# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1562 data_global #======================================================================= # SUBMISSION DETAILS _publ_contact_author # Name and address of author for correspondence ; Prof. Israel Goldberg School of Chemistry Tel-Aviv University Ramat-Aviv 69978 Tel-Aviv Israel ; _publ_contact_author_phone '972 3 6409965' _publ_contact_author_fax '972 3 6409293' _publ_contact_author_email goldberg@post.tau.ac.il _publ_requested_journal 'Chemical Communications' _publ_contact_letter ; February 7, 2000 Dear Editor, This CIF file contains the crystallographic data for compounds 1 & 2, the structural features of which are discussed in a manuscript submitted for a possible publication in Chemical Communications. The manuscript is entitled: "New Effective Synthons for Supramolecular Self-Assembly of meso-Carboxyphenylporphyrins" and co-authored by: Y. Diskin-Posner, S. Dahal and I. Goldberg It has been submitted to the office of Prof. Dermot O'Hare. Sincerely, Israel Goldberg ; #======================================================================= data_Compound1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; (C48 H30 N4 O8).3(C9 H10 O2).(C7H5O2-).(Na+) ; _chemical_formula_sum 'C82 H65 N4 Na O16' _chemical_formula_weight 1385.37 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 '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' 'Na' 'Na' 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'P21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.8540(3) _cell_length_b 32.3380(6) _cell_length_c 11.3580(15) _cell_angle_alpha 90.0000(18) _cell_angle_beta 110.521(3) _cell_angle_gamma 90.000(2) _cell_volume 3389.7(5) _cell_formula_units_Z 2 _cell_measurement_temperature 110 _cell_measurement_reflns_used 10388 _cell_measurement_theta_min 1.9 _cell_measurement_theta_max 25.7 _exptl_crystal_description 'prisms' _exptl_crystal_colour 'shining purple' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.357 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1448 _exptl_absorpt_coefficient_mu 0.100 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 110 _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '1 degree Phi scans' _diffrn_detector_area_resol_mean '56 microns' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10388 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0759 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -39 