0921 0.0025 0.051 Uiso 1 1 calc R . . C36 C 0.80800(17) 0.4146(2) 0.10561(15) 0.0316(9) Uani 1 1 d . . . H36 H 0.844 0.4121 0.1338 0.038 Uiso 1 1 calc R . . C37 C 0.75997(17) 0.4631(2) 0.10831(15) 0.0311(9) Uani 1 1 d . . . H37 H 0.764 0.4935 0.1375 0.037 Uiso 1 1 calc R . . C38 C 0.70509(16) 0.4665(2) 0.06696(14) 0.0257(8) Uani 1 1 d . . . C39 C 0.70339(17) 0.4227(2) 0.02325(14) 0.0266(8) Uani 1 1 d . . . H39 H 0.6685 0.4252 -0.0059 0.032 Uiso 1 1 calc R . . C40 C 0.75359(16) 0.3757(2) 0.02331(14) 0.0241(8) Uani 1 1 d . . . H40 H 0.7518 0.3463 -0.0061 0.029 Uiso 1 1 calc R . . N1 N 1.04484(13) 0.09956(17) 0.07861(11) 0.0260(7) Uani 1 1 d . . . N2 N 0.80526(13) 0.37081(16) 0.06436(11) 0.0241(7) Uani 1 1 d . . . O1 O 1.00757(11) 0.23940(14) 0.12328(10) 0.0291(6) Uani 1 1 d . . . O2 O 0.95703(11) 0.34560(14) 0.09384(10) 0.0309(6) Uani 1 1 d . . . O3 O 0.86063(11) 0.19609(14) 0.09222(10) 0.0285(6) Uani 1 1 d . . . O4 O 0.85754(12) 0.26804(14) 0.15992(10) 0.0326(6) Uani 1 1 d . . . O5 O 1.25417(13) 0.45542(16) 0.27383(11) 0.0417(7) Uani 1 1 d . . . O6 O 0.93435(11) 0.17659(14) 0.00972(9) 0.0261(6) Uani 1 1 d . . . O7 O 0.86267(11) 0.26961(14) -0.00725(9) 0.0286(6) Uani 1 1 d . . . O8 O 0.91856(11) 0.03965(14) 0.08790(9) 0.0280(6) Uani 1 1 d . . . O9 O 0.96411(11) 0.09960(13) 0.16048(9) 0.0265(6) Uani 1 1 d . . . O10 O 0.81629(18) 0.2369(2) -0.27158(12) 0.0629(10) Uani 1 1 d . . . Zn1 Zn 0.960248(18) 0.15082(2) 0.086917(15) 0.02304(17) Uani 1 1 d . . . Zn2 Zn 0.875251(18) 0.29685(2) 0.067062(15) 0.02372(18) Uani 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 C1 0.019(2) 0.042(2) 0.020(2) 0.0032(17) 0.0059(16) 0.0004(17) C2 0.0214(19) 0.038(2) 0.027(2) 0.0019(17) 0.0052(17) -0.0019(16) C3 0.034(2) 0.037(2) 0.051(3) 0.010(2) -0.006(2) -0.010(2) C4 0.031(2) 0.044(3) 0.046(3) 0.013(2) -0.010(2) -0.0080(19) C5 0.0257(19) 0.039(2) 0.025(2) 0.0013(17) 0.0050(16) -0.0036(17) C6 0.031(2) 0.038(2) 0.039(2) 0.0079(18) 0.0052(18) -0.0055(18) C7 0.024(2) 0.039(2) 0.031(2) 0.0053(18) -0.0010(17) -0.0046(17) C8 0.0181(18) 0.036(2) 0.021(2) 0.0026(17) -0.0014(16) 0.0031(16) C9 0.0172(18) 0.035(2) 0.023(2) 0.0025(16) 0.0019(15) 0.0065(15) C10 0.0215(18) 0.042(2) 0.0164(19) -0.0026(17) 0.0000(15) -0.0003(17) C11 0.0221(19) 0.036(2) 0.026(2) -0.0027(17) 0.0001(16) -0.0075(16) C12 0.0193(18) 0.041(2) 0.020(2) 0.0008(17) 0.0017(15) -0.0013(16) C13 0.0251(19) 0.042(2) 0.020(2) -0.0016(17) 0.0055(16) -0.0015(17) C14 0.0234(19) 0.032(2) 