# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Carpentier, Jean-Francois' _publ_contact_author_email jean-francois.carpentier@univ-rennes1.fr _publ_section_title ; Zinc and Magnesium Complexes Supported by Bulky Multidentate Amino-Ether Phenolate Ligands: Potent Pre-Catalysts for the Immortal Ring-Opening Polymerisation of Cyclic Esters ; _publ_requested_category FM loop_ _publ_author_name V.Poirier T.Roisnel J.-F.Carpentier Y.Sarazin # Attachment '- CIF files and Check Cif.doc' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2009-06-08 at 14:17:06 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : d:\progs\wingx\files\archive.dat # CIF files read : job struct data_job _database_code_depnum_ccdc_archive 'CCDC 780416' _audit_creation_date 2009-06-08T14:17:06-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #--------------------------------------------------------------------------- # CHEMICAL INFORMATION # #--------------------------------------------------------------------------- _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C27 H47 N O5 Zn, C27 H47 N O5 Zn' _chemical_formula_sum 'C54 H94 N2 O10 Zn2' _chemical_formula_weight 1062.05 _chemical_compound_source 'synthesis as described' #--------------------------------------------------------------------------- # UNIT CELL INFORMATION # #--------------------------------------------------------------------------- _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.9972(5) _cell_length_b 16.8148(9) _cell_length_c 17.4778(10) _cell_angle_alpha 74.056(3) _cell_angle_beta 86.334(3) _cell_angle_gamma 85.641(3) _cell_volume 2814.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5227 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 27.4 _cell_measurement_wavelength 0.71073 #--------------------------------------------------------------------------- # CRYSTAL INFORMATION # #--------------------------------------------------------------------------- _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.49 _exptl_crystal_size_min 0.31 _exptl_crystal_density_diffrn 1.253 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1144 _exptl_special_details ; ? ; #--------------------------------------------------------------------------- # ABSORPTION CORRECTION # #--------------------------------------------------------------------------- _exptl_absorpt_coefficient_mu 0.907 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_absorpt_correction_T_min 0.621 _exptl_absorpt_correction_T_max 0.755 #--------------------------------------------------------------------------- # DATA COLLECTION # #--------------------------------------------------------------------------- _diffrn_measurement_device_type 'APEXII, Bruker-AXS' _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_detector 'CCD plate' _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0509 _diffrn_reflns_av_unetI/netI 0.0577 _diffrn_reflns_number 42261 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 27.47 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.984 _diffrn_measured_fraction_theta_max 0.984 _reflns_number_total 12674 _reflns_number_gt 9621 _reflns_threshold_expression >2sigma(I) #--------------------------------------------------------------------------- # COMPUTER PROGRAMS USED # #--------------------------------------------------------------------------- _computing_data_collection 'Bruker SAINT' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _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^)+(0.0598P)^2^+1.3050P] 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 12674 _refine_ls_number_parameters 627 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0565 _refine_ls_R_factor_gt 0.0372 _refine_ls_wR_factor_ref 0.1039 _refine_ls_wR_factor_gt 0.0925 _refine_ls_goodness_of_fit_ref 0.892 _refine_ls_restrained_S_all 0.892 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.493 _refine_diff_density_min -0.338 _refine_diff_density_rms 0.069 #--------------------------------------------------------------------------- # 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 and6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and6.1.1.4' 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 0.60418(2) 0.531307(14) 0.244051(14) 0.01398(7) Uani 1 1 d . . . C1 C 0.4672(2) 0.51764(14) 0.33343(13) 0.0238(5) Uani 1 1 d . . . H1A H 0.4618 0.5681 0.3524 0.029 Uiso 1 1 calc R . . H1B H 0.3788 0.5138 0.3126 0.029 Uiso 1 1 calc R . . C2 C 0.4919(3) 0.44198(16) 0.40509(14) 0.0320(6) Uani 1 1 d . . . H2A H 0.4945 0.3912 0.3877 0.048 Uiso 1 1 calc R . . H2B H 0.4192 0.4408 0.4457 0.048 Uiso 1 1 calc R . . H2C H 0.5778 0.4457 0.4276 0.048 Uiso 1 1 calc R . . O11 O 0.60617(14) 0.42986(8) 0.18825(8) 0.0169(3) Uani 1 1 d . . . C12 C 0.5375(2) 0.35353(13) 0.21624(14) 0.0210(5) Uani 1 1 d . . . H12A H 0.56 0.3267 0.2722 0.025 Uiso 1 1 calc R . . H12B H 0.5712 0.3155 0.1841 0.025 Uiso 1 1 calc R . . C13 C 0.3873(2) 0.36558(14) 0.21182(13) 0.0219(5) Uani 1 1 d . . . H13A H 0.3454 0.3154 0.2454 0.026 Uiso 1 1 calc R . . H13B H 0.3546 0.413 0.2327 0.026 Uiso 1 1 calc R . . O14 O 0.34902(14) 0.38081(9) 0.13166(9) 0.0192(3) Uani 1 1 d . . . C15 C 0.2085(2) 0.37536(14) 0.12589(14) 0.0229(5) Uani 1 1 d . . . H15A H 0.1753 0.3323 0.1727 0.027 Uiso 1 1 calc R . . H15B H 0.1938 0.3576 0.0777 0.027 Uiso 1 1 calc R . . C16 C 0.1274(2) 0.45612(14) 0.12171(14) 0.0247(5) Uani 1 1 d . . . H16A H 0.0302 0.447 0.126 0.03 Uiso 1 1 calc R . . H16B H 0.149 0.4783 0.1661 0.03 Uiso 1 1 calc R . . O17 O 0.16063(15) 0.51301(9) 0.04738(9) 0.0222(3) Uani 1 1 d . . . C18 C 0.0977(2) 0.59423(15) 0.03775(15) 0.0268(5) Uani 1 1 d . . . H18A H -0.0002 0.5896 0.0487 0.032 Uiso 1 1 calc R . . H18B H 0.1119 0.6268 -0.0183 0.032 Uiso 1 1 calc R . . C19 C 0.1497(2) 0.64024(15) 0.09127(15) 0.0277(5) Uani 1 1 d . . . H19A H 0.1052 0.6966 0.0809 0.033 Uiso 1 1 calc R . . H19B H 0.1313 0.6105 0.1478 0.033 Uiso 1 1 calc R . . O20 O 0.29009(15) 0.64501(10) 0.07469(9) 0.0239(4) Uani 1 1 d . . . C21 C 0.3576(2) 0.67020(14) 0.13279(14) 0.0215(5) Uani 1 1 d . . . H21A H 0.3507 0.6282 0.1849 0.026 Uiso 1 1 calc R . . H21B H 0.316 0.7235 0.1391 0.026 Uiso 1 1 calc R . . C22 C 0.5035(2) 0.67966(12) 0.10494(13) 0.0179(4) Uani 1 1 d . . . H22A H 0.507 0.7053 0.0467 0.021 Uiso 1 1 calc R . . H22B H 0.5403 0.7188 0.1301 0.021 Uiso 1 1 calc R . . N23 N 0.59336(16) 0.60256(10) 0.12155(10) 0.0126(3) Uani 1 1 d . . . C24 C 0.5551(2) 0.54531(12) 0.07517(12) 0.0138(4) Uani 1 1 d . . . H24A H 0.5774 0.5695 0.0178 0.017 Uiso 1 1 calc R . . H24B H 0.457 0.5392 0.0818 0.017 Uiso 1 1 calc R . . C25 C 0.6283(2) 0.46064(12) 0.10301(12) 0.0154(4) Uani 1 1 d . . . H25A H 0.5942 0.422 0.0762 0.018 Uiso 1 1 calc R . . H25B H 0.7256 0.465 0.0894 0.018 Uiso 1 1 calc R . . O31 O 0.79694(14) 0.54209(8) 0.24774(8) 0.0147(3) Uani 1 1 d . . . C32 C 0.82851(19) 0.62175(12) 0.22464(12) 0.0126(4) Uani 1 1 d . . . C33 C 0.89625(19) 0.65905(12) 0.27415(12) 0.0131(4) Uani 1 1 d . . . C34 C 0.9408(2) 0.60872(12) 0.35675(12) 0.0158(4) Uani 1 1 d . . . C35 C 0.8202(2) 0.56942(14) 0.40848(13) 0.0217(5) Uani 1 1 d . . . H35A H 0.7512 0.6129 0.4125 0.033 Uiso 1 1 calc R . . H35B H 0.8494 0.5399 0.4618 0.033 Uiso 1 1 calc R . . H35C H 0.783 0.5304 0.3841 0.033 Uiso 1 1 calc R . . C36 C 1.0464(2) 0.54108(15) 0.34646(14) 0.0276(5) Uani 1 1 d . . . H36A H 1.0087 0.5064 0.3173 0.041 Uiso 1 1 calc R . . H36B H 1.0725 0.5067 0.3989 0.041 Uiso 1 1 calc R . . H36C H 1.1254 0.5668 0.3165 0.041 Uiso 1 1 calc R . . C37 C 1.0047(2) 0.66211(14) 0.40177(13) 0.0235(5) Uani 1 1 d . . . H37A H 1.0864 0.6846 0.3723 0.035 Uiso 1 1 calc R . . H37B H 1.0276 0.6279 0.4549 0.035 Uiso 1 1 calc R . . H37C H 0.9409 0.7078 0.4067 0.035 Uiso 1 1 calc R . . C38 C 0.92477(19) 0.74218(12) 0.24329(12) 0.0146(4) Uani 1 1 d . . . H38 H 0.9717 0.7667 0.2757 0.017 Uiso 1 1 calc R . . C39 C 0.8894(2) 0.79205(12) 0.16828(12) 0.0140(4) Uani 1 1 d . . . C40 C 0.9254(2) 0.88299(12) 0.14161(12) 0.0164(4) Uani 1 1 d . . . C41 C 1.0787(2) 0.88658(14) 0.13026(15) 0.0251(5) Uani 1 1 d . . . H41A H 1.1204 0.8573 0.1803 0.038 Uiso 1 1 calc R . . H41B H 1.1023 0.9445 0.1147 0.038 Uiso 1 1 calc R . . H41C H 1.1112 0.8602 0.0885 0.038 Uiso 1 1 calc R . . C42 C 0.8741(2) 0.92681(13) 0.20574(13) 0.0235(5) Uani 1 1 d . . . H42A H 0.777 0.9219 0.2152 0.035 Uiso 1 1 calc R . . H42B H 0.8933 0.9855 0.1874 0.035 Uiso 1 1 calc R . . H42C H 0.9194 0.9008 0.2554 0.035 Uiso 1 1 calc R . . C43 C 0.8622(2) 0.93039(13) 0.06306(13) 0.0223(5) Uani 1 1 d . . . H43A H 0.8964 0.9053 0.0207 0.033 Uiso 1 1 calc R . . H43B H 0.8854 0.9884 0.0491 0.033 Uiso 1 1 calc R . . H43C H 0.7644 0.9278 0.0692 0.033 Uiso 1 1 calc R . . C44 C 0.82371(19) 0.75450(12) 0.12107(12) 0.0133(4) Uani 1 1 d . . . H44 H 0.7982 0.7859 0.0695 0.016 Uiso 1 1 calc R . . C45 C 0.79453(19) 0.67083(12) 0.14844(12) 0.0129(4) Uani 1 1 d . . . C46 C 0.7324(2) 0.62872(12) 0.09485(12) 0.0141(4) Uani 1 1 d . . . H46A H 0.7297 0.667 0.0406 0.017 Uiso 1 1 calc R . . H46B H 0.7905 0.5792 0.0918 0.017 Uiso 1 1 calc R . . Zn2 Zn 0.80422(2) 1.169801(14) 0.266664(14) 0.01425(7) Uani 1 1 d . . . C51 C 0.9502(2) 1.21305(14) 0.18694(13) 0.0211(5) Uani 1 1 d . . . H51A H 0.9298 1.2734 0.1657 0.025 Uiso 1 1 calc R . . H51B H 1.0339 1.2062 0.2161 0.025 Uiso 1 1 calc R . . C52 C 0.9815(3) 1.17794(17) 0.11549(14) 0.0324(6) Uani 1 1 d . . . H52A H 1.0088 1.1189 0.1342 0.049 Uiso 1 1 calc R . . H52B H 1.0545 1.2074 0.0821 0.049 Uiso 1 1 calc R . . H52C H 0.9012 1.185 0.0843 0.049 Uiso 1 1 calc R . . O61 O 0.78101(14) 1.25493(8) 0.34392(8) 0.0178(3) Uani 1 1 d . . . C62 C 0.8332(2) 1.33676(12) 0.32177(14) 0.0189(5) Uani 1 1 d . . . H62A H 0.7922 1.3684 0.3584 0.023 Uiso 1 1 calc R . . H62B H 0.8061 1.3663 0.2673 0.023 Uiso 1 1 calc R . . C63 C 0.9827(2) 1.33527(14) 0.32401(13) 0.0198(5) Uani 1 1 d . . . H63A H 1.0241 1.2891 0.3039 0.024 Uiso 1 1 calc R . . H63B H 1.0153 1.3877 0.289 0.024 Uiso 1 1 calc R . . O64 O 1.02159(14) 1.32505(9) 0.40369(9) 0.0190(3) Uani 1 1 d . . . C65 C 1.1620(2) 1.33149(14) 0.40809(13) 0.0201(5) Uani 1 1 d . . . H65A H 1.1765 1.359 0.4499 0.024 Uiso 1 1 calc R . . H65B H 1.197 1.3668 0.3567 0.024 Uiso 1 1 calc R . . C66 C 1.2397(2) 1.24877(14) 0.42634(13) 0.0222(5) Uani 1 1 d . . . H66A H 1.3362 1.2566 0.4294 0.027 Uiso 1 1 calc R . . H66B H 1.2076 1.2136 0.4785 0.027 Uiso 1 1 calc R . . O67 O 1.22265(14) 1.20910(9) 0.36593(9) 0.0192(3) Uani 1 1 d . . . C68 C 1.3044(2) 1.13381(13) 0.37603(14) 0.0200(5) Uani 1 1 d . . . H68A H 1.3158 1.1072 0.4334 0.024 Uiso 1 1 calc R . . H68B H 1.3942 1.1456 0.3499 0.024 Uiso 1 1 calc R . . C69 C 1.2373(2) 1.07688(13) 0.33945(13) 0.0195(5) Uani 1 1 d . . . H69A H 1.2167 1.1056 0.2836 0.023 Uiso 1 1 calc R . . H69B H 1.2974 1.0272 0.3398 0.023 Uiso 1 1 calc R . . O70 O 1.11594(14) 1.05323(9) 0.38551(8) 0.0179(3) Uani 1 1 d . . . C71 C 1.0310(2) 1.01405(13) 0.34691(13) 0.0174(4) Uani 1 1 d . . . H71A H 1.0726 0.9591 0.3454 0.021 Uiso 1 1 calc R . . H71B H 1.0197 1.048 0.2914 0.021 Uiso 1 1 calc R . . C72 C 0.8947(2) 1.00351(12) 0.39087(13) 0.0162(4) Uani 1 1 d . . . H72A H 0.8455 0.9648 0.371 0.019 Uiso 1 1 calc R . . H72B H 0.9087 0.9775 0.4481 0.019 Uiso 1 1 calc R . . N73 N 0.80863(16) 1.08194(10) 0.38289(10) 0.0128(3) Uani 1 1 d . . . C74 C 0.8530(2) 1.12790(12) 0.43826(12) 0.0156(4) Uani 1 1 d . . . H74A H 0.9505 1.1354 0.4288 0.019 Uiso 1 1 calc R . . H74B H 0.8379 1.0943 0.4939 0.019 Uiso 1 1 calc R . . C75 C 0.7786(2) 1.21227(13) 0.42748(12) 0.0168(4) Uani 1 1 d . . . H75A H 0.6846 1.2054 0.4485 0.02 Uiso 1 1 calc R . . H75B H 0.8223 1.2448 0.4571 0.02 Uiso 1 1 calc R . . O81 O 0.61840(14) 1.15481(8) 0.25121(8) 0.0159(3) Uani 1 1 d . . . C82 C 0.58337(19) 1.07606(12) 0.26864(12) 0.0137(4) Uani 1 1 d . . . C83 C 0.5192(2) 1.04524(12) 0.21322(12) 0.0153(4) Uani 1 1 d . . . C84 C 0.4897(2) 1.10074(13) 0.12942(12) 0.0179(4) Uani 1 1 d . . . C85 C 0.6219(2) 1.13206(15) 0.08520(13) 0.0242(5) Uani 1 1 d . . . H85A H 0.6614 1.1675 0.1127 0.036 Uiso 1 1 calc R . . H85B H 0.6037 1.1639 0.0305 0.036 Uiso 1 1 calc R . . H85C H 0.6848 1.0847 0.0843 0.036 Uiso 1 1 calc R . . C86 C 0.3937(2) 1.17491(13) 0.13498(13) 0.0210(5) Uani 1 1 d . . . H86A H 0.3056 1.1553 0.1565 0.032 Uiso 1 1 calc R . . H86B H 0.3845 1.2132 0.0818 0.032 Uiso 1 1 calc R . . H86C H 0.4299 1.2036 0.1702 0.032 Uiso 1 1 calc R . . C87 C 0.4231(3) 1.05418(15) 0.07875(14) 0.0293(6) Uani 1 1 d . . . H87A H 0.4826 1.0068 0.0732 0.044 Uiso 1 1 calc R . . H87B H 0.4069 1.0917 0.0259 0.044 Uiso 1 1 calc R . . H87C H 0.3376 1.0344 0.1049 0.044 Uiso 1 1 calc R . . C88 C 0.4858(2) 0.96245(12) 0.23750(12) 0.0153(4) Uani 1 1 d . . . H88 H 0.4424 0.9417 0.2008 0.018 Uiso 1 1 calc R . . C89 C 0.51193(19) 0.90793(12) 0.31231(12) 0.0139(4) Uani 1 1 d . . . C90 C 0.4712(2) 0.81805(12) 0.33283(13) 0.0167(4) Uani 1 1 d . . . C91 C 0.3173(2) 0.81726(15) 0.34358(15) 0.0290(6) Uani 1 1 d . . . H91A H 0.2866 0.8413 0.3872 0.044 Uiso 1 1 calc R . . H91B H 0.2906 0.7601 0.3561 0.044 Uiso 1 1 calc R . . H91C H 0.2767 0.8499 0.2943 0.044 Uiso 1 1 calc R . . C92 C 0.5193(3) 0.77842(14) 0.26558(14) 0.0291(6) Uani 1 1 d . . . H92A H 0.479 0.8102 0.2158 0.044 Uiso 1 1 calc R . . H92B H 0.492 0.7213 0.2792 0.044 Uiso 1 1 calc R . . H92C H 0.6173 0.7785 0.2588 0.044 Uiso 1 1 calc R . . C93 C 0.5323(2) 0.76416(13) 0.40960(14) 0.0242(5) Uani 1 1 d . . . H93A H 0.6305 0.7636 0.4035 0.036 Uiso 1 1 calc R . . H93B H 0.5039 0.7075 0.4203 0.036 Uiso 1 1 calc R . . H93C H 0.5016 0.7869 0.4541 0.036 Uiso 1 1 calc R . . C94 C 0.57306(19) 0.94039(12) 0.36574(12) 0.0137(4) Uani 1 1 d . . . H94 H 0.592 0.9057 0.4172 0.016 Uiso 1 1 calc R . . C95 C 0.60691(19) 1.02299(12) 0.34484(12) 0.0137(4) Uani 1 1 d . . . C96 C 0.66596(19) 1.05887(13) 0.40464(12) 0.0139(4) Uani 1 1 d . . . H96A H 0.6101 1.1088 0.4089 0.017 Uiso 1 1 calc R . . H96B H 0.6628 1.0179 0.4575 0.017 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 #--------------------------------------------------------------------------- # MOLECULAR GEOMETRY # #--------------------------------------------------------------------------- Zn1 0.01376(13) 0.01452(13) 0.01385(13) -0.00335(10) -0.00119(9) -0.00345(9) C1 0.0219(12) 0.0261(12) 0.0222(12) -0.0049(10) 0.0043(9) -0.0038(9) C2 0.0322(14) 0.0374(14) 0.0233(13) -0.0027(11) 0.0072(10) -0.0098(11) O11 0.0207(8) 0.0123(7) 0.0176(8) -0.0024(6) -0.0055(6) -0.0040(6) C12 0.0268(12) 0.0117(10) 0.0234(12) -0.0005(9) -0.0073(9) -0.0056(9) C13 0.0257(12) 0.0217(11) 0.0194(12) -0.0048(9) -0.0018(9) -0.0102(9) O14 0.0169(8) 0.0242(8) 0.0170(8) -0.0053(6) -0.0006(6) -0.0066(6) C15 0.0177(11) 0.0292(12) 0.0243(12) -0.0096(10) 0.0015(9) -0.0106(9) C16 0.0178(11) 0.0322(13) 0.0247(13) -0.0088(10) 0.0036(9) -0.0041(9) O17 0.0195(8) 0.0259(8) 0.0208(8) -0.0064(7) 0.0008(6) -0.0011(6) C18 0.0125(11) 0.0311(13) 0.0374(14) -0.0106(11) -0.0036(10) 0.0018(9) C19 0.0155(11) 0.0315(13) 0.0389(15) -0.0152(11) 0.0009(10) 0.0002(9) O20 0.0139(8) 0.0341(9) 0.0269(9) -0.0134(7) -0.0022(6) -0.0018(6) C21 0.0189(11) 0.0215(11) 0.0258(12) -0.0099(10) -0.0044(9) 0.0041(9) C22 0.0176(11) 0.0130(10) 0.0238(12) -0.0054(9) -0.0073(9) 0.0004(8) N23 0.0131(8) 0.0122(8) 0.0139(9) -0.0049(7) -0.0038(7) -0.0022(6) C24 0.0122(10) 0.0153(10) 0.0150(10) -0.0049(8) -0.0033(8) -0.0036(8) C25 0.0160(10) 0.0163(10) 0.0153(10) -0.0059(8) -0.0015(8) -0.0036(8) O31 0.0148(7) 0.0104(7) 0.0189(8) -0.0029(6) -0.0041(6) -0.0029(5) C32 0.0098(9) 0.0122(9) 0.0163(10) -0.0043(8) -0.0020(8) -0.0005(7) C33 0.0117(10) 0.0138(10) 0.0134(10) -0.0024(8) -0.0023(8) -0.0008(7) C34 0.0165(11) 0.0155(10) 0.0155(11) -0.0029(8) -0.0054(8) -0.0014(8) C35 0.0266(12) 0.0241(12) 0.0134(11) -0.0003(9) -0.0043(9) -0.0101(9) C36 0.0296(13) 0.0289(13) 0.0243(13) -0.0071(10) -0.0140(10) 0.0097(10) C37 0.0272(13) 0.0247(12) 0.0192(12) -0.0032(10) -0.0081(9) -0.0086(10) C38 0.0122(10) 0.0166(10) 0.0175(11) -0.0080(9) -0.0030(8) -0.0025(8) C39 0.0135(10) 0.0118(10) 0.0165(10) -0.0030(8) -0.0010(8) -0.0028(8) C40 0.0175(11) 0.0129(10) 0.0192(11) -0.0034(8) -0.0030(8) -0.0045(8) C41 0.0200(12) 0.0196(11) 0.0331(14) -0.0013(10) -0.0012(10) -0.0071(9) C42 0.0345(14) 0.0133(11) 0.0231(12) -0.0047(9) -0.0008(10) -0.0049(9) C43 0.0273(13) 0.0144(11) 0.0234(12) -0.0006(9) -0.0048(10) -0.0040(9) C44 0.0115(10) 0.0149(10) 0.0123(10) -0.0018(8) -0.0012(8) 0.0002(8) C45 0.0102(10) 0.0146(10) 0.0144(10) -0.0040(8) -0.0010(8) -0.0030(7) C46 0.0145(10) 0.0153(10) 0.0125(10) -0.0033(8) -0.0008(8) -0.0034(8) Zn2 0.01403(13) 0.01465(13) 0.01439(13) -0.00369(10) -0.00127(9) -0.00322(9) C51 0.0181(11) 0.0236(12) 0.0215(12) -0.0056(9) 0.0002(9) -0.0038(9) C52 0.0312(14) 0.0440(15) 0.0260(13) -0.0148(12) 0.0087(10) -0.0150(11) O61 0.0223(8) 0.0138(7) 0.0175(8) -0.0032(6) -0.0049(6) -0.0032(6) C62 0.0216(11) 0.0101(10) 0.0255(12) -0.0047(9) -0.0060(9) -0.0011(8) C63 0.0210(11) 0.0206(11) 0.0187(11) -0.0055(9) -0.0037(9) -0.0042(9) O64 0.0163(8) 0.0251(8) 0.0176(8) -0.0081(6) -0.0029(6) -0.0036(6) C65 0.0155(11) 0.0260(12) 0.0226(12) -0.0122(10) -0.0031(9) -0.0028(9) C66 0.0204(12) 0.0270(12) 0.0208(12) -0.0073(10) -0.0077(9) -0.0025(9) O67 0.0193(8) 0.0168(8) 0.0221(8) -0.0061(6) -0.0046(6) 0.0021(6) C68 0.0136(10) 0.0189(11) 0.0260(12) -0.0042(9) -0.0014(9) 0.0009(8) C69 0.0128(10) 0.0196(11) 0.0251(12) -0.0057(9) 0.0021(9) 0.0018(8) O70 0.0135(7) 0.0225(8) 0.0187(8) -0.0066(6) -0.0009(6) -0.0036(6) C71 0.0148(11) 0.0176(10) 0.0207(11) -0.0066(9) -0.0033(8) 0.0014(8) C72 0.0143(10) 0.0143(10) 0.0196(11) -0.0036(9) -0.0036(8) 0.0006(8) N73 0.0107(8) 0.0139(8) 0.0151(9) -0.0053(7) -0.0024(7) -0.0010(6) C74 0.0159(10) 0.0181(10) 0.0138(10) -0.0046(8) -0.0046(8) -0.0026(8) C75 0.0170(11) 0.0201(11) 0.0152(11) -0.0072(9) -0.0003(8) -0.0037(8) O81 0.0158(7) 0.0118(7) 0.0200(8) -0.0028(6) -0.0057(6) -0.0019(5) C82 0.0105(10) 0.0129(10) 0.0170(11) -0.0029(8) -0.0019(8) 0.0005(7) C83 0.0137(10) 0.0143(10) 0.0180(11) -0.0050(8) -0.0020(8) 0.0012(8) C84 0.0197(11) 0.0188(11) 0.0155(11) -0.0044(9) -0.0050(8) 0.0001(8) C85 0.0248(12) 0.0270(12) 0.0165(11) 0.0002(10) -0.0009(9) 0.0034(10) C86 0.0186(11) 0.0200(11) 0.0218(12) -0.0016(9) -0.0050(9) 0.0038(9) C87 0.0447(16) 0.0258(13) 0.0191(12) -0.0056(10) -0.0145(11) -0.0043(11) C88 0.0138(10) 0.0179(10) 0.0171(11) -0.0087(9) -0.0040(8) -0.0019(8) C89 0.0093(10) 0.0154(10) 0.0177(11) -0.0057(8) 0.0004(8) -0.0010(7) C90 0.0172(11) 0.0129(10) 0.0202(11) -0.0039(9) -0.0020(8) -0.0039(8) C91 0.0211(12) 0.0250(13) 0.0399(15) -0.0050(11) -0.0029(10) -0.0077(10) C92 0.0446(15) 0.0167(11) 0.0277(13) -0.0085(10) 0.0034(11) -0.0072(10) C93 0.0278(13) 0.0158(11) 0.0274(13) -0.0015(10) -0.0054(10) -0.0047(9) C94 0.0098(10) 0.0138(10) 0.0155(10) -0.0006(8) -0.0009(8) 0.0004(7) C95 0.0099(10) 0.0165(10) 0.0162(10) -0.0064(8) -0.0019(8) -0.0020(8) C96 0.0122(10) 0.0162(10) 0.0146(10) -0.0057(8) 0.0000(8) -0.0032(8) _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 O31 1.9560(14) . ? Zn1 C1 1.987(2) . ? Zn1 N23 2.1522(17) . ? Zn1 O11 2.1836(14) . ? C1 C2 1.538(3) . ? C1 H1A 0.99 . ? C1 H1B 0.99 . ? C2 H2A 0.98 . ? C2 H2B 0.98 . ? C2 H2C 0.98 . ? O11 C25 1.445(2) . ? O11 C12 1.450(2) . ? C12 C13 1.504(3) . ? C12 H12A 0.99 . ? C12 H12B 0.99 . ? C13 O14 1.425(3) . ? C13 H13A 0.99 . ? C13 H13B 0.99 . ? O14 C15 1.427(2) . ? C15 C16 1.514(3) . ? C15 H15A 0.99 . ? C15 H15B 0.99 . ? C16 O17 1.422(3) . ? C16 H16A 0.99 . ? C16 H16B 0.99 . ? O17 C18 1.430(3) . ? C18 C19 1.505(3) . ? C18 H18A 0.99 . ? C18 H18B 0.99 . ? C19 O20 1.418(3) . ? C19 H19A 0.99 . ? C19 H19B 0.99 . ? O20 C21 1.426(3) . ? C21 C22 1.514(3) . ? C21 H21A 0.99 . ? C21 H21B 0.99 . ? C22 N23 1.491(3) . ? C22 H22A 0.99 . ? C22 H22B 0.99 . ? N23 C46 1.496(2) . ? N23 C24 1.502(2) . ? C24 C25 1.518(3) . ? C24 H24A 0.99 . ? C24 H24B 0.99 . ? C25 H25A 0.99 . ? C25 H25B 0.99 . ? O31 C32 1.344(2) . ? C32 C45 1.408(3) . ? C32 C33 1.428(3) . ? C33 C38 1.397(3) . ? C33 C34 1.534(3) . ? C34 C36 1.531(3) . ? C34 C35 1.537(3) . ? C34 C37 1.540(3) . ? C35 H35A 0.98 . ? C35 H35B 0.98 . ? C35 H35C 0.98 . ? C36 H36A 0.98 . ? C36 H36B 0.98 . ? C36 H36C 0.98 . ? C37 H37A 0.98 . ? C37 H37B 0.98 . ? C37 H37C 0.98 . ? C38 C39 1.399(3) . ? C38 H38 0.95 . ? C39 C44 1.389(3) . ? C39 C40 1.535(3) . ? C40 C43 1.534(3) . ? C40 C41 1.537(3) . ? C40 C42 1.544(3) . ? C41 H41A 0.98 . ? C41 H41B 0.98 . ? C41 H41C 0.98 . ? C42 H42A 0.98 . ? C42 H42B 0.98 . ? C42 H42C 0.98 . ? C43 H43A 0.98 . ? C43 H43B 0.98 . ? C43 H43C 0.98 . ? C44 C45 1.403(3) . ? C44 H44 0.95 . ? C45 C46 1.507(3) . ? C46 H46A 0.99 . ? C46 H46B 0.99 . ? Zn2 O81 1.9391(14) . ? Zn2 C51 1.986(2) . ? Zn2 N73 2.1595(17) . ? Zn2 O61 2.2130(14) . ? C51 C52 1.527(3) . ? C51 H51A 0.99 . ? C51 H51B 0.99 . ? C52 H52A 0.98 . ? C52 H52B 0.98 . ? C52 H52C 0.98 . ? O61 C75 1.439(2) . ? O61 C62 1.451(2) . ? C62 C63 1.496(3) . ? C62 H62A 0.99 . ? C62 H62B 0.99 . ? C63 O64 1.431(2) . ? C63 H63A 0.99 . ? C63 H63B 0.99 . ? O64 C65 1.425(2) . ? C65 C66 1.505(3) . ? C65 H65A 0.99 . ? C65 H65B 0.99 . ? C66 O67 1.420(3) . ? C66 H66A 0.99 . ? C66 H66B 0.99 . ? O67 C68 1.428(2) . ? C68 C69 1.504(3) . ? C68 H68A 0.99 . ? C68 H68B 0.99 . ? C69 O70 1.432(2) . ? C69 H69A 0.99 . ? C69 H69B 0.99 . ? O70 C71 1.419(2) . ? C71 C72 1.519(3) . ? C71 H71A 0.99 . ? C71 H71B 0.99 . ? C72 N73 1.497(3) . ? C72 H72A 0.99 . ? C72 H72B 0.99 . ? N73 C74 1.499(2) . ? N73 C96 1.504(2) . ? C74 C75 1.520(3) . ? C74 H74A 0.99 . ? C74 H74B 0.99 . ? C75 H75A 0.99 . ? C75 H75B 0.99 . ? O81 C82 1.343(2) . ? C82 C95 1.407(3) . ? C82 C83 1.423(3) . ? C83 C88 1.399(3) . ? C83 C84 1.538(3) . ? C84 C86 1.535(3) . ? C84 C85 1.541(3) . ? C84 C87 1.541(3) . ? C85 H85A 0.98 . ? C85 H85B 0.98 . ? C85 H85C 0.98 . ? C86 H86A 0.98 . ? C86 H86B 0.98 . ? C86 H86C 0.98 . ? C87 H87A 0.98 . ? C87 H87B 0.98 . ? C87 H87C 0.98 . ? C88 C89 1.402(3) . ? C88 H88 0.95 . ? C89 C94 1.395(3) . ? C89 C90 1.535(3) . ? C90 C93 1.532(3) . ? C90 C92 1.538(3) . ? C90 C91 1.538(3) . ? C91 H91A 0.98 . ? C91 H91B 0.98 . ? C91 H91C 0.98 . ? C92 H92A 0.98 . ? C92 H92B 0.98 . ? C92 H92C 0.98 . ? C93 H93A 0.98 . ? C93 H93B 0.98 . ? C93 H93C 0.98 . ? C94 C95 1.398(3) . ? C94 H94 0.95 . ? C95 C96 1.512(3) . ? C96 H96A 0.99 . ? C96 H96B 0.99 . ? 