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 25.74 _reflns_number_total 10388 _reflns_number_gt 7865 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius, B.V.' _computing_cell_refinement 'Denzo' _computing_data_reduction 'Denzo' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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^)+(0.0857P)^2^+3.4332P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.2(8) _refine_ls_number_reflns 10388 _refine_ls_number_parameters 945 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0949 _refine_ls_R_factor_gt 0.0653 _refine_ls_wR_factor_ref 0.1778 _refine_ls_wR_factor_gt 0.1545 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.333 _refine_ls_shift/su_mean 0.027 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 N1 N -0.3909(4) 0.27355(15) 0.0848(4) 0.0260(10) Uani 1 1 d . . . N2 N -0.3454(4) 0.33397(16) -0.0960(4) 0.0259(10) Uani 1 1 d . . . H2 H -0.4172 0.3308 -0.0621 0.023(14) Uiso 1 1 d R . . N3 N -0.5752(4) 0.38306(15) -0.0671(4) 0.0251(10) Uani 1 1 d . . . N4 N -0.6185(4) 0.32270(15) 0.1130(3) 0.0239(10) Uani 1 1 d . . . H4 H -0.5480 0.3217 0.0817 0.05(4) Uiso 1 1 d R . . C5 C -0.6114(5) 0.29253(19) 0.2017(4) 0.0255(12) Uani 1 1 d . . . C6 C -0.5205(6) 0.25819(18) 0.2304(5) 0.0263(12) Uani 1 1 d . . . C7 C -0.4162(5) 0.24888(19) 0.1738(5) 0.0273(12) Uani 1 1 d . . . C8 C -0.3239(6) 0.21316(19) 0.2014(5) 0.0323(13) Uani 1 1 d . . . H8 H -0.3206 0.1926 0.2595 0.039 Uiso 1 1 calc . . . C9 C -0.2437(6) 0.2150(2) 0.1281(5) 0.0341(13) Uani 1 1 d . . . H9 H -0.1753 0.1958 0.1237 0.041 Uiso 1 1 calc . . . C10 C -0.2853(5) 0.25339(18) 0.0560(5) 0.0271(12) Uani 1 1 d . . . C11 C -0.2195(6) 0.26691(19) -0.0303(5) 0.0278(12) Uani 1 1 d . . . C12 C -0.2508(6) 0.30329(19) -0.0994(5) 0.0282(12) Uani 1 1 d . . . C13 C -0.1908(6) 0.31553(18) -0.1918(4) 0.0265(12) Uani 1 1 d . . . H13 H -0.1211 0.3010 -0.2129 0.032 Uiso 1 1 calc . . . C14 C -0.2521(5) 0.35166(19) -0.2434(4) 0.0287(12) Uani 1 1 d . . . H14 H -0.2326 0.3662 -0.3062 0.034 Uiso 1 1 calc . . . C15 C -0.3522(5) 0.36340(19) -0.1842(5) 0.0266(12) Uani 1 1 d . . . C16 C -0.4443(6) 0.39802(19) -0.2118(5) 0.0289(12) Uani 1 1 d . . . C17 C -0.5473(6) 0.40682(18) -0.1554(4) 0.0247(11) Uani 1 1 d . . . C18 C -0.6377(6) 0.44352(18) -0.1817(5) 0.0307(13) Uani 1 1 d . . . H18 H -0.6378 0.4646 -0.2375 0.037 Uiso 1 1 calc . . . C19 C -0.7217(6) 0.44141(19) -0.1100(5) 0.0336(13) Uani 1 1 d . . . H19 H -0.7917 0.4604 -0.1076 0.040 Uiso 1 1 calc . . . C20 C -0.6802(6) 0.40342(19) -0.0371(4) 0.0274(12) Uani 1 1 d . . . C21 C -0.7456(5) 0.38997(19) 0.0467(5) 0.0260(12) Uani 1 1 d . . . C22 C -0.7167(5) 0.35292(18) 0.1162(4) 0.0237(11) Uani 1 1 d . . . C23 C -0.7735(5) 0.34128(19) 0.2113(5) 0.0276(12) Uani 1 1 d . . . H23 H -0.8408 0.3560 0.2351 0.033 Uiso 1 1 calc . . . C24 C -0.7116(5) 0.30489(18) 0.2604(5) 0.0255(11) Uani 1 1 d . . . H24 H -0.7313 0.2902 0.3229 0.031 Uiso 1 1 calc . . . C26 C -0.6603(6) 0.21027(19) 0.3182(5) 0.0295(13) Uani 1 1 d . . . H26 H -0.7418 0.2152 0.2473 0.035 Uiso 1 1 calc . . . C25 C -0.5315(5) 0.22924(18) 0.3305(5) 0.0245(12) Uani 1 1 d . . . C27 C -0.6694(6) 0.18343(19) 0.4122(5) 0.0291(13) Uani 1 1 d . . . H27 H -0.7569 0.1708 0.4043 0.035 Uiso 1 1 calc . . . C28 C -0.5463(6) 0.17582(19) 0.5176(5) 0.0274(12) Uani 1 1 d . . . C29 C -0.4170(5) 0.19552(19) 0.5286(5) 0.0267(12) Uani 1 1 d . . . H29 H -0.3349 0.1908 0.5991 0.032 Uiso 1 1 calc . . . C30 C -0.4095(5) 0.22186(18) 0.4364(5) 0.0259(12) Uani 1 1 d . . . H30 H -0.3224 0.2348 0.4447 0.031 Uiso 1 1 calc . . . C31 C -0.5601(6) 0.1468(2) 0.6165(5) 0.0292(13) Uani 1 1 d . . . O32 O -0.6702(4) 0.12978(16) 0.6081(4) 0.0438(11) Uani 1 1 d . . . O33 O -0.4370(4) 0.14280(17) 0.7135(3) 0.0392(10) Uani 1 1 d . . . H33 H -0.435(10) 0.117(3) 0.762(9) 0.05(3) Uiso 1 1 d . . . C34 C -0.1061(6) 0.23886(18) -0.0504(5) 0.0268(12) Uani 1 1 d . . . C35 C -0.1504(6) 0.2010(2) -0.1113(5) 0.0344(14) Uani 1 1 d . . . H35 H -0.2471 0.1930 -0.1364 0.041 Uiso 1 1 calc . . . C36 C -0.0482(7) 0.17535(19) -0.1341(5) 0.0372(14) Uani 1 1 d . . . H36 H -0.0768 0.1504 -0.1762 0.045 Uiso 1 1 calc . . . C37 C 0.0961(6) 0.18723(19) -0.0937(5) 0.0318(13) Uani 1 1 d . . . C38 C 0.1372(6) 0.22488(19) -0.0321(5) 0.0317(13) Uani 1 1 d . . . H38 H 0.2342 0.2326 -0.0045 0.038 Uiso 1 1 calc . . . C39 C 0.0381(6) 0.25070(19) -0.0111(5) 0.0275(12) Uani 1 1 d . . . H39 H 0.0672 0.2759 0.0291 0.033 Uiso 1 1 calc . . . C40 C 0.2031(7) 0.1596(2) -0.1187(6) 0.0410(16) Uani 1 1 d . . . O41 O 0.1680(5) 0.12650(15) -0.1742(4) 0.0482(11) Uani 1 1 d . . . O42 O 0.3375(5) 0.17347(16) -0.0783(4) 0.0475(11) Uani 1 1 d . . . H42 H 0.400(6) 0.148(2) -0.090(5) 0.053(17) Uiso 1 1 d . . . C43 C -0.4332(6) 0.42624(19) -0.3125(5) 0.0273(12) Uani 1 1 d . . . C44 C -0.3036(6) 0.4455(2) -0.3043(5) 0.0307(13) Uani 1 1 d . . . H44 H -0.2204 0.4406 -0.2349 0.037 Uiso 1 1 calc . . . C45 C -0.2974(6) 