0.023(2) -0.0040(16) 0.0010(16) -0.0002(16) C15 0.0250(19) 0.043(2) 0.024(2) -0.0003(18) 0.0054(17) -0.0038(17) C16 0.0168(18) 0.034(2) 0.021(2) 0.0005(17) 0.0039(16) 0.0018(17) C17 0.027(2) 0.032(2) 0.019(2) 0.0014(15) 0.0049(16) 0.0040(16) C18 0.027(2) 0.039(2) 0.020(2) -0.0001(17) 0.0004(16) 0.0086(17) C19 0.030(2) 0.040(2) 0.026(2) -0.0014(17) 0.0070(17) 0.0081(18) C20 0.042(2) 0.039(2) 0.022(2) -0.0019(17) 0.0021(18) 0.0099(19) C21 0.035(2) 0.052(2) 0.026(3) -0.0020(19) -0.0038(18) 0.019(2) C22 0.028(2) 0.049(2) 0.020(2) -0.0034(18) 0.0028(17) 0.0118(18) C23 0.0183(18) 0.037(2) 0.022(2) 0.0024(17) 0.0050(15) 0.0073(17) C24 0.0217(18) 0.038(2) 0.019(2) 0.0014(16) 0.0023(15) 0.0034(16) C25 0.042(2) 0.041(2) 0.017(2) -0.0015(17) 0.0072(17) -0.0008(19) C26 0.053(3) 0.038(2) 0.021(2) -0.0022(17) 0.0036(19) -0.0074(19) C27 0.032(2) 0.042(2) 0.022(2) -0.0012(17) 0.0005(17) -0.0051(18) C28 0.029(2) 0.049(2) 0.0128(19) 0.0000(17) 0.0018(16) -0.0007(18) C29 0.0251(19) 0.034(2) 0.019(2) -0.0001(16) 0.0003(15) -0.0007(16) C30 0.048(3) 0.049(3) 0.018(2) 0.0005(19) -0.0004(19) 0.016(2) C31 0.032(2) 0.058(3) 0.025(2) -0.0068(19) 0.0051(18) 0.011(2) C32 0.029(2) 0.060(3) 0.026(2) -0.0019(19) -0.0010(17) 0.016(2) C33 0.0266(19) 0.034(2) 0.018(2) -0.0015(16) 0.0042(16) 0.0046(16) C34 0.043(2) 0.062(3) 0.018(2) -0.0035(19) 0.0028(18) 0.027(2) C35 0.037(2) 0.067(3) 0.018(2) 0.0030(19) -0.0012(18) 0.023(2) C36 0.025(2) 0.043(2) 0.023(2) -0.0043(18) -0.0014(16) 0.0068(17) C37 0.027(2) 0.041(2) 0.023(2) -0.0066(17) 0.0016(16) 0.0092(17) C38 0.0219(18) 0.035(2) 0.020(2) 0.0015(16) 0.0049(15) 0.0035(16) C39 0.0209(18) 0.037(2) 0.020(2) 0.0005(16) 0.0012(15) 0.0018(16) C40 0.0207(19) 0.032(2) 0.020(2) -0.0012(15) 0.0052(16) 0.0044(16) N1 0.0231(16) 0.0380(17) 0.0162(17) 0.0027(13) 0.0036(13) 0.0052(13) N2 0.0207(16) 0.0324(16) 0.0177(17) -0.0003(14) 0.0023(13) 0.0026(13) O1 0.0259(13) 0.0325(16) 0.0271(15) 0.0000(11) 0.0031(11) 0.0005(11) O2 0.0215(14) 0.0374(15) 0.0313(16) 0.0039(11) 0.0021(12) -0.0002(11) O3 0.0226(13) 0.0392(15) 0.0233(16) 0.0019(11) 0.0052(11) 0.0034(11) O4 0.0363(15) 0.0344(15) 0.0274(15) 0.0013(13) 0.0084(12) -0.0010(12) O5 0.0396(16) 0.0559(18) 0.0258(18) 0.0051(13) 0.0010(13) -0.0163(14) O6 0.0212(13) 0.0375(14) 0.0183(14) 0.0005(11) 0.0026(11) 0.0062(12) O7 0.0275(13) 0.0371(14) 0.0206(14) 0.0010(11) 0.0049(11) 0.0083(12) O8 0.0279(13) 0.0371(14) 0.0180(16) 0.0018(11) 0.0041(11) 0.0034(11) O9 0.0234(13) 0.0339(14) 0.0212(14) 