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 O31 Zn1 C1 127.63(8) . . ? O31 Zn1 N23 94.15(6) . . ? C1 Zn1 N23 130.36(8) . . ? O31 Zn1 O11 100.56(6) . . ? C1 Zn1 O11 111.14(8) . . ? N23 Zn1 O11 80.89(6) . . ? C2 C1 Zn1 115.77(16) . . ? C2 C1 H1A 108.3 . . ? Zn1 C1 H1A 108.3 . . ? C2 C1 H1B 108.3 . . ? Zn1 C1 H1B 108.3 . . ? H1A C1 H1B 107.4 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C25 O11 C12 116.24(15) . . ? C25 O11 Zn1 110.21(11) . . ? C12 O11 Zn1 127.86(13) . . ? O11 C12 C13 113.78(17) . . ? O11 C12 H12A 108.8 . . ? C13 C12 H12A 108.8 . . ? O11 C12 H12B 108.8 . . ? C13 C12 H12B 108.8 . . ? H12A C12 H12B 107.7 . . ? O14 C13 C12 110.54(18) . . ? O14 C13 H13A 109.5 . . ? C12 C13 H13A 109.5 . . ? O14 C13 H13B 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 108.1 . . ? C13 O14 C15 112.76(16) . . ? O14 C15 C16 113.41(17) . . ? O14 C15 H15A 108.9 . . ? C16 C15 H15A 108.9 . . ? O14 C15 H15B 108.9 . . ? C16 C15 H15B 108.9 . . ? H15A C15 H15B 107.7 . . ? O17 C16 C15 107.92(18) . . ? O17 C16 H16A 110.1 . . ? C15 C16 H16A 110.1 . . ? O17 C16 H16B 110.1 . . ? C15 C16 H16B 110.1 . . ? H16A C16 H16B 108.4 . . ? C16 O17 C18 113.83(17) . . ? O17 C18 C19 113.60(19) . . ? O17 C18 H18A 108.8 . . ? C19 C18 H18A 108.8 . . ? O17 C18 H18B 108.8 . . ? C19 C18 H18B 108.8 . . ? H18A C18 H18B 107.7 . . ? O20 C19 C18 107.43(18) . . ? O20 C19 H19A 110.2 . . ? C18 C19 H19A 110.2 . . ? O20 C19 H19B 110.2 . . ? C18 C19 H19B 110.2 . . ? H19A C19 H19B 108.5 . . ? C19 O20 C21 113.40(17) . . ? O20 C21 C22 108.19(17) . . ? O20 C21 H21A 110.1 . . ? C22 C21 H21A 110.1 . . ? O20 C21 H21B 110.1 . . ? C22 C21 H21B 110.1 . . ? H21A C21 H21B 108.4 . . ? N23 C22 C21 116.75(17) . . ? N23 C22 H22A 108.1 . . ? C21 C22 H22A 108.1 . . ? N23 C22 H22B 108.1 . . ? C21 C22 H22B 108.1 . . ? H22A C22 H22B 107.3 . . ? C22 N23 C46 106.58(15) . . ? C22 N23 C24 110.91(15) . . ? C46 N23 C24 108.86(15) . . ? C22 N23 Zn1 116.80(13) . . ? C46 N23 Zn1 106.21(12) . . ? C24 N23 Zn1 107.17(11) . . ? N23 C24 C25 111.14(16) . . ? N23 C24 H24A 109.4 . . ? C25 C24 H24A 109.4 . . ? N23 C24 H24B 109.4 . . ? C25 C24 H24B 109.4 . . ? H24A C24 H24B 108 . . ? O11 C25 C24 108.77(16) . . ? O11 C25 H25A 109.9 . . ? C24 C25 H25A 109.9 . . ? O11 C25 H25B 109.9 . . ? C24 C25 H25B 109.9 . . ? H25A C25 H25B 108.3 . . ? C32 O31 Zn1 111.90(12) . . ? O31 C32 C45 119.13(16) . . ? O31 C32 C33 122.71(18) . . ? C45 C32 C33 118.15(17) . . ? C38 C33 C32 117.47(18) . . ? C38 C33 C34 121.34(17) . . ? C32 C33 C34 121.15(17) . . ? C36 C34 C33 108.61(17) . . ? C36 C34 C35 110.06(18) . . ? C33 C34 C35 110.47(16) . . ? C36 C34 C37 107.67(18) . . ? C33 C34 C37 112.52(17) . . ? C35 C34 C37 107.46(17) . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C34 C37 H37A 109.5 . . ? C34 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C34 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C33 C38 C39 124.94(18) . . ? C33 C38 H38 117.5 . . ? C39 C38 H38 117.5 . . ? C44 C39 C38 116.62(17) . . ? C44 C39 C40 123.48(18) . . ? C38 C39 C40 119.89(17) . . ? C43 C40 C39 112.16(16) . . ? C43 C40 C41 108.58(17) . . ? C39 C40 C41 109.19(17) . . ? C43 C40 C42 107.86(18) . . ? C39 C40 C42 109.66(17) . . ? C41 C40 C42 109.34(17) . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C40 C43 H43A 109.5 . . ? C40 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C40 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C39 C44 C45 120.90(19) . . ? C39 C44 H44 119.6 . . ? C45 C44 H44 119.6 . . ? C44 C45 C32 121.90(18) . . ? C44 C45 C46 120.69(18) . . ? C32 C45 C46 117.31(17) . . ? N23 C46 C45 114.10(16) . . ? N23 C46 H46A 108.7 . . ? C45 C46 H46A 108.7 . . ? N23 C46 H46B 108.7 . . ? C45 C46 H46B 108.7 . . ? H46A C46 H46B 107.6 . . ? O81 Zn2 C51 129.80(8) . . ? O81 Zn2 N73 94.43(6) . . ? C51 Zn2 N73 131.56(8) . . ? O81 Zn2 O61 101.40(6) . . ? C51 Zn2 O61 105.37(7) . . ? N73 Zn2 O61 79.47(6) . . ? C52 C51 Zn2 120.76(15) . . ? C52 C51 H51A 107.1 . . ? Zn2 C51 H51A 107.1 . . ? C52 C51 H51B 107.1 . . ? Zn2 C51 H51B 107.1 . . ? H51A C51 H51B 106.8 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C75 O61 C62 116.09(15) . . ? C75 O61 Zn2 113.02(11) . . ? C62 O61 Zn2 123.37(12) . . ? O61 C62 C63 113.56(17) . . ? O61 C62 H62A 108.9 . . ? C63 C62 H62A 108.9 . . ? O61 C62 H62B 108.9 . . ? C63 C62 H62B 108.9 . . ? H62A C62 H62B 107.7 . . ? O64 C63 C62 110.29(17) . . ? O64 C63 H63A 109.6 . . ? C62 C63 H63A 109.6 . . ? O64 C63 H63B 109.6 . . ? C62 C63 H63B 109.6 . . ? H63A C63 H63B 108.1 . . ? C65 O64 C63 112.61(16) . . ? O64 C65 C66 112.93(17) . . ? O64 C65 H65A 109 . . ? C66 C65 H65A 109 . . ? O64 C65 H65B 109 . . ? C66 C65 H65B 109 . . ? H65A C65 H65B 107.8 . . ? O67 C66 C65 109.87(17) . . ? O67 C66 H66A 109.7 . . ? C65 C66 H66A 109.7 . . ? O67 C66 H66B 109.7 . . ? C65 C66 H66B 109.7 . . ? H66A C66 H66B 108.2 . . ? C66 O67 C68 112.35(16) . . ? O67 C68 C69 108.77(17) . . ? O67 C68 H68A 109.9 . . ? C69 C68 H68A 109.9 . . ? O67 C68 H68B 109.9 . . ? C69 C68 H68B 109.9 . . ? H68A C68 H68B 108.3 . . ? O70 C69 C68 107.88(17) . . ? O70 C69 H69A 110.1 . . ? C68 C69 H69A 110.1 . . ? O70 C69 H69B 110.1 . . ? C68 C69 H69B 110.1 . . ? H69A C69 H69B 108.4 . . ? C71 O70 C69 112.35(16) . . ? O70 C71 C72 110.26(17) . . ? O70 C71 H71A 109.6 . . ? C72 C71 H71A 109.6 . . ? O70 C71 H71B 109.6 . . ? C72 C71 H71B 109.6 . . ? H71A C71 H71B 108.1 . . ? N73 C72 C71 115.02(16) . . ? N73 C72 H72A 108.5 . . ? C71 C72 H72A 108.5 . . ? N73 C72 H72B 108.5 . . ? C71 C72 H72B 108.5 . . ? H72A C72 H72B 107.5 . . ? C72 N73 C74 109.80(15) . . ? C72 N73 C96 107.83(15) . . ? C74 N73 C96 109.71(15) . . ? C72 N73 Zn2 117.42(12) . . ? C74 N73 Zn2 106.05(12) . . ? C96 N73 Zn2 105.84(12) . . ? N73 C74 C75 112.55(16) . . ? N73 C74 H74A 109.1 . . ? C75 C74 H74A 109.1 . . ? N73 C74 H74B 109.1 . . ? C75 C74 H74B 109.1 . . ? H74A C74 H74B 107.8 . . ? O61 C75 C74 108.66(16) . . ? O61 C75 H75A 110 . . ? C74 C75 H75A 110 . . ? O61 C75 H75B 110 . . ? C74 C75 H75B 110 . . ? H75A C75 H75B 108.3 . . ? C82 O81 Zn2 116.03(12) . . ? O81 C82 C95 119.15(17) . . ? O81 C82 C83 121.99(18) . . ? C95 C82 C83 118.83(17) . . ? C88 C83 C82 117.50(18) . . ? C88 C83 C84 121.44(18) . . ? C82 C83 C84 121.06(17) . . ? C86 C84 C83 110.31(17) . . ? C86 C84 C85 109.63(18) . . ? C83 C84 C85 109.63(17) . . ? C86 C84 C87 107.32(18) . . ? C83 C84 C87 112.32(17) . . ? C85 C84 C87 107.57(19) . . ? C84 C85 H85A 109.5 . . ? C84 C85 H85B 109.5 . . ? H85A C85 H85B 109.5 . . ? C84 C85 H85C 109.5 . . ? H85A C85 H85C 109.5 . . ? H85B C85 H85C 109.5 . . ? C84 C86 H86A 109.5 . . ? C84 C86 H86B 109.5 . . ? H86A C86 H86B 109.5 . . ? C84 C86 H86C 109.5 . . ? H86A C86 H86C 109.5 . . ? H86B C86 H86C 109.5 . . ? C84 C87 H87A 109.5 . . ? C84 C87 H87B 109.5 . . ? H87A C87 H87B 109.5 . . ? C84 C87 H87C 109.5 . . ? H87A C87 H87C 109.5 . . ? H87B C87 H87C 109.5 . . ? C83 C88 C89 124.51(18) . . ? C83 C88 H88 117.7 . . ? C89 C88 H88 117.7 . . ? C94 C89 C88 116.60(18) . . ? C94 C89 C90 123.11(18) . . ? C88 C89 C90 120.27(17) . . ? C93 C90 C89 112.31(16) . . ? C93 C90 C92 107.33(18) . . ? C89 C90 C92 110.31(17) . . ? C93 C90 C91 108.45(18) . . ? C89 C90 C91 109.07(17) . . ? C92 C90 C91 109.30(18) . . ? C90 C91 H91A 109.5 . . ? C90 C91 H91B 109.5 . . ? H91A C91 H91B 109.5 . . ? C90 C91 H91C 109.5 . . ? H91A C91 H91C 109.5 . . ? H91B C91 H91C 109.5 . . ? C90 C92 H92A 109.5 . . ? C90 C92 H92B 109.5 . . ? H92A C92 H92B 109.5 . . ? C90 C92 H92C 109.5 . . ? H92A C92 H92C 109.5 . . ? H92B C92 H92C 109.5 . . ? C90 C93 H93A 109.5 . . ? C90 C93 H93B 109.5 . . ? H93A C93 H93B 109.5 . . ? C90 C93 H93C 109.5 . . ? H93A C93 H93C 109.5 . . ? H93B C93 H93C 109.5 . . ? C89 C94 C95 121.17(19) . . ? C89 C94 H94 119.4 . . ? C95 C94 H94 119.4 . . ? C94 C95 C82 121.35(18) . . ? C94 C95 C96 120.77(18) . . ? C82 C95 C96 117.85(17) . . ? N73 C96 C95 113.06(16) . . ? N73 C96 H96A 109 . . ? C95 C96 H96A 109 . . ? N73 C96 H96B 109 . . ? C95 C96 H96B 109 . . ? H96A C96 H96B 107.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O31 Zn1 C1 C2 -58.0(2) . . . . ? N23 Zn1 C1 C2 161.20(14) . . . . ? O11 Zn1 C1 C2 65.13(18) . . . . ? O31 Zn1 O11 C25 -80.41(12) . . . . ? C1 Zn1 O11 C25 142.03(13) . . . . ? N23 Zn1 O11 C25 12.15(12) . . . . ? O31 Zn1 O11 C12 127.59(15) . . . . ? C1 Zn1 O11 C12 -9.97(17) . . . . ? N23 Zn1 O11 C12 -139.85(16) . . . . ? C25 O11 C12 C13 -81.4(2) . . . . ? Zn1 O11 C12 C13 69.2(2) . . . . ? O11 C12 C13 O14 75.5(2) . . . . ? C12 C13 O14 C15 167.60(17) . . . . ? C13 O14 C15 C16 87.5(2) . . . . ? O14 C15 C16 O17 68.3(2) . . . . ? C15 C16 O17 C18 -175.92(17) . . . . ? C16 O17 C18 C19 68.9(2) . . . . ? O17 C18 C19 O20 58.0(3) . . . . ? C18 C19 O20 C21 -166.66(19) . . . . ? C19 O20 C21 C22 -175.42(18) . . . . ? O20 C21 C22 N23 -82.3(2) . . . . ? C21 C22 N23 C46 -175.40(17) . . . . ? C21 C22 N23 C24 66.3(2) . . . . ? C21 C22 N23 Zn1 -56.9(2) . . . . ? O31 Zn1 N23 C22 -119.39(13) . . . . ? C1 Zn1 N23 C22 30.51(17) . . . . ? O11 Zn1 N23 C22 140.57(13) . . . . ? O31 Zn1 N23 C46 -0.71(12) . . . . ? C1 Zn1 N23 C46 149.19(13) . . . . ? O11 Zn1 N23 C46 -100.75(12) . . . . ? O31 Zn1 N23 C24 115.54(12) . . . . ? C1 Zn1 N23 C24 -94.57(15) . . . . ? O11 Zn1 N23 C24 15.49(12) . . . . ? C22 N23 C24 C25 -169.42(16) . . . . ? C46 N23 C24 C25 73.62(19) . . . . ? Zn1 N23 C24 C25 -40.86(18) . . . . ? C12 O11 C25 C24 118.45(18) . . . . ? Zn1 O11 C25 C24 -37.14(17) . . . . ? N23 C24 C25 O11 53.2(2) . . . . ? C1 Zn1 O31 C32 -97.03(15) . . . . ? N23 Zn1 O31 C32 54.11(13) . . . . ? O11 Zn1 O31 C32 135.60(12) . . . . ? Zn1 O31 C32 C45 -57.7(2) . . . . ? Zn1 O31 C32 C33 122.66(17) . . . . ? O31 C32 C33 C38 179.42(18) . . . . ? C45 C32 C33 C38 -0.2(3) . . . . ? O31 C32 C33 C34 1.8(3) . . . . ? C45 C32 C33 C34 -177.86(18) . . . . ? C38 C33 C34 C36 -113.5(2) . . . . ? C32 C33 C34 C36 64.1(2) . . . . ? C38 C33 C34 C35 125.7(2) . . . . ? C32 C33 C34 C35 -56.7(2) . . . . ? C38 C33 C34 C37 5.6(3) . . . . ? C32 C33 C34 C37 -176.79(19) . . . . ? C32 C33 C38 C39 1.5(3) . . . . ? C34 C33 C38 C39 179.11(18) . . . . ? C33 C38 C39 C44 -1.5(3) . . . . ? C33 C38 C39 C40 179.37(19) . . . . ? C44 C39 C40 C43 8.7(3) . . . . ? C38 C39 C40 C43 -172.29(18) . . . . ? C44 C39 C40 C41 -111.7(2) . . . . ? C38 C39 C40 C41 67.3(2) . . . . ? C44 C39 C40 C42 128.5(2) . . . . ? C38 C39 C40 C42 -52.5(2) . . . . ? C38 C39 C44 C45 0.3(3) . . . . ? C40 C39 C44 C45 179.41(18) . . . . ? C39 C44 C45 C32 0.8(3) . . . . ? C39 C44 C45 C46 -175.53(19) . . . . ? O31 C32 C45 C44 179.48(18) . . . . ? C33 C32 C45 C44 -0.9(3) . . . . ? O31 C32 C45 C46 -4.0(3) . . . . ? C33 C32 C45 C46 175.58(18) . . . . ? C22 N23 C46 C45 73.0(2) . . . . ? C24 N23 C46 C45 -167.29(16) . . . . ? Zn1 N23 C46 C45 -52.19(18) . . . . ? C44 C45 C46 N23 -114.3(2) . . . . ? C32 C45 C46 N23 69.2(2) . . . . ? O81 Zn2 C51 C52 -51.2(2) . . . . ? N73 Zn2 C51 C52 99.6(2) . . . . ? O61 Zn2 C51 C52 -170.93(18) . . . . ? O81 Zn2 O61 C75 91.66(13) . . . . ? C51 Zn2 O61 C75 -131.23(13) . . . . ? N73 Zn2 O61 C75 -0.79(12) . . . . ? O81 Zn2 O61 C62 -119.90(14) . . . . ? C51 Zn2 O61 C62 17.21(16) . . . . ? N73 Zn2 O61 C62 147.65(15) . . . . ? C75 O61 C62 C63 75.0(2) . . . . ? Zn2 O61 C62 C63 -72.5(2) . . . . ? O61 C62 C63 O64 -82.1(2) . . . . ? C62 C63 O64 C65 -174.12(16) . . . . ? C63 O64 C65 C66 -94.4(2) . . . . ? O64 C65 C66 O67 60.0(2) . . . . ? C65 C66 O67 C68 174.41(17) . . . . ? C66 O67 C68 C69 152.56(17) . . . . ? O67 C68 C69 O70 -66.8(2) . . . . ? C68 C69 O70 C71 167.51(17) . . . . ? C69 O70 C71 C72 -170.37(16) . . . . ? O70 C71 C72 N73 71.5(2) . . . . ? C71 C72 N73 C74 -79.4(2) . . . . ? C71 C72 N73 C96 161.08(17) . . . . ? C71 C72 N73 Zn2 41.8(2) . . . . ? O81 Zn2 N73 C72 112.28(13) . . . . ? C51 Zn2 N73 C72 -45.65(17) . . . . ? O61 Zn2 N73 C72 -146.93(13) . . . . ? O81 Zn2 N73 C74 -124.61(12) . . . . ? C51 Zn2 N73 C74 77.46(15) . . . . ? O61 Zn2 N73 C74 -23.82(12) . . . . ? O81 Zn2 N73 C96 -8.10(12) . . . . ? C51 Zn2 N73 C96 -166.03(12) . . . . ? O61 Zn2 N73 C96 92.69(11) . . . . ? C72 N73 C74 C75 174.44(16) . . . . ? C96 N73 C74 C75 -67.2(2) . . . . ? Zn2 N73 C74 C75 46.65(18) . . . . ? C62 O61 C75 C74 -125.67(17) . . . . ? Zn2 O61 C75 C74 25.20(18) . . . . ? N73 C74 C75 O61 -48.7(2) . . . . ? C51 Zn2 O81 C82 111.94(15) . . . . ? N73 Zn2 O81 C82 -46.59(14) . . . . ? O61 Zn2 O81 C82 -126.73(13) . . . . ? Zn2 O81 C82 C95 55.2(2) . . . . ? Zn2 O81 C82 C83 -126.81(17) . . . . ? O81 C82 C83 C88 -179.44(18) . . . . ? C95 C82 C83 C88 -1.5(3) . . . . ? O81 C82 C83 C84 1.4(3) . . . . ? C95 C82 C83 C84 179.38(18) . . . . ? C88 C83 C84 C86 119.1(2) . . . . ? C82 C83 C84 C86 -61.8(2) . . . . ? C88 C83 C84 C85 -120.1(2) . . . . ? C82 C83 C84 C85 59.0(3) . . . . ? C88 C83 C84 C87 -0.6(3) . . . . ? C82 C83 C84 C87 178.5(2) . . . . ? C82 C83 C88 C89 -0.4(3) . . . . ? C84 C83 C88 C89 178.75(19) . . . . ? C83 C88 C89 C94 1.4(3) . . . . ? C83 C88 C89 C90 -179.87(19) . . . . ? C94 C89 C90 C93 -12.7(3) . . . . ? C88 C89 C90 C93 168.64(19) . . . . ? C94 C89 C90 C92 -132.4(2) . . . . ? C88 C89 C90 C92 49.0(3) . . . . ? C94 C89 C90 C91 107.6(2) . . . . ? C88 C89 C90 C91 -71.1(2) . . . . ? C88 C89 C94 C95 -0.5(3) . . . . ? C90 C89 C94 C95 -179.17(18) . . . . ? C89 C94 C95 C82 -1.4(3) . . . . ? C89 C94 C95 C96 176.56(19) . . . . ? O81 C82 C95 C94 -179.59(18) . . . . ? C83 C82 C95 C94 2.4(3) . . . . ? O81 C82 C95 C96 2.4(3) . . . . ? C83 C82 C95 C96 -175.65(18) . . . . ? C72 N73 C96 C95 -68.5(2) . . . . ? C74 N73 C96 C95 171.93(16) . . . . ? Zn2 N73 C96 C95 57.92(17) . . . . ? C94 C95 C96 N73 113.9(2) . . . . ? C82 C95 C96 N73 -68.1(2) . . . . ? # Attachment 'VP313_120K_KCCD_03sept09_archive.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2009-09-04 at 10:27:47 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : d:\progs\wingx\files\archive.dat # CIF files read : job struct data_job2 _database_code_depnum_ccdc_archive 'CCDC 780417' #TrackingRef 'VP313_120K_KCCD_03sept09_archive.cif' _audit_creation_date 2009-09-04T10:27:47-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C23 H39 N O2 Zn' _chemical_formula_sum 'C23 H39 N O2 Zn' _chemical_formula_weight 426.92 _chemical_compound_source 'synthesis as described' _chemical_absolute_configuration ad #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 8.4855(2) _cell_length_b 14.4219(4) _cell_length_c 19.4610(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2381.58(11) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 24351 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.485 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.32 _exptl_crystal_density_diffrn 1.191 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 920 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.047 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_absorpt_correction_T_min 0.551 _exptl_absorpt_correction_T_max 0.715 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0303 _diffrn_reflns_av_unetI/netI 0.028 _diffrn_reflns_number 31311 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.5 _diffrn_reflns_theta_full 27.5 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _reflns_number_total 5426 _reflns_number_gt 5095 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _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^)+(0.0237P)^2^+0.2406P] 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 5426 _refine_ls_number_parameters 252 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0257 _refine_ls_R_factor_gt 0.0218 _refine_ls_wR_factor_ref 0.0536 _refine_ls_wR_factor_gt 0.052 _refine_ls_goodness_of_fit_ref 1.162 _refine_ls_restrained_S_all 1.162 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.001 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.031(7) _refine_diff_density_max 0.273 _refine_diff_density_min -0.429 _refine_diff_density_rms 0.08 #----------------------------------------------------------------------------# # 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 0.154738(19) 0.230343(12) 0.671207(8) 0.01524(5) Uani 1 1 d . . . O1 O 0.27335(13) 0.31655(7) 0.61609(5) 0.0183(2) Uani 1 1 d . . . C2 C 0.20129(17) 0.37990(10) 0.57719(7) 0.0143(3) Uani 1 1 d . . . C3 C 0.25202(18) 0.47446(10) 0.57582(7) 0.0160(3) Uani 1 1 d . . . C4 C 0.17000(19) 0.53607(10) 0.53357(7) 0.0177(3) Uani 1 1 d . . . H4 H 0.2029 0.599 0.5332 0.021 Uiso 1 1 calc R . . C5 C 0.04231(19) 0.51128(10) 0.49164(7) 0.0184(3) Uani 1 1 d . . . C6 C -0.00370(17) 0.41875(11) 0.49337(7) 0.0170(3) Uani 1 1 d . . . H6 H -0.0893 0.3992 0.4654 0.02 Uiso 1 1 calc R . . C7 C 0.07238(18) 0.35373(10) 0.53505(7) 0.0153(3) Uani 1 1 d . . . C8 C 0.39934(18) 0.50602(11) 0.61529(8) 0.0184(3) Uani 1 1 d . . . C9 C 0.4301(2) 0.61073(12) 0.60795(10) 0.0307(4) Uani 1 1 d . . . H9A H 0.5239 0.6277 0.6345 0.046 Uiso 1 1 calc R . . H9B H 0.3389 0.6453 0.6253 0.046 Uiso 1 1 calc R . . H9C H 0.447 0.6259 0.5594 0.046 Uiso 1 1 calc R . . C10 C 0.5425(2) 0.45499(12) 0.58613(9) 0.0259(4) Uani 1 1 d . . . H10A H 0.6375 0.4745 0.6109 0.039 Uiso 1 1 calc R . . H10B H 0.5539 0.4698 0.5372 0.039 Uiso 1 1 calc R . . H10C H 0.5278 0.388 0.5916 0.039 Uiso 1 1 calc R . . C11 C 0.3846(2) 0.48584(14) 0.69244(8) 0.0324(4) Uani 1 1 d . . . H11A H 0.3678 0.4193 0.6994 0.049 Uiso 1 1 calc R . . H11B H 0.2951 0.5204 0.7113 0.049 Uiso 1 1 calc R . . H11C H 0.4816 0.505 0.7159 0.049 Uiso 1 1 calc R . . C12 C -0.0397(2) 0.58577(11) 0.44788(8) 0.0234(3) Uani 1 1 d . . . C13 C -0.1229(2) 0.65529(14) 0.49542(10) 0.0391(5) Uani 1 1 d . . . H13A H -0.1765 0.7024 0.4676 0.059 Uiso 1 1 calc R . . H13B H -0.0449 0.6853 0.5251 0.059 Uiso 1 1 calc R . . H13C H -0.2004 0.6225 0.5238 0.059 Uiso 1 1 calc R . . C14 C -0.1611(3) 0.54307(15) 0.39912(12) 0.0569(7) Uani 1 1 d . . . H14A H -0.2444 0.513 0.426 0.085 Uiso 1 1 calc R . . H14B H -0.1095 0.497 0.3698 0.085 Uiso 1 1 calc R . . H14C H -0.2072 0.5919 0.3704 0.085 Uiso 1 1 calc R . . C15 C 0.0812(2) 0.63878(13) 0.40404(9) 0.0311(4) Uani 1 1 d . . . H15A H 0.1364 0.5952 0.3738 0.047 Uiso 1 1 calc R . . H15B H 0.1576 0.6695 0.4342 0.047 Uiso 1 1 calc R . . H15C H 0.0267 0.6854 0.3762 0.047 Uiso 1 1 calc R . . C16 C 0.01993(17) 0.25424(10) 0.53427(7) 0.0155(3) Uani 1 1 d . . . H16A H -0.0648 0.247 0.4997 0.019 Uiso 1 1 calc R . . H16B H 0.1096 0.2149 0.5197 0.019 Uiso 1 1 calc R . . N17 N -0.03915(14) 0.22034(9) 0.60215(6) 0.0145(2) Uani 1 1 d . . . C18 C -0.0927(2) 0.12202(10) 0.59653(8) 0.0199(3) Uani 1 1 d . . . H18A H -0.002 0.0789 0.5962 0.024 Uiso 1 1 calc R . . H18B H -0.156 0.1123 0.5544 0.024 Uiso 1 1 calc R . . C19 C -0.1926(2) 0.10901(13) 0.66071(8) 0.0292(4) Uani 1 1 d . . . H19A H -0.1257 0.0994 0.7018 0.035 Uiso 1 1 calc R . . H19B H -0.2652 0.0557 0.6557 0.035 Uiso 1 1 calc R . . C20 C -0.2831(2) 0.20011(13) 0.66544(10) 0.0316(4) Uani 1 1 d . . . H20A H -0.2989 0.2181 0.714 0.038 Uiso 1 1 calc R . . H20B H -0.3874 0.1943 0.6431 0.038 Uiso 1 1 calc R . . C21 C -0.18035(16) 0.27291(12) 0.62773(7) 0.0197(3) Uani 1 1 d . . . H21 H -0.2405 0.2969 0.5873 0.024 Uiso 1 1 calc R . . C22 C -0.13299(18) 0.35433(10) 0.67272(8) 0.0213(3) Uani 1 1 d . . . H22A H -0.0848 0.4038 0.6444 0.026 Uiso 1 1 calc R . . H22B H -0.2266 0.3802 0.6963 0.026 Uiso 1 1 calc R . . O23 O -0.02145(14) 0.32034(8) 0.72217(6) 0.0227(2) Uani 1 1 d . . . C24 C 0.0220(2) 0.38982(14) 0.77100(9) 0.0358(4) Uani 1 1 d . . . H24A H 0.0573 0.4456 0.7467 0.054 Uiso 1 1 calc R . . H24B H 0.1076 0.3665 0.8 0.054 Uiso 1 1 calc R . . H24C H -0.0693 0.4051 0.7998 0.054 Uiso 1 1 calc R . . C25 C 0.2195(2) 0.13487(12) 0.73811(8) 0.0256(4) Uani 1 1 d . . . H25A H 0.196 0.0731 0.7184 0.031 Uiso 1 1 calc R . . H25B H 0.335 0.1389 0.7445 0.031 Uiso 1 1 calc R . . C26 C 0.1405(3) 0.14180(13) 0.80856(8) 0.0329(4) Uani 1 1 d . . . H26A H 0.1736 0.1992 0.8312 0.049 Uiso 1 1 calc R . . H26B H 0.1714 0.0885 0.8368 0.049 Uiso 1 1 calc R . . H26C H 0.0257 0.1421 0.8028 0.049 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 0.01749(8) 0.01351(8) 0.01471(7) 0.00165(7) -0.00304(7) 0.00141(7) O1 0.0166(5) 0.0168(5) 0.0215(5) 0.0047(4) -0.0032(4) 0.0000(4) C2 0.0142(7) 0.0153(7) 0.0136(6) 0.0015(5) 0.0015(5) 0.0008(5) C3 0.0147(7) 0.0162(7) 0.0173(7) -0.0027(6) 0.0011(6) -0.0011(6) C4 0.0182(8) 0.0131(7) 0.0217(7) 0.0008(5) 0.0000(6) -0.0012(6) C5 0.0189(7) 0.0176(7) 0.0187(7) 0.0035(6) -0.0018(6) -0.0003(6) C6 0.0154(7) 0.0208(7) 0.0149(7) 0.0016(6) -0.0019(5) -0.0031(6) C7 0.0168(8) 0.0158(7) 0.0134(7) 0.0009(6) 0.0020(6) -0.0027(6) C8 0.0181(7) 0.0153(8) 0.0219(7) -0.0011(6) -0.0032(6) -0.0026(6) C9 0.0265(10) 0.0165(8) 0.0491(11) -0.0026(8) -0.0135(8) -0.0029(7) C10 0.0164(8) 0.0253(9) 0.0359(9) -0.0053(7) -0.0040(7) -0.0003(7) C11 0.0384(11) 0.0384(10) 0.0203(8) -0.0052(7) -0.0054(7) -0.0131(8) C12 0.0235(8) 0.0181(8) 0.0287(8) 0.0075(7) -0.0063(7) -0.0003(7) C13 0.0385(12) 0.0374(10) 0.0414(11) 0.0163(8) 0.0097(9) 0.0190(9) C14 0.0652(15) 0.0379(12) 0.0674(15) 0.0270(11) -0.0479(14) -0.0143(13) C15 0.0348(10) 0.0259(9) 0.0325(9) 0.0116(8) 0.0065(8) 0.0058(8) C16 0.0179(7) 0.0172(8) 0.0113(6) 0.0001(5) -0.0009(5) -0.0021(6) N17 0.0162(6) 0.0133(6) 0.0139(5) 0.0013(5) -0.0004(4) -0.0009(5) C18 0.0254(8) 0.0134(7) 0.0209(7) 0.0031(6) -0.0056(6) -0.0052(6) C19 0.0340(10) 0.0312(9) 0.0223(8) 0.0081(7) -0.0034(7) -0.0156(8) C20 0.0250(8) 0.0404(10) 0.0292(9) -0.0040(8) 0.0070(7) -0.0135(7) C21 0.0160(7) 0.0249(7) 0.0182(6) 0.0043(6) -0.0015(5) 0.0042(7) C22 0.0224(8) 0.0188(7) 0.0226(7) 0.0029(6) 0.0026(7) 0.0077(6) O23 0.0237(6) 0.0225(6) 0.0220(5) -0.0074(5) -0.0037(4) 0.0038(5) C24 0.0351(10) 0.0382(11) 0.0341(10) -0.0223(8) -0.0005(8) 0.0020(9) C25 0.0281(9) 0.0248(9) 0.0239(8) 0.0071(7) -0.0049(7) 0.0046(7) C26 0.0427(11) 0.0334(9) 0.0226(8) 0.0089(7) -0.0052(8) 0.0012(9) #----------------------------------------------------------------------------# # 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 1.9259(11) . ? Zn1 C25 1.9730(15) . ? Zn1 N17 2.1293(12) . ? Zn1 O23 2.2144(11) . ? O1 C2 1.3348(18) . ? C2 C7 1.418(2) . ? C2 C3 1.430(2) . ? C3 C4 1.396(2) . ? C3 C8 1.536(2) . ? C4 C5 1.403(2) . ? C4 H4 0.95 . ? C5 C6 1.391(2) . ? C5 C12 1.537(2) . ? C6 C7 1.398(2) . ? C6 H6 0.95 . ? C7 C16 1.502(2) . ? C8 C10 1.529(2) . ? C8 C11 1.534(2) . ? C8 C9 1.539(2) . ? C9 H9A 0.98 . ? C9 H9B 0.98 . ? C9 H9C 0.98 . ? C10 H10A 0.98 . ? C10 H10B 0.98 . ? C10 H10C 0.98 . ? C11 H11A 0.98 . ? C11 H11B 0.98 . ? C11 H11C 0.98 . ? C12 C14 1.530(3) . ? C12 C13 1.536(3) . ? C12 C15 1.538(2) . ? C13 H13A 0.98 . ? C13 H13B 0.98 . ? C13 H13C 0.98 . ? C14 H14A 0.98 . ? C14 H14B 0.98 . ? C14 H14C 0.98 . ? C15 H15A 0.98 . ? C15 H15B 0.98 . ? C15 H15C 0.98 . ? C16 N17 1.4951(17) . ? C16 H16A 0.99 . ? C16 H16B 0.99 . ? N17 C18 1.4931(19) . ? N17 C21 1.5026(19) . ? C18 C19 1.521(2) . ? C18 H18A 0.99 . ? C18 H18B 0.99 . ? C19 C20 1.525(3) . ? C19 H19A 0.99 . ? C19 H19B 0.99 . ? C20 C21 1.550(2) . ? C20 H20A 0.99 . ? C20 H20B 0.99 . ? C21 C22 1.519(2) . ? C21 H21 1 . ? C22 O23 1.4360(19) . ? C22 H22A 0.99 . ? C22 H22B 0.99 . ? O23 C24 1.4293(19) . ? C24 H24A 0.98 . ? C24 H24B 0.98 . ? C24 H24C 0.98 . ? C25 C26 1.529(2) . ? C25 H25A 0.99 . ? C25 H25B 0.99 . ? C26 H26A 0.98 . ? C26 H26B 0.98 . ? C26 H26C 0.98 . ? 