0.4719(2) -0.3987(5) 0.0315(13) Uani 1 1 d . . . H45 H -0.2106 0.4848 -0.3919 0.038 Uiso 1 1 calc . . . C46 C -0.4213(6) 0.47913(19) -0.5038(5) 0.0278(12) Uani 1 1 d . . . C47 C -0.5490(6) 0.46072(19) -0.5138(5) 0.0287(13) Uani 1 1 d . . . H47 H -0.6317 0.4660 -0.5833 0.034 Uiso 1 1 calc . . . C48 C -0.5560(6) 0.43373(19) -0.4193(5) 0.0284(12) Uani 1 1 d . . . H48 H -0.6430 0.4207 -0.4276 0.034 Uiso 1 1 calc . . . C49 C -0.4082(6) 0.5080(2) -0.6039(5) 0.0307(13) Uani 1 1 d . . . O50 O -0.2927(4) 0.52263(15) -0.6010(4) 0.0414(10) Uani 1 1 d . . . O51 O -0.5329(4) 0.51540(17) -0.6937(4) 0.0389(10) Uani 1 1 d . . . H51 H -0.514(5) 0.5269(16) -0.759(5) 0.025(13) Uiso 1 1 d . . . C52 C -0.8545(6) 0.41713(19) 0.0687(5) 0.0276(13) Uani 1 1 d . . . C53 C -1.0004(6) 0.4070(2) 0.0287(5) 0.0312(13) Uani 1 1 d . . . H53 H -1.0316 0.3825 -0.0151 0.037 Uiso 1 1 calc . . . C54 C -1.1020(6) 0.4328(2) 0.0523(5) 0.0357(14) Uani 1 1 d . . . H54 H -1.1993 0.4253 0.0247 0.043 Uiso 1 1 calc . . . C55 C -1.0567(6) 0.4694(2) 0.1171(5) 0.0304(13) Uani 1 1 d . . . C56 C -0.9113(6) 0.4799(2) 0.1570(5) 0.0379(15) Uani 1 1 d . . . H56 H -0.8805 0.5045 0.2004 0.045 Uiso 1 1 calc . . . C57 C -0.8123(6) 0.45469(19) 0.1338(5) 0.0316(13) Uani 1 1 d . . . H57 H -0.7153 0.4625 0.1616 0.038 Uiso 1 1 calc . . . C58 C -1.1607(7) 0.4983(2) 0.1448(5) 0.0341(14) Uani 1 1 d . . . O59 O -1.1246(5) 0.53118(15) 0.1982(4) 0.0450(11) Uani 1 1 d . . . O60 O -1.2964(5) 0.48453(16) 0.1053(4) 0.0455(11) Uani 1 1 d . . . H60 H -1.38(2) 0.509(7) 0.072(18) 0.05(10) Uiso 1 1 d . . . Na61 Na -0.7792(2) 0.0790 0.69513(15) 0.0321(4) Uani 1 1 d . . . C62 C -1.2159(6) 0.3575(2) 0.2575(5) 0.0395(14) Uani 1 1 d . . . H62 H -1.1625 0.3562 0.2044 0.047 Uiso 1 1 calc . . . C63 C -1.3190(6) 0.3871(2) 0.2397(5) 0.0418(15) Uani 1 1 d . . . H63 H -1.3363 0.4058 0.1738 0.050 Uiso 1 1 calc . . . C64 C -1.3979(6) 0.3898(2) 0.3178(6) 0.0416(15) Uani 1 1 d . . . H64 H -1.4661 0.4108 0.3056 0.050 Uiso 1 1 calc . . . C65 C -1.3773(6) 0.3620(2) 0.4136(5) 0.0374(14) Uani 1 1 d . . . H65 H -1.4326 0.3634 0.4652 0.045 Uiso 1 1 calc . . . C66 C -1.2718(6) 0.3313(2) 0.4323(5) 0.0344(13) Uani 1 1 d . . . H66 H -1.2563 0.3123 0.4970 0.041 Uiso 1 1 calc . . . C67 C -1.1903(6) 0.32922(19) 0.3550(5) 0.0312(12) Uani 1 1 d . . . C68 C -1.0791(6) 0.2962(2) 0.3684(5) 0.0367(14) Uani 1 1 d . . . O69 O -1.0016(5) 0.29493(17) 0.3059(4) 0.0510(12) Uani 1 1 d . . . O70 O -1.0754(4) 0.26834(14) 0.4562(4) 0.0357(9) Uani 