0.0002(11) 0.0041(10) -0.0001(11) O10 0.086(3) 0.072(2) 0.0259(18) 0.0031(16) 0.0044(16) 0.043(2) Zn1 0.0206(3) 0.0310(3) 0.0167(3) 0.00109(16) 0.00309(19) 0.00384(16) Zn2 0.0180(3) 0.0320(3) 0.0198(3) -0.00147(17) 0.00216(19) 0.00361(16) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.255(4) . ? C1 O2 1.270(4) . ? C1 C2 1.507(5) . ? C2 C3 1.369(6) . ? C2 C7 1.378(5) . ? C3 C4 1.383(6) . ? C4 C5 1.388(6) . ? C5 C6 1.392(6) . ? C5 C15 1.485(5) . ? C6 C7 1.389(5) . ? C8 O4 1.233(4) . ? C8 O3 1.309(5) . ? C8 C9 1.491(5) . ? C9 C14 1.391(5) . ? C9 C10 1.393(5) . ? C10 C11 1.381(5) . ? C11 C12 1.389(5) . ? C12 C13 1.401(5) . ? C12 C15 1.497(5) 3_445 ? C13 C14 1.371(5) . ? C15 O5 1.226(5) . ? C15 C12 1.497(5) 3 ? C16 O7 1.262(4) . ? C16 O6 1.268(4) . ? C16 C17 1.496(5) . ? C17 C18 1.388(5) . ? C17 C22 1.391(5) . ? C18 C19 1.379(5) . ? C19 C20 1.402(6) . ? C20 C21 1.391(6) . ? C20 C30 1.480(6) . ? C21 C22 1.374(6) . ? C23 O8 1.255(4) . ? C23 O9 1.273(4) . ? C23 C24 1.496(5) . ? C23 Zn1 2.487(4) . ? C24 C29 1.390(5) . ? C24 C25 1.396(5) . ? C25 C26 1.374(6) . ? C26 C27 1.392(6) . ? C27 C28 1.397(6) . ? C27 C30 1.485(6) 6_556 ? C28 C29 1.381(5) . ? C30 O10 1.244(5) . ? C30 C27 1.485(6) 6 ? C31 N1 1.346(5) . ? C31 C32 1.374(6) . ? C32 C33 1.390(5) . ? C33 C34 1.378(5) . ? C33 C38 1.485(5) 3_545 ? C34 C35 1.376(6) . ? C35 N1 1.322(5) . ? C36 N2 1.331(5) . ? C36 C37 1.371(5) . ? C37 C38 1.392(5) . ? C38 C39 1.388(5) . ? C38 C33 1.485(5) 3_455 ? C39 C40 1.374(5) . ? C40 N2 1.345(5) . ? N1 Zn1 2.103(3) . ? N2 Zn2 2.001(3) . ? O1 Zn1 2.005(2) . ? O2 Zn2 1.936(2) . ? O3 Zn2 1.987(3) . ? O3 Zn1 2.332(2) . ? O6 Zn1 2.020(2) . ? O7 Zn2 1.967(2) . ? O8 Zn1 2.201(3) . ? O9 Zn1 2.127(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 O2 125.5(3) . . ? O1 C1 C2 117.7(3) . . ? O2 C1 C2 116.9(3) . . ? C3 C2 C7 120.3(4) . . ? C3 C2 C1 119.6(3) . . ? C7 C2 C1 120.1(3) . . ? C2 C3 C4 120.8(4) . . ? C3 C4 C5 119.8(4) . . ? C4 C5 C6 119.0(4) . . ? C4 C5 C15 118.9(4) . . ? C6 C5 C15 121.9(4) . . ? C7 C6 C5 120.6(4) . . ? C2 C7 C6 119.4(4) . . ? O4 C8 O3 121.5(3) . . ? O4 C8 C9 120.6(3) . . ? O3 C8 C9 117.8(3) . . ? C14 C9 C10 119.0(3) . . ? C14 C9 C8 119.9(3) . . ? C10 C9 C8 121.1(3) . . ? C11 C10 C9 120.1(3) . . ? C10 C11 C12 120.5(3) . . ? C11 C12 C13 119.4(3) . . ? C11 C12 C15 121.4(3) . 3_445 ? C13 C12 C15 118.9(3) . 3_445 ? C14 C13 C12 119.6(3) . . ? C13 C14 C9 121.3(3) . . ? O5 C15 C5 120.1(3) . . ? O5 C15 C12 119.6(3) . 