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 C25 132.26(6) . . ? O1 Zn1 N17 95.51(4) . . ? C25 Zn1 N17 125.76(6) . . ? O1 Zn1 O23 102.94(5) . . ? C25 Zn1 O23 107.55(6) . . ? N17 Zn1 O23 78.50(4) . . ? C2 O1 Zn1 121.22(9) . . ? O1 C2 C7 119.94(13) . . ? O1 C2 C3 121.69(13) . . ? C7 C2 C3 118.36(13) . . ? C4 C3 C2 117.88(13) . . ? C4 C3 C8 120.76(13) . . ? C2 C3 C8 121.20(13) . . ? C3 C4 C5 124.43(13) . . ? C3 C4 H4 117.8 . . ? C5 C4 H4 117.8 . . ? C6 C5 C4 116.57(13) . . ? C6 C5 C12 123.84(14) . . ? C4 C5 C12 119.58(13) . . ? C5 C6 C7 121.87(14) . . ? C5 C6 H6 119.1 . . ? C7 C6 H6 119.1 . . ? C6 C7 C2 120.88(14) . . ? C6 C7 C16 119.86(13) . . ? C2 C7 C16 119.24(13) . . ? C10 C8 C11 109.65(14) . . ? C10 C8 C3 108.56(12) . . ? C11 C8 C3 111.52(13) . . ? C10 C8 C9 107.64(14) . . ? C11 C8 C9 106.89(14) . . ? C3 C8 C9 112.47(13) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C14 C12 C13 109.06(17) . . ? C14 C12 C5 111.53(14) . . ? C13 C12 C5 109.30(13) . . ? C14 C12 C15 107.77(15) . . ? C13 C12 C15 108.44(15) . . ? C5 C12 C15 110.67(14) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N17 C16 C7 113.74(11) . . ? N17 C16 H16A 108.8 . . ? C7 C16 H16A 108.8 . . ? N17 C16 H16B 108.8 . . ? C7 C16 H16B 108.8 . . ? H16A C16 H16B 107.7 . . ? C18 N17 C16 110.36(11) . . ? C18 N17 C21 105.11(12) . . ? C16 N17 C21 113.27(11) . . ? C18 N17 Zn1 110.23(9) . . ? C16 N17 Zn1 106.05(8) . . ? C21 N17 Zn1 111.89(8) . . ? N17 C18 C19 103.09(12) . . ? N17 C18 H18A 111.1 . . ? C19 C18 H18A 111.1 . . ? N17 C18 H18B 111.1 . . ? C19 C18 H18B 111.1 . . ? H18A C18 H18B 109.1 . . ? C18 C19 C20 102.94(13) . . ? C18 C19 H19A 111.2 . . ? C20 C19 H19A 111.2 . . ? C18 C19 H19B 111.2 . . ? C20 C19 H19B 111.2 . . ? H19A C19 H19B 109.1 . . ? C19 C20 C21 105.77(14) . . ? C19 C20 H20A 110.6 . . ? C21 C20 H20A 110.6 . . ? C19 C20 H20B 110.6 . . ? C21 C20 H20B 110.6 . . ? H20A C20 H20B 108.7 . . ? N17 C21 C22 111.72(11) . . ? N17 C21 C20 105.29(13) . . ? C22 C21 C20 113.55(12) . . ? N17 C21 H21 108.7 . . ? C22 C21 H21 108.7 . . ? C20 C21 H21 108.7 . . ? O23 C22 C21 107.26(11) . . ? O23 C22 H22A 110.3 . . ? C21 C22 H22A 110.3 . . ? O23 C22 H22B 110.3 . . ? C21 C22 H22B 110.3 . . ? H22A C22 H22B 108.5 . . ? C24 O23 C22 112.09(13) . . ? C24 O23 Zn1 122.32(10) . . ? C22 O23 Zn1 110.18(8) . . ? O23 C24 H24A 109.5 . . ? O23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? O23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 Zn1 115.08(12) . . ? C26 C25 H25A 108.5 . . ? Zn1 C25 H25A 108.5 . . ? C26 C25 H25B 108.5 . . ? Zn1 C25 H25B 108.5 . . ? H25A C25 H25B 107.5 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C25 Zn1 O1 C2 -175.43(11) . . . . ? N17 Zn1 O1 C2 32.82(11) . . . . ? O23 Zn1 O1 C2 -46.62(11) . . . . ? Zn1 O1 C2 C7 -46.34(16) . . . . ? Zn1 O1 C2 C3 134.59(12) . . . . ? O1 C2 C3 C4 179.90(13) . . . . ? C7 C2 C3 C4 0.8(2) . . . . ? O1 C2 C3 C8 4.4(2) . . . . ? C7 C2 C3 C8 -174.73(13) . . . . ? C2 C3 C4 C5 -0.8(2) . . . . ? C8 C3 C4 C5 174.72(14) . . . . ? C3 C4 C5 C6 0.2(2) . . . . ? C3 C4 C5 C12 179.36(14) . . . . ? C4 C5 C6 C7 0.5(2) . . . . ? C12 C5 C6 C7 -178.66(14) . . . . ? C5 C6 C7 C2 -0.4(2) . . . . ? C5 C6 C7 C16 -179.03(14) . . . . ? O1 C2 C7 C6 -179.32(13) . . . . ? C3 C2 C7 C6 -0.2(2) . . . . ? O1 C2 C7 C16 -0.7(2) . . . . ? C3 C2 C7 C16 178.38(13) . . . . ? C4 C3 C8 C10 -113.19(16) . . . . ? C2 C3 C8 C10 62.23(18) . . . . ? C4 C3 C8 C11 125.90(16) . . . . ? C2 C3 C8 C11 -58.69(19) . . . . ? C4 C3 C8 C9 5.8(2) . . . . ? C2 C3 C8 C9 -178.77(14) . . . . ? C6 C5 C12 C14 -8.3(2) . . . . ? C4 C5 C12 C14 172.63(17) . . . . ? C6 C5 C12 C13 112.39(18) . . . . ? C4 C5 C12 C13 -66.70(19) . . . . ? C6 C5 C12 C15 -128.24(17) . . . . ? C4 C5 C12 C15 52.7(2) . . . . ? C6 C7 C16 N17 -118.33(14) . . . . ? C2 C7 C16 N17 63.06(17) . . . . ? C7 C16 N17 C18 178.50(12) . . . . ? C7 C16 N17 C21 60.97(16) . . . . ? C7 C16 N17 Zn1 -62.12(13) . . . . ? O1 Zn1 N17 C18 138.38(9) . . . . ? C25 Zn1 N17 C18 -16.05(12) . . . . ? O23 Zn1 N17 C18 -119.50(10) . . . . ? O1 Zn1 N17 C16 18.92(9) . . . . ? C25 Zn1 N17 C16 -135.51(10) . . . . ? O23 Zn1 N17 C16 121.04(9) . . . . ? O1 Zn1 N17 C21 -105.04(10) . . . . ? C25 Zn1 N17 C21 100.53(11) . . . . ? O23 Zn1 N17 C21 -2.93(9) . . . . ? C16 N17 C18 C19 -163.15(12) . . . . ? C21 N17 C18 C19 -40.69(14) . . . . ? Zn1 N17 C18 C19 80.04(12) . . . . ? N17 C18 C19 C20 40.66(15) . . . . ? C18 C19 C20 C21 -25.46(17) . . . . ? C18 N17 C21 C22 147.99(12) . . . . ? C16 N17 C21 C22 -91.45(14) . . . . ? Zn1 N17 C21 C22 28.36(14) . . . . ? C18 N17 C21 C20 24.29(14) . . . . ? C16 N17 C21 C20 144.85(12) . . . . ? Zn1 N17 C21 C20 -95.34(12) . . . . ? C19 C20 C21 N17 1.17(16) . . . . ? C19 C20 C21 C22 -121.36(14) . . . . ? N17 C21 C22 O23 -48.70(15) . . . . ? C20 C21 C22 O23 70.21(16) . . . . ? C21 C22 O23 C24 -175.30(13) . . . . ? C21 C22 O23 Zn1 44.88(13) . . . . ? O1 Zn1 O23 C24 -65.87(13) . . . . ? C25 Zn1 O23 C24 76.91(14) . . . . ? N17 Zn1 O23 C24 -158.96(13) . . . . ? O1 Zn1 O23 C22 69.10(10) . . . . ? C25 Zn1 O23 C22 -148.12(10) . . . . ? N17 Zn1 O23 C22 -23.98(10) . . . . ? O1 Zn1 C25 C26 126.74(13) . . . . ? N17 Zn1 C25 C26 -88.75(14) . . . . ? O23 Zn1 C25 C26 -0.46(15) . . . . ? # Attachment 'VP356_150K_APEX_20oct09_archive.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2009-10-20 at 14:29:54 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : d:\progs\wingx\files\archive.dat # CIF files read : job struct data_job3 _database_code_depnum_ccdc_archive 'CCDC 780418' #TrackingRef 'VP356_150K_APEX_20oct09_archive.cif' _audit_creation_date 2009-10-20T14:29:54-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C31 H60 N2 O5 Si2 Zn1' _chemical_formula_sum 'C31 H60 N2 O5 Si2 Zn' _chemical_formula_weight 662.36 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.7067(4) _cell_length_b 13.1381(5) _cell_length_c 13.9560(6) _cell_angle_alpha 76.371(2) _cell_angle_beta 72.957(2) _cell_angle_gamma 83.477(2) _cell_volume 1821.97(12) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5553 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 27.4 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.47 _exptl_crystal_size_min 0.4 _exptl_crystal_density_diffrn 1.207 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 716 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.777 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_absorpt_correction_T_min 0.526 _exptl_absorpt_correction_T_max 0.733 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_measurement_device_type 'APEXII, Bruker-AXS' _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_detector 'CCD plate' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0404 _diffrn_reflns_av_unetI/netI 0.0434 _diffrn_reflns_number 23988 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 27.46 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.986 _diffrn_measured_fraction_theta_max 0.986 _reflns_number_total 8218 _reflns_number_gt 7065 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SAINT (Bruker, 2002)' _computing_cell_refinement 'Bruker SMART (Bruker, 2002)' _computing_data_reduction 'Bruker SAINT (Bruker, 2002)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _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^)+(0.0297P)^2^+0.4111P] 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 8218 _refine_ls_number_parameters 382 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0387 _refine_ls_R_factor_gt 0.0303 _refine_ls_wR_factor_ref 0.0772 _refine_ls_wR_factor_gt 0.0735 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.384 _refine_diff_density_min -0.373 _refine_diff_density_rms 0.051 #----------------------------------------------------------------------------# # 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.172245(15) 0.323905(13) 0.411253(13) 0.01661(6) Uani 1 1 d . . . N1 N 0.34940(12) 0.28419(10) 0.34559(10) 0.0211(3) Uani 1 1 d . . . Si1 Si 0.46396(4) 0.36400(4) 0.34768(4) 0.02536(11) Uani 1 1 d . . . C2 C 0.38481(17) 0.47973(13) 0.40370(14) 0.0318(4) Uani 1 1 d . . . H2A H 0.3218 0.5161 0.367 0.048 Uiso 1 1 calc R . . H2B H 0.4519 0.5278 0.397 0.048 Uiso 1 1 calc R . . H2C H 0.3394 0.4557 0.4764 0.048 Uiso 1 1 calc R . . C3 C 0.57557(17) 0.29917(17) 0.42768(16) 0.0433(5) Uani 1 1 d . . . H3A H 0.5239 0.2608 0.494 0.065 Uiso 1 1 calc R . . H3B H 0.6236 0.3526 0.4388 0.065 Uiso 1 1 calc R . . H3C H 0.6377 0.2502 0.3922 0.065 Uiso 1 1 calc R . . C4 C 0.57150(19) 0.41788(16) 0.21497(15) 0.0426(5) Uani 1 1 d . . . H4A H 0.6165 0.3597 0.1835 0.064 Uiso 1 1 calc R . . H4B H 0.6362 0.462 0.2199 0.064 Uiso 1 1 calc R . . H4C H 0.5175 0.4598 0.1727 0.064 Uiso 1 1 calc R . . Si2 Si 0.38158(4) 0.16728(3) 0.30730(4) 0.02354(10) Uani 1 1 d . . . C5 C 0.55943(17) 0.12341(15) 0.27582(16) 0.0387(5) Uani 1 1 d . . . H5A H 0.6107 0.1787 0.2242 0.058 Uiso 1 1 calc R . . H5B H 0.5714 0.0595 0.2488 0.058 Uiso 1 1 calc R . . H5C H 0.589 0.1091 0.338 0.058 Uiso 1 1 calc R . . C6 C 0.33341(19) 0.17489(14) 0.18685(14) 0.0350(4) Uani 1 1 d . . . H6A H 0.2425 0.2019 0.1961 0.053 Uiso 1 1 calc R . . H6B H 0.342 0.1048 0.1719 0.053 Uiso 1 1 calc R . . H6C H 0.3906 0.222 0.1297 0.053 Uiso 1 1 calc R . . C7 C 0.29499(19) 0.05817(14) 0.41024(15) 0.0368(4) Uani 1 1 d . . . H7A H 0.3397 0.0387 0.4645 0.055 Uiso 1 1 calc R . . H7B H 0.2958 -0.0027 0.3807 0.055 Uiso 1 1 calc R . . H7C H 0.2044 0.0816 0.4392 0.055 Uiso 1 1 calc R . . O11 O 0.14269(10) 0.33944(8) 0.55107(8) 0.0188(2) Uani 1 1 d . . . C12 C 0.04888(14) 0.28929(11) 0.62836(11) 0.0167(3) Uani 1 1 d . . . C13 C 0.07211(14) 0.23448(11) 0.72269(11) 0.0177(3) Uani 1 1 d . . . C14 C -0.03469(14) 0.19078(11) 0.80113(11) 0.0192(3) Uani 1 1 d . . . H14 H -0.0198 0.1561 0.865 0.023 Uiso 1 1 calc R . . C15 C -0.16237(14) 0.19464(11) 0.79211(11) 0.0185(3) Uani 1 1 d . . . C16 C -0.18027(14) 0.24443(11) 0.69739(11) 0.0188(3) Uani 1 1 d . . . H16 H -0.2644 0.2467 0.6869 0.023 Uiso 1 1 calc R . . C17 C -0.07789(14) 0.29121(11) 0.61727(11) 0.0172(3) Uani 1 1 d . . . C18 C 0.21185(14) 0.21957(12) 0.73501(12) 0.0212(3) Uani 1 1 d . . . C19 C 0.21856(16) 0.15072(13) 0.83918(13) 0.0274(4) Uani 1 1 d . . . H19A H 0.1853 0.0818 0.8472 0.041 Uiso 1 1 calc R . . H19B H 0.1652 0.1843 0.8944 0.041 Uiso 1 1 calc R . . H19C H 0.3095 0.1421 0.8423 0.041 Uiso 1 1 calc R . . C20 C 0.26725(16) 0.32585(13) 0.72501(13) 0.0271(4) Uani 1 1 d . . . H20A H 0.3573 0.3147 0.7302 0.041 Uiso 1 1 calc R . . H20B H 0.2135 0.3595 0.7801 0.041 Uiso 1 1 calc R . . H20C H 0.2662 0.371 0.6584 0.041 Uiso 1 1 calc R . . C21 C 0.29983(15) 0.16405(14) 0.65148(13) 0.0286(4) Uani 1 1 d . . . H21A H 0.2639 0.0967 0.6576 0.043 Uiso 1 1 calc R . . H21B H 0.3883 0.152 0.6601 0.043 Uiso 1 1 calc R . . H21C H 0.3032 0.2082 0.5836 0.043 Uiso 1 1 calc R . . C22 C -0.27643(15) 0.15045(13) 0.88411(12) 0.0238(3) Uani 1 1 d . . . C23 C -0.39643(17) 0.13716(16) 0.85117(15) 0.0380(4) Uani 1 1 d . . . H23A H -0.3726 0.0918 0.8014 0.057 Uiso 1 1 calc R . . H23B H -0.4289 0.2059 0.8197 0.057 Uiso 1 1 calc R . . H23C H -0.4649 0.1053 0.9113 0.057 Uiso 1 1 calc R . . C24 C -0.3149(2) 0.22724(16) 0.95720(14) 0.0413(5) Uani 1 1 d . . . H24A H -0.3503 0.2933 0.9231 0.062 Uiso 1 1 calc R . . H24B H -0.2375 0.2406 0.9755 0.062 Uiso 1 1 calc R . . H24C H -0.3812 0.1966 1.0195 0.062 Uiso 1 1 calc R . . C25 C -0.23788(18) 0.04395(14) 0.94348(15) 0.0370(4) Uani 1 1 d . . . H25A H -0.3126 0.0178 1.0012 0.056 Uiso 1 1 calc R . . H25B H -0.1645 0.0515 0.9694 0.056 Uiso 1 1 calc R . . H25C H -0.2119 -0.0058 0.8979 0.056 Uiso 1 1 calc R . . C26 C -0.10109(14) 0.34706(12) 0.51655(11) 0.0176(3) Uani 1 1 d . . . H26A H -0.0761 0.4206 0.5015 0.021 Uiso 1 1 calc R . . H26B H -0.1956 0.3481 0.5224 0.021 Uiso 1 1 calc R . . N31 N -0.02546(11) 0.29697(9) 0.42840(9) 0.0160(3) Uani 1 1 d . . . C32 C -0.06510(15) 0.18576(11) 0.45485(12) 0.0207(3) Uani 1 1 d . . . H32A H -0.1617 0.1856 0.4795 0.025 Uiso 1 1 calc R . . H32B H -0.0306 0.147 0.5124 0.025 Uiso 1 1 calc R . . C33 C -0.02009(15) 0.12705(12) 0.36905(13) 0.0244(3) Uani 1 1 d . . . H33A H 0.0671 0.1497 0.3247 0.029 Uiso 1 1 calc R . . H33B H -0.0129 0.0508 0.3977 0.029 Uiso 1 1 calc R . . O34 O -0.11188(11) 0.14802(9) 0.31068(9) 0.0275(3) Uani 1 1 d . . . C35 C -0.07593(19) 0.10082(14) 0.22367(14) 0.0359(4) Uani 1 1 d . . . H35A H -0.1404 0.0488 0.2319 0.043 Uiso 1 1 calc R . . H35B H 0.0109 0.0637 0.2184 0.043 Uiso 1 1 calc R . . C36 C -0.07118(18) 0.18266(16) 0.12818(14) 0.0354(4) Uani 1 1 d . . . H36A H -0.0619 0.1488 0.07 0.042 Uiso 1 1 calc R . . H36B H -0.1535 0.2267 0.1372 0.042 Uiso 1 1 calc R . . O37 O 0.03607(11) 0.24576(9) 0.10708(9) 0.0315(3) Uani 1 1 d . . . C38 C 0.03494(19) 0.33538(14) 0.02758(13) 0.0341(4) Uani 1 1 d . . . H38A H -0.0461 0.3793 0.0467 0.041 Uiso 1 1 calc R . . H38B H 0.0381 0.3139 -0.0365 0.041 Uiso 1 1 calc R . . C39 C 0.1520(2) 0.39616(15) 0.01190(13) 0.0371(4) Uani 1 1 d . . . H39A H 0.2306 0.3482 0.0102 0.045 Uiso 1 1 calc R . . H39B H 0.1676 0.448 -0.0541 0.045 Uiso 1 1 calc R . . O40 O 0.12758(12) 0.44855(10) 0.09483(9) 0.0333(3) Uani 1 1 d . . . C41 C 0.24132(17) 0.46841(14) 0.11837(13) 0.0315(4) Uani 1 1 d . . . H41A H 0.2989 0.5129 0.0578 0.038 Uiso 1 1 calc R . . H41B H 0.2902 0.4015 0.1367 0.038 Uiso 1 1 calc R . . C42 C 0.20230(16) 0.52328(12) 0.20690(12) 0.0261(4) Uani 1 1 d . . . H42A H 0.2822 0.5409 0.2203 0.031 Uiso 1 1 calc R . . H42B H 0.153 0.5898 0.1878 0.031 Uiso 1 1 calc R . . O43 O 0.12322(10) 0.46087(8) 0.29922(8) 0.0231(2) Uani 1 1 d . . . C44 C -0.01444(14) 0.46711(12) 0.30446(12) 0.0208(3) Uani 1 1 d . . . H44A H -0.028 0.503 0.2372 0.025 Uiso 1 1 calc R . . H44B H -0.0648 0.5071 0.3565 0.025 Uiso 1 1 calc R . . C45 C -0.05919(14) 0.35659(11) 0.33337(11) 0.0186(3) Uani 1 1 d . . . H45A H -0.155 0.3583 0.3447 0.022 Uiso 1 1 calc R . . H45B H -0.0171 0.3205 0.2764 0.022 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 0.01300(9) 0.01888(9) 0.01708(10) -0.00428(7) -0.00244(7) -0.00083(6) N1 0.0130(6) 0.0235(7) 0.0263(7) -0.0086(6) -0.0022(5) 0.0002(5) Si1 0.0150(2) 0.0300(2) 0.0300(3) -0.0097(2) -0.00060(18) -0.00484(17) C2 0.0271(9) 0.0337(9) 0.0360(10) -0.0136(8) -0.0031(8) -0.0093(7) C3 0.0216(9) 0.0590(13) 0.0532(13) -0.0129(11) -0.0145(9) -0.0048(8) C4 0.0324(10) 0.0431(11) 0.0429(12) -0.0108(9) 0.0093(9) -0.0126(8) Si2 0.0184(2) 0.0227(2) 0.0286(2) -0.00843(19) -0.00376(18) 0.00185(17) C5 0.0254(9) 0.0376(10) 0.0535(12) -0.0203(9) -0.0074(9) 0.0100(8) C6 0.0396(10) 0.0323(9) 0.0371(10) -0.0163(8) -0.0106(8) 0.0012(8) C7 0.0402(10) 0.0265(9) 0.0407(11) -0.0048(8) -0.0088(9) -0.0012(8) O11 0.0160(5) 0.0238(5) 0.0161(5) -0.0028(4) -0.0031(4) -0.0055(4) C12 0.0163(7) 0.0175(7) 0.0161(7) -0.0051(6) -0.0025(6) -0.0019(5) C13 0.0175(7) 0.0181(7) 0.0189(8) -0.0057(6) -0.0057(6) -0.0010(5) C14 0.0215(7) 0.0210(7) 0.0158(7) -0.0030(6) -0.0063(6) -0.0022(6) C15 0.0187(7) 0.0199(7) 0.0169(7) -0.0050(6) -0.0029(6) -0.0036(6) C16 0.0153(7) 0.0227(7) 0.0193(8) -0.0059(6) -0.0047(6) -0.0015(6) C17 0.0178(7) 0.0193(7) 0.0154(7) -0.0048(6) -0.0051(6) -0.0007(6) C18 0.0162(7) 0.0249(8) 0.0224(8) -0.0022(7) -0.0072(6) -0.0016(6) C19 0.0237(8) 0.0309(9) 0.0287(9) -0.0007(7) -0.0138(7) -0.0002(7) C20 0.0226(8) 0.0300(9) 0.0320(9) -0.0020(7) -0.0144(7) -0.0059(7) C21 0.0205(8) 0.0332(9) 0.0301(9) -0.0054(8) -0.0071(7) 0.0045(7) C22 0.0209(8) 0.0279(8) 0.0193(8) -0.0008(7) -0.0019(6) -0.0069(6) C23 0.0246(9) 0.0507(12) 0.0328(10) 0.0078(9) -0.0071(8) -0.0157(8) C24 0.0401(11) 0.0473(11) 0.0270(10) -0.0091(9) 0.0104(8) -0.0124(9) C25 0.0303(9) 0.0373(10) 0.0349(10) 0.0110(8) -0.0066(8) -0.0129(8) C26 0.0140(7) 0.0229(8) 0.0148(7) -0.0044(6) -0.0026(6) 0.0006(6) N31 0.0170(6) 0.0169(6) 0.0142(6) -0.0031(5) -0.0043(5) -0.0015(5) C32 0.0218(7) 0.0181(7) 0.0216(8) -0.0019(6) -0.0058(6) -0.0043(6) C33 0.0223(8) 0.0222(8) 0.0294(9) -0.0077(7) -0.0058(7) -0.0025(6) O34 0.0274(6) 0.0331(6) 0.0268(6) -0.0141(5) -0.0082(5) -0.0032(5) C35 0.0437(11) 0.0349(10) 0.0330(10) -0.0171(8) -0.0053(8) -0.0119(8) C36 0.0333(10) 0.0509(11) 0.0292(10) -0.0164(9) -0.0098(8) -0.0114(8) O37 0.0296(6) 0.0374(7) 0.0292(7) -0.0060(6) -0.0094(5) -0.0068(5) C38 0.0444(11) 0.0383(10) 0.0212(9) -0.0094(8) -0.0095(8) -0.0008(8) C39 0.0506(12) 0.0366(10) 0.0199(9) -0.0103(8) 0.0016(8) -0.0065(8) O40 0.0359(7) 0.0394(7) 0.0251(6) -0.0146(6) -0.0024(5) -0.0042(5) C41 0.0320(9) 0.0293(9) 0.0273(9) -0.0026(7) -0.0002(8) -0.0062(7) C42 0.0293(9) 0.0224(8) 0.0226(8) 0.0010(7) -0.0029(7) -0.0083(6) O43 0.0210(5) 0.0218(5) 0.0229(6) 0.0031(5) -0.0056(5) -0.0042(4) C44 0.0206(7) 0.0213(8) 0.0188(8) -0.0017(6) -0.0060(6) 0.0019(6) C45 0.0183(7) 0.0226(7) 0.0154(7) -0.0032(6) -0.0060(6) -0.0007(6) #----------------------------------------------------------------------------# # 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 N1 1.9213(12) . ? Zn1 O11 1.9392(10) . ? Zn1 N31 2.1206(12) . ? Zn1 O43 2.2134(10) . ? N1 Si2 1.7095(13) . ? N1 Si1 1.7123(14) . ? Si1 C3 1.872(2) . ? Si1 C2 1.8763(17) . ? Si1 C4 1.8906(19) . ? C2 H2A 0.98 . ? C2 H2B 0.98 . ? C2 H2C 0.98 . ? C3 H3A 0.98 . ? C3 H3B 0.98 . ? C3 H3C 0.98 . ? C4 H4A 0.98 . ? C4 H4B 0.98 . ? C4 H4C 0.98 . ? Si2 C6 1.8758(19) . ? Si2 C7 1.8785(18) . ? Si2 C5 1.8791(17) . ? C5 H5A 0.98 . ? C5 H5B 0.98 . ? C5 H5C 0.98 . ? C6 H6A 0.98 . ? C6 H6B 0.98 . ? C6 H6C 0.98 . ? C7 H7A 0.98 . ? C7 H7B 0.98 . ? C7 H7C 0.98 . ? O11 C12 1.3367(17) . ? C12 C17 1.407(2) . ? C12 C13 1.421(2) . ? C13 C14 1.398(2) . ? C13 C18 1.541(2) . ? C14 C15 1.403(2) . ? C14 H14 0.95 . ? C15 C16 1.387(2) . ? C15 C22 1.539(2) . ? C16 C17 1.393(2) . ? C16 H16 0.95 . ? C17 C26 1.501(2) . ? C18 C19 1.537(2) . ? C18 C20 1.539(2) . ? C18 C21 1.543(2) . ? C19 H19A 0.98 . ? C19 H19B 0.98 . ? C19 H19C 0.98 . ? C20 H20A 0.98 . ? C20 H20B 0.98 . ? C20 H20C 0.98 . ? C21 H21A 0.98 . ? C21 H21B 0.98 . ? C21 H21C 0.98 . ? C22 C23 1.526(2) . ? C22 C25 1.529(2) . ? C22 C24 1.540(2) . ? C23 H23A 0.98 . ? C23 H23B 0.98 . ? C23 H23C 0.98 . ? C24 H24A 0.98 . ? C24 H24B 0.98 . ? C24 H24C 0.98 . ? C25 H25A 0.98 . ? C25 H25B 0.98 . ? C25 H25C 0.98 . ? C26 N31 1.5096(17) . ? C26 H26A 0.99 . ? C26 H26B 0.99 . ? N31 C45 1.4932(18) . ? N31 C32 1.4987(18) . ? C32 C33 1.508(2) . ? C32 H32A 0.99 . ? C32 H32B 0.99 . ? C33 O34 1.4167(19) . ? C33 H33A 0.99 . ? C33 H33B 0.99 . ? O34 C35 1.426(2) . ? C35 C36 1.494(3) . ? C35 H35A 0.99 . ? C35 H35B 0.99 . ? C36 O37 1.413(2) . ? C36 H36A 0.99 . ? C36 H36B 0.99 . ? O37 C38 1.417(2) . ? C38 C39 1.497(3) . ? C38 H38A 0.99 . ? C38 H38B 0.99 . ? C39 O40 1.428(2) . ? C39 H39A 0.99 . ? C39 H39B 0.99 . ? O40 C41 1.416(2) . ? C41 C42 1.507(2) . ? C41 H41A 0.99 . ? C41 H41B 0.99 . ? C42 O43 1.4386(18) . ? C42 H42A 0.99 . ? C42 H42B 0.99 . ? O43 C44 1.4479(18) . ? C44 C45 1.507(2) . ? C44 H44A 0.99 . ? C44 H44B 0.99 . ? C45 H45A 0.99 . ? C45 H45B 0.99 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Zn1 O11 114.52(5) . . ? N1 Zn1 N31 142.96(5) . . ? O11 Zn1 N31 94.96(4) . . ? N1 Zn1 O43 103.70(5) . . ? O11 Zn1 O43 117.74(4) . . ? N31 Zn1 O43 79.52(4) . . ? Si2 N1 Si1 125.71(7) . . ? Si2 N1 Zn1 119.17(7) . . ? Si1 N1 Zn1 114.47(7) . . ? N1 Si1 C3 114.13(8) . . ? N1 Si1 C2 111.28(7) . . ? C3 Si1 C2 104.96(9) . . ? N1 Si1 C4 112.28(8) . . ? C3 Si1 C4 106.82(9) . . ? C2 Si1 C4 106.81(8) . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si1 C3 H3A 109.5 . . ? Si1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si1 C4 H4A 109.5 . . ? Si1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Si1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N1 Si2 C6 111.35(7) . . ? N1 Si2 C7 111.39(8) . . ? C6 Si2 C7 109.32(9) . . ? N1 Si2 C5 114.07(8) . . ? C6 Si2 C5 104.79(9) . . ? C7 Si2 C5 105.53(9) . . ? Si2 C5 H5A 109.5 . . ? Si2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si2 C6 H6A 109.5 . . ? Si2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si2 C7 H7A 109.5 . . ? Si2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C12 O11 Zn1 121.73(9) . . ? O11 C12 C17 119.46(13) . . ? O11 C12 C13 122.20(13) . . ? C17 C12 C13 118.33(13) . . ? C14 C13 C12 117.67(13) . . ? C14 C13 C18 121.75(13) . . ? C12 C13 C18 120.51(13) . . ? C13 C14 C15 124.54(14) . . ? C13 C14 H14 117.7 . . ? C15 C14 H14 117.7 . . ? C16 C15 C14 116.23(13) . . ? C16 C15 C22 122.32(14) . . ? C14 C15 C22 121.39(13) . . ? C15 C16 C17 121.60(14) . . ? C15 C16 H16 119.2 . . ? C17 C16 H16 119.2 . . ? C16 C17 C12 121.52(13) . . ? C16 C17 C26 120.38(13) . . ? C12 C17 C26 118.10(13) . . ? C19 C18 C20 107.59(13) . . ? C19 C18 C13 112.76(13) . . ? C20 C18 C13 110.89(12) . . ? C19 C18 C21 107.03(13) . . ? C20 C18 C21 109.63(13) . . ? C13 C18 C21 108.83(13) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 C25 108.00(14) . . ? C23 C22 C15 112.02(13) . . ? C25 C22 C15 111.47(13) . . ? C23 C22 C24 108.24(15) . . ? C25 C22 C24 108.30(15) . . ? C15 C22 C24 108.69(13) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C17 C26 N31 113.20(11) . . ? C17 C26 H26A 108.9 . . ? N31 C26 H26A 108.9 . . ? C17 C26 H26B 108.9 . . ? N31 C26 H26B 108.9 . . ? H26A C26 H26B 107.8 . . ? C45 N31 C32 111.17(11) . . ? C45 N31 C26 108.55(11) . . ? C32 N31 C26 107.17(11) . . ? C45 N31 Zn1 107.43(9) . . ? C32 N31 Zn1 118.17(9) . . ? C26 N31 Zn1 103.81(8) . . ? N31 C32 C33 115.80(12) . . ? N31 C32 H32A 108.3 . . ? C33 C32 H32A 108.3 . . ? N31 C32 H32B 108.3 . . ? C33 C32 H32B 108.3 . . ? H32A C32 H32B 107.4 . . ? O34 C33 C32 108.86(12) . . ? O34 C33 H33A 109.9 . . ? C32 C33 H33A 109.9 . . ? O34 C33 H33B 109.9 . . ? C32 C33 H33B 109.9 . . ? H33A C33 H33B 108.3 . . ? C33 O34 C35 113.92(12) . . ? O34 C35 C36 110.13(14) . . ? O34 C35 H35A 109.6 . . ? C36 C35 H35A 109.6 . . ? O34 C35 H35B 109.6 . . ? C36 C35 H35B 109.6 . . ? H35A C35 H35B 108.1 . . ? O37 C36 C35 109.35(15) . . ? O37 C36 H36A 109.8 . . ? C35 C36 H36A 109.8 . . ? O37 C36 H36B 109.8 . . ? C35 C36 H36B 109.8 . . ? H36A C36 H36B 108.3 . . ? C36 O37 C38 112.65(14) . . ? O37 C38 C39 108.08(15) . . ? O37 C38 H38A 110.1 . . ? C39 C38 H38A 110.1 . . ? O37 C38 H38B 110.1 . . ? C39 C38 H38B 110.1 . . ? H38A C38 H38B 108.4 . . ? O40 C39 C38 108.18(14) . . ? O40 C39 H39A 110.1 . . ? C38 C39 H39A 110.1 . . ? O40 C39 H39B 110.1 . . ? C38 C39 H39B 110.1 . . ? H39A C39 H39B 108.4 . . ? C41 O40 C39 114.57(13) . . ? O40 C41 C42 109.30(13) . . ? O40 C41 H41A 109.8 . . ? C42 C41 H41A 109.8 . . ? O40 C41 H41B 109.8 . . ? C42 C41 H41B 109.8 . . ? H41A C41 H41B 108.3 . . ? O43 C42 C41 112.80(13) . . ? O43 C42 H42A 109 . . ? C41 C42 H42A 109 . . ? O43 C42 H42B 109 . . ? C41 C42 H42B 109 . . ? H42A C42 H42B 107.8 . . ? C42 O43 C44 113.80(11) . . ? C42 O43 Zn1 132.02(9) . . ? C44 O43 Zn1 111.32(8) . . ? O43 C44 C45 107.44(11) . . ? O43 C44 H44A 110.2 . . ? C45 C44 H44A 110.2 . . ? O43 C44 H44B 110.2 . . ? C45 C44 H44B 110.2 . . ? H44A C44 H44B 108.5 . . ? N31 C45 C44 111.12(12) . . ? N31 C45 H45A 109.4 . . ? C44 C45 H45A 109.4 . . ? N31 C45 H45B 109.4 . . ? C44 C45 H45B 109.4 . . ? H45A C45 H45B 108 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O11 Zn1 N1 Si2 117.52(8) . . . . ? N31 Zn1 N1 Si2 -22.15(14) . . . . ? O43 Zn1 N1 Si2 -112.86(8) . . . . ? O11 Zn1 N1 Si1 -53.74(9) . . . . ? N31 Zn1 N1 Si1 166.59(6) . . . . ? O43 Zn1 N1 Si1 75.89(8) . . . . ? Si2 N1 Si1 C3 -57.51(13) . . . . ? Zn1 N1 Si1 C3 113.08(9) . . . . ? Si2 N1 Si1 C2 -176.07(10) . . . . ? Zn1 N1 Si1 C2 -5.48(11) . . . . ? Si2 N1 Si1 C4 64.25(12) . . . . ? Zn1 N1 Si1 C4 -125.16(9) . . . . ? Si1 N1 Si2 C6 -113.40(11) . . . . ? Zn1 N1 Si2 C6 76.42(10) . . . . ? Si1 N1 Si2 C7 124.28(11) . . . . ? Zn1 N1 Si2 C7 -45.90(11) . . . . ? Si1 N1 Si2 C5 4.95(13) . . . . ? Zn1 N1 Si2 C5 -165.24(9) . . . . ? N1 Zn1 O11 C12 -126.88(10) . . . . ? N31 Zn1 O11 C12 30.08(10) . . . . ? O43 Zn1 O11 C12 110.84(10) . . . . ? Zn1 O11 C12 C17 -47.57(16) . . . . ? Zn1 O11 C12 C13 133.12(12) . . . . ? O11 C12 C13 C14 175.69(13) . . . . ? C17 C12 C13 C14 -3.6(2) . . . . ? O11 C12 C13 C18 -7.4(2) . . . . ? C17 C12 C13 C18 173.32(13) . . . . ? C12 C13 C14 C15 2.0(2) . . . . ? C18 C13 C14 C15 -174.93(14) . . . . ? C13 C14 C15 C16 1.0(2) . . . . ? C13 C14 C15 C22 -176.23(14) . . . . ? C14 C15 C16 C17 -2.3(2) . . . . ? C22 C15 C16 C17 174.89(13) . . . . ? C15 C16 C17 C12 0.6(2) . . . . ? C15 C16 C17 C26 -178.32(13) . . . . ? O11 C12 C17 C16 -176.86(13) . . . . ? C13 C12 C17 C16 2.5(2) . . . . ? O11 C12 C17 C26 2.1(2) . . . . ? C13 C12 C17 C26 -178.57(13) . . . . ? C14 C13 C18 C19 1.6(2) . . . . ? C12 C13 C18 C19 -175.26(14) . . . . ? C14 C13 C18 C20 -119.16(15) . . . . ? C12 C13 C18 C20 64.01(18) . . . . ? C14 C13 C18 C21 120.17(15) . . . . ? C12 C13 C18 C21 -56.66(18) . . . . ? C16 C15 C22 C23 17.7(2) . . . . ? C14 C15 C22 C23 -165.22(14) . . . . ? C16 C15 C22 C25 138.87(16) . . . . ? C14 C15 C22 C25 -44.1(2) . . . . ? C16 C15 C22 C24 -101.84(18) . . . . ? C14 C15 C22 C24 75.22(18) . . . . ? C16 C17 C26 N31 -116.70(14) . . . . ? C12 C17 C26 N31 64.34(17) . . . . ? C17 C26 N31 C45 178.19(12) . . . . ? C17 C26 N31 C32 58.04(15) . . . . ? C17 C26 N31 Zn1 -67.74(13) . . . . ? N1 Zn1 N31 C45 -77.70(12) . . . . ? O11 Zn1 N31 C45 138.53(9) . . . . ? O43 Zn1 N31 C45 21.21(8) . . . . ? N1 Zn1 N31 C32 48.98(14) . . . . ? O11 Zn1 N31 C32 -94.79(10) . . . . ? O43 Zn1 N31 C32 147.89(10) . . . . ? N1 Zn1 N31 C26 167.44(9) . . . . ? O11 Zn1 N31 C26 23.67(9) . . . . ? O43 Zn1 N31 C26 -93.66(8) . . . . ? C45 N31 C32 C33 50.68(16) . . . . ? C26 N31 C32 C33 169.14(12) . . . . ? Zn1 N31 C32 C33 -74.19(14) . . . . ? N31 C32 C33 O34 -85.70(15) . . . . ? C32 C33 O34 C35 176.87(13) . . . . ? C33 O34 C35 C36 -123.28(16) . . . . ? O34 C35 C36 O37 69.50(19) . . . . ? C35 C36 O37 C38 -170.34(14) . . . . ? C36 O37 C38 C39 179.92(13) . . . . ? O37 C38 C39 O40 -74.76(18) . . . . ? C38 C39 O40 C41 152.60(15) . . . . ? C39 O40 C41 C42 -179.79(14) . . . . ? O40 C41 C42 O43 62.18(18) . . . . ? C41 C42 O43 C44 -83.55(16) . . . . ? C41 C42 O43 Zn1 75.27(17) . . . . ? N1 Zn1 O43 C42 -10.52(14) . . . . ? O11 Zn1 O43 C42 117.13(13) . . . . ? N31 Zn1 O43 C42 -152.74(13) . . . . ? N1 Zn1 O43 C44 148.69(9) . . . . ? O11 Zn1 O43 C44 -83.66(10) . . . . ? N31 Zn1 O43 C44 6.46(9) . . . . ? C42 O43 C44 C45 130.89(13) . . . . ? Zn1 O43 C44 C45 -32.35(13) . . . . ? C32 N31 C45 C44 -177.72(11) . . . . ? C26 N31 C45 C44 64.65(14) . . . . ? Zn1 N31 C45 C44 -47.02(13) . . . . ? O43 C44 C45 N31 53.25(15) . . . . ? # Attachment 'YS23_100K_APEX_05dec08_archive.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2008-12-05 at 18:38:12 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.4 # Request file : f:\progs\wingx\files\archive.dat # CIF files read : job struct data_job4 _database_code_depnum_ccdc_archive 'CCDC 780419' #TrackingRef 'YS23_100K_APEX_05dec08_archive.cif' _audit_creation_date 2008-12-05T18:38:12-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C19 H31 N1 O2' _chemical_formula_sum 'C19 H31 N O2' _chemical_formula_weight 305.45 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P c a b' _symmetry_space_group_name_Hall '-P 2bc 2ac' _symmetry_Int_Tables_number 61 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z+1/2' 'x+1/2, -y, -z+1/2' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, y-1/2, -z-1/2' '-x-1/2, y, z-1/2' 'x-1/2, -y-1/2, z' _cell_length_a 8.8637(19) _cell_length_b 10.150(2) _cell_length_c 40.261(9) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3622.1(13) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2708 _cell_measurement_theta_min 3.04 _cell_measurement_theta_max 27.45 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.12 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1344 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.071 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_absorpt_correction_T_min 0.960 _exptl_absorpt_correction_T_max 0.989 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_measurement_device_type 'APEXII, Bruker-AXS' _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_detector 'CCD plate' _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0815 _diffrn_reflns_av_unetI/netI 0.0751 _diffrn_reflns_number 16205 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 52 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _reflns_number_total 4140 _reflns_number_gt 2996 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SAINT' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _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^)+(0.0386P)^2^+2.3214P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 4140 _refine_ls_number_parameters 178 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.098 _refine_ls_R_factor_gt 0.0682 _refine_ls_wR_factor_ref 0.1481 _refine_ls_wR_factor_gt 0.1359 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.083 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.259 _refine_diff_density_min -0.203 _refine_diff_density_rms 0.05 #----------------------------------------------------------------------------# # 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' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6065(2) -0.0021(2) 0.69004(5) 0.0225(4) Uani 1 1 d . . . H1A H 0.6222 -0.0447 0.6682 0.027 Uiso 1 1 calc R . . H1B H 0.5144 0.0527 0.6887 0.027 Uiso 1 1 calc R . . C2 C 0.5866(3) -0.1061(2) 0.71638(5) 0.0268(5) Uani 1 1 d . . . H2A H 0.4981 -0.1614 0.7108 0.032 Uiso 1 1 calc R . . H2B H 0.6767 -0.1638 0.7168 0.032 Uiso 1 1 calc R . . O3 O 0.56564(16) -0.04960(15) 0.74826(4) 0.0275(4) Uani 1 1 d . . . C4 C 0.6914(2) 0.0325(2) 0.75632(5) 0.0264(5) Uani 1 1 d . . . H4A H 0.7839 -0.0219 0.7575 0.032 Uiso 1 1 calc R . . H4B H 0.6752 0.0727 0.7784 0.032 Uiso 1 1 calc R . . C5 C 0.7128(2) 0.1402(2) 0.73082(5) 0.0241(5) Uani 1 1 d . . . H5A H 0.6225 0.1976 0.7303 0.029 Uiso 1 1 calc R . . H5B H 0.801 0.1949 0.7368 0.029 Uiso 1 1 calc R . . N6 N 0.73634(19) 0.08093(17) 0.69803(4) 0.0207(4) Uani 1 1 d . . . C7 C 0.7592(2) 0.1809(2) 0.67200(5) 0.0231(4) Uani 1 1 d . . . H7A H 0.8323 0.2478 0.6799 0.028 Uiso 1 1 calc R . . H7B H 0.6625 0.226 0.6673 0.028 Uiso 1 1 calc R . . C8 C 0.8177(2) 0.11790(19) 0.64064(5) 0.0209(4) Uani 1 1 d . . . C9 C 0.9477(2) 0.04013(19) 0.64230(5) 0.0205(4) Uani 1 1 d . . . O10 O 1.01296(17) 0.01736(15) 0.67271(4) 0.0252(3) Uani 1 1 d . . . H10 H 0.941(3) 0.029(3) 0.6873(7) 0.05 Uiso 1 1 d . . . C11 C 1.0127(2) -0.01336(18) 0.61357(5) 0.019 Uani 1 1 d . . . C12 C 1.1607(2) -0.0913(2) 0.61453(5) 0.02 Uani 1 1 d . . . C13 C 1.2857(2) -0.0058(2) 0.62975(5) 0.025 Uani 1 1 d . . . H13A H 1.2969 0.0752 0.6167 0.038 Uiso 1 1 calc R . . H13B H 1.381 -0.0547 0.6296 0.038 Uiso 1 1 calc R . . H13C H 1.259 0.0168 0.6527 0.038 Uiso 1 1 calc R . . C14 C 1.1413(3) -0.2174(2) 0.63542(6) 0.0297(5) Uani 1 1 d . . . H14A H 1.1115 -0.1936 0.6581 0.044 Uiso 1 1 calc R . . H14B H 1.237 -0.2658 0.636 0.044 Uiso 1 1 calc R . . H14C H 1.0632 -0.2731 0.6254 0.044 Uiso 1 1 calc R . . C15 C 1.2126(2) -0.1335(2) 0.57992(5) 0.0259(5) Uani 1 1 d . . . H15A H 1.1349 -0.1889 0.5697 0.039 Uiso 1 1 calc R . . H15B H 1.3068 -0.1835 0.5817 0.039 Uiso 1 1 calc R . . H15C H 1.2292 -0.0552 0.5662 0.039 Uiso 1 1 calc R . . C16 C 0.9357(2) 0.00918(19) 0.58380(5) 0.0203(4) Uani 1 1 d . . . H16 H 0.9773 -0.0265 0.564 0.024 Uiso 1 1 calc R . . C17 C 0.8023(2) 0.0805(2) 0.58132(5) 0.0201(4) Uani 1 1 d . . . C18 C 0.7459(2) 0.1353(2) 0.61046(5) 0.0206(4) Uani 1 1 d . . . H18 H 0.6558 0.1859 0.6096 0.025 Uiso 1 1 calc R . . C19 C 0.7166(2) 0.0965(2) 0.54849(5) 0.021 Uani 1 1 d . . . C20 C 0.5635(3) 0.0282(2) 0.55178(6) 0.034 Uani 1 1 d . . . H20A H 0.579 -0.0653 0.5568 0.051 Uiso 1 1 calc R . . H20B H 0.5078 0.0365 0.5309 0.051 Uiso 1 1 calc R . . H20C H 0.5058 0.0694 0.5697 0.051 Uiso 1 1 calc R . . C21 C 0.8003(3) 0.0350(3) 0.51920(5) 0.0367(6) Uani 1 1 d . . . H21A H 0.8998 0.0762 0.517 0.055 Uiso 1 1 calc R . . H21B H 0.7424 0.0491 0.4988 0.055 Uiso 1 1 calc R . . H21C H 0.8126 -0.0597 0.523 0.055 Uiso 1 1 calc R . . C22 C 0.6911(3) 0.2423(2) 0.54099(6) 0.0350(6) Uani 1 1 d . . . H22A H 0.6357 0.283 0.5594 0.053 Uiso 1 1 calc R . . H22B H 0.6325 0.251 0.5205 0.053 Uiso 1 1 calc R . . H22C H 0.7887 0.2863 0.5383 0.053 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 C1 0.0212(10) 0.0212(11) 0.0250(11) -0.0034(9) -0.0012(8) 0.0016(8) C2 0.0304(12) 0.0261(12) 0.0238(11) 0.0005(9) 0.0010(9) -0.0043(9) O3 0.0262(8) 0.0311(9) 0.0251(8) 0.0005(7) 0.0037(6) -0.0042(6) C4 0.0281(12) 0.0306(12) 0.0206(11) -0.0011(9) 0.0003(9) -0.0039(9) C5 0.0258(11) 0.0249(12) 0.0216(11) -0.0040(9) 0.0010(8) -0.0011(8) N6 0.0257(9) 0.0207(9) 0.0157(8) -0.0014(7) 0.0003(7) -0.0006(7) C7 0.0271(11) 0.0207(11) 0.0214(11) -0.0006(8) 0.0011(9) 0.0005(8) C8 0.0243(11) 0.0163(10) 0.0219(11) -0.0003(8) 0.0026(8) -0.0019(8) C9 0.0236(11) 0.0181(10) 0.0199(10) 0.0026(8) -0.0010(8) -0.0024(8) O10 0.0244(8) 0.0320(9) 0.0193(8) 0.0012(6) -0.0001(6) 0.0037(6) C11 0.018 0.013 0.024 0.002 0.001 -0.003 C12 0.02 0.017 0.023 0 0.001 0 C13 0.023 0.026 0.026 -0.002 -0.003 -0.001 C14 0.0305(12) 0.0221(12) 0.0364(13) 0.0072(10) 0.0003(10) 0.0022(9) C15 0.0225(11) 0.0243(12) 0.0309(12) -0.0026(9) 0.0008(9) 0.0044(8) C16 0.0226(10) 0.0173(10) 0.0211(11) -0.0006(8) 0.0025(8) -0.0021(8) C17 0.0210(10) 0.0167(10) 0.0226(11) 0.0013(8) -0.0008(8) -0.0027(8) C18 0.0215(10) 0.0168(10) 0.0235(11) 0.0026(8) 0.0009(8) 0.0016(8) C19 0.022 0.022 0.02 0 -0.001 0.001 C20 0.031 0.041 0.03 0.006 -0.004 -0.006 C21 0.0328(14) 0.0564(17) 0.0210(12) -0.0069(11) -0.0039(9) 0.0094(11) C22 0.0457(15) 0.0296(13) 0.0298(12) 0.0071(10) -0.0077(11) 0.0011(10) #----------------------------------------------------------------------------# # 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 N6 1.462(3) . ? C1 C2 1.507(3) . ? C1 H1A 0.99 . ? C1 H1B 0.99 . ? C2 O3 1.418(3) . ? C2 H2A 0.99 . ? C2 H2B 0.99 . ? O3 C4 1.429(2) . ? C4 C5 1.511(3) . ? C4 H4A 0.99 . ? C4 H4B 0.99 . ? C5 N6 1.465(3) . ? C5 H5A 0.99 . ? C5 H5B 0.99 . ? N6 C7 1.473(3) . ? C7 C8 1.508(3) . ? C7 H7A 0.99 . ? C7 H7B 0.99 . ? C8 C18 1.383(3) . ? C8 C9 1.398(3) . ? C9 O10 1.374(2) . ? C9 C11 1.402(3) . ? O10 H10 0.88(3) . ? C11 C16 1.398(3) . ? C11 C12 1.533(3) . ? C12 C15 1.529(3) . ? C12 C13 1.535(3) . ? C12 C14 1.541(3) . ? C13 H13A 0.98 . ? C13 H13B 0.98 . ? C13 H13C 0.98 . ? C14 H14A 0.98 . ? C14 H14B 0.98 . ? C14 H14C 0.98 . ? C15 H15A 0.98 . ? C15 H15B 0.98 . ? C15 H15C 0.98 . ? C16 C17 1.390(3) . ? C16 H16 0.95 . ? C17 C18 1.391(3) . ? C17 C19 1.533(3) . ? C18 H18 0.95 . ? C19 C22 1.526(3) . ? C19 C21 1.527(3) . ? C19 C20 1.529(3) . ? C20 H20A 0.98 . ? C20 H20B 0.98 . ? C20 H20C 0.98 . ? C21 H21A 0.98 . ? C21 H21B 0.98 . ? C21 H21C 0.98 . ? C22 H22A 0.98 . ? C22 H22B 0.98 . ? C22 H22C 0.98 . ? 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 N6 C1 C2 109.96(17) . . ? N6 C1 H1A 109.7 . . ? C2 C1 H1A 109.7 . . ? N6 C1 H1B 109.7 . . ? C2 C1 H1B 109.7 . . ? H1A C1 H1B 108.2 . . ? O3 C2 C1 111.64(18) . . ? O3 C2 H2A 109.3 . . ? C1 C2 H2A 109.3 . . ? O3 C2 H2B 109.3 . . ? C1 C2 H2B 109.3 . . ? H2A C2 H2B 108 . . ? C2 O3 C4 109.84(15) . . ? O3 C4 C5 111.40(17) . . ? O3 C4 H4A 109.3 . . ? C5 C4 H4A 109.3 . . ? O3 C4 H4B 109.3 . . ? C5 C4 H4B 109.3 . . ? H4A C4 H4B 108 . . ? N6 C5 C4 109.46(17) . . ? N6 C5 H5A 109.8 . . ? C4 C5 H5A 109.8 . . ? N6 C5 H5B 109.8 . . ? C4 C5 H5B 109.8 . . ? H5A C5 H5B 108.2 . . ? C1 N6 C5 108.82(16) . . ? C1 N6 C7 110.43(16) . . ? C5 N6 C7 112.20(16) . . ? N6 C7 C8 110.55(16) . . ? N6 C7 H7A 109.5 . . ? C8 C7 H7A 109.5 . . ? N6 C7 H7B 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 108.1 . . ? C18 C8 C9 119.58(18) . . ? C18 C8 C7 121.55(18) . . ? C9 C8 C7 118.87(18) . . ? O10 C9 C8 119.00(18) . . ? O10 C9 C11 119.81(18) . . ? C8 C9 C11 121.18(18) . . ? C9 O10 H10 105.7(18) . . ? C16 C11 C9 116.35(18) . . ? C16 C11 C12 121.58(17) . . ? C9 C11 C12 122.07(17) . . ? C15 C12 C11 112.27(16) . . ? C15 C12 C13 107.78(17) . . ? C11 C12 C13 109.64(16) . . ? C15 C12 C14 107.35(17) . . ? C11 C12 C14 110.31(16) . . ? C13 C12 C14 109.41(17) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C11 124.17(18) . . ? C17 C16 H16 117.9 . . ? C11 C16 H16 117.9 . . ? C16 C17 C18 116.97(18) . . ? C16 C17 C19 122.61(18) . . ? C18 C17 C19 120.40(18) . . ? C8 C18 C17 121.60(19) . . ? C8 C18 H18 119.2 . . ? C17 C18 H18 119.2 . . ? C22 C19 C21 108.38(18) . . ? C22 C19 C20 109.01(18) . . ? C21 C19 C20 108.22(18) . . ? C22 C19 C17 110.28(17) . . ? C21 C19 C17 112.41(17) . . ? C20 C19 C17 108.48(17) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N6 C1 C2 O3 58.6(2) . . . . ? C1 C2 O3 C4 -57.8(2) . . . . ? C2 O3 C4 C5 58.1(2) . . . . ? O3 C4 C5 N6 -58.8(2) . . . . ? C2 C1 N6 C5 -57.9(2) . . . . ? C2 C1 N6 C7 178.57(17) . . . . ? C4 C5 N6 C1 58.0(2) . . . . ? C4 C5 N6 C7 -179.52(17) . . . . ? C1 N6 C7 C8 -71.3(2) . . . . ? C5 N6 C7 C8 167.09(16) . . . . ? N6 C7 C8 C18 125.7(2) . . . . ? N6 C7 C8 C9 -54.2(2) . . . . ? C18 C8 C9 O10 -176.24(18) . . . . ? C7 C8 C9 O10 3.7(3) . . . . ? C18 C8 C9 C11 4.4(3) . . . . ? C7 C8 C9 C11 -175.61(18) . . . . ? O10 C9 C11 C16 177.15(17) . . . . ? C8 C9 C11 C16 -3.5(3) . . . . ? O10 C9 C11 C12 -3.4(3) . . . . ? C8 C9 C11 C12 175.92(18) . . . . ? C16 C11 C12 C15 2.3(3) . . . . ? C9 C11 C12 C15 -177.15(18) . . . . ? C16 C11 C12 C13 122.0(2) . . . . ? C9 C11 C12 C13 -57.4(2) . . . . ? C16 C11 C12 C14 -117.4(2) . . . . ? C9 C11 C12 C14 63.2(2) . . . . ? C9 C11 C16 C17 0.3(3) . . . . ? C12 C11 C16 C17 -179.11(18) . . . . ? C11 C16 C17 C18 1.9(3) . . . . ? C11 C16 C17 C19 -176.47(18) . . . . ? C9 C8 C18 C17 -2.1(3) . . . . ? C7 C8 C18 C17 177.99(18) . . . . ? C16 C17 C18 C8 -1.0(3) . . . . ? C19 C17 C18 C8 177.38(18) . . . . ? C16 C17 C19 C22 -125.4(2) . . . . ? C18 C17 C19 C22 56.3(3) . . . . ? C16 C17 C19 C21 -4.4(3) . . . . ? C18 C17 C19 C21 177.34(19) . . . . ? C16 C17 C19 C20 115.3(2) . . . . ? C18 C17 C19 C20 -63.0(2) . . . . ? # Attachment 'YS94_100K_APEX_07mai09_archive.