1 1 d . . . C71 C -0.9692(7) 0.2355(2) 0.4724(6) 0.0444(16) Uani 1 1 d . . . H71A H -0.8719 0.2468 0.5031 0.053 Uiso 1 1 calc . . . H71B H -0.9844 0.2218 0.3929 0.053 Uiso 1 1 calc . . . C72 C -0.9887(7) 0.2056(3) 0.5656(8) 0.063(2) Uani 1 1 d . . . H72A H -0.9191 0.1836 0.5796 0.094 Uiso 1 1 calc . . . H72B H -1.0848 0.1942 0.5336 0.094 Uiso 1 1 calc . . . H72C H -0.9747 0.2196 0.6435 0.094 Uiso 1 1 calc . . . C73 C -0.7443(6) 0.2969(2) 0.7629(5) 0.0351(14) Uani 1 1 d . . . H73 H -0.7973 0.2983 0.8163 0.042 Uiso 1 1 calc . . . C74 C -0.6427(7) 0.2664(2) 0.7791(6) 0.0418(15) Uani 1 1 d . . . H74 H -0.6272 0.2471 0.8430 0.050 Uiso 1 1 calc . . . C75 C -0.5627(6) 0.2645(2) 0.6993(5) 0.0373(14) Uani 1 1 d . . . H75 H -0.4929 0.2441 0.7105 0.045 Uiso 1 1 calc . . . C76 C -0.5877(6) 0.2931(2) 0.6038(6) 0.0403(15) Uani 1 1 d . . . H76 H -0.5342 0.2917 0.5508 0.048 Uiso 1 1 calc . . . C77 C -0.6912(6) 0.3236(2) 0.5857(5) 0.0329(13) Uani 1 1 d . . . H77 H -0.7088 0.3423 0.5199 0.039 Uiso 1 1 calc . . . C78 C -0.7684(6) 0.3260(2) 0.6665(5) 0.0327(13) Uani 1 1 d . . . C79 C -0.8820(6) 0.3580(2) 0.6529(5) 0.0360(14) Uani 1 1 d . . . O80 O -0.9598(4) 0.35918(16) 0.7140(4) 0.0489(11) Uani 1 1 d . . . O81 O -0.8879(4) 0.38683(14) 0.5651(3) 0.0362(9) Uani 1 1 d . . . C82 C -0.9962(6) 0.4189(2) 0.5473(6) 0.0386(14) Uani 1 1 d . . . H82A H -0.9808 0.4332 0.6260 0.046 Uiso 1 1 calc . . . H82B H -1.0923 0.4068 0.5192 0.046 Uiso 1 1 calc . . . C83 C -0.9836(7) 0.4482(3) 0.4523(8) 0.061(2) Uani 1 1 d . . . H83A H -1.0549 0.4696 0.4393 0.092 Uiso 1 1 calc . . . H83B H -0.9993 0.4339 0.3747 0.092 Uiso 1 1 calc . . . H83C H -0.8886 0.4603 0.4812 0.092 Uiso 1 1 calc . . . C84 C -1.0853(7) 0.5865(3) 0.7303(7) 0.072(2) Uani 1 1 d . . . H84 H -1.1616 0.5958 0.6605 0.087 Uiso 1 1 calc . . . C85 C -1.0988(9) 0.5861(5) 0.8474(8) 0.114(4) Uani 1 1 d . . . H85 H -1.1862 0.5945 0.8539 0.137 Uiso 1 1 calc . . . C86 C -0.9932(8) 0.5744(3) 0.9502(6) 0.0683(19) Uani 1 1 d . . . H86 H -1.0004 0.5781 1.0291 0.082 Uiso 1 1 calc . . . C87 C -0.8722(8) 0.5566(3) 0.9375(7) 0.073(2) Uani 1 1 d . . . H87 H -0.8001 0.5460 1.0079 0.088 Uiso 1 1 calc . . . C88 C -0.8564(8) 0.5544(3) 0.8201(7) 0.069(2) Uani 1 1 d . . . H88 H -0.7783 0.5406 0.8102 0.082 Uiso 1 1 calc . . . C89 C -0.9619(6) 0.5736(3) 0.7174(5) 0.0589(17) Uani 1 1 d . . . C90 C -0.9491(7) 0.5725(3) 0.5907(6) 0.0602(18) Uani 1 1 d . . . O91 O -1.0444(5) 0.5815(2) 0.4964(4) 0.0674(12) Uani 