3 ? C5 C15 C12 120.3(3) . 3 ? O7 C16 O6 125.4(3) . . ? O7 C16 C17 116.3(3) . . ? O6 C16 C17 118.3(3) . . ? C18 C17 C22 119.5(3) . . ? C18 C17 C16 121.4(3) . . ? C22 C17 C16 119.1(3) . . ? C19 C18 C17 120.4(3) . . ? C18 C19 C20 120.2(3) . . ? C21 C20 C19 118.7(4) . . ? C21 C20 C30 118.0(4) . . ? C19 C20 C30 123.2(4) . . ? C22 C21 C20 120.9(4) . . ? C21 C22 C17 120.2(3) . . ? O8 C23 O9 120.9(3) . . ? O8 C23 C24 120.0(3) . . ? O9 C23 C24 119.1(3) . . ? O8 C23 Zn1 62.15(19) . . ? O9 C23 Zn1 58.77(18) . . ? C24 C23 Zn1 177.5(3) . . ? C29 C24 C25 119.7(3) . . ? C29 C24 C23 119.8(3) . . ? C25 C24 C23 120.4(3) . . ? C26 C25 C24 119.8(4) . . ? C25 C26 C27 120.9(4) . . ? C26 C27 C28 119.1(4) . . ? C26 C27 C30 119.4(4) . 6_556 ? C28 C27 C30 121.3(3) . 6_556 ? C29 C28 C27 120.2(3) . . ? C28 C29 C24 120.2(3) . . ? O10 C30 C20 118.2(4) . . ? O10 C30 C27 118.8(4) . 6 ? C20 C30 C27 122.9(3) . 6 ? N1 C31 C32 122.9(4) . . ? C31 C32 C33 119.6(4) . . ? C34 C33 C32 117.0(3) . . ? C34 C33 C38 122.3(3) . 3_545 ? C32 C33 C38 120.5(3) . 3_545 ? C35 C34 C33 119.7(4) . . ? N1 C35 C34 123.6(4) . . ? N2 C36 C37 122.8(3) . . ? C36 C37 C38 119.5(3) . . ? C39 C38 C37 117.5(3) . . ? C39 C38 C33 121.7(3) . 3_455 ? C37 C38 C33 120.7(3) . 3_455 ? C40 C39 C38 119.6(3) . . ? N2 C40 C39 122.3(3) . . ? C35 N1 C31 117.0(3) . . ? C35 N1 Zn1 122.6(2) . . ? C31 N1 Zn1 119.6(2) . . ? C36 N2 C40 118.3(3) . . ? C36 N2 Zn2 119.2(2) . . ? C40 N2 Zn2 122.5(2) . . ? C1 O1 Zn1 138.4(2) . . ? C1 O2 Zn2 119.9(2) . . ? C8 O3 Zn2 104.3(2) . . ? C8 O3 Zn1 121.3(2) . . ? Zn2 O3 Zn1 94.33(10) . . ? C16 O6 Zn1 138.8(2) . . ? C16 O7 Zn2 121.5(2) . . ? C23 O8 Zn1 87.6(2) . . ? C23 O9 Zn1 90.4(2) . . ? O1 Zn1 O6 105.94(10) . . ? O1 Zn1 N1 92.89(11) . . ? O6 Zn1 N1 91.41(10) . . ? O1 Zn1 O9 90.78(10) . . ? O6 Zn1 O9 162.21(10) . . ? N1 Zn1 O9 93.80(10) . . ? O1 Zn1 O8 151.80(10) . . ? O6 Zn1 O8 102.20(10) . . ? N1 Zn1 O8 88.10(10) . . ? O9 Zn1 O8 61.05(9) . . ? O1 Zn1 O3 93.28(9) . . ? O6 Zn1 O3 87.34(9) . . ? N1 Zn1 O3 173.81(10) . . ? O9 Zn1 O3 85.65(9) . . ? O8 Zn1 O3 86.24(9) . . ? O1 Zn1 C23 121.55(11) . . ? O6 Zn1 C23 132.22(11) . . ? N1 Zn1 C23 91.16(11) . . ? O9 Zn1 C23 30.78(11) . . ? O8 Zn1 C23 30.27(11) . . ? O3 Zn1 C23 85.21(10) . . ? O2 Zn2 O7 111.14(11) . . ? O2 Zn2 O3 120.04(11) . . ? O7 Zn2 O3 96.21(11) . . ? O2 Zn2 N2 108.55(11) . . ? O7 Zn2 N2 102.53(11) . . ? O3 Zn2 N2 116.18(11) . . ? #=============================================================================# # End of CIF