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2009-05-07 at 11:45:42 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : d:\progs\wingx\files\archive.dat # CIF files read : job struct data_job5 _database_code_depnum_ccdc_archive 'CCDC 780420' #TrackingRef 'YS94_100K_APEX_07mai09_archive.cif' _audit_creation_date 2009-05-07T11:45:42-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety '2(C21 H35 N O2)' _chemical_formula_sum 'C42 H70 N2 O4' _chemical_formula_weight 667 _chemical_compound_source 'synthesis as described' _chemical_absolute_configuration unk #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'P 32' _symmetry_space_group_name_Hall 'P 32' _symmetry_Int_Tables_number 145 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z-1/3' '-x+y, -x, z-2/3' _cell_length_a 10.7292(3) _cell_length_b 10.7292 _cell_length_c 29.5051(9) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 2941.45(12) _cell_formula_units_Z 3 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9912 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 27.12 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.58 _exptl_crystal_size_mid 0.52 _exptl_crystal_size_min 0.47 _exptl_crystal_density_diffrn 1.13 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1104 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.071 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_absorpt_correction_T_min 0.939 _exptl_absorpt_correction_T_max 0.967 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_measurement_device_type 'APEXII, Bruker-AXS' _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_detector 'CCD plate' _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0585 _diffrn_reflns_av_unetI/netI 0.0342 _diffrn_reflns_number 37354 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 4476 _reflns_number_gt 4105 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SAINT' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _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^)+(0.0482P)^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_number_reflns 4476 _refine_ls_number_parameters 449 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0412 _refine_ls_R_factor_gt 0.0367 _refine_ls_wR_factor_ref 0.0903 _refine_ls_wR_factor_gt 0.0879 _refine_ls_goodness_of_fit_ref 1.198 _refine_ls_restrained_S_all 1.198 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.001 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -10(10) _refine_diff_density_max 0.193 _refine_diff_density_min -0.2 _refine_diff_density_rms 0.041 #----------------------------------------------------------------------------# # 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 '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 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0 '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 O1 O 0.98909(15) 1.57555(15) -0.04171(5) 0.0192(3) Uani 1 1 d . . . H1 H 0.8993 1.5362 -0.0391 0.029 Uiso 1 1 calc R . . C2 C 1.0435(2) 1.5326(2) -0.00640(6) 0.0156(4) Uani 1 1 d . . . C3 C 1.1813(2) 1.5486(2) -0.00978(6) 0.0146(4) Uani 1 1 d . . . C4 C 1.2745(2) 1.6139(2) -0.05233(6) 0.0177(4) Uani 1 1 d . . . C5 C 1.4226(2) 1.6252(3) -0.04777(7) 0.0241(5) Uani 1 1 d . . . H5A H 1.4791 1.6688 -0.0753 0.036 Uiso 1 1 calc R . . H5B H 1.4099 1.5289 -0.0436 0.036 Uiso 1 1 calc R . . H5C H 1.4733 1.6852 -0.0215 0.036 Uiso 1 1 calc R . . C6 C 1.3012(2) 1.7669(2) -0.06085(8) 0.0248(5) Uani 1 1 d . . . H6A H 1.2087 1.7636 -0.0642 0.037 Uiso 1 1 calc R . . H6B H 1.3579 1.8056 -0.0886 0.037 Uiso 1 1 calc R . . H6C H 1.3538 1.8288 -0.0351 0.037 Uiso 1 1 calc R . . C7 C 1.1991(2) 1.5173(2) -0.09361(7) 0.0231(4) Uani 1 1 d . . . H7A H 1.259 1.5588 -0.1206 0.035 Uiso 1 1 calc R . . H7B H 1.1056 1.5109 -0.0983 0.035 Uiso 1 1 calc R . . H7C H 1.1847 1.4209 -0.0882 0.035 Uiso 1 1 calc R . . C8 C 1.2281(2) 1.5008(2) 0.02736(6) 0.0154(4) Uani 1 1 d . . . H8 H 1.3211 1.5108 0.0259 0.018 Uiso 1 1 calc R . . C9 C 1.1460(2) 1.4398(2) 0.06612(6) 0.0159(4) Uani 1 1 d . . . C10 C 1.2005(2) 1.3918(2) 0.10692(6) 0.0162(4) Uani 1 1 d . . . C11 C 1.0893(2) 1.2365(2) 0.12069(7) 0.0216(4) Uani 1 1 d . . . H11A H 1.1244 1.2086 0.1473 0.032 Uiso 1 1 calc R . . H11B H 1.0751 1.1711 0.0955 0.032 Uiso 1 1 calc R . . H11C H 0.9976 1.2312 0.128 0.032 Uiso 1 1 calc R . . C12 C 1.3436(2) 1.3979(2) 0.09726(7) 0.0218(4) Uani 1 1 d . . . H12A H 1.4177 1.4973 0.0907 0.033 Uiso 1 1 calc R . . H12B H 1.3325 1.3369 0.0711 0.033 Uiso 1 1 calc R . . H12C H 1.3723 1.3632 0.1238 0.033 Uiso 1 1 calc R . . C13 C 1.2222(2) 1.4935(2) 0.14677(7) 0.0202(4) Uani 1 1 d . . . H13A H 1.295 1.5921 0.1386 0.03 Uiso 1 1 calc R . . H13B H 1.2543 1.4632 0.1735 0.03 Uiso 1 1 calc R . . H13C H 1.131 1.49 0.1535 0.03 Uiso 1 1 calc R . . C14 C 1.0103(2) 1.4274(2) 0.06802(6) 0.0165(4) Uani 1 1 d . . . H14 H 0.9521 1.3868 0.0942 0.02 Uiso 1 1 calc R . . C15 C 0.9587(2) 1.4735(2) 0.03233(6) 0.0163(4) Uani 1 1 d . . . C16 C 0.8151(2) 1.4669(2) 0.03655(6) 0.0179(4) Uani 1 1 d . . . H16A H 0.763 1.4068 0.0631 0.022 Uiso 1 1 calc R . . H16B H 0.8318 1.5651 0.0421 0.022 Uiso 1 1 calc R . . N17 N 0.72440(18) 1.40701(18) -0.00427(5) 0.0166(3) Uani 1 1 d . . . C18 C 0.5973(2) 1.4267(2) -0.00209(7) 0.0210(4) Uani 1 1 d . . . H18A H 0.6191 1.5198 -0.0158 0.025 Uiso 1 1 calc R . . H18B H 0.5663 1.4239 0.0297 0.025 Uiso 1 1 calc R . . C19 C 0.4820(2) 1.3017(2) -0.02902(7) 0.0230(4) Uani 1 1 d . . . H19A H 0.4952 1.3207 -0.062 0.028 Uiso 1 1 calc R . . H19B H 0.3845 1.2812 -0.0203 0.028 Uiso 1 1 calc R . . C20 C 0.5070(2) 1.1784(2) -0.01562(7) 0.0230(4) Uani 1 1 d . . . H20A H 0.4696 1.1023 -0.0391 0.028 Uiso 1 1 calc R . . H20B H 0.4598 1.1354 0.0136 0.028 Uiso 1 1 calc R . . C21 C 0.6715(2) 1.2505(2) -0.01160(7) 0.0185(4) Uani 1 1 d . . . H21 H 0.6972 1.2103 0.0151 0.022 Uiso 1 1 calc R . . C22 C 0.7393(2) 1.2311(2) -0.05431(7) 0.0199(4) Uani 1 1 d . . . H22A H 0.7089 1.2647 -0.0811 0.024 Uiso 1 1 calc R . . H22B H 0.8456 1.2877 -0.0521 0.024 Uiso 1 1 calc R . . O23 O 0.69276(16) 1.08203(15) -0.05855(5) 0.0231(3) Uani 1 1 d . . . C24 C 0.7371(3) 1.0510(3) -0.10026(7) 0.0297(5) Uani 1 1 d . . . H24A H 0.8423 1.106 -0.1023 0.045 Uiso 1 1 calc R . . H24B H 0.6954 1.0777 -0.1254 0.045 Uiso 1 1 calc R . . H24C H 0.7042 0.9479 -0.1019 0.045 Uiso 1 1 calc R . . O51 O 0.58337(15) 0.76285(16) 0.15036(5) 0.0195(3) Uani 1 1 d . . . H51 H 0.5383 0.8081 0.1494 0.029 Uiso 1 1 calc R . . C52 C 0.6802(2) 0.8063(2) 0.11509(6) 0.0161(4) Uani 1 1 d . . . C53 C 0.8014(2) 0.7891(2) 0.11811(6) 0.0148(4) Uani 1 1 d . . . C54 C 0.8278(2) 0.7205(2) 0.16012(6) 0.0178(4) Uani 1 1 d . . . C55 C 0.6996(2) 0.5681(2) 0.16772(8) 0.0242(5) Uani 1 1 d . . . H55A H 0.6133 0.574 0.1746 0.036 Uiso 1 1 calc R . . H55B H 0.7207 0.5227 0.1931 0.036 Uiso 1 1 calc R . . H55C H 0.683 0.5105 0.1402 0.036 Uiso 1 1 calc R . . C56 C 0.9635(2) 0.7074(2) 0.15539(7) 0.0227(4) Uani 1 1 d . . . H56A H 0.9537 0.648 0.1289 0.034 Uiso 1 1 calc R . . H56B H 0.9755 0.6626 0.1827 0.034 Uiso 1 1 calc R . . H56C H 1.0478 0.8034 0.1515 0.034 Uiso 1 1 calc R . . C57 C 0.8494(2) 0.8149(2) 0.20210(7) 0.0238(4) Uani 1 1 d . . . H57A H 0.8651 0.7704 0.2289 0.036 Uiso 1 1 calc R . . H57B H 0.7636 0.8236 0.2067 0.036 Uiso 1 1 calc R . . H57C H 0.9333 0.9107 0.1974 0.036 Uiso 1 1 calc R . . C58 C 0.8962(2) 0.8371(2) 0.08120(6) 0.0166(4) Uani 1 1 d . . . H58 H 0.9788 0.8264 0.0826 0.02 Uiso 1 1 calc R . . C59 C 0.8758(2) 0.8998(2) 0.04247(6) 0.0165(4) Uani 1 1 d . . . C60 C 0.9780(2) 0.9491(2) 0.00160(6) 0.0170(4) Uani 1 1 d . . . C61 C 1.1147(2) 0.9417(3) 0.01070(7) 0.0237(5) Uani 1 1 d . . . H61A H 1.1649 1.0014 0.0371 0.036 Uiso 1 1 calc R . . H61B H 1.1778 0.9772 -0.0159 0.036 Uiso 1 1 calc R . . H61C H 1.0888 0.8418 0.0167 0.036 Uiso 1 1 calc R . . C62 C 1.0223(2) 1.1045(2) -0.01160(7) 0.0221(4) Uani 1 1 d . . . H62A H 1.0812 1.1314 -0.0392 0.033 Uiso 1 1 calc R . . H62B H 1.0781 1.1698 0.0131 0.033 Uiso 1 1 calc R . . H62C H 0.9359 1.1115 -0.0172 0.033 Uiso 1 1 calc R . . C63 C 0.8979(2) 0.8482(2) -0.03850(7) 0.0208(4) Uani 1 1 d . . . H63A H 0.9607 0.8785 -0.0652 0.031 Uiso 1 1 calc R . . H63B H 0.8108 0.8526 -0.0453 0.031 Uiso 1 1 calc R . . H63C H 0.8712 0.7492 -0.0305 0.031 Uiso 1 1 calc R . . C64 C 0.7526(2) 0.9129(2) 0.04093(6) 0.0171(4) Uani 1 1 d . . . H64 H 0.7355 0.9547 0.015 0.02 Uiso 1 1 calc R . . C65 C 0.6550(2) 0.8664(2) 0.07639(6) 0.0170(4) Uani 1 1 d . . . C66 C 0.5182(2) 0.8732(2) 0.07264(7) 0.0190(4) Uani 1 1 d . . . H66A H 0.5255 0.9329 0.0461 0.023 Uiso 1 1 calc R . . H66B H 0.4365 0.775 0.0674 0.023 Uiso 1 1 calc R . . N67 N 0.48858(17) 0.93379(18) 0.11346(6) 0.0177(3) Uani 1 1 d . . . C68 C 0.3419(2) 0.9135(2) 0.11183(8) 0.0225(5) Uani 1 1 d . . . H68A H 0.2713 0.82 0.1254 0.027 Uiso 1 1 calc R . . H68B H 0.313 0.9169 0.0802 0.027 Uiso 1 1 calc R . . C69 C 0.3516(2) 1.0379(2) 0.13933(7) 0.0240(5) Uani 1 1 d . . . H69A H 0.3476 1.0189 0.1723 0.029 Uiso 1 1 calc R . . H69B H 0.2738 1.058 0.1311 0.029 Uiso 1 1 calc R . . C70 C 0.4993(2) 1.1613(2) 0.12516(7) 0.0224(4) Uani 1 1 d . . . H70A H 0.5389 1.238 0.1485 0.027 Uiso 1 1 calc R . . H70B H 0.4933 1.2034 0.0959 0.027 Uiso 1 1 calc R . . C71 C 0.5923(2) 1.0901(2) 0.12065(7) 0.0182(4) Uani 1 1 d . . . H71 H 0.6573 1.1304 0.0938 0.022 Uiso 1 1 calc R . . C72 C 0.6809(2) 1.1105(2) 0.16320(7) 0.0198(4) Uani 1 1 d . . . H72A H 0.6173 1.075 0.1901 0.024 Uiso 1 1 calc R . . H72B H 0.7323 1.0556 0.1606 0.024 Uiso 1 1 calc R . . O73 O 0.78151(15) 1.26002(15) 0.16788(5) 0.0222(3) Uani 1 1 d . . . C74 C 0.8608(2) 1.2903(3) 0.20893(7) 0.0264(5) Uani 1 1 d . . . H74A H 0.9157 1.2398 0.2091 0.04 Uiso 1 1 calc R . . H74B H 0.7942 1.2579 0.2347 0.04 Uiso 1 1 calc R . . H74C H 0.9271 1.3942 0.2113 0.04 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 O1 0.0165(7) 0.0225(8) 0.0202(7) 0.0038(6) -0.0014(5) 0.0109(6) C2 0.0168(9) 0.0135(9) 0.0167(9) -0.0011(7) -0.0023(7) 0.0077(8) C3 0.0141(9) 0.0129(9) 0.0151(9) -0.0024(7) -0.0008(7) 0.0055(8) C4 0.0168(10) 0.0193(10) 0.0170(10) 0.0007(7) -0.0002(7) 0.0091(8) C5 0.0194(10) 0.0337(12) 0.0221(10) 0.0058(9) 0.0050(8) 0.0154(10) C6 0.0256(11) 0.0212(11) 0.0274(11) 0.0076(9) 0.0056(9) 0.0116(9) C7 0.0243(11) 0.0294(12) 0.0173(10) 0.0008(8) 0.0012(8) 0.0147(10) C8 0.0141(9) 0.0154(9) 0.0162(9) -0.0017(7) -0.0002(7) 0.0071(8) C9 0.0182(10) 0.0147(9) 0.0154(9) -0.0017(7) -0.0019(7) 0.0087(8) C10 0.0169(10) 0.0180(10) 0.0150(9) 0.0008(7) -0.0001(7) 0.0097(8) C11 0.0249(11) 0.0218(11) 0.0194(10) 0.0024(8) -0.0018(8) 0.0127(9) C12 0.0205(10) 0.0317(12) 0.0192(10) 0.0005(8) -0.0014(8) 0.0175(10) C13 0.0221(11) 0.0232(11) 0.0167(10) -0.0020(8) -0.0040(8) 0.0124(9) C14 0.0156(9) 0.0165(9) 0.0154(9) -0.0017(7) 0.0006(7) 0.0066(8) C15 0.0153(9) 0.0175(10) 0.0167(9) -0.0024(7) -0.0010(7) 0.0086(8) C16 0.0155(10) 0.0220(10) 0.0182(10) -0.0006(8) 0.0000(7) 0.0106(8) N17 0.0176(8) 0.0182(8) 0.0171(8) -0.0015(6) -0.0020(6) 0.0114(7) C18 0.0151(10) 0.0234(11) 0.0279(11) 0.0004(8) -0.0005(8) 0.0122(9) C19 0.0147(10) 0.0248(11) 0.0293(11) 0.0011(9) -0.0024(8) 0.0097(9) C20 0.0177(10) 0.0200(10) 0.0290(11) 0.0016(8) 0.0018(8) 0.0078(9) C21 0.0169(10) 0.0172(10) 0.0201(10) 0.0014(8) -0.0012(8) 0.0077(8) C22 0.0223(10) 0.0144(10) 0.0228(11) -0.0022(8) -0.0027(8) 0.0089(8) O23 0.0281(8) 0.0186(7) 0.0229(7) -0.0026(6) -0.0008(6) 0.0120(7) C24 0.0433(14) 0.0322(13) 0.0221(11) -0.0051(9) -0.0045(10) 0.0252(12) O51 0.0170(7) 0.0227(8) 0.0225(7) 0.0037(6) 0.0056(6) 0.0127(6) C52 0.0150(9) 0.0127(9) 0.0169(9) -0.0010(7) 0.0020(7) 0.0042(8) C53 0.0164(9) 0.0117(9) 0.0163(9) -0.0027(7) -0.0012(7) 0.0070(8) C54 0.0190(10) 0.0188(10) 0.0161(9) 0.0019(7) -0.0003(7) 0.0098(8) C55 0.0237(11) 0.0206(11) 0.0265(11) 0.0047(9) -0.0002(9) 0.0098(9) C56 0.0232(11) 0.0260(11) 0.0225(10) 0.0030(9) -0.0009(8) 0.0149(9) C57 0.0253(11) 0.0293(12) 0.0177(10) -0.0031(8) -0.0025(8) 0.0144(10) C58 0.0150(9) 0.0162(10) 0.0191(10) -0.0022(7) -0.0008(7) 0.0082(8) C59 0.0191(10) 0.0150(9) 0.0153(9) -0.0027(7) -0.0007(7) 0.0084(8) C60 0.0160(9) 0.0188(10) 0.0164(9) 0.0013(7) 0.0018(7) 0.0089(8) C61 0.0204(11) 0.0300(12) 0.0223(10) 0.0040(9) 0.0049(8) 0.0136(10) C62 0.0244(11) 0.0192(10) 0.0206(10) 0.0020(8) 0.0038(8) 0.0093(9) C63 0.0233(11) 0.0223(11) 0.0164(10) -0.0006(8) 0.0025(8) 0.0112(9) C64 0.0206(10) 0.0168(10) 0.0141(9) 0.0011(7) -0.0007(7) 0.0096(8) C65 0.0179(10) 0.0161(10) 0.0180(9) -0.0033(8) -0.0012(7) 0.0092(8) C66 0.0161(10) 0.0219(10) 0.0200(10) -0.0019(8) -0.0011(8) 0.0103(9) N67 0.0130(8) 0.0191(9) 0.0214(9) -0.0001(7) 0.0012(6) 0.0083(7) C68 0.0152(10) 0.0231(11) 0.0324(12) 0.0021(9) 0.0024(8) 0.0119(9) C69 0.0227(11) 0.0275(11) 0.0280(11) 0.0024(9) 0.0046(9) 0.0173(10) C70 0.0228(11) 0.0184(10) 0.0267(11) 0.0007(8) 0.0004(9) 0.0109(9) C71 0.0170(10) 0.0165(10) 0.0208(10) 0.0024(8) 0.0029(8) 0.0080(8) C72 0.0191(10) 0.0173(10) 0.0223(10) 0.0021(8) 0.0017(8) 0.0085(8) O73 0.0232(8) 0.0174(7) 0.0218(7) -0.0007(6) -0.0028(6) 0.0071(6) C74 0.0251(12) 0.0286(12) 0.0213(11) -0.0037(9) -0.0015(9) 0.0104(10) #----------------------------------------------------------------------------# # 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 O1 C2 1.381(2) . ? O1 H1 0.84 . ? C2 C15 1.399(3) . ? C2 C3 1.404(3) . ? C3 C8 1.404(3) . ? C3 C4 1.539(3) . ? C4 C5 1.538(3) . ? C4 C6 1.540(3) . ? C4 C7 1.540(3) . ? C5 H5A 0.98 . ? C5 H5B 0.98 . ? C5 H5C 0.98 . ? C6 H6A 0.98 . ? C6 H6B 0.98 . ? C6 H6C 0.98 . ? C7 H7A 0.98 . ? C7 H7B 0.98 . ? C7 H7C 0.98 . ? C8 C9 1.391(3) . ? C8 H8 0.95 . ? C9 C14 1.395(3) . ? C9 C10 1.536(3) . ? C10 C12 1.531(3) . ? C10 C13 1.541(3) . ? C10 C11 1.541(3) . ? C11 H11A 0.98 . ? C11 H11B 0.98 . ? C11 H11C 0.98 . ? C12 H12A 0.98 . ? C12 H12B 0.98 . ? C12 H12C 0.98 . ? C13 H13A 0.98 . ? C13 H13B 0.98 . ? C13 H13C 0.98 . ? C14 C15 1.390(3) . ? C14 H14 0.95 . ? C15 C16 1.511(3) . ? C16 N17 1.478(2) . ? C16 H16A 0.99 . ? C16 H16B 0.99 . ? N17 C18 1.482(3) . ? N17 C21 1.495(3) . ? C18 C19 1.517(3) . ? C18 H18A 0.99 . ? C18 H18B 0.99 . ? C19 C20 1.528(3) . ? C19 H19A 0.99 . ? C19 H19B 0.99 . ? C20 C21 1.537(3) . ? C20 H20A 0.99 . ? C20 H20B 0.99 . ? C21 C22 1.521(3) . ? C21 H21 1 . ? C22 O23 1.423(2) . ? C22 H22A 0.99 . ? C22 H22B 0.99 . ? O23 C24 1.418(3) . ? C24 H24A 0.98 . ? C24 H24B 0.98 . ? C24 H24C 0.98 . ? O51 C52 1.377(2) . ? O51 H51 0.84 . ? C52 C65 1.402(3) . ? C52 C53 1.404(3) . ? C53 C58 1.401(3) . ? C53 C54 1.539(3) . ? C54 C56 1.537(3) . ? C54 C55 1.538(3) . ? C54 C57 1.543(3) . ? C55 H55A 0.98 . ? C55 H55B 0.98 . ? C55 H55C 0.98 . ? C56 H56A 0.98 . ? C56 H56B 0.98 . ? C56 H56C 0.98 . ? C57 H57A 0.98 . ? C57 H57B 0.98 . ? C57 H57C 0.98 . ? C58 C59 1.397(3) . ? C58 H58 0.95 . ? C59 C64 1.398(3) . ? C59 C60 1.535(3) . ? C60 C61 1.531(3) . ? C60 C62 1.539(3) . ? C60 C63 1.543(3) . ? C61 H61A 0.98 . ? C61 H61B 0.98 . ? C61 H61C 0.98 . ? C62 H62A 0.98 . ? C62 H62B 0.98 . ? C62 H62C 0.98 . ? C63 H63A 0.98 . ? C63 H63B 0.98 . ? C63 H63C 0.98 . ? C64 C65 1.385(3) . ? C64 H64 0.95 . ? C65 C66 1.510(3) . ? C66 N67 1.477(3) . ? C66 H66A 0.99 . ? C66 H66B 0.99 . ? N67 C68 1.478(3) . ? N67 C71 1.493(3) . ? C68 C69 1.521(3) . ? C68 H68A 0.99 . ? C68 H68B 0.99 . ? C69 C70 1.530(3) . ? C69 H69A 0.99 . ? C69 H69B 0.99 . ? C70 C71 1.537(3) . ? C70 H70A 0.99 . ? C70 H70B 0.99 . ? C71 C72 1.523(3) . ? C71 H71 1 . ? C72 O73 1.424(2) . ? C72 H72A 0.99 . ? C72 H72B 0.99 . ? O73 C74 1.421(3) . ? C74 H74A 0.98 . ? C74 H74B 0.98 . ? C74 H74C 0.98 . ? 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 C2 O1 H1 109.5 . . ? O1 C2 C15 118.68(17) . . ? O1 C2 C3 120.02(16) . . ? C15 C2 C3 121.30(17) . . ? C2 C3 C8 116.52(17) . . ? C2 C3 C4 121.24(16) . . ? C8 C3 C4 122.24(17) . . ? C3 C4 C5 112.05(16) . . ? C3 C4 C6 110.52(16) . . ? C5 C4 C6 107.23(17) . . ? C3 C4 C7 109.62(16) . . ? C5 C4 C7 107.27(17) . . ? C6 C4 C7 110.07(17) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C3 123.74(17) . . ? C9 C8 H8 118.1 . . ? C3 C8 H8 118.1 . . ? C8 C9 C14 117.58(17) . . ? C8 C9 C10 122.99(17) . . ? C14 C9 C10 119.39(16) . . ? C12 C10 C9 112.47(16) . . ? C12 C10 C13 108.59(16) . . ? C9 C10 C13 107.97(15) . . ? C12 C10 C11 108.24(17) . . ? C9 C10 C11 110.52(16) . . ? C13 C10 C11 108.98(16) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C10 C13 H13A 109.5 . . ? C10 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C10 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 C9 121.17(17) . . ? C15 C14 H14 119.4 . . ? C9 C14 H14 119.4 . . ? C14 C15 C2 119.69(17) . . ? C14 C15 C16 119.90(17) . . ? C2 C15 C16 120.33(17) . . ? N17 C16 C15 112.80(16) . . ? N17 C16 H16A 109 . . ? C15 C16 H16A 109 . . ? N17 C16 H16B 109 . . ? C15 C16 H16B 109 . . ? H16A C16 H16B 107.8 . . ? C16 N17 C18 110.83(15) . . ? C16 N17 C21 113.81(15) . . ? C18 N17 C21 107.86(15) . . ? N17 C18 C19 104.62(17) . . ? N17 C18 H18A 110.8 . . ? C19 C18 H18A 110.8 . . ? N17 C18 H18B 110.8 . . ? C19 C18 H18B 110.8 . . ? H18A C18 H18B 108.9 . . ? C18 C19 C20 102.25(16) . . ? C18 C19 H19A 111.3 . . ? C20 C19 H19A 111.3 . . ? C18 C19 H19B 111.3 . . ? C20 C19 H19B 111.3 . . ? H19A C19 H19B 109.2 . . ? C19 C20 C21 103.78(17) . . ? C19 C20 H20A 111 . . ? C21 C20 H20A 111 . . ? C19 C20 H20B 111 . . ? C21 C20 H20B 111 . . ? H20A C20 H20B 109 . . ? N17 C21 C22 109.54(16) . . ? N17 C21 C20 105.80(16) . . ? C22 C21 C20 112.03(17) . . ? N17 C21 H21 109.8 . . ? C22 C21 H21 109.8 . . ? C20 C21 H21 109.8 . . ? O23 C22 C21 107.68(16) . . ? O23 C22 H22A 110.2 . . ? C21 C22 H22A 110.2 . . ? O23 C22 H22B 110.2 . . ? C21 C22 H22B 110.2 . . ? H22A C22 H22B 108.5 . . ? C24 O23 C22 111.70(16) . . ? O23 C24 H24A 109.5 . . ? O23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? O23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C52 O51 H51 109.5 . . ? O51 C52 C65 118.99(17) . . ? O51 C52 C53 119.94(17) . . ? C65 C52 C53 121.07(17) . . ? C58 C53 C52 116.87(17) . . ? C58 C53 C54 121.91(17) . . ? C52 C53 C54 121.21(16) . . ? C56 C54 C55 107.52(17) . . ? C56 C54 C53 112.33(16) . . ? C55 C54 C53 110.18(16) . . ? C56 C54 C57 107.12(16) . . ? C55 C54 C57 109.99(17) . . ? C53 C54 C57 109.62(16) . . ? C54 C55 H55A 109.5 . . ? C54 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C54 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C54 C56 H56A 109.5 . . ? C54 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C54 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C54 C57 H57A 109.5 . . ? C54 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C54 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C59 C58 C53 123.58(18) . . ? C59 C58 H58 118.2 . . ? C53 C58 H58 118.2 . . ? C58 C59 C64 117.28(17) . . ? C58 C59 C60 123.46(17) . . ? C64 C59 C60 119.22(17) . . ? C61 C60 C59 112.47(16) . . ? C61 C60 C62 108.41(17) . . ? C59 C60 C62 110.65(16) . . ? C61 C60 C63 108.08(16) . . ? C59 C60 C63 108.01(15) . . ? C62 C60 C63 109.16(16) . . ? C60 C61 H61A 109.5 . . ? C60 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C60 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C60 C62 H62A 109.5 . . ? C60 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C60 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C60 C63 H63A 109.5 . . ? C60 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C60 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C65 C64 C59 121.42(18) . . ? C65 C64 H64 119.3 . . ? C59 C64 H64 119.3 . . ? C64 C65 C52 119.76(18) . . ? C64 C65 C66 120.34(17) . . ? C52 C65 C66 119.84(17) . . ? N67 C66 C65 112.97(16) . . ? N67 C66 H66A 109 . . ? C65 C66 H66A 109 . . ? N67 C66 H66B 109 . . ? C65 C66 H66B 109 . . ? H66A C66 H66B 107.8 . . ? C66 N67 C68 110.90(15) . . ? C66 N67 C71 113.99(15) . . ? C68 N67 C71 108.11(16) . . ? N67 C68 C69 104.66(17) . . ? N67 C68 H68A 110.8 . . ? C69 C68 H68A 110.8 . . ? N67 C68 H68B 110.8 . . ? C69 C68 H68B 110.8 . . ? H68A C68 H68B 108.9 . . ? C68 C69 C70 101.57(17) . . ? C68 C69 H69A 111.5 . . ? C70 C69 H69A 111.5 . . ? C68 C69 H69B 111.5 . . ? C70 C69 H69B 111.5 . . ? H69A C69 H69B 109.3 . . ? C69 C70 C71 104.03(16) . . ? C69 C70 H70A 111 . . ? C71 C70 H70A 111 . . ? C69 C70 H70B 111 . . ? C71 C70 H70B 111 . . ? H70A C70 H70B 109 . . ? N67 C71 C72 109.85(16) . . ? N67 C71 C70 105.46(16) . . ? C72 C71 C70 111.81(17) . . ? N67 C71 H71 109.9 . . ? C72 C71 H71 109.9 . . ? C70 C71 H71 109.9 . . ? O73 C72 C71 107.99(16) . . ? O73 C72 H72A 110.1 . . ? C71 C72 H72A 110.1 . . ? O73 C72 H72B 110.1 . . ? C71 C72 H72B 110.1 . . ? H72A C72 H72B 108.4 . . ? C74 O73 C72 111.74(16) . . ? O73 C74 H74A 109.5 . . ? O73 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? O73 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C2 C3 C8 -179.32(17) . . . . ? C15 C2 C3 C8 0.7(3) . . . . ? O1 C2 C3 C4 0.1(3) . . . . ? C15 C2 C3 C4 -179.87(17) . . . . ? C2 C3 C4 C5 178.12(18) . . . . ? C8 C3 C4 C5 -2.4(3) . . . . ? C2 C3 C4 C6 58.6(2) . . . . ? C8 C3 C4 C6 -122.0(2) . . . . ? C2 C3 C4 C7 -62.9(2) . . . . ? C8 C3 C4 C7 116.53(19) . . . . ? C2 C3 C8 C9 0.2(3) . . . . ? C4 C3 C8 C9 -179.25(17) . . . . ? C3 C8 C9 C14 -0.8(3) . . . . ? C3 C8 C9 C10 -178.39(17) . . . . ? C8 C9 C10 C12 -8.5(3) . . . . ? C14 C9 C10 C12 173.94(17) . . . . ? C8 C9 C10 C13 111.3(2) . . . . ? C14 C9 C10 C13 -66.3(2) . . . . ? C8 C9 C10 C11 -129.56(19) . . . . ? C14 C9 C10 C11 52.8(2) . . . . ? C8 C9 C14 C15 0.4(3) . . . . ? C10 C9 C14 C15 178.15(17) . . . . ? C9 C14 C15 C2 0.4(3) . . . . ? C9 C14 C15 C16 -176.31(17) . . . . ? O1 C2 C15 C14 179.00(17) . . . . ? C3 C2 C15 C14 -1.0(3) . . . . ? O1 C2 C15 C16 -4.3(3) . . . . ? C3 C2 C15 C16 175.73(18) . . . . ? C14 C15 C16 N17 -134.69(18) . . . . ? C2 C15 C16 N17 48.6(2) . . . . ? C15 C16 N17 C18 -169.77(16) . . . . ? C15 C16 N17 C21 68.5(2) . . . . ? C16 N17 C18 C19 -150.83(17) . . . . ? C21 N17 C18 C19 -25.6(2) . . . . ? N17 C18 C19 C20 38.7(2) . . . . ? C18 C19 C20 C21 -36.9(2) . . . . ? C16 N17 C21 C22 -113.45(18) . . . . ? C18 N17 C21 C22 123.15(17) . . . . ? C16 N17 C21 C20 125.61(17) . . . . ? C18 N17 C21 C20 2.2(2) . . . . ? C19 C20 C21 N17 21.8(2) . . . . ? C19 C20 C21 C22 -97.5(2) . . . . ? N17 C21 C22 O23 176.68(15) . . . . ? C20 C21 C22 O23 -66.2(2) . . . . ? C21 C22 O23 C24 173.14(17) . . . . ? O51 C52 C53 C58 -179.31(17) . . . . ? C65 C52 C53 C58 1.2(3) . . . . ? O51 C52 C53 C54 0.8(3) . . . . ? C65 C52 C53 C54 -178.79(17) . . . . ? C58 C53 C54 C56 -2.0(3) . . . . ? C52 C53 C54 C56 177.90(17) . . . . ? C58 C53 C54 C55 -121.9(2) . . . . ? C52 C53 C54 C55 58.0(2) . . . . ? C58 C53 C54 C57 116.93(19) . . . . ? C52 C53 C54 C57 -63.1(2) . . . . ? C52 C53 C58 C59 0.0(3) . . . . ? C54 C53 C58 C59 179.94(18) . . . . ? C53 C58 C59 C64 -0.7(3) . . . . ? C53 C58 C59 C60 -178.52(17) . . . . ? C58 C59 C60 C61 -8.1(3) . . . . ? C64 C59 C60 C61 174.12(18) . . . . ? C58 C59 C60 C62 -129.5(2) . . . . ? C64 C59 C60 C62 52.7(2) . . . . ? C58 C59 C60 C63 111.1(2) . . . . ? C64 C59 C60 C63 -66.7(2) . . . . ? C58 C59 C64 C65 0.3(3) . . . . ? C60 C59 C64 C65 178.19(18) . . . . ? C59 C64 C65 C52 0.8(3) . . . . ? C59 C64 C65 C66 -176.12(18) . . . . ? O51 C52 C65 C64 178.87(17) . . . . ? C53 C52 C65 C64 -1.6(3) . . . . ? O51 C52 C65 C66 -4.2(3) . . . . ? C53 C52 C65 C66 175.39(18) . . . . ? C64 C65 C66 N67 -133.88(19) . . . . ? C52 C65 C66 N67 49.2(2) . . . . ? C65 C66 N67 C68 -169.43(17) . . . . ? C65 C66 N67 C71 68.3(2) . . . . ? C66 N67 C68 C69 -151.72(17) . . . . ? C71 N67 C68 C69 -26.1(2) . . . . ? N67 C68 C69 C70 39.1(2) . . . . ? C68 C69 C70 C71 -37.4(2) . . . . ? C66 N67 C71 C72 -113.35(17) . . . . ? C68 N67 C71 C72 122.85(17) . . . . ? C66 N67 C71 C70 126.01(17) . . . . ? C68 N67 C71 C70 2.2(2) . . . . ? C69 C70 C71 N67 22.3(2) . . . . ? C69 C70 C71 C72 -97.09(19) . . . . ? N67 C71 C72 O73 