1 1 d . . . O92 O -0.8291(5) 0.55533(18) 0.5872(4) 0.0656(13) Uani 1 1 d . . . C93 C -0.8098(9) 0.5515(3) 0.4627(7) 0.074(2) Uani 1 1 d . . . H93A H -0.7250 0.5348 0.4719 0.089 Uiso 1 1 calc . . . H93B H -0.8935 0.5378 0.4035 0.089 Uiso 1 1 calc . . . C94 C -0.7924(9) 0.5932(3) 0.4131(8) 0.076(2) Uani 1 1 d . . . H94A H -0.7787 0.5901 0.3339 0.115 Uiso 1 1 calc . . . H94B H -0.7097 0.6068 0.4718 0.115 Uiso 1 1 calc . . . H94C H -0.8777 0.6094 0.4017 0.115 Uiso 1 1 calc . . . C95 C -0.5120(7) 0.6133(2) 0.8525(6) 0.0476(16) Uani 1 1 d . . . H95 H -0.5335 0.6377 0.8858 0.057 Uiso 1 1 calc . . . C96 C -0.5054(9) 0.6135(2) 0.7329(6) 0.0556(19) Uani 1 1 d . . . H96 H -0.5209 0.6380 0.6871 0.067 Uiso 1 1 calc . . . C97 C -0.4761(7) 0.5780(3) 0.6820(4) 0.0512(14) Uani 1 1 d . . . H97 H -0.4677 0.5782 0.6029 0.061 Uiso 1 1 calc . . . C98 C -0.4590(9) 0.5416(2) 0.7494(6) 0.060(2) Uani 1 1 d . . . H98 H -0.4429 0.5171 0.7139 0.071 Uiso 1 1 calc . . . C99 C -0.4656(8) 0.5413(2) 0.8681(6) 0.0516(17) Uani 1 1 d . . . H99 H -0.4552 0.5165 0.9119 0.062 Uiso 1 1 calc . . . C100 C -0.4876(5) 0.5778(2) 0.9228(4) 0.0319(10) Uani 1 1 d . . . C101 C -0.4938(5) 0.5782(2) 1.0529(4) 0.0305(10) Uani 1 1 d . . . O102 O -0.5151(5) 0.61271(15) 1.0954(4) 0.0436(11) Uani 1 1 d . . . O103 O -0.4768(5) 0.54525(16) 1.1138(4) 0.0459(11) 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 N1 0.035(2) 0.026(3) 0.022(2) 0.0030(18) 0.0173(18) 0.0001(19) N2 0.032(2) 0.027(3) 0.026(2) 0.0040(19) 0.0193(18) 0.001(2) N3 0.042(3) 0.019(2) 0.020(2) -0.0010(17) 0.0186(18) 0.0008(19) N4 0.037(2) 0.023(2) 0.018(2) 0.0045(17) 0.0165(18) 0.0000(19) C5 0.040(3) 0.028(3) 0.015(2) -0.002(2) 0.017(2) -0.003(2) C6 0.041(3) 0.019(3) 0.022(3) 0.004(2) 0.016(2) 0.001(2) C7 0.034(3) 0.032(3) 0.019(2) 0.001(2) 0.013(2) 0.000(2) C8 0.046(3) 0.028(3) 0.028(3) 0.010(2) 0.020(2) 0.010(3) C9 0.052(3) 0.036(4) 0.024(3) 0.006(2) 0.026(3) 0.009(3) C10 0.036(3) 0.025(3) 0.025(3) 0.001(2) 0.017(2) 0.003(2) C11 0.044(3) 0.024(3) 0.022(3) -0.004(2) 0.019(2) -0.004(2) C12 0.037(3) 0.025(3) 0.026(3) 0.003(2) 0.016(2) 0.003(2) C13 0.040(3) 0.026(3) 0.020(2) -0.002(2) 0.019(2) 0.005(2) C14 0.035(3) 0.038(3) 0.020(2) 0.000(2) 0.018(2) 0.002(2) C15 0.037(3) 0.023(3) 0.024(3) 0.003(2) 0.017(2) -0.002(2) C16 0.045(3) 0.028(3) 0.021(3) 0.001(2) 0.021(2) -0.002(2) C17 0.042(3) 0.019(3) 0.021(2) 0.007(2) 0.021(2) 0.004(2) C18 0.058(4) 0.019(3) 0.029(3) 0.007(2) 0.032(3) 0.003(2) C19 