177.99(15) . . . . ? C70 C71 C72 O73 -65.3(2) . . . . ? C71 C72 O73 C74 175.02(16) . . . . ? data_job _database_code_depnum_ccdc_archive 'CCDC 782555' #TrackingRef 'VP498_150K_APEX_27mai10_archive.cif' _audit_creation_date 2010-05-27T09:11:24-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C29 H56 N2 O5 Si2 Zn' _chemical_formula_sum 'C29 H56 N2 O5 Si2 Zn' _chemical_formula_weight 634.31 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 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 13.9506(17) _cell_length_b 10.7275(7) _cell_length_c 23.4443(16) _cell_angle_alpha 90 _cell_angle_beta 95.431(4) _cell_angle_gamma 90 _cell_volume 3492.8(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5111 _cell_measurement_theta_min 2.58 _cell_measurement_theta_max 27.45 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.07 _exptl_crystal_density_diffrn 1.206 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1368 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.807 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_absorpt_correction_T_min 0.809 _exptl_absorpt_correction_T_max 0.945 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_measurement_device_type 'APEXII, Bruker-AXS' _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_detector 'CCD plate' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0459 _diffrn_reflns_av_unetI/netI 0.0418 _diffrn_reflns_number 31084 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 7992 _reflns_number_gt 6530 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SAINT (Bruker, 2002)' _computing_cell_refinement 'Bruker SMART (Bruker, 2002)' _computing_data_reduction 'Bruker SAINT (Bruker, 2002)' _computing_structure_solution 'SIR97 (Altomare et al., 1999))' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material ; WinGX publication routines (Farrugia, 1999), CRYSCAL (T. Roisnel, local program) ; #----------------------------------------------------------------------------# # 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^)+(0.0326P)^2^+1.3500P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 7992 _refine_ls_number_parameters 368 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0451 _refine_ls_R_factor_gt 0.0323 _refine_ls_wR_factor_ref 0.0816 _refine_ls_wR_factor_gt 0.0756 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.379 _refine_diff_density_min -0.227 _refine_diff_density_rms 0.055 #----------------------------------------------------------------------------# # 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.244560(13) 0.279881(18) 0.125416(8) 0.01773(6) Uani 1 1 d . . . N1 N 0.36673(10) 0.24097(13) 0.09925(6) 0.0212(3) Uani 1 1 d . . . Si1 Si 0.41141(3) 0.32942(5) 0.04767(2) 0.02141(11) Uani 1 1 d . . . HSI1 H 0.3570(16) 0.442(2) 0.0410(9) 0.05 Uiso 1 1 d . . . C2 C 0.53900(14) 0.3813(2) 0.06602(10) 0.0378(5) Uani 1 1 d . . . H2A H 0.5462 0.4144 0.1052 0.057 Uiso 1 1 calc R . . H2B H 0.555 0.4464 0.0392 0.057 Uiso 1 1 calc R . . H2C H 0.5824 0.3102 0.0633 0.057 Uiso 1 1 calc R . . C3 C 0.40032(17) 0.2532(2) -0.02477(8) 0.0368(5) Uani 1 1 d . . . H3A H 0.4436 0.1812 -0.0242 0.055 Uiso 1 1 calc R . . H3B H 0.4178 0.3132 -0.0536 0.055 Uiso 1 1 calc R . . H3C H 0.3338 0.2256 -0.0343 0.055 Uiso 1 1 calc R . . Si2 Si 0.42403(4) 0.11841(5) 0.13396(2) 0.02425(12) Uani 1 1 d . . . HSI2 H 0.3625(16) 0.012(2) 0.1353(10) 0.05 Uiso 1 1 d . . . C4 C 0.53074(18) 0.0622(2) 0.09878(10) 0.0520(7) Uani 1 1 d . . . H4A H 0.513 0.0522 0.0576 0.078 Uiso 1 1 calc R . . H4B H 0.5521 -0.0181 0.1154 0.078 Uiso 1 1 calc R . . H4C H 0.5831 0.1231 0.1049 0.078 Uiso 1 1 calc R . . C5 C 0.46296(16) 0.1602(2) 0.20992(9) 0.0366(5) Uani 1 1 d . . . H5A H 0.5032 0.2352 0.2109 0.055 Uiso 1 1 calc R . . H5B H 0.5 0.0912 0.2284 0.055 Uiso 1 1 calc R . . H5C H 0.4061 0.1762 0.2304 0.055 Uiso 1 1 calc R . . O11 O 0.14673(9) 0.37326(11) 0.06542(5) 0.0230(3) Uani 1 1 d . . . C12 C 0.12080(14) 0.35008(18) 0.00552(8) 0.0290(4) Uani 1 1 d . . . H12A H 0.0498 0.3543 -0.0018 0.035 Uiso 1 1 calc R . . H12B H 0.1405 0.2641 -0.0033 0.035 Uiso 1 1 calc R . . C13 C 0.16387(14) 0.43774(19) -0.03502(8) 0.0305(4) Uani 1 1 d . . . H13A H 0.2302 0.46 -0.0196 0.037 Uiso 1 1 calc R . . H13B H 0.1673 0.3962 -0.0725 0.037 Uiso 1 1 calc R . . O14 O 0.10709(9) 0.54770(13) -0.04256(6) 0.0322(3) Uani 1 1 d . . . C15 C 0.15193(16) 0.6459(2) -0.07177(9) 0.0401(5) Uani 1 1 d . . . H15A H 0.1046 0.682 -0.1014 0.048 Uiso 1 1 calc R . . H15B H 0.2059 0.6113 -0.0913 0.048 Uiso 1 1 calc R . . C16 C 0.18926(16) 0.7471(2) -0.03120(9) 0.0368(5) Uani 1 1 d . . . H16A H 0.2161 0.8159 -0.0529 0.044 Uiso 1 1 calc R . . H16B H 0.136 0.7808 -0.0108 0.044 Uiso 1 1 calc R . . O17 O 0.26158(9) 0.69757(12) 0.00870(6) 0.0294(3) Uani 1 1 d . . . C18 C 0.30380(15) 0.78790(17) 0.04809(9) 0.0318(4) Uani 1 1 d . . . H18A H 0.2529 0.8374 0.0642 0.038 Uiso 1 1 calc R . . H18B H 0.3452 0.8454 0.0283 0.038 Uiso 1 1 calc R . . C19 C 0.36281(14) 0.71990(18) 0.09515(9) 0.0287(4) Uani 1 1 d . . . H19A H 0.4041 0.6571 0.0785 0.034 Uiso 1 1 calc R . . H19B H 0.405 0.7794 0.1179 0.034 Uiso 1 1 calc R . . O20 O 0.29990(9) 0.66006(11) 0.13108(6) 0.0259(3) Uani 1 1 d . . . C21 C 0.34722(12) 0.56280(16) 0.16393(7) 0.0215(4) Uani 1 1 d . . . H21A H 0.4055 0.5965 0.186 0.026 Uiso 1 1 calc R . . H21B H 0.3678 0.4975 0.1378 0.026 Uiso 1 1 calc R . . C22 C 0.28209(12) 0.50583(16) 0.20460(7) 0.0218(4) Uani 1 1 d . . . H22A H 0.3227 0.4579 0.2338 0.026 Uiso 1 1 calc R . . H22B H 0.2522 0.5746 0.2248 0.026 Uiso 1 1 calc R . . C24 C 0.12132(12) 0.49137(16) 0.14852(7) 0.0205(4) Uani 1 1 d . . . H24A H 0.1198 0.577 0.1642 0.025 Uiso 1 1 calc R . . H24B H 0.0601 0.45 0.1555 0.025 Uiso 1 1 calc R . . C25 C 0.12816(12) 0.49880(15) 0.08463(7) 0.0208(4) Uani 1 1 d . . . H25A H 0.0672 0.5308 0.0649 0.025 Uiso 1 1 calc R . . H25B H 0.1811 0.5553 0.0762 0.025 Uiso 1 1 calc R . . O31 O 0.17694(8) 0.14441(11) 0.15629(5) 0.0224(3) Uani 1 1 d . . . C32 C 0.09523(12) 0.16155(15) 0.18058(7) 0.0181(3) Uani 1 1 d . . . C33 C 0.01863(12) 0.07395(15) 0.17226(7) 0.0193(3) Uani 1 1 d . . . C34 C 0.02564(13) -0.03902(17) 0.13272(8) 0.0251(4) Uani 1 1 d . . . C35 C 0.03902(18) 0.0063(2) 0.07206(8) 0.0428(6) Uani 1 1 d . . . H35A H -0.0148 0.0608 0.0585 0.064 Uiso 1 1 calc R . . H35B H 0.0408 -0.0656 0.0464 0.064 Uiso 1 1 calc R . . H35C H 0.0996 0.0527 0.0724 0.064 Uiso 1 1 calc R . . C36 C 0.11040(14) -0.12319(16) 0.15387(8) 0.0252(4) Uani 1 1 d . . . H36A H 0.1158 -0.1914 0.1265 0.038 Uiso 1 1 calc R . . H36B H 0.0996 -0.1577 0.1914 0.038 Uiso 1 1 calc R . . H36C H 0.17 -0.0743 0.1572 0.038 Uiso 1 1 calc R . . C37 C -0.06562(15) -0.1211(2) 0.12961(11) 0.0477(6) Uani 1 1 d . . . H37A H -0.1211 -0.0726 0.1134 0.071 Uiso 1 1 calc R . . H37B H -0.0768 -0.1491 0.1682 0.071 Uiso 1 1 calc R . . H37C H -0.0569 -0.1937 0.1053 0.071 Uiso 1 1 calc R . . C38 C -0.06360(12) 0.09530(16) 0.20032(7) 0.0217(4) Uani 1 1 d . . . H38 H -0.1144 0.0362 0.1952 0.026 Uiso 1 1 calc R . . C39 C -0.07615(12) 0.19820(15) 0.23557(7) 0.0202(4) Uani 1 1 d . . . C40 C -0.17029(13) 0.21204(17) 0.26443(8) 0.0263(4) Uani 1 1 d . . . C41 C -0.18278(17) 0.0996(2) 0.30316(10) 0.0448(6) Uani 1 1 d . . . H41A H -0.1288 0.0959 0.3331 0.067 Uiso 1 1 calc R . . H41B H -0.1843 0.0231 0.2803 0.067 Uiso 1 1 calc R . . H41C H -0.2432 0.1078 0.321 0.067 Uiso 1 1 calc R . . C42 C -0.25566(14) 0.2190(2) 0.21825(10) 0.0433(6) Uani 1 1 d . . . H42A H -0.3158 0.2255 0.2366 0.065 Uiso 1 1 calc R . . H42B H -0.2572 0.1436 0.1946 0.065 Uiso 1 1 calc R . . H42C H -0.2486 0.2924 0.1941 0.065 Uiso 1 1 calc R . . C43 C -0.16947(15) 0.3286(2) 0.30149(10) 0.0410(5) Uani 1 1 d . . . H43A H -0.1619 0.4023 0.2777 0.061 Uiso 1 1 calc R . . H43B H -0.1157 0.324 0.3315 0.061 Uiso 1 1 calc R . . H43C H -0.2302 0.3344 0.3192 0.061 Uiso 1 1 calc R . . C44 C -0.00048(12) 0.28247(15) 0.24270(7) 0.0187(3) Uani 1 1 d . . . H44 H -0.0064 0.3537 0.2662 0.022 Uiso 1 1 calc R . . C45 C 0.08437(12) 0.26508(15) 0.21616(7) 0.0170(3) Uani 1 1 d . . . C46 C 0.16779(12) 0.35321(15) 0.23013(7) 0.0189(3) Uani 1 1 d . . . H46A H 0.2222 0.3051 0.2493 0.023 Uiso 1 1 calc R . . H46B H 0.1485 0.4157 0.2579 0.023 Uiso 1 1 calc R . . N47 N 0.20310(9) 0.42166(12) 0.17974(6) 0.0167(3) 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 Zn1 0.01913(10) 0.01736(10) 0.01735(10) 0.00176(8) 0.00521(7) 0.00184(8) N1 0.0211(7) 0.0201(7) 0.0234(8) 0.0021(6) 0.0081(6) 0.0049(6) Si1 0.0219(2) 0.0217(2) 0.0216(2) 0.0009(2) 0.00699(19) 0.00087(19) C2 0.0263(10) 0.0402(12) 0.0477(13) 0.0031(10) 0.0090(9) -0.0047(9) C3 0.0490(13) 0.0388(12) 0.0240(10) -0.0029(9) 0.0109(9) 0.0010(10) Si2 0.0281(3) 0.0195(2) 0.0255(3) 0.0023(2) 0.0045(2) 0.0056(2) C4 0.0595(15) 0.0527(15) 0.0466(14) 0.0118(12) 0.0194(12) 0.0373(12) C5 0.0398(12) 0.0363(11) 0.0328(11) 0.0038(9) -0.0013(9) 0.0039(9) O11 0.0287(6) 0.0217(6) 0.0178(6) 0.0003(5) -0.0026(5) 0.0044(5) C12 0.0340(10) 0.0297(10) 0.0218(9) -0.0024(8) -0.0056(8) 0.0000(8) C13 0.0304(10) 0.0399(11) 0.0211(9) 0.0010(9) 0.0016(8) 0.0042(8) O14 0.0289(7) 0.0373(8) 0.0305(7) 0.0127(6) 0.0031(6) 0.0034(6) C15 0.0434(12) 0.0485(13) 0.0284(11) 0.0147(10) 0.0038(9) -0.0008(10) C16 0.0385(11) 0.0349(11) 0.0378(12) 0.0154(10) 0.0073(10) 0.0039(9) O17 0.0305(7) 0.0261(7) 0.0321(7) 0.0044(6) 0.0058(6) 0.0030(5) C18 0.0389(11) 0.0220(9) 0.0363(11) 0.0050(9) 0.0134(9) -0.0036(8) C19 0.0291(10) 0.0251(9) 0.0336(11) 0.0030(8) 0.0114(8) -0.0078(8) O20 0.0242(6) 0.0218(6) 0.0332(7) 0.0060(6) 0.0112(5) -0.0021(5) C21 0.0221(8) 0.0199(8) 0.0229(9) -0.0024(7) 0.0045(7) -0.0035(7) C22 0.0241(9) 0.0214(8) 0.0199(9) -0.0036(7) 0.0019(7) -0.0064(7) C24 0.0211(8) 0.0184(8) 0.0223(9) 0.0011(7) 0.0038(7) 0.0033(7) C25 0.0237(8) 0.0171(8) 0.0215(9) 0.0026(7) 0.0010(7) 0.0020(7) O31 0.0257(6) 0.0163(6) 0.0270(7) 0.0024(5) 0.0115(5) 0.0004(5) C32 0.0216(8) 0.0168(8) 0.0164(8) 0.0041(7) 0.0044(7) 0.0022(6) C33 0.0233(8) 0.0185(8) 0.0159(8) -0.0006(7) -0.0001(7) 0.0015(7) C34 0.0285(9) 0.0246(9) 0.0216(9) -0.0080(8) -0.0004(7) 0.0020(7) C35 0.0696(16) 0.0417(12) 0.0159(9) -0.0043(9) -0.0019(10) 0.0210(11) C36 0.0360(10) 0.0166(8) 0.0229(9) -0.0008(7) 0.0021(8) 0.0009(7) C37 0.0351(12) 0.0468(13) 0.0607(15) -0.0359(12) 0.0021(11) -0.0085(10) C38 0.0204(8) 0.0208(8) 0.0234(9) -0.0017(7) -0.0009(7) -0.0029(7) C39 0.0198(8) 0.0203(8) 0.0207(9) -0.0003(7) 0.0033(7) 0.0010(7) C40 0.0203(9) 0.0281(10) 0.0316(10) -0.0041(8) 0.0089(8) -0.0016(7) C41 0.0492(13) 0.0422(13) 0.0470(13) 0.0023(11) 0.0255(11) -0.0071(11) C42 0.0216(10) 0.0586(15) 0.0500(14) -0.0065(12) 0.0051(9) 0.0029(10) C43 0.0308(11) 0.0419(12) 0.0534(14) -0.0163(11) 0.0210(10) -0.0028(9) C44 0.0214(8) 0.0169(8) 0.0181(8) -0.0005(7) 0.0032(7) 0.0016(7) C45 0.0189(8) 0.0167(8) 0.0154(8) 0.0026(7) 0.0026(6) -0.0001(6) C46 0.0221(8) 0.0194(8) 0.0156(8) 0.0009(7) 0.0039(7) -0.0008(7) N47 0.0180(7) 0.0151(7) 0.0172(7) 0.0010(6) 0.0031(5) -0.0009(5) #----------------------------------------------------------------------------# # 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 N1 1.9114(14) . ? Zn1 O31 1.9117(11) . ? Zn1 N47 2.0998(13) . ? Zn1 O11 2.1169(12) . ? N1 Si1 1.7011(15) . ? N1 Si2 1.7049(15) . ? Si1 C2 1.876(2) . ? Si1 C3 1.878(2) . ? Si1 HSI1 1.43(2) . ? C2 H2A 0.98 . ? C2 H2B 0.98 . ? C2 H2C 0.98 . ? C3 H3A 0.98 . ? C3 H3B 0.98 . ? C3 H3C 0.98 . ? Si2 C5 1.867(2) . ? Si2 C4 1.869(2) . ? Si2 HSI2 1.43(2) . ? C4 H4A 0.98 . ? C4 H4B 0.98 . ? C4 H4C 0.98 . ? C5 H5A 0.98 . ? C5 H5B 0.98 . ? C5 H5C 0.98 . ? O11 C12 1.438(2) . ? O11 C25 1.451(2) . ? C12 C13 1.502(3) . ? C12 H12A 0.99 . ? C12 H12B 0.99 . ? C13 O14 1.423(2) . ? C13 H13A 0.99 . ? C13 H13B 0.99 . ? O14 C15 1.432(2) . ? C15 C16 1.503(3) . ? C15 H15A 0.99 . ? C15 H15B 0.99 . ? C16 O17 1.413(2) . ? C16 H16A 0.99 . ? C16 H16B 0.99 . ? O17 C18 1.427(2) . ? C18 C19 1.502(3) . ? C18 H18A 0.99 . ? C18 H18B 0.99 . ? C19 O20 1.425(2) . ? C19 H19A 0.99 . ? C19 H19B 0.99 . ? O20 C21 1.422(2) . ? C21 C22 1.508(2) . ? C21 H21A 0.99 . ? C21 H21B 0.99 . ? C22 N47 1.499(2) . ? C22 H22A 0.99 . ? C22 H22B 0.99 . ? C24 N47 1.496(2) . ? C24 C25 1.512(2) . ? C24 H24A 0.99 . ? C24 H24B 0.99 . ? C25 H25A 0.99 . ? C25 H25B 0.99 . ? O31 C32 1.334(2) . ? C32 C45 1.406(2) . ? C32 C33 1.423(2) . ? C33 C38 1.394(2) . ? C33 C34 1.535(2) . ? C34 C35 1.531(3) . ? C34 C36 1.532(2) . ? C34 C37 1.544(3) . ? C35 H35A 0.98 . ? C35 H35B 0.98 . ? C35 H35C 0.98 . ? C36 H36A 0.98 . ? C36 H36B 0.98 . ? C36 H36C 0.98 . ? C37 H37A 0.98 . ? C37 H37B 0.98 . ? C37 H37C 0.98 . ? C38 C39 1.400(2) . ? C38 H38 0.95 . ? C39 C44 1.388(2) . ? C39 C40 1.541(2) . ? C40 C43 1.522(3) . ? C40 C41 1.529(3) . ? C40 C42 1.534(3) . ? C41 H41A 0.98 . ? C41 H41B 0.98 . ? C41 H41C 0.98 . ? C42 H42A 0.98 . ? C42 H42B 0.98 . ? C42 H42C 0.98 . ? C43 H43A 0.98 . ? C43 H43B 0.98 . ? C43 H43C 0.98 . ? C44 C45 1.401(2) . ? C44 H44 0.95 . ? C45 C46 1.511(2) . ? C46 N47 1.512(2) . ? C46 H46A 0.99 . ? C46 H46B 0.99 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Zn1 O31 116.26(6) . . ? N1 Zn1 N47 131.15(6) . . ? O31 Zn1 N47 98.45(5) . . ? N1 Zn1 O11 115.37(6) . . ? O31 Zn1 O11 107.52(5) . . ? N47 Zn1 O11 82.13(5) . . ? Si1 N1 Si2 125.64(9) . . ? Si1 N1 Zn1 120.28(8) . . ? Si2 N1 Zn1 114.03(8) . . ? N1 Si1 C2 113.96(9) . . ? N1 Si1 C3 113.31(9) . . ? C2 Si1 C3 109.37(10) . . ? N1 Si1 HSI1 108.9(9) . . ? C2 Si1 HSI1 104.9(9) . . ? C3 Si1 HSI1 105.8(9) . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si1 C3 H3A 109.5 . . ? Si1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N1 Si2 C5 110.56(9) . . ? N1 Si2 C4 113.28(9) . . ? C5 Si2 C4 109.07(11) . . ? N1 Si2 HSI2 111.8(9) . . ? C5 Si2 HSI2 107.0(9) . . ? C4 Si2 HSI2 104.8(9) . . ? Si2 C4 H4A 109.5 . . ? Si2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Si2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si2 C5 H5A 109.5 . . ? Si2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C12 O11 C25 115.32(13) . . ? C12 O11 Zn1 130.82(11) . . ? C25 O11 Zn1 110.84(9) . . ? O11 C12 C13 115.52(16) . . ? O11 C12 H12A 108.4 . . ? C13 C12 H12A 108.4 . . ? O11 C12 H12B 108.4 . . ? C13 C12 H12B 108.4 . . ? H12A C12 H12B 107.5 . . ? O14 C13 C12 110.26(15) . . ? O14 C13 H13A 109.6 . . ? C12 C13 H13A 109.6 . . ? O14 C13 H13B 109.6 . . ? C12 C13 H13B 109.6 . . ? H13A C13 H13B 108.1 . . ? C13 O14 C15 113.97(15) . . ? O14 C15 C16 111.68(17) . . ? O14 C15 H15A 109.3 . . ? C16 C15 H15A 109.3 . . ? O14 C15 H15B 109.3 . . ? C16 C15 H15B 109.3 . . ? H15A C15 H15B 107.9 . . ? O17 C16 C15 109.32(17) . . ? O17 C16 H16A 109.8 . . ? C15 C16 H16A 109.8 . . ? O17 C16 H16B 109.8 . . ? C15 C16 H16B 109.8 . . ? H16A C16 H16B 108.3 . . ? C16 O17 C18 113.49(15) . . ? O17 C18 C19 108.03(15) . . ? O17 C18 H18A 110.1 . . ? C19 C18 H18A 110.1 . . ? O17 C18 H18B 110.1 . . ? C19 C18 H18B 110.1 . . ? H18A C18 H18B 108.4 . . ? O20 C19 C18 109.12(15) . . ? O20 C19 H19A 109.9 . . ? C18 C19 H19A 109.9 . . ? O20 C19 H19B 109.9 . . ? C18 C19 H19B 109.9 . . ? H19A C19 H19B 108.3 . . ? C21 O20 C19 111.73(13) . . ? O20 C21 C22 111.31(14) . . ? O20 C21 H21A 109.4 . . ? C22 C21 H21A 109.4 . . ? O20 C21 H21B 109.4 . . ? C22 C21 H21B 109.4 . . ? H21A C21 H21B 108 . . ? N47 C22 C21 117.59(14) . . ? N47 C22 H22A 107.9 . . ? C21 C22 H22A 107.9 . . ? N47 C22 H22B 107.9 . . ? C21 C22 H22B 107.9 . . ? H22A C22 H22B 107.2 . . ? N47 C24 C25 113.22(13) . . ? N47 C24 H24A 108.9 . . ? C25 C24 H24A 108.9 . . ? N47 C24 H24B 108.9 . . ? C25 C24 H24B 108.9 . . ? H24A C24 H24B 107.7 . . ? O11 C25 C24 106.76(13) . . ? O11 C25 H25A 110.4 . . ? C24 C25 H25A 110.4 . . ? O11 C25 H25B 110.4 . . ? C24 C25 H25B 110.4 . . ? H25A C25 H25B 108.6 . . ? C32 O31 Zn1 121.93(10) . . ? O31 C32 C45 120.43(15) . . ? O31 C32 C33 120.76(15) . . ? C45 C32 C33 118.78(15) . . ? C38 C33 C32 117.89(15) . . ? C38 C33 C34 121.14(15) . . ? C32 C33 C34 120.96(15) . . ? C35 C34 C36 109.24(16) . . ? C35 C34 C33 109.32(15) . . ? C36 C34 C33 111.18(14) . . ? C35 C34 C37 108.03(18) . . ? C36 C34 C37 106.67(16) . . ? C33 C34 C37 112.30(15) . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C34 C37 H37A 109.5 . . ? C34 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C34 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C33 C38 C39 124.23(16) . . ? C33 C38 H38 117.9 . . ? C39 C38 H38 117.9 . . ? C44 C39 C38 116.66(15) . . ? C44 C39 C40 123.69(15) . . ? C38 C39 C40 119.65(15) . . ? C43 C40 C41 107.69(18) . . ? C43 C40 C42 109.05(17) . . ? C41 C40 C42 109.46(17) . . ? C43 C40 C39 111.67(15) . . ? C41 C40 C39 109.54(15) . . ? C42 C40 C39 109.39(16) . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C40 C43 H43A 109.5 . . ? C40 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C40 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C39 C44 C45 121.65(16) . . ? C39 C44 H44 119.2 . . ? C45 C44 H44 119.2 . . ? C44 C45 C32 120.78(15) . . ? C44 C45 C46 119.09(15) . . ? C32 C45 C46 119.93(15) . . ? C45 C46 N47 115.82(13) . . ? C45 C46 H46A 108.3 . . ? N47 C46 H46A 108.3 . . ? C45 C46 H46B 108.3 . . ? N47 C46 H46B 108.3 . . ? H46A C46 H46B 107.4 . . ? C24 N47 C22 112.80(13) . . ? C24 N47 C46 109.58(12) . . ? C22 N47 C46 105.69(12) . . ? C24 N47 Zn1 107.84(10) . . ? C22 N47 Zn1 115.95(10) . . ? C46 N47 Zn1 104.53(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O31 Zn1 N1 Si1 154.19(8) . . . . ? N47 Zn1 N1 Si1 -75.38(12) . . . . ? O11 Zn1 N1 Si1 26.92(11) . . . . ? O31 Zn1 N1 Si2 -28.29(11) . . . . ? N47 Zn1 N1 Si2 102.14(9) . . . . ? O11 Zn1 N1 Si2 -155.56(7) . . . . ? Si2 N1 Si1 C2 -46.71(14) . . . . ? Zn1 N1 Si1 C2 130.51(11) . . . . ? Si2 N1 Si1 C3 79.22(14) . . . . ? Zn1 N1 Si1 C3 -103.57(11) . . . . ? Si1 N1 Si2 C5 108.90(12) . . . . ? Zn1 N1 Si2 C5 -68.46(11) . . . . ? Si1 N1 Si2 C4 -13.86(16) . . . . ? Zn1 N1 Si2 C4 168.77(11) . . . . ? N1 Zn1 O11 C12 45.21(16) . . . . ? O31 Zn1 O11 C12 -86.33(15) . . . . ? N47 Zn1 O11 C12 177.25(15) . . . . ? N1 Zn1 O11 C25 -113.79(11) . . . . ? O31 Zn1 O11 C25 114.66(10) . . . . ? N47 Zn1 O11 C25 18.24(10) . . . . ? C25 O11 C12 C13 54.4(2) . . . . ? Zn1 O11 C12 C13 -103.86(17) . . . . ? O11 C12 C13 O14 -84.20(19) . . . . ? C12 C13 O14 C15 168.90(16) . . . . ? C13 O14 C15 C16 -104.6(2) . . . . ? O14 C15 C16 O17 63.0(2) . . . . ? C15 C16 O17 C18 178.10(16) . . . . ? C16 O17 C18 C19 168.00(16) . . . . ? O17 C18 C19 O20 -72.88(19) . . . . ? C18 C19 O20 C21 160.50(15) . . . . ? C19 O20 C21 C22 176.22(14) . . . . ? O20 C21 C22 N47 74.30(19) . . . . ? C12 O11 C25 C24 157.77(14) . . . . ? Zn1 O11 C25 C24 -39.69(15) . . . . ? N47 C24 C25 O11 49.11(18) . . . . ? N1 Zn1 O31 C32 173.92(12) . . . . ? N47 Zn1 O31 C32 29.33(13) . . . . ? O11 Zn1 O31 C32 -55.02(13) . . . . ? Zn1 O31 C32 C45 -40.2(2) . . . . ? Zn1 O31 C32 C33 141.52(13) . . . . ? O31 C32 C33 C38 177.99(15) . . . . ? C45 C32 C33 C38 -0.3(2) . . . . ? O31 C32 C33 C34 -3.2(2) . . . . ? C45 C32 C33 C34 178.50(15) . . . . ? C38 C33 C34 C35 119.12(19) . . . . ? C32 C33 C34 C35 -59.7(2) . . . . ? C38 C33 C34 C36 -120.20(18) . . . . ? C32 C33 C34 C36 61.0(2) . . . . ? C38 C33 C34 C37 -0.8(2) . . . . ? C32 C33 C34 C37 -179.56(17) . . . . ? C32 C33 C38 C39 0.9(3) . . . . ? C34 C33 C38 C39 -177.98(16) . . . . ? C33 C38 C39 C44 -0.5(3) . . . . ? C33 C38 C39 C40 -179.98(16) . . . . ? C44 C39 C40 C43 -0.2(3) . . . . ? C38 C39 C40 C43 179.23(17) . . . . ? C44 C39 C40 C41 -119.4(2) . . . . ? C38 C39 C40 C41 60.0(2) . . . . ? C44 C39 C40 C42 120.65(19) . . . . ? C38 C39 C40 C42 -60.0(2) . . . . ? C38 C39 C44 C45 -0.3(2) . . . . ? C40 C39 C44 C45 179.12(16) . . . . ? C39 C44 C45 C32 0.8(3) . . . . ? C39 C44 C45 C46 -174.12(15) . . . . ? O31 C32 C45 C44 -178.77(15) . . . . ? C33 C32 C45 C44 -0.4(2) . . . . ? O31 C32 C45 C46 -3.9(2) . . . . ? C33 C32 C45 C46 174.40(15) . . . . ? C44 C45 C46 N47 -122.43(16) . . . . ? C32 C45 C46 N47 62.6(2) . . . . ? C25 C24 N47 C22 95.94(16) . . . . ? C25 C24 N47 C46 -146.62(14) . . . . ? C25 C24 N47 Zn1 -33.40(15) . . . . ? C21 C22 N47 C24 -74.80(19) . . . . ? C21 C22 N47 C46 165.48(15) . . . . ? C21 C22 N47 Zn1 50.24(18) . . . . ? C45 C46 N47 C24 55.92(17) . . . . ? C45 C46 N47 C22 177.73(14) . . . . ? C45 C46 N47 Zn1 -59.43(15) . . . . ? N1 Zn1 N47 C24 125.12(10) . . . . ? O31 Zn1 N47 C24 -98.52(10) . . . . ? O11 Zn1 N47 C24 8.14(10) . . . . ? N1 Zn1 N47 C22 -2.42(14) . . . . ? O31 Zn1 N47 C22 133.94(11) . . . . ? O11 Zn1 N47 C22 -119.39(11) . . . . ? N1 Zn1 N47 C46 -118.32(10) . . . . ? O31 Zn1 N47 C46 18.04(10) . . . . ? O11 Zn1 N47 C46 124.71(10) . . . . ? data_hklf5 _database_code_depnum_ccdc_archive 'CCDC 786156' #TrackingRef 'VP514_150K_KCCD_09juin10_archive.cif' _audit_creation_date 2010-06-10T16:00:50-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C56 H88 N4 O22 Zn5, C4 H8 O' _chemical_formula_sum 'C60 H96 N4 O23 Zn5' _chemical_formula_weight 1568.26 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.7988(4) _cell_length_b 14.6192(4) _cell_length_c 18.6856(5) _cell_angle_alpha 73.213(2) _cell_angle_beta 80.247(2) _cell_angle_gamma 85.375(2) _cell_volume 3554.60(17) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 15317 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.485 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.465 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1636 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.737 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0 _diffrn_reflns_av_unetI/netI 0.0847 _diffrn_reflns_number 28712 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 27.71 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.974 _reflns_number_total 28712 _reflns_number_gt 18101 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1999))' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material ; WinGX publication routines (Farrugia, 1999), CRYSCAL (T. Roisnel, local program) ; #----------------------------------------------------------------------------# # 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^)+(0.1016P)^2^+8.2403P] 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 SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.0057(5) _refine_ls_number_reflns 28712 _refine_ls_number_parameters 816 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1263 _refine_ls_R_factor_gt 0.0732 _refine_ls_wR_factor_ref 0.2211 _refine_ls_wR_factor_gt 0.186 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.298 _refine_diff_density_min -0.865 _refine_diff_density_rms 0.121 #----------------------------------------------------------------------------# # 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 0.73210(4) 0.15003(4) 0.55085(3) 0.03952(16) Uani 1 1 d . . . Zn2 Zn 0.52070(5) 0.16366(4) 0.67849(4) 0.04578(17) Uani 1 1 d . . . Zn3 Zn 0.77397(5) 0.24365(4) 0.74369(3) 0.04069(16) Uani 1 1 d . . . Zn4 Zn 1.00945(4) 0.36962(4) 0.81530(3) 0.03847(15) Uani 1 1 d . . . Zn5 Zn 0.80358(4) 0.29345(4) 0.94727(3) 0.03966(16) Uani 1 1 d . . . N1 N 0.7237(3) 0.0786(3) 0.4690(2) 0.0398(9) Uani 1 1 d . . . C2 C 0.7999(4) 0.0018(4) 0.4656(3) 0.0483(13) Uani 1 1 d . . . H2A H 0.7826 -0.0364 0.4339 0.058 Uiso 1 1 calc R . . H2B H 0.8019 -0.0412 0.5171 0.058 Uiso 1 1 calc R . . C3 C 0.9004(5) 0.0429(5) 0.4328(4) 0.0611(16) Uani 1 1 d . . . H3A H 0.9195 0.0778 0.4661 0.073 Uiso 1 1 calc R . . H3B H 0.9495 -0.0099 0.4307 0.073 Uiso 1 1 calc R . . O4 O 0.9008(4) 0.1061(4) 0.3589(2) 0.0686(12) Uani 1 1 d . . . C5 C 0.8316(5) 0.1817(5) 0.3625(3) 0.0591(16) Uani 1 1 d . . . H5A H 0.833 0.2269 0.3114 0.071 Uiso 1 1 calc R . . H5B H 0.8499 0.2167 0.3961 0.071 Uiso 1 1 calc R . . C6 C 0.7281(4) 0.1453(4) 0.3921(3) 0.0469(13) Uani 1 1 d . . . H6A H 0.6813 0.2 0.3934 0.056 Uiso 1 1 calc R . . H6B H 0.7087 0.1121 0.3577 0.056 Uiso 1 1 calc R . . C7 C 0.6234(4) 0.0356(3) 0.4924(3) 0.0403(11) Uani 1 1 d . . . H7A H 0.5728 0.0878 0.4915 0.048 Uiso 1 1 calc R . . H7B H 0.6125 0.003 0.455 0.048 Uiso 1 1 calc R . . C8 C 0.6101(4) -0.0339(3) 0.5689(3) 0.0377(11) Uani 1 1 d . . . C9 C 0.5966(4) -0.1300(3) 0.5777(3) 0.0404(11) Uani 1 1 d . . . H9A H 0.6564 -0.1539 0.5503 0.048 Uiso 1 1 calc R . . H9B H 0.5418 -0.1324 0.5503 0.048 Uiso 1 1 calc R . . C10 C 0.5773(4) -0.1967(3) 0.6485(3) 0.0402(12) Uani 1 1 d . . . C11 C 0.5636(4) -0.3033(3) 0.6578(3) 0.0465(13) Uani 1 1 d . . . C12 C 0.4726(7) -0.3357(5) 0.7125(5) 0.098(3) Uani 1 1 d . . . H12A H 0.4155 -0.2987 0.693 0.147 Uiso 1 1 calc R . . H12B H 0.4781 -0.3258 0.7614 0.147 Uiso 1 1 calc R . . H12C H 0.4644 -0.4037 0.7191 0.147 Uiso 1 1 calc R . . C14 C 0.5532(8) -0.3214(4) 0.5843(4) 0.095(3) Uani 1 1 d . . . H14A H 0.4959 -0.285 0.5648 0.142 Uiso 1 1 calc R . . H14B H 0.5445 -0.3898 0.5927 0.142 Uiso 1 1 calc R . . H14C H 0.6126 -0.3014 0.5475 0.142 Uiso 1 1 calc R . . C15 C 0.6509(7) -0.3591(5) 0.6873(7) 0.115(4) Uani 1 1 d . . . H15A H 0.6577 -0.3476 0.7353 0.173 Uiso 1 1 calc R . . H15B H 0.7102 -0.3391 0.6505 0.173 Uiso 1 1 calc R . . H15C H 0.642 -0.4274 0.6954 0.173 Uiso 1 1 calc R . . C16 C 0.5709(4) -0.1627(3) 0.7114(3) 0.0402(11) Uani 1 1 d . . . H16A H 0.6192 -0.201 0.7426 0.048 Uiso 1 1 calc R . . H16B H 0.5049 -0.1784 0.7412 0.048 Uiso 1 1 calc R . . C17 C 0.5850(4) -0.0654(3) 0.7049(3) 0.0410(12) Uani 1 1 d . . . C18 C 0.6046(4) -0.0031(3) 0.6336(3) 0.0347(10) Uani 1 1 d . . . O19 O 0.6190(3) 0.0912(2) 0.6256(2) 0.0400(8) Uani 1 1 d . . . C20 C 0.5817(4) -0.0293(3) 0.7728(3) 0.0383(11) Uani 1 1 d . . . H20A H 0.5783 -0.0846 0.8186 0.046 Uiso 1 1 calc R . . H20B H 0.6436 0.0034 0.768 0.046 Uiso 1 1 calc R . . N21 N 0.4970(3) 0.0379(3) 0.7830(3) 0.0421(10) Uani 1 1 d . . . C22 C 0.4032(4) -0.0117(4) 0.7965(4) 0.0516(14) Uani 1 1 d . . . H22A H 0.4064 -0.0727 0.8367 0.062 Uiso 1 1 calc R . . H22B H 0.3941 -0.0268 0.7497 0.062 Uiso 1 1 calc R . . C23 C 0.3161(5) 0.0488(5) 0.8197(4) 0.0656(17) Uani 1 1 d . . . H23A H 0.3096 0.1073 0.7776 0.079 Uiso 1 1 calc R . . H23B H 0.2554 0.0126 0.8296 0.079 Uiso 1 1 calc R . . O24 O 0.3259(3) 0.0751(3) 0.8850(3) 0.0672(12) Uani 1 1 d . . . C25 C 0.4150(5) 0.1260(4) 0.8714(4) 0.0578(16) Uani 1 1 d . . . H25A H 0.4219 0.1447 0.9172 0.069 Uiso 1 1 calc R . . H25B H 0.4116 0.1851 0.8293 0.069 Uiso 1 1 calc R . . C26 C 0.5027(4) 0.0657(4) 0.8520(3) 0.0481(13) Uani 1 1 d . . . H26A H 0.5632 0.1017 0.8443 0.058 Uiso 1 1 calc R . . H26B H 0.5068 0.0074 0.8947 0.058 Uiso 1 1 calc R . . O31 O 0.3937(3) 0.2325(3) 0.6692(2) 0.0539(10) Uani 1 1 d . . . C32 C 0.3491(5) 0.1935(4) 0.6326(4) 0.0536(14) Uani 1 1 d . . . O33 O 0.3848(4) 0.1224(4) 0.6144(3) 0.0845(17) Uani 1 1 d . . . C34 C 0.2508(6) 0.2366(6) 0.6154(5) 0.091(3) Uani 1 1 d . . . H34A H 0.2366 0.2929 0.6343 0.136 Uiso 1 1 calc R . . H34B H 0.2 0.1895 0.6401 0.136 Uiso 1 1 calc R . . H34C H 0.2512 0.2554 0.5606 0.136 Uiso 1 1 calc R . . O35 O 0.5926(3) 0.2338(2) 0.7309(2) 0.0418(8) Uani 1 1 d . . . C36 C 0.6020(4) 0.3230(3) 0.7164(3) 0.0431(12) Uani 1 1 d . . . O37 O 0.6826(3) 0.3548(2) 0.7201(2) 0.0515(10) Uani 1 1 d . . . C38 C 0.5168(5) 0.3913(4) 0.6996(4) 0.0593(16) Uani 1 1 d . . . H38A H 0.4595 0.356 0.6993 0.089 Uiso 1 1 calc R . . H38B H 0.5337 0.4375 0.65 0.089 Uiso 1 1 calc R . . H38C H 0.5012 0.4252 0.7386 0.089 Uiso 1 1 calc R . . O41 O 0.5914(4) 0.2937(3) 0.5718(3) 0.0731(13) Uani 1 1 d . . . C42 C 0.6593(6) 0.3294(5) 0.5216(4) 0.0690(19) Uani 1 1 d . . . C43 C 0.6598(7) 0.4387(4) 0.4870(4) 0.087(3) Uani 1 1 d . . . H43A H 0.7179 0.4556 0.4482 0.13 Uiso 1 1 calc R . . H43B H 0.6618 0.4696 0.5268 0.13 Uiso 1 1 calc R . . H43C H 0.6002 0.4603 0.4641 0.13 Uiso 1 1 calc R . . O44 O 0.7313(4) 0.2846(3) 0.4954(3) 0.0699(13) Uani 1 1 d . . . O45 O 0.8540(3) 0.0875(3) 0.5927(2) 0.0482(9) Uani 1 1 d . . . C46 C 0.8627(4) 0.1260(4) 0.6438(3) 0.0462(13) Uani 1 1 d . . . C47 C 0.9461(5) 0.0941(5) 0.6892(4) 0.0607(16) Uani 1 1 d . . . H47A H 0.9419 0.1301 0.7265 0.091 Uiso 1 1 calc R . . H47B H 1.0091 0.1058 0.6552 0.091 Uiso 1 1 calc R . . H47C H 0.9416 0.0257 0.7153 0.091 Uiso 1 1 calc R . . O48 O 0.8030(3) 0.1928(3) 0.6543(2) 0.0449(9) Uani 1 1 d . . . O51 O 0.7664(3) 0.1188(2) 0.8234(2) 0.0474(9) Uani 1 1 d . . . C52 C 0.7528(4) 0.1415(3) 0.8840(3) 0.0403(11) Uani 1 1 d . . . C53 C 0.7404(5) 0.0654(4) 0.9578(3) 0.0538(15) Uani 1 1 d . . . H53A H 0.7301 0.0951 0.9994 0.081 Uiso 1 1 calc R . . H53B H 0.7997 0.0236 0.9612 0.081 Uiso 1 1 calc R . . H53C H 0.6834 0.0276 0.9613 0.081 Uiso 1 1 calc R . . O54 O 0.7446(3) 0.2292(2) 0.88229(19) 0.0385(8) Uani 1 1 d . . . O55 O 0.8960(3) 0.3093(3) 0.7402(2) 0.0462(9) Uani 1 1 d . . . C56 C 0.9361(5) 0.3789(4) 0.6909(3) 0.0537(14) Uani 1 1 d . . . C57 C 0.9060(7) 0.4118(6) 0.6130(4) 0.093(3) Uani 1 1 d . . . H57A H 0.8567 0.3692 0.6097 0.139 Uiso 1 1 calc R . . H57B H 0.9637 0.4104 0.5747 0.139 Uiso 1 1 calc R . . H57C H 0.8779 0.4772 0.6043 0.139 Uiso 1 1 calc R . . O58 O 1.0008(3) 0.4241(3) 0.7061(2) 0.0556(10) Uani 1 1 d . . . N61 N 0.6695(3) 0.3980(3) 0.9398(3) 0.0428(10) Uani 1 1 d . . . C62 C 0.5799(4) 0.3552(4) 0.9292(4) 0.0532(15) Uani 1 1 d . . . H62A H 0.5295 0.4063 0.9143 0.064 Uiso 1 1 calc R . . H62B H 0.5971 0.3238 0.8881 0.064 Uiso 1 1 calc R . . C63 C 0.5387(5) 0.2834(5) 1.0007(4) 0.071(2) Uani 1 1 d . . . H63A H 0.4822 0.2528 0.9918 0.085 Uiso 1 1 calc R . . H63B H 0.5895 0.233 1.0161 0.085 Uiso 1 1 calc R . . O64 O 0.5071(3) 0.3283(3) 1.0607(3) 0.0776(14) Uani 1 1 d . . . C65 C 0.5905(5) 0.3694(5) 1.0737(4) 0.0712(19) Uani 1 1 d . . . H65A H 0.6385 0.3175 1.0924 0.085 Uiso 1 1 calc R . . H65B H 0.5692 0.4016 1.1139 0.085 Uiso 1 1 calc R . . C66 C 0.6406(4) 0.4399(4) 1.0051(3) 0.0517(14) Uani 1 1 d . . . H66A H 0.7001 0.4619 1.0175 0.062 Uiso 1 1 calc R . . H66B H 0.5958 0.4963 0.9903 0.062 Uiso 1 1 calc R . . C67 C 0.6971(4) 0.4772(3) 0.8697(3) 0.0392(11) Uani 1 1 d . . . H67A H 0.6393 0.5209 0.8598 0.047 Uiso 1 1 calc R . . H67B H 0.7163 0.4502 0.8263 0.047 Uiso 1 1 calc R . . C68 C 0.7807(4) 0.5329(3) 0.8759(3) 0.0357(10) Uani 1 1 d . . . C69 C 0.7667(4) 0.6274(3) 0.8784(3) 0.0393(11) Uani 1 1 d . . . H69 H 0.7038 0.6578 0.873 0.047 Uiso 1 1 calc R . . C70 C 0.8420(4) 0.6795(3) 0.8886(3) 0.0398(11) Uani 1 1 d . . . C71 C 0.8235(4) 0.7840(4) 0.8897(4) 0.0529(15) Uani 1 1 d . . . C72 C 0.7252(5) 0.7959(4) 0.9376(4) 0.0670(19) Uani 1 1 d . . . H72A H 0.6726 0.7745 0.9176 0.1 Uiso 1 1 calc R . . H72B H 0.7131 0.8633 0.9362 0.1 Uiso 1 1 calc R . . H72C H 0.7265 0.7574 0.99 0.1 Uiso 1 1 calc R . . C73 C 0.9049(5) 0.8192(5) 0.9204(6) 0.093(3) Uani 1 1 d . . . H73A H 0.9683 0.8126 0.8892 0.139 Uiso 1 1 calc R . . H73B H 0.907 0.781 0.9727 0.139 Uiso 1 1 calc R . . H73C H 0.8915 0.8865 0.9188 0.139 Uiso 1 1 calc R . . C74 C 0.8199(6) 0.8466(4) 0.8083(5) 0.080(2) Uani 1 1 d . . . H74A H 0.8828 0.84 0.7766 0.12 Uiso 1 1 calc R . . H74B H 0.8079 0.9136 0.8083 0.12 Uiso 1 1 calc R . . H74C H 0.7668 0.8261 0.7883 0.12 Uiso 1 1 calc R . . C75 C 0.9328(4) 0.6329(3) 0.8952(3) 0.0428(12) Uani 1 1 d . . . H75 H 0.9856 0.6665 0.9014 0.051 Uiso 1 1 calc R . . C76 C 0.9497(4) 0.5369(3) 0.8930(3) 0.0365(11) Uani 1 1 d . . . C77 C 0.8729(3) 0.4888(3) 0.8819(3) 0.0337(10) Uani 1 1 d . . . C78 C 1.0458(4) 0.4859(3) 0.9072(3) 0.0396(11) Uani 1 1 d . . . H78A H 1.0333 0.4269 0.9494 0.047 Uiso 1 1 calc R . . H78B H 1.0863 0.5271 0.9233 0.047 Uiso 1 1 calc R . . N79 N 1.1033(3) 0.4595(3) 0.8398(3) 0.0412(10) Uani 1 1 d . . . C80 C 1.1332(4) 0.5476(4) 0.7785(4) 0.0499(14) Uani 1 1 d . . . H80A H 1.1662 0.5899 0.799 0.06 Uiso 1 1 calc R . . H80B H 1.0738 0.5824 0.7596 0.06 Uiso 1 1 calc R . . C81 C 1.2025(5) 0.5239(4) 0.7132(4) 0.0647(18) Uani 1 1 d . . . H81A H 1.1684 0.4846 0.6906 0.078 Uiso 1 1 calc R . . H81B H 1.2217 0.5838 0.6736 0.078 Uiso 1 1 calc R . . O82 O 1.2887(3) 0.4729(3) 0.7388(3) 0.0779(15) Uani 1 1 d . . . C83 C 1.2601(5) 0.3870(4) 0.7943(5) 0.074(2) Uani 1 1 d . . . H83A H 1.3196 0.3495 0.8105 0.089 Uiso 1 1 calc R . . H83B H 1.2246 0.3485 0.772 0.089 Uiso 1 1 calc R . . C84 C 1.1952(4) 0.4052(4) 0.8620(4) 0.0532(15) Uani 1 1 d . . . H84A H 1.1779 0.3435 0.8999 0.064 Uiso 1 1 calc R . . H84B H 1.231 0.4421 0.8854 0.064 Uiso 1 1 calc R . . O85 O 1.0652(3) 0.2427(2) 0.8434(2) 0.0508(9) Uani 1 1 d . . . C86 C 1.0117(4) 0.1790(4) 0.8898(3) 0.0452(12) Uani 1 1 d . . . C87 C 1.0500(5) 0.0766(4) 0.8972(4) 0.0666(18) Uani 1 1 d . . . H87A H 1.1127 0.0769 0.8634 0.1 Uiso 1 1 calc R . . H87B H 1.0021 0.0414 0.8832 0.1 Uiso 1 1 calc R . . H87C H 1.0598 0.0457 0.9495 0.1 Uiso 1 1 calc R . . O88 O 0.9329(3) 0.1935(3) 0.9281(2) 0.0512(9) Uani 1 1 d . . . O89 O 0.8882(2) 0.3968(2) 0.87852(19) 0.0348(7) Uani 1 1 d . . . O91 O 0.7704(3) 0.2015(3) 1.0529(2) 0.0551(10) Uani 1 1 d . . . C92 C 0.8142(4) 0.2452(4) 1.0874(3) 0.0482(13) Uani 1 1 d . . . C93 C 0.8164(6) 0.1996(6) 1.1705(4) 0.079(2) Uani 1 1 d . . . H93A H 0.7824 0.139 1.1867 0.119 Uiso 1 1 calc R . . H93B H 0.7834 0.2426 1.1994 0.119 Uiso 1 1 calc R . . H93C H 0.8849 0.1875 1.1794 0.119 Uiso 1 1 calc R . . O94 O 0.8517(3) 0.3230(3) 1.0548(3) 0.0624(11) Uani 1 1 d . . . O101 O 0.1220(8) 0.2135(7) 0.4539(6) 0.168(3) Uiso 1 1 d . . . C102 C 0.0529(10) 0.2858(9) 0.4671(8) 0.144(4) Uiso 1 1 d . . . H10A H -0.0071 0.2577 0.5008 0.173 Uiso 1 1 calc R . . H10B H 0.0813 0.3283 0.4903 0.173 Uiso 1 1 calc R . . C103 C 0.0315(10) 0.3362(9) 0.3950(7) 0.140(4) Uiso 1 1 d . . . H10C H 0.0578 0.4011 0.381 0.167 Uiso 1 1 calc R . . H10D H -0.0408 0.3433 0.3971 0.167 Uiso 1 1 calc R . . C104 C 0.0727(7) 0.2896(7) 0.3356(5) 0.105(3) Uani 1 1 d . . . H10E H 0.1198 0.3308 0.2957 0.126 Uiso 1 1 calc R . . H10F H 0.0204 0.272 0.3123 0.126 Uiso 1 1 calc R . . C105 C 0.1251(7) 0.2001(6) 0.3822(5) 0.088(2) Uani 1 1 d . . . H10G H 0.0907 0.1415 0.3862 0.105 Uiso 1 1 calc R . . H10H H 0.1941 0.194 0.3581 0.105 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 0.0410(3) 0.0376(3) 0.0424(3) -0.0146(3) -0.0053(3) -0.0047(2) Zn2 0.0459(4) 0.0409(3) 0.0580(4) -0.0271(3) -0.0092(3) 0.0066(3) Zn3 0.0471(4) 0.0379(3) 0.0426(3) -0.0191(3) -0.0080(3) -0.0018(3) Zn4 0.0361(3) 0.0334(3) 0.0468(3) -0.0166(3) 0.0008(3) -0.0018(2) Zn5 0.0434(3) 0.0349(3) 0.0419(3) -0.0152(2) 0.0015(3) -0.0093(2) N1 0.045(3) 0.041(2) 0.034(2) -0.0110(18) -0.0076(19) -0.0004(18) C2 0.054(3) 0.050(3) 0.048(3) -0.024(3) -0.014(3) 0.010(3) C3 0.062(4) 0.077(4) 0.051(4) -0.035(3) 0.001(3) 0.004(3) O4 0.072(3) 0.089(3) 0.048(3) -0.034(2) 0.011(2) -0.012(3) C5 0.072(4) 0.062(4) 0.041(3) -0.013(3) -0.001(3) -0.017(3) C6 0.060(4) 0.045(3) 0.037(3) -0.009(2) -0.013(3) -0.006(2) C7 0.051(3) 0.031(2) 0.042(3) -0.007(2) -0.019(2) -0.007(2) C8 0.040(3) 0.031(2) 0.046(3) -0.014(2) -0.011(2) -0.001(2) C9 0.046(3) 0.033(2) 0.047(3) -0.016(2) -0.010(2) -0.004(2) C10 0.046(3) 0.027(2) 0.052(3) -0.016(2) -0.014(2) 0.001(2) C11 0.062(4) 0.025(2) 0.057(3) -0.012(2) -0.017(3) -0.002(2) C12 0.115(7) 0.049(4) 0.126(8) -0.040(4) 0.032(6) -0.032(4) C14 0.178(9) 0.040(3) 0.078(5) -0.023(3) -0.028(6) -0.028(4) C15 0.117(7) 0.036(3) 0.215(11) -0.029(5) -0.104(8) 0.009(4) C16 0.046(3) 0.032(2) 0.044(3) -0.012(2) -0.008(2) 0.003(2) C17 0.046(3) 0.035(2) 0.048(3) -0.016(2) -0.019(2) 0.008(2) C18 0.037(3) 0.027(2) 0.044(3) -0.016(2) -0.007(2) 0.0018(18) O19 0.045(2) 0.0311(16) 0.049(2) -0.0206(15) -0.0035(16) -0.0057(14) C20 0.048(3) 0.033(2) 0.035(3) -0.012(2) -0.008(2) 0.001(2) N21 0.040(2) 0.041(2) 0.047(3) -0.017(2) -0.001(2) -0.0068(18) C22 0.047(3) 0.044(3) 0.065(4) -0.020(3) 0.002(3) -0.010(2) C23 0.045(4) 0.071(4) 0.077(5) -0.026(4) 0.012(3) -0.010(3) O24 0.069(3) 0.059(2) 0.063(3) -0.020(2) 0.027(2) -0.010(2) C25 0.074(4) 0.043(3) 0.054(4) -0.020(3) 0.009(3) -0.003(3) C26 0.062(4) 0.038(3) 0.044(3) -0.015(2) 0.002(3) -0.006(2) O31 0.049(2) 0.052(2) 0.063(3) -0.019(2) -0.010(2) -0.0066(18) C32 0.050(3) 0.061(4) 0.054(4) -0.021(3) -0.012(3) -0.004(3) O33 0.099(4) 0.090(3) 0.090(4) -0.059(3) -0.043(3) 0.033(3) C34 0.074(5) 0.095(6) 0.122(7) -0.046(5) -0.050(5) 0.021(4) O35 0.052(2) 0.0272(16) 0.046(2) -0.0129(15) -0.0022(17) -0.0016(15) C36 0.048(3) 0.032(2) 0.047(3) -0.014(2) 0.003(2) -0.001(2) O37 0.052(2) 0.0396(19) 0.071(3) -0.0238(19) -0.014(2) -0.0052(17) C38 0.055(4) 0.036(3) 0.086(5) -0.017(3) -0.012(3) 0.002(2) O41 0.095(4) 0.048(2) 0.069(3) -0.007(2) -0.006(3) -0.004(2) C42 0.104(6) 0.065(4) 0.046(4) -0.025(3) -0.018(4) 0.009(4) C43 0.140(8) 0.041(3) 0.062(5) -0.007(3) 0.009(5) 0.015(4) O44 0.100(4) 0.050(2) 0.058(3) -0.018(2) -0.004(3) 0.006(2) O45 0.050(2) 0.058(2) 0.049(2) -0.0335(19) -0.0146(18) 0.0091(18) C46 0.045(3) 0.058(3) 0.042(3) -0.025(3) -0.006(2) 0.000(3) C47 0.057(4) 0.079(4) 0.059(4) -0.039(3) -0.017(3) 0.015(3) O48 0.046(2) 0.051(2) 0.046(2) -0.0249(18) -0.0120(17) 0.0048(17) O51 0.061(2) 0.0426(19) 0.044(2) -0.0209(17) -0.0051(18) -0.0043(17) C52 0.041(3) 0.039(3) 0.044(3) -0.017(2) -0.005(2) -0.003(2) C53 0.083(4) 0.032(3) 0.049(3) -0.013(2) -0.013(3) -0.002(3) O54 0.044(2) 0.0301(16) 0.044(2) -0.0145(15) -0.0039(16) -0.0058(14) O55 0.054(2) 0.050(2) 0.036(2) -0.0125(17) -0.0047(17) -0.0102(17) C56 0.070(4) 0.052(3) 0.041(3) -0.014(3) -0.007(3) -0.012(3) C57 0.145(8) 0.086(5) 0.047(4) 0.000(4) -0.025(4) -0.052(5) O58 0.062(3) 0.058(2) 0.049(2) -0.0156(19) -0.0021(19) -0.020(2) N61 0.032(2) 0.044(2) 0.058(3) -0.029(2) 0.009(2) -0.0091(18) C62 0.031(3) 0.052(3) 0.084(4) -0.035(3) 0.003(3) -0.011(2) C63 0.046(4) 0.063(4) 0.099(6) -0.029(4) 0.015(4) -0.016(3) O64 0.052(3) 0.075(3) 0.097(4) -0.033(3) 0.031(3) -0.011(2) C65 0.072(5) 0.072(4) 0.067(4) -0.033(4) 0.019(4) 0.002(4) C66 0.051(3) 0.050(3) 0.058(4) -0.030(3) 0.006(3) 0.000(3) C67 0.032(3) 0.039(2) 0.051(3) -0.021(2) -0.003(2) -0.008(2) C68 0.035(3) 0.031(2) 0.044(3) -0.017(2) -0.003(2) -0.0018(19) C69 0.032(3) 0.037(2) 0.053(3) -0.019(2) -0.007(2) -0.001(2) C70 0.036(3) 0.029(2) 0.058(3) -0.020(2) -0.005(2) 0.0010(19) C71 0.038(3) 0.034(3) 0.096(5) -0.034(3) -0.009(3) 0.000(2) C72 0.060(4) 0.043(3) 0.108(6) -0.042(4) -0.005(4) 0.006(3) C73 0.064(4) 0.061(4) 0.188(10) -0.078(5) -0.038(5) 0.003(3) C74 0.074(5) 0.035(3) 0.113(6) -0.005(4) 0.004(4) 0.005(3) C75 0.042(3) 0.033(2) 0.061(3) -0.019(2) -0.018(3) -0.005(2) C76 0.035(3) 0.034(2) 0.045(3) -0.019(2) -0.005(2) -0.0033(19) C77 0.034(3) 0.030(2) 0.038(3) -0.012(2) -0.001(2) -0.0066(18) C78 0.038(3) 0.034(2) 0.054(3) -0.019(2) -0.018(2) 0.004(2) N79 0.031(2) 0.034(2) 0.059(3) -0.016(2) -0.008(2) 0.0046(17) C80 0.040(3) 0.035(3) 0.072(4) -0.014(3) 0.003(3) -0.010(2) C81 0.052(4) 0.051(3) 0.081(5) -0.019(3) 0.021(3) -0.007(3) O82 0.037(2) 0.052(2) 0.131(5) -0.022(3) 0.020(3) -0.0043(19) C83 0.040(3) 0.047(3) 0.128(7) -0.026(4) 0.003(4) 0.013(3) C84 0.030(3) 0.043(3) 0.088(5) -0.017(3) -0.016(3) 0.007(2) O85 0.041(2) 0.0351(18) 0.074(3) -0.0154(19) -0.0023(19) -0.0017(16) C86 0.037(3) 0.039(3) 0.056(3) -0.008(2) -0.008(3) 0.002(2) C87 0.056(4) 0.034(3) 0.099(5) -0.013(3) 0.003(4) 0.005(3) O88 0.045(2) 0.042(2) 0.060(2) -0.0113(18) 0.0001(19) 0.0037(16) O89 0.0344(18) 0.0290(15) 0.0440(19) -0.0174(14) -0.0005(15) -0.0028(13) O91 0.060(3) 0.065(2) 0.050(2) -0.030(2) -0.0071(19) -0.014(2) C92 0.051(3) 0.054(3) 0.042(3) -0.016(3) -0.006(3) -0.014(3) C93 0.108(6) 0.090(5) 0.043(4) -0.016(4) -0.009(4) -0.036(5) O94 0.063(3) 0.062(3) 0.063(3) -0.010(2) -0.015(2) -0.017(2) C104 0.078(6) 0.109(7) 0.097(7) 0.025(6) -0.020(5) -0.006(5) C105 0.093(6) 0.076(5) 0.088(6) -0.006(4) -0.035(5) 0.012(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 O44 1.941(4) . ? Zn1 O19 1.977(4) . ? Zn1 O45 2.015(4) . ? Zn1 N1 2.108(4) . ? Zn2 O31 1.957(4) . ? Zn2 O19 1.964(3) . ? Zn2 O35 2.017(3) . ? Zn2 N21 2.259(4) . ? Zn2 O41 2.448(5) . ? Zn3 O37 1.967(4) . ? Zn3 O55 1.987(4) . ? Zn3 O48 1.987(3) . ? Zn3 O51 1.992(4) . ? Zn3 C52 2.595(5) . ? Zn4 O85 1.911(3) . ? Zn4 O89 1.961(3) . ? Zn4 O58 1.985(4) . ? Zn4 N79 2.106(4) . ? Zn5 O89 1.987(3) . ? Zn5 O54 2.033(3) . ? Zn5 O91 2.042(4) . ? Zn5 O88 2.261(4) . ? Zn5 N61 2.299(4) . ? Zn5 O94 2.379(4) . ? Zn5 C92 2.534(6) . ? N1 C6 1.480(7) . ? N1 C2 1.483(6) . ? N1 C7 1.510(7) . ? C2 C3 1.514(9) . ? C2 H2A 0.99 . ? C2 H2B 0.99 . ? C3 O4 1.422(8) . ? C3 H3A 0.99 . ? C3 H3B 0.99 . ? O4 C5 1.410(8) . ? C5 C6 1.522(8) . ? C5 H5A 0.99 . ? C5 H5B 0.99 . ? C6 H6A 0.99 . ? C6 H6B 0.99 . ? C7 C8 1.487(7) . ? C7 H7A 0.99 . ? C7 H7B 0.99 . ? C8 C9 1.390(6) . ? C8 C18 1.396(7) . ? C9 C10 1.396(7) . ? C9 H9A 0.99 . ? C9 H9B 0.99 . ? C10 C16 1.391(7) . ? C10 C11 1.540(6) . ? C11 C12 1.493(10) . ? C11 C15 1.493(9) . ? C11 C14 1.504(9) . ? C12 H12A 0.98 . ? C12 H12B 0.98 . ? C12 H12C 0.98 . ? C14 H14A 0.98 . ? C14 H14B 0.98 . ? C14 H14C 0.98 . ? C15 H15A 0.98 . ? C15 H15B 0.98 . ? C15 H15C 0.98 . ? C16 C17 1.418(6) . ? C16 H16A 0.99 . ? C16 H16B 0.99 . ? C17 C18 1.376(7) . ? C17 C20 1.502(7) . ? C18 O19 1.369(5) . ? C20 N21 1.489(6) . ? C20 H20A 0.99 . ? C20 H20B 0.99 . ? N21 C26 1.476(7) . ? N21 C22 1.483(7) . ? C22 C23 1.513(8) . ? C22 H22A 0.99 . ? C22 H22B 0.99 . ? C23 O24 1.410(8) . ? C23 H23A 0.99 . ? C23 H23B 0.99 . ? O24 C25 1.437(8) . ? C25 C26 1.496(8) . ? C25 H25A 0.99 . ? C25 H25B 0.99 . ? C26 H26A 0.99 . ? C26 H26B 0.99 . ? O31 C32 1.262(7) . ? C32 O33 1.227(7) . ? C32 C34 1.495(9) . ? C34 H34A 0.98 . ? C34 H34B 0.98 . ? C34 H34C 0.98 . ? O35 C36 1.265(6) . ? C36 O37 1.260(6) . ? C36 C38 1.494(7) . ? C38 H38A 0.98 . ? C38 H38B 0.98 . ? C38 H38C 0.98 . ? O41 C42 1.237(9) . ? C42 O44 1.254(8) . ? C42 C43 1.540(9) . ? C43 H43A 0.98 . ? C43 H43B 0.98 . ? C43 H43C 0.98 . ? O45 C46 1.266(6) . ? C46 O48 1.264(6) . ? C46 C47 1.509(8) . ? C47 H47A 0.98 . ? C47 H47B 0.98 . ? C47 H47C 0.98 . ? O51 C52 1.250(6) . ? C52 O54 1.271(5) . ? C52 C53 1.495(8) . ? C53 H53A 0.98 . ? C53 H53B 0.98 . ? C53 H53C 0.98 . ? O55 C56 1.253(7) . ? C56 O58 1.266(7) . ? C56 C57 1.514(9) . ? C57 H57A 0.98 . ? C57 H57B 0.98 . ? C57 H57C 0.98 . ? N61 C67 1.493(7) . ? N61 C62 1.497(6) . ? N61 C66 1.501(6) . ? C62 C63 1.496(9) . ? C62 H62A 0.99 . ? C62 H62B 0.99 . ? C63 O64 1.445(8) . ? C63 H63A 0.99 . ? C63 H63B 0.99 . ? O64 C65 1.426(9) . ? C65 C66 1.495(9) . ? C65 H65A 0.99 . ? C65 H65B 0.99 . ? C66 H66A 0.99 . ? C66 H66B 0.99 . ? C67 C68 1.503(6) . ? C67 H67A 0.99 . ? C67 H67B 0.99 . ? C68 C77 1.386(7) . ? C68 C69 1.392(6) . ? C69 C70 1.406(7) . ? C69 H69 0.95 . ? C70 C75 1.384(7) . ? C70 C71 1.534(6) . ? C71 C72 1.520(9) . ? C71 C73 1.528(8) . ? C71 C74 1.538(10) . ? C72 H72A 0.98 . ? C72 H72B 0.98 . ? C72 H72C 0.98 . ? C73 H73A 0.98 . ? C73 H73B 0.98 . ? C73 H73C 0.98 . ? C74 H74A 0.98 . ? C74 H74B 0.98 . ? C74 H74C 0.98 . ? C75 C76 1.415(6) . ? C75 H75 0.95 . ? C76 C77 1.393(6) . ? C76 C78 1.494(7) . ? C77 O89 1.363(5) . ? C78 N79 1.502(7) . ? C78 H78A 0.99 . ? C78 H78B 0.99 . ? N79 C80 1.488(7) . ? N79 C84 1.496(6) . ? C80 C81 1.523(8) . ? C80 H80A 0.99 . ? C80 H80B 0.99 . ? C81 O82 1.430(8) . ? C81 H81A 0.99 . ? C81 H81B 0.99 . ? O82 C83 1.413(8) . ? C83 C84 1.498(9) . ? C83 H83A 0.99 . ? C83 H83B 0.99 . ? C84 H84A 0.99 . ? C84 H84B 0.99 . ? O85 C86 1.262(7) . ? C86 O88 1.235(7) . ? C86 C87 1.522(7) . ? C87 H87A 0.98 . ? C87 H87B 0.98 . ? C87 H87C 0.98 . ? O91 C92 1.273(6) . ? C92 O94 1.233(7) . ? C92 C93 1.507(8) . ? C93 H93A 0.98 . ? C93 H93B 0.98 . ? C93 H93C 0.98 . ? O101 C105 1.402(12) . ? O101 C102 1.413(14) . ? C102 C103 1.404(15) . ? C102 H10A 0.99 . ? C102 H10B 0.99 . ? C103 C104 1.477(14) . ? C103 H10C 0.99 . ? C103 H10D 0.99 . ? C104 C105 1.548(10) . ? C104 H10E 0.99 . ? C104 H10F 0.99 . ? C105 H10G 0.99 . ? C105 H10H 0.99 . ? 