0.049(3) 0.028(3) 0.030(3) 0.004(2) 0.021(3) 0.012(3) C20 0.044(3) 0.025(3) 0.020(2) 0.001(2) 0.020(2) 0.003(2) C21 0.033(3) 0.027(3) 0.024(3) -0.003(2) 0.017(2) 0.000(2) C22 0.033(3) 0.025(3) 0.019(2) -0.004(2) 0.016(2) 0.000(2) C23 0.033(3) 0.030(3) 0.027(3) 0.003(2) 0.019(2) 0.000(2) C24 0.036(3) 0.023(3) 0.024(3) 0.005(2) 0.018(2) 0.000(2) C26 0.040(3) 0.029(3) 0.021(3) 0.005(2) 0.012(2) 0.003(3) C25 0.034(3) 0.020(3) 0.028(3) -0.002(2) 0.021(2) -0.002(2) C27 0.041(3) 0.024(3) 0.029(3) -0.003(2) 0.021(3) -0.010(2) C28 0.042(3) 0.024(3) 0.021(3) 0.002(2) 0.017(2) 0.004(2) C29 0.030(3) 0.028(3) 0.025(3) 0.004(2) 0.014(2) 0.000(2) C30 0.034(3) 0.024(3) 0.024(3) 0.002(2) 0.015(2) 0.001(2) C31 0.041(3) 0.026(3) 0.030(3) 0.000(2) 0.025(3) -0.006(3) O32 0.049(3) 0.054(3) 0.030(2) 0.0112(19) 0.0154(18) -0.015(2) O33 0.047(2) 0.050(3) 0.025(2) 0.0161(18) 0.0182(18) 0.003(2) C34 0.043(3) 0.020(3) 0.024(3) 0.008(2) 0.021(2) 0.014(2) C35 0.041(3) 0.039(4) 0.029(3) -0.001(3) 0.021(3) -0.008(3) C36 0.066(4) 0.018(3) 0.040(3) -0.001(2) 0.034(3) 0.006(3) C37 0.043(4) 0.027(3) 0.033(3) 0.003(2) 0.023(3) 0.006(2) C38 0.046(3) 0.026(3) 0.030(3) -0.001(2) 0.021(2) 0.005(3) C39 0.033(3) 0.026(3) 0.027(3) 0.003(2) 0.014(2) 0.006(2) C40 0.061(4) 0.029(4) 0.044(3) 0.008(3) 0.032(3) 0.015(3) O41 0.075(3) 0.030(3) 0.056(3) -0.009(2) 0.044(2) 0.002(2) O42 0.049(3) 0.039(3) 0.065(3) -0.001(2) 0.033(2) 0.009(2) C43 0.042(3) 0.026(3) 0.022(3) 0.004(2) 0.021(2) 0.005(2) C44 0.039(3) 0.037(4) 0.024(3) 0.008(2) 0.020(2) 0.003(3) C45 0.036(3) 0.036(3) 0.028(3) 0.007(2) 0.018(2) 0.001(3) C46 0.042(3) 0.027(3) 0.025(3) 0.003(2) 0.025(2) -0.002(2) C47 0.043(3) 0.030(3) 0.020(2) 0.002(2) 0.019(2) 0.004(2) C48 0.035(3) 0.031(3) 0.029(3) 0.000(2) 0.024(2) 0.000(2) C49 0.047(4) 0.030(3) 0.021(3) 0.002(2) 0.019(3) 0.004(3) O50 0.049(2) 0.040(2) 0.040(2) 0.0170(18) 0.0217(18) -0.0085(19) O51 0.043(2) 0.048(3) 0.031(2) 0.0157(19) 0.0186(19) 0.0016(19) C52 0.042(3) 0.029(3) 0.019(2) 0.002(2) 0.020(2) 0.000(2) C53 0.041(3) 0.031(3) 0.023(3) -0.003(2) 0.013(2) 0.004(3) C54 0.041(3) 0.043(4) 0.028(3) 0.002(3) 0.019(2) 0.002(3) C55 0.046(3) 0.030(3) 0.022(3) 0.003(2) 0.021(2) 0.008(3) C56 0.052(4) 0.039(4) 0.035(3) -0.008(3) 0.031(3) -0.004(3) C57 0.048(3) 0.025(3) 0.030(3) -0.003(2) 0.024(2) -0.001(2) C58 0.052(4) 0.036(4) 0.026(3) 0.004(2) 0.028(3) 0.006(3) O59 0.067(3) 0.033(3) 0.050(2) 0.001(2) 0.039(2) 0.011(2) O60 0.050(3) 0.046(3) 0.047(2) 0.005(2) 