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 O44 Zn1 O19 122.26(18) . . ? O44 Zn1 O45 119.7(2) . . ? O19 Zn1 O45 106.33(16) . . ? O44 Zn1 N1 104.40(18) . . ? O19 Zn1 N1 98.02(15) . . ? O45 Zn1 N1 101.57(15) . . ? O31 Zn2 O19 141.10(16) . . ? O31 Zn2 O35 105.09(15) . . ? O19 Zn2 O35 107.85(14) . . ? O31 Zn2 N21 107.01(17) . . ? O19 Zn2 N21 92.16(15) . . ? O35 Zn2 N21 91.77(14) . . ? O31 Zn2 O41 87.02(17) . . ? O19 Zn2 O41 79.83(15) . . ? O35 Zn2 O41 78.61(16) . . ? N21 Zn2 O41 164.79(17) . . ? O37 Zn3 O55 99.98(15) . . ? O37 Zn3 O48 108.08(16) . . ? O55 Zn3 O48 103.63(15) . . ? O37 Zn3 O51 133.51(17) . . ? O55 Zn3 O51 110.81(15) . . ? O48 Zn3 O51 97.74(15) . . ? O37 Zn3 C52 115.74(17) . . ? O55 Zn3 C52 99.08(15) . . ? O48 Zn3 C52 125.55(15) . . ? O51 Zn3 C52 27.85(14) . . ? O85 Zn4 O89 116.89(16) . . ? O85 Zn4 O58 115.58(18) . . ? O89 Zn4 O58 111.27(16) . . ? O85 Zn4 N79 107.10(16) . . ? O89 Zn4 N79 98.48(15) . . ? O58 Zn4 N79 105.22(17) . . ? O89 Zn5 O54 107.87(13) . . ? O89 Zn5 O91 147.74(14) . . ? O54 Zn5 O91 102.25(14) . . ? O89 Zn5 O88 85.62(13) . . ? O54 Zn5 O88 82.42(14) . . ? O91 Zn5 O88 87.14(16) . . ? O89 Zn5 N61 90.08(14) . . ? O54 Zn5 N61 87.80(14) . . ? O91 Zn5 N61 102.53(17) . . ? O88 Zn5 N61 167.54(15) . . ? O89 Zn5 O94 90.75(14) . . ? O54 Zn5 O94 160.96(14) . . ? O91 Zn5 O94 58.71(14) . . ? O88 Zn5 O94 95.39(15) . . ? N61 Zn5 O94 96.36(16) . . ? O89 Zn5 C92 118.67(16) . . ? O54 Zn5 C92 132.12(16) . . ? O91 Zn5 C92 29.92(15) . . ? O88 Zn5 C92 90.13(17) . . ? N61 Zn5 C92 102.18(18) . . ? O94 Zn5 C92 28.85(15) . . ? C6 N1 C2 107.8(4) . . ? C6 N1 C7 108.6(4) . . ? C2 N1 C7 109.4(4) . . ? C6 N1 Zn1 112.1(3) . . ? C2 N1 Zn1 114.9(3) . . ? C7 N1 Zn1 103.9(3) . . ? N1 C2 C3 111.2(5) . . ? N1 C2 H2A 109.4 . . ? C3 C2 H2A 109.4 . . ? N1 C2 H2B 109.4 . . ? C3 C2 H2B 109.4 . . ? H2A C2 H2B 108 . . ? O4 C3 C2 111.3(5) . . ? O4 C3 H3A 109.4 . . ? C2 C3 H3A 109.4 . . ? O4 C3 H3B 109.4 . . ? C2 C3 H3B 109.4 . . ? H3A C3 H3B 108 . . ? C5 O4 C3 109.0(4) . . ? O4 C5 C6 111.5(5) . . ? O4 C5 H5A 109.3 . . ? C6 C5 H5A 109.3 . . ? O4 C5 H5B 109.3 . . ? C6 C5 H5B 109.3 . . ? H5A C5 H5B 108 . . ? N1 C6 C5 110.4(4) . . ? N1 C6 H6A 109.6 . . ? C5 C6 H6A 109.6 . . ? N1 C6 H6B 109.6 . . ? C5 C6 H6B 109.6 . . ? H6A C6 H6B 108.1 . . ? C8 C7 N1 113.7(4) . . ? C8 C7 H7A 108.8 . . ? N1 C7 H7A 108.8 . . ? C8 C7 H7B 108.8 . . ? N1 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? C9 C8 C18 118.6(5) . . ? C9 C8 C7 120.7(4) . . ? C18 C8 C7 120.6(4) . . ? C8 C9 C10 122.8(5) . . ? C8 C9 H9A 106.6 . . ? C10 C9 H9A 106.6 . . ? C8 C9 H9B 106.6 . . ? C10 C9 H9B 106.6 . . ? H9A C9 H9B 106.6 . . ? C16 C10 C9 116.8(4) . . ? C16 C10 C11 120.7(5) . . ? C9 C10 C11 122.5(4) . . ? C12 C11 C15 109.7(7) . . ? C12 C11 C14 107.9(6) . . ? C15 C11 C14 109.2(7) . . ? C12 C11 C10 109.4(5) . . ? C15 C11 C10 108.6(5) . . ? C14 C11 C10 112.0(5) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 C15 H15A 109.5 . . ? C11 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C11 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C10 C16 C17 122.1(5) . . ? C10 C16 H16A 106.8 . . ? C17 C16 H16A 106.8 . . ? C10 C16 H16B 106.8 . . ? C17 C16 H16B 106.8 . . ? H16A C16 H16B 106.6 . . ? C18 C17 C16 118.4(4) . . ? C18 C17 C20 119.4(4) . . ? C16 C17 C20 122.2(5) . . ? O19 C18 C17 119.6(4) . . ? O19 C18 C8 119.1(4) . . ? C17 C18 C8 121.3(4) . . ? C18 O19 Zn2 119.5(3) . . ? C18 O19 Zn1 116.6(3) . . ? Zn2 O19 Zn1 123.53(16) . . ? N21 C20 C17 113.6(4) . . ? N21 C20 H20A 108.8 . . ? C17 C20 H20A 108.8 . . ? N21 C20 H20B 108.8 . . ? C17 C20 H20B 108.8 . . ? H20A C20 H20B 107.7 . . ? C26 N21 C22 106.9(4) . . ? C26 N21 C20 107.4(4) . . ? C22 N21 C20 110.0(4) . . ? C26 N21 Zn2 111.5(3) . . ? C22 N21 Zn2 116.1(3) . . ? C20 N21 Zn2 104.6(3) . . ? N21 C22 C23 111.7(4) . . ? N21 C22 H22A 109.3 . . ? C23 C22 H22A 109.3 . . ? N21 C22 H22B 109.3 . . ? C23 C22 H22B 109.3 . . ? H22A C22 H22B 107.9 . . ? O24 C23 C22 112.1(6) . . ? O24 C23 H23A 109.2 . . ? C22 C23 H23A 109.2 . . ? O24 C23 H23B 109.2 . . ? C22 C23 H23B 109.2 . . ? H23A C23 H23B 107.9 . . ? C23 O24 C25 109.4(5) . . ? O24 C25 C26 110.9(4) . . ? O24 C25 H25A 109.5 . . ? C26 C25 H25A 109.5 . . ? O24 C25 H25B 109.5 . . ? C26 C25 H25B 109.5 . . ? H25A C25 H25B 108 . . ? N21 C26 C25 111.5(5) . . ? N21 C26 H26A 109.3 . . ? C25 C26 H26A 109.3 . . ? N21 C26 H26B 109.3 . . ? C25 C26 H26B 109.3 . . ? H26A C26 H26B 108 . . ? C32 O31 Zn2 106.6(4) . . ? O33 C32 O31 120.7(6) . . ? O33 C32 C34 122.6(6) . . ? O31 C32 C34 116.6(6) . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 O35 Zn2 128.2(4) . . ? O37 C36 O35 119.9(5) . . ? O37 C36 C38 119.0(4) . . ? O35 C36 C38 121.0(5) . . ? C36 O37 Zn3 106.5(3) . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C42 O41 Zn2 152.1(5) . . ? O41 C42 O44 125.9(7) . . ? O41 C42 C43 119.3(7) . . ? O44 C42 C43 114.7(7) . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C42 O44 Zn1 111.4(5) . . ? C46 O45 Zn1 105.1(3) . . ? O48 C46 O45 119.2(5) . . ? O48 C46 C47 121.0(5) . . ? O45 C46 C47 119.7(5) . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C46 O48 Zn3 128.7(3) . . ? C52 O51 Zn3 104.0(3) . . ? O51 C52 O54 119.6(5) . . ? O51 C52 C53 119.8(4) . . ? O54 C52 C53 120.4(5) . . ? O51 C52 Zn3 48.1(3) . . ? O54 C52 Zn3 71.5(3) . . ? C53 C52 Zn3 167.9(3) . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C52 O54 Zn5 127.3(3) . . ? C56 O55 Zn3 130.2(4) . . ? O55 C56 O58 120.4(5) . . ? O55 C56 C57 120.4(5) . . ? O58 C56 C57 119.1(6) . . ? C56 C57 H57A 109.5 . . ? C56 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C56 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C56 O58 Zn4 107.3(4) . . ? C67 N61 C62 106.6(4) . . ? C67 N61 C66 108.6(4) . . ? C62 N61 C66 107.3(4) . . ? C67 N61 Zn5 105.2(3) . . ? C62 N61 Zn5 112.7(3) . . ? C66 N61 Zn5 115.9(3) . . ? C63 C62 N61 110.5(5) . . ? C63 C62 H62A 109.5 . . ? N61 C62 H62A 109.5 . . ? C63 C62 H62B 109.5 . . ? N61 C62 H62B 109.5 . . ? H62A C62 H62B 108.1 . . ? O64 C63 C62 110.9(5) . . ? O64 C63 H63A 109.5 . . ? C62 C63 H63A 109.5 . . ? O64 C63 H63B 109.5 . . ? C62 C63 H63B 109.5 . . ? H63A C63 H63B 108.1 . . ? C65 O64 C63 108.3(5) . . ? O64 C65 C66 113.8(6) . . ? O64 C65 H65A 108.8 . . ? C66 C65 H65A 108.8 . . ? O64 C65 H65B 108.8 . . ? C66 C65 H65B 108.8 . . ? H65A C65 H65B 107.7 . . ? C65 C66 N61 112.0(5) . . ? C65 C66 H66A 109.2 . . ? N61 C66 H66A 109.2 . . ? C65 C66 H66B 109.2 . . ? N61 C66 H66B 109.2 . . ? H66A C66 H66B 107.9 . . ? N61 C67 C68 112.1(4) . . ? N61 C67 H67A 109.2 . . ? C68 C67 H67A 109.2 . . ? N61 C67 H67B 109.2 . . ? C68 C67 H67B 109.2 . . ? H67A C67 H67B 107.9 . . ? C77 C68 C69 119.1(4) . . ? C77 C68 C67 119.6(4) . . ? C69 C68 C67 121.3(4) . . ? C68 C69 C70 122.6(4) . . ? C68 C69 H69 118.7 . . ? C70 C69 H69 118.7 . . ? C75 C70 C69 116.8(4) . . ? C75 C70 C71 122.5(4) . . ? C69 C70 C71 120.6(4) . . ? C72 C71 C73 109.2(6) . . ? C72 C71 C70 110.4(5) . . ? C73 C71 C70 111.9(5) . . ? C72 C71 C74 108.3(5) . . ? C73 C71 C74 108.4(6) . . ? C70 C71 C74 108.7(5) . . ? C71 C72 H72A 109.5 . . ? C71 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C71 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C71 C73 H73A 109.5 . . ? C71 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C71 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? C71 C74 H74A 109.5 . . ? C71 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C71 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? C70 C75 C76 122.1(4) . . ? C70 C75 H75 118.9 . . ? C76 C75 H75 118.9 . . ? C77 C76 C75 118.7(4) . . ? C77 C76 C78 120.4(4) . . ? C75 C76 C78 120.8(4) . . ? O89 C77 C68 119.8(4) . . ? O89 C77 C76 119.5(4) . . ? C68 C77 C76 120.6(4) . . ? C76 C78 N79 113.9(4) . . ? C76 C78 H78A 108.8 . . ? N79 C78 H78A 108.8 . . ? C76 C78 H78B 108.8 . . ? N79 C78 H78B 108.8 . . ? H78A C78 H78B 107.7 . . ? C80 N79 C84 107.5(4) . . ? C80 N79 C78 109.9(4) . . ? C84 N79 C78 108.9(4) . . ? C80 N79 Zn4 116.4(3) . . ? C84 N79 Zn4 110.1(3) . . ? C78 N79 Zn4 103.9(3) . . ? N79 C80 C81 111.4(4) . . ? N79 C80 H80A 109.4 . . ? C81 C80 H80A 109.4 . . ? N79 C80 H80B 109.4 . . ? C81 C80 H80B 109.4 . . ? H80A C80 H80B 108 . . ? O82 C81 C80 110.7(6) . . ? O82 C81 H81A 109.5 . . ? C80 C81 H81A 109.5 . . ? O82 C81 H81B 109.5 . . ? C80 C81 H81B 109.5 . . ? H81A C81 H81B 108.1 . . ? C83 O82 C81 108.6(5) . . ? O82 C83 C84 112.0(5) . . ? O82 C83 H83A 109.2 . . ? C84 C83 H83A 109.2 . . ? O82 C83 H83B 109.2 . . ? C84 C83 H83B 109.2 . . ? H83A C83 H83B 107.9 . . ? N79 C84 C83 110.6(5) . . ? N79 C84 H84A 109.5 . . ? C83 C84 H84A 109.5 . . ? N79 C84 H84B 109.5 . . ? C83 C84 H84B 109.5 . . ? H84A C84 H84B 108.1 . . ? C86 O85 Zn4 117.4(3) . . ? O88 C86 O85 125.6(5) . . ? O88 C86 C87 119.2(5) . . ? O85 C86 C87 115.3(5) . . ? C86 C87 H87A 109.5 . . ? C86 C87 H87B 109.5 . . ? H87A C87 H87B 109.5 . . ? C86 C87 H87C 109.5 . . ? H87A C87 H87C 109.5 . . ? H87B C87 H87C 109.5 . . ? C86 O88 Zn5 148.8(4) . . ? C77 O89 Zn4 116.2(3) . . ? C77 O89 Zn5 121.0(3) . . ? Zn4 O89 Zn5 122.11(15) . . ? C92 O91 Zn5 96.9(3) . . ? O94 C92 O91 121.5(5) . . ? O94 C92 C93 120.9(5) . . ? O91 C92 C93 117.5(5) . . ? O94 C92 Zn5 68.6(3) . . ? O91 C92 Zn5 53.1(3) . . ? C93 C92 Zn5 170.1(4) . . ? C92 C93 H93A 109.5 . . ? C92 C93 H93B 109.5 . . ? H93A C93 H93B 109.5 . . ? C92 C93 H93C 109.5 . . ? H93A C93 H93C 109.5 . . ? H93B C93 H93C 109.5 . . ? C92 O94 Zn5 82.5(3) . . ? C105 O101 C102 112.7(10) . . ? C103 C102 O101 104.4(12) . . ? C103 C102 H10A 110.9 . . ? O101 C102 H10A 110.9 . . ? C103 C102 H10B 110.9 . . ? O101 C102 H10B 110.9 . . ? H10A C102 H10B 108.9 . . ? C102 C103 C104 113.6(11) . . ? C102 C103 H10C 108.8 . . ? C104 C103 H10C 108.8 . . ? C102 C103 H10D 108.8 . . ? C104 C103 H10D 108.8 . . ? H10C C103 H10D 107.7 . . ? C103 C104 C105 100.9(8) . . ? C103 C104 H10E 111.6 . . ? C105 C104 H10E 111.6 . . ? C103 C104 H10F 111.6 . . ? C105 C104 H10F 111.6 . . ? H10E C104 H10F 109.4 . . ? O101 C105 C104 105.9(8) . . ? O101 C105 H10G 110.6 . . ? C104 C105 H10G 110.6 . . ? O101 C105 H10H 110.6 . . ? C104 C105 H10H 110.6 . . ? H10G C105 H10H 108.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O44 Zn1 N1 C6 4.9(4) . . . . ? O19 Zn1 N1 C6 131.2(3) . . . . ? O45 Zn1 N1 C6 -120.2(4) . . . . ? O44 Zn1 N1 C2 128.3(4) . . . . ? O19 Zn1 N1 C2 -105.3(4) . . . . ? O45 Zn1 N1 C2 3.2(4) . . . . ? O44 Zn1 N1 C7 -112.2(3) . . . . ? O19 Zn1 N1 C7 14.2(3) . . . . ? O45 Zn1 N1 C7 122.8(3) . . . . ? C6 N1 C2 C3 54.9(5) . . . . ? C7 N1 C2 C3 172.8(4) . . . . ? Zn1 N1 C2 C3 -70.8(5) . . . . ? N1 C2 C3 O4 -58.4(6) . . . . ? C2 C3 O4 C5 59.8(6) . . . . ? C3 O4 C5 C6 -60.6(6) . . . . ? C2 N1 C6 C5 -55.1(6) . . . . ? C7 N1 C6 C5 -173.5(4) . . . . ? Zn1 N1 C6 C5 72.2(5) . . . . ? O4 C5 C6 N1 59.9(6) . . . . ? C6 N1 C7 C8 179.3(4) . . . . ? C2 N1 C7 C8 62.0(5) . . . . ? Zn1 N1 C7 C8 -61.2(4) . . . . ? N1 C7 C8 C9 -114.6(5) . . . . ? N1 C7 C8 C18 69.6(6) . . . . ? C18 C8 C9 C10 0.4(8) . . . . ? C7 C8 C9 C10 -175.6(5) . . . . ? C8 C9 C10 C16 0.6(8) . . . . ? C8 C9 C10 C11 -179.3(5) . . . . ? C16 C10 C11 C12 49.1(8) . . . . ? C9 C10 C11 C12 -131.1(7) . . . . ? C16 C10 C11 C15 -70.6(8) . . . . ? C9 C10 C11 C15 109.2(7) . . . . ? C16 C10 C11 C14 168.7(6) . . . . ? C9 C10 C11 C14 -11.5(8) . . . . ? C9 C10 C16 C17 -1.1(8) . . . . ? C11 C10 C16 C17 178.8(5) . . . . ? C10 C16 C17 C18 0.6(8) . . . . ? C10 C16 C17 C20 -177.8(5) . . . . ? C16 C17 C18 O19 -179.7(4) . . . . ? C20 C17 C18 O19 -1.2(7) . . . . ? C16 C17 C18 C8 0.4(8) . . . . ? C20 C17 C18 C8 178.8(5) . . . . ? C9 C8 C18 O19 179.2(4) . . . . ? C7 C8 C18 O19 -4.9(7) . . . . ? C9 C8 C18 C17 -0.9(7) . . . . ? C7 C8 C18 C17 175.1(5) . . . . ? C17 C18 O19 Zn2 -52.4(5) . . . . ? C8 C18 O19 Zn2 127.5(4) . . . . ? C17 C18 O19 Zn1 134.5(4) . . . . ? C8 C18 O19 Zn1 -45.5(5) . . . . ? O31 Zn2 O19 C18 -81.5(4) . . . . ? O35 Zn2 O19 C18 131.9(3) . . . . ? N21 Zn2 O19 C18 39.3(3) . . . . ? O41 Zn2 O19 C18 -153.7(4) . . . . ? O31 Zn2 O19 Zn1 91.0(3) . . . . ? O35 Zn2 O19 Zn1 -55.5(2) . . . . ? N21 Zn2 O19 Zn1 -148.1(2) . . . . ? O41 Zn2 O19 Zn1 18.9(2) . . . . ? O44 Zn1 O19 C18 149.2(3) . . . . ? O45 Zn1 O19 C18 -68.1(3) . . . . ? N1 Zn1 O19 C18 36.5(3) . . . . ? O44 Zn1 O19 Zn2 -23.6(3) . . . . ? O45 Zn1 O19 Zn2 119.1(2) . . . . ? N1 Zn1 O19 Zn2 -136.3(2) . . . . ? C18 C17 C20 N21 68.1(6) . . . . ? C16 C17 C20 N21 -113.5(5) . . . . ? C17 C20 N21 C26 179.1(4) . . . . ? C17 C20 N21 C22 63.1(6) . . . . ? C17 C20 N21 Zn2 -62.3(4) . . . . ? O31 Zn2 N21 C26 -83.9(4) . . . . ? O19 Zn2 N21 C26 130.5(3) . . . . ? O35 Zn2 N21 C26 22.5(4) . . . . ? O41 Zn2 N21 C26 72.8(7) . . . . ? O31 Zn2 N21 C22 38.9(4) . . . . ? O19 Zn2 N21 C22 -106.7(3) . . . . ? O35 Zn2 N21 C22 145.3(3) . . . . ? O41 Zn2 N21 C22 -164.4(5) . . . . ? O31 Zn2 N21 C20 160.4(3) . . . . ? O19 Zn2 N21 C20 14.7(3) . . . . ? O35 Zn2 N21 C20 -93.3(3) . . . . ? O41 Zn2 N21 C20 -43.0(7) . . . . ? C26 N21 C22 C23 54.4(6) . . . . ? C20 N21 C22 C23 170.7(5) . . . . ? Zn2 N21 C22 C23 -70.8(6) . . . . ? N21 C22 C23 O24 -57.3(7) . . . . ? C22 C23 O24 C25 57.8(7) . . . . ? C23 O24 C25 C26 -59.3(7) . . . . ? C22 N21 C26 C25 -56.5(6) . . . . ? C20 N21 C26 C25 -174.5(4) . . . . ? Zn2 N21 C26 C25 71.4(5) . . . . ? O24 C25 C26 N21 60.5(6) . . . . ? O19 Zn2 O31 C32 29.2(5) . . . . ? O35 Zn2 O31 C32 176.3(4) . . . . ? N21 Zn2 O31 C32 -87.0(4) . . . . ? O41 Zn2 O31 C32 99.0(4) . . . . ? Zn2 O31 C32 O33 4.2(8) . . . . ? Zn2 O31 C32 C34 -177.6(6) . . . . ? O31 Zn2 O35 C36 -46.6(5) . . . . ? O19 Zn2 O35 C36 112.4(4) . . . . ? N21 Zn2 O35 C36 -154.8(4) . . . . ? O41 Zn2 O35 C36 37.1(4) . . . . ? Zn2 O35 C36 O37 -140.9(4) . . . . ? Zn2 O35 C36 C38 43.0(7) . . . . ? O35 C36 O37 Zn3 3.4(6) . . . . ? C38 C36 O37 Zn3 179.6(4) . . . . ? O55 Zn3 O37 C36 176.5(4) . . . . ? O48 Zn3 O37 C36 68.5(4) . . . . ? O51 Zn3 O37 C36 -51.9(4) . . . . ? C52 Zn3 O37 C36 -78.3(4) . . . . ? O31 Zn2 O41 C42 -168.7(10) . . . . ? O19 Zn2 O41 C42 -25.5(10) . . . . ? O35 Zn2 O41 C42 85.2(10) . . . . ? N21 Zn2 O41 C42 33.6(14) . . . . ? Zn2 O41 C42 O44 19.3(15) . . . . ? Zn2 O41 C42 C43 -159.7(7) . . . . ? O41 C42 O44 Zn1 -6.0(9) . . . . ? C43 C42 O44 Zn1 173.0(5) . . . . ? O19 Zn1 O44 C42 10.5(5) . . . . ? O45 Zn1 O44 C42 -127.4(4) . . . . ? N1 Zn1 O44 C42 119.9(5) . . . . ? O44 Zn1 O45 C46 67.1(4) . . . . ? O19 Zn1 O45 C46 -76.7(4) . . . . ? N1 Zn1 O45 C46 -178.8(4) . . . . ? Zn1 O45 C46 O48 -3.8(6) . . . . ? Zn1 O45 C46 C47 178.5(5) . . . . ? O45 C46 O48 Zn3 162.3(4) . . . . ? C47 C46 O48 Zn3 -20.0(8) . . . . ? O37 Zn3 O48 C46 175.1(5) . . . . ? O55 Zn3 O48 C46 69.6(5) . . . . ? O51 Zn3 O48 C46 -44.1(5) . . . . ? C52 Zn3 O48 C46 -42.3(5) . . . . ? O37 Zn3 O51 C52 -59.0(4) . . . . ? O55 Zn3 O51 C52 69.0(4) . . . . ? O48 Zn3 O51 C52 176.9(3) . . . . ? Zn3 O51 C52 O54 1.9(6) . . . . ? Zn3 O51 C52 C53 178.4(4) . . . . ? O37 Zn3 C52 O51 136.4(3) . . . . ? O55 Zn3 C52 O51 -117.9(3) . . . . ? O48 Zn3 C52 O51 -3.8(4) . . . . ? O37 Zn3 C52 O54 -41.9(3) . . . . ? O55 Zn3 C52 O54 63.8(3) . . . . ? O48 Zn3 C52 O54 177.9(2) . . . . ? O51 Zn3 C52 O54 -178.3(5) . . . . ? O37 Zn3 C52 C53 129.5(19) . . . . ? O55 Zn3 C52 C53 -124.7(19) . . . . ? O48 Zn3 C52 C53 -11(2) . . . . ? O51 Zn3 C52 C53 -6.8(18) . . . . ? O51 C52 O54 Zn5 -138.7(4) . . . . ? C53 C52 O54 Zn5 44.8(7) . . . . ? Zn3 C52 O54 Zn5 -137.3(3) . . . . ? O89 Zn5 O54 C52 122.0(4) . . . . ? O91 Zn5 O54 C52 -46.3(4) . . . . ? O88 Zn5 O54 C52 39.1(4) . . . . ? N61 Zn5 O54 C52 -148.6(4) . . . . ? O94 Zn5 O54 C52 -45.4(7) . . . . ? C92 Zn5 O54 C52 -44.2(5) . . . . ? O37 Zn3 O55 C56 -49.6(5) . . . . ? O48 Zn3 O55 C56 61.9(5) . . . . ? O51 Zn3 O55 C56 165.8(5) . . . . ? C52 Zn3 O55 C56 -168.0(5) . . . . ? Zn3 O55 C56 O58 164.0(4) . . . . ? Zn3 O55 C56 C57 -14.3(9) . . . . ? O55 C56 O58 Zn4 -4.5(7) . . . . ? C57 C56 O58 Zn4 173.8(6) . . . . ? O85 Zn4 O58 C56 69.5(4) . . . . ? O89 Zn4 O58 C56 -66.9(4) . . . . ? N79 Zn4 O58 C56 -172.6(4) . . . . ? O89 Zn5 N61 C67 20.0(3) . . . . ? O54 Zn5 N61 C67 -87.8(3) . . . . ? O91 Zn5 N61 C67 170.1(3) . . . . ? O88 Zn5 N61 C67 -49.6(8) . . . . ? O94 Zn5 N61 C67 110.8(3) . . . . ? C92 Zn5 N61 C67 139.4(3) . . . . ? O89 Zn5 N61 C62 135.8(4) . . . . ? O54 Zn5 N61 C62 27.9(4) . . . . ? O91 Zn5 N61 C62 -74.1(4) . . . . ? O88 Zn5 N61 C62 66.1(8) . . . . ? O94 Zn5 N61 C62 -133.4(4) . . . . ? C92 Zn5 N61 C62 -104.8(4) . . . . ? O89 Zn5 N61 C66 -99.9(4) . . . . ? O54 Zn5 N61 C66 152.2(4) . . . . ? O91 Zn5 N61 C66 50.1(4) . . . . ? O88 Zn5 N61 C66 -169.6(6) . . . . ? O94 Zn5 N61 C66 -9.2(4) . . . . ? C92 Zn5 N61 C66 19.5(4) . . . . ? C67 N61 C62 C63 -172.6(4) . . . . ? C66 N61 C62 C63 -56.3(6) . . . . ? Zn5 N61 C62 C63 72.5(5) . . . . ? N61 C62 C63 O64 62.8(7) . . . . ? C62 C63 O64 C65 -60.8(7) . . . . ? C63 O64 C65 C66 57.3(7) . . . . ? O64 C65 C66 N61 -55.0(7) . . . . ? C67 N61 C66 C65 167.0(5) . . . . ? C62 N61 C66 C65 52.2(7) . . . . ? Zn5 N61 C66 C65 -74.8(6) . . . . ? C62 N61 C67 C68 174.3(4) . . . . ? C66 N61 C67 C68 59.0(5) . . . . ? Zn5 N61 C67 C68 -65.7(4) . . . . ? N61 C67 C68 C77 65.6(6) . . . . ? N61 C67 C68 C69 -112.2(5) . . . . ? C77 C68 C69 C70 -1.6(8) . . . . ? C67 C68 C69 C70 176.2(5) . . . . ? C68 C69 C70 C75 0.9(8) . . . . ? C68 C69 C70 C71 179.0(5) . . . . ? C75 C70 C71 C72 -137.7(6) . . . . ? C69 C70 C71 C72 44.3(8) . . . . ? C75 C70 C71 C73 -16.0(9) . . . . ? C69 C70 C71 C73 166.0(6) . . . . ? C75 C70 C71 C74 103.7(6) . . . . ? C69 C70 C71 C74 -74.3(7) . . . . ? C69 C70 C75 C76 -0.9(8) . . . . ? C71 C70 C75 C76 -179.0(5) . . . . ? C70 C75 C76 C77 1.7(8) . . . . ? C70 C75 C76 C78 -174.4(5) . . . . ? C69 C68 C77 O89 -179.1(5) . . . . ? C67 C68 C77 O89 3.0(7) . . . . ? C69 C68 C77 C76 2.4(8) . . . . ? C67 C68 C77 C76 -175.5(5) . . . . ? C75 C76 C77 O89 179.1(5) . . . . ? C78 C76 C77 O89 -4.8(7) . . . . ? C75 C76 C77 C68 -2.4(8) . . . . ? C78 C76 C77 C68 173.7(5) . . . . ? C77 C76 C78 N79 69.2(6) . . . . ? C75 C76 C78 N79 -114.8(5) . . . . ? C76 C78 N79 C80 65.1(5) . . . . ? C76 C78 N79 C84 -177.4(4) . . . . ? C76 C78 N79 Zn4 -60.1(4) . . . . ? O85 Zn4 N79 C80 130.7(3) . . . . ? O89 Zn4 N79 C80 -107.7(3) . . . . ? O58 Zn4 N79 C80 7.2(4) . . . . ? O85 Zn4 N79 C84 8.0(4) . . . . ? O89 Zn4 N79 C84 129.7(4) . . . . ? O58 Zn4 N79 C84 -115.5(4) . . . . ? O85 Zn4 N79 C78 -108.4(3) . . . . ? O89 Zn4 N79 C78 13.2(3) . . . . ? O58 Zn4 N79 C78 128.1(3) . . . . ? C84 N79 C80 C81 54.3(6) . . . . ? C78 N79 C80 C81 172.7(5) . . . . ? Zn4 N79 C80 C81 -69.6(5) . . . . ? N79 C80 C81 O82 -58.6(6) . . . . ? C80 C81 O82 C83 60.2(7) . . . . ? C81 O82 C83 C84 -61.9(7) . . . . ? C80 N79 C84 C83 -54.6(6) . . . . ? C78 N79 C84 C83 -173.7(4) . . . . ? Zn4 N79 C84 C83 73.1(5) . . . . ? O82 C83 C84 N79 60.4(7) . . . . ? O89 Zn4 O85 C86 14.8(5) . . . . ? O58 Zn4 O85 C86 -119.2(4) . . . . ? N79 Zn4 O85 C86 124.0(4) . . . . ? Zn4 O85 C86 O88 -12.7(8) . . . . ? Zn4 O85 C86 C87 167.0(4) . . . . ? O85 C86 O88 Zn5 18.4(12) . . . . ? C87 C86 O88 Zn5 -161.4(5) . . . . ? O89 Zn5 O88 C86 -17.7(7) . . . . ? O54 Zn5 O88 C86 91.0(7) . . . . ? O91 Zn5 O88 C86 -166.2(7) . . . . ? N61 Zn5 O88 C86 52.4(11) . . . . ? O94 Zn5 O88 C86 -108.0(7) . . . . ? C92 Zn5 O88 C86 -136.4(7) . . . . ? C68 C77 O89 Zn4 135.7(4) . . . . ? C76 C77 O89 Zn4 -45.8(5) . . . . ? C68 C77 O89 Zn5 -54.2(5) . . . . ? C76 C77 O89 Zn5 124.4(4) . . . . ? O85 Zn4 O89 C77 151.4(3) . . . . ? O58 Zn4 O89 C77 -72.8(3) . . . . ? N79 Zn4 O89 C77 37.3(3) . . . . ? O85 Zn4 O89 Zn5 -18.6(3) . . . . ? O58 Zn4 O89 Zn5 117.2(2) . . . . ? N79 Zn4 O89 Zn5 -132.8(2) . . . . ? O54 Zn5 O89 C77 123.8(3) . . . . ? O91 Zn5 O89 C77 -78.1(4) . . . . ? O88 Zn5 O89 C77 -155.7(3) . . . . ? N61 Zn5 O89 C77 36.0(3) . . . . ? O94 Zn5 O89 C77 -60.3(3) . . . . ? C92 Zn5 O89 C77 -67.9(4) . . . . ? O54 Zn5 O89 Zn4 -66.7(2) . . . . ? O91 Zn5 O89 Zn4 91.5(3) . . . . ? O88 Zn5 O89 Zn4 13.9(2) . . . . ? N61 Zn5 O89 Zn4 -154.4(2) . . . . ? O94 Zn5 O89 Zn4 109.3(2) . . . . ? C92 Zn5 O89 Zn4 101.7(2) . . . . ? O89 Zn5 O91 C92 18.1(5) . . . . ? O54 Zn5 O91 C92 176.9(3) . . . . ? O88 Zn5 O91 C92 95.2(4) . . . . ? N61 Zn5 O91 C92 -92.7(4) . . . . ? O94 Zn5 O91 C92 -2.8(3) . . . . ? Zn5 O91 C92 O94 5.5(6) . . . . ? Zn5 O91 C92 C93 -176.0(5) . . . . ? O89 Zn5 C92 O94 15.9(4) . . . . ? O54 Zn5 C92 O94 -179.1(3) . . . . ? O91 Zn5 C92 O94 -175.0(6) . . . . ? O88 Zn5 C92 O94 101.0(4) . . . . ? N61 Zn5 C92 O94 -81.0(4) . . . . ? O89 Zn5 C92 O91 -169.1(3) . . . . ? O54 Zn5 C92 O91 -4.1(4) . . . . ? O88 Zn5 C92 O91 -84.0(3) . . . . ? N61 Zn5 C92 O91 94.0(3) . . . . ? O94 Zn5 C92 O91 175.0(6) . . . . ? O91 C92 O94 Zn5 -4.7(6) . . . . ? C93 C92 O94 Zn5 176.9(6) . . . . ? O89 Zn5 O94 C92 -166.1(4) . . . . ? O54 Zn5 O94 C92 1.9(7) . . . . ? O91 Zn5 O94 C92 2.9(3) . . . . ? O88 Zn5 O94 C92 -80.4(4) . . . . ? N61 Zn5 O94 C92 103.7(4) . . . . ? C105 O101 C102 C103 -15.9(15) . . . . ? O101 C102 C103 C104 9.3(16) . . . . ? C102 C103 C104 C105 -0.2(14) . . . . ? C102 O101 C105 C104 16.0(13) . . . . ? C103 C104 C105 O101 -9.1(11) . . . . ?