0.025(2) 0.016(2) Na61 0.0472(12) 0.0260(8) 0.0337(9) -0.0014(11) 0.0273(8) -0.0017(11) C62 0.050(4) 0.042(4) 0.035(3) 0.006(3) 0.025(3) 0.001(3) C63 0.049(4) 0.049(4) 0.027(3) 0.002(3) 0.013(3) -0.008(3) C64 0.043(3) 0.038(4) 0.039(3) -0.006(3) 0.009(3) 0.001(3) C65 0.044(3) 0.038(4) 0.036(3) -0.004(3) 0.021(3) -0.003(3) C66 0.044(3) 0.031(3) 0.032(3) 0.000(2) 0.019(2) -0.005(3) C67 0.042(3) 0.029(3) 0.030(3) -0.003(2) 0.020(2) 0.002(3) C68 0.045(3) 0.042(4) 0.026(3) 0.000(3) 0.015(3) -0.002(3) O69 0.059(3) 0.057(3) 0.055(3) 0.009(2) 0.042(2) 0.008(2) O70 0.038(2) 0.036(2) 0.041(2) 0.0051(18) 0.0232(17) 0.0014(18) C71 0.050(4) 0.032(4) 0.057(4) -0.003(3) 0.026(3) 0.007(3) C72 0.057(4) 0.055(5) 0.083(5) 0.034(4) 0.032(4) 0.013(4) C73 0.047(3) 0.033(4) 0.028(3) -0.004(2) 0.018(2) -0.005(3) C74 0.055(4) 0.026(3) 0.041(3) 0.005(3) 0.013(3) 0.002(3) C75 0.044(3) 0.032(3) 0.037(3) -0.008(3) 0.016(3) 0.002(3) C76 0.047(4) 0.036(4) 0.042(3) -0.016(3) 0.021(3) -0.005(3) C77 0.040(3) 0.033(3) 0.033(3) -0.008(2) 0.021(2) -0.007(3) C78 0.035(3) 0.031(3) 0.032(3) -0.008(2) 0.012(2) -0.007(3) C79 0.049(3) 0.035(4) 0.031(3) 0.005(3) 0.022(3) -0.010(3) O80 0.057(3) 0.050(3) 0.057(3) 0.011(2) 0.042(2) 0.007(2) O81 0.044(2) 0.036(2) 0.037(2) 0.0065(18) 0.0240(17) 0.0045(18) C82 0.041(3) 0.042(4) 0.037(3) 0.002(3) 0.020(3) 0.001(3) C83 0.051(4) 0.067(5) 0.070(5) 0.025(4) 0.026(4) 0.016(4) C84 0.047(4) 0.103(8) 0.062(4) 0.006(4) 0.013(3) 0.014(4) C85 0.070(6) 0.210(13) 0.074(6) 0.001(8) 0.041(5) 0.037(7) C86 0.076(5) 0.074(5) 0.062(4) 0.018(5) 0.034(4) 0.007(5) C87 0.074(5) 0.091(6) 0.058(4) 0.016(4) 0.027(4) -0.004(4) C88 0.065(5) 0.080(5) 0.068(5) 0.020(4) 0.032(4) -0.002(4) C89 0.037(3) 0.093(5) 0.044(3) 0.001(4) 0.010(3) 0.010(4) C90 0.033(4) 0.087(6) 0.055(4) 0.006(4) 0.008(3) 0.006(4) O91 0.060(3) 0.081(3) 0.053(3) 0.005(3) 0.010(2) 0.003(3) O92 0.074(3) 0.069(3) 0.060(3) 0.016(2) 0.031(2) 0.014(3) C93 0.091(6) 0.066(5) 0.068(5) 0.000(4) 0.031(4) -0.002(4) C94 0.072(5) 0.069(6) 0.087(6) 0.021(4) 0.026(4) -0.004(4) C95 0.073(4) 0.045(4) 0.031(3) -0.005(3) 0.026(3) 0.000(3) C96 0.100(6) 0.035(4) 0.038(4) 0.007(3) 0.033(4) 0.001(4) C97 0.078(4) 0.052(3) 0.034(3) 0.003(4) 0.032(3) 0.006(4) C98 0.107(6) 0.043(4) 0.042(4) 0.005(3) 0.043(4) 0.025(4) C99 0.083(5) 0.036(4) 0.045(4) 0.007(3) 0.033(3) 0.015(3) C100 0.049(3) 0.027(2) 0.025(2) 0.000(3) 0.019(2) -0.004(3) C101 0.032(3) 0.036(2) 0.026(2) -0.003(3) 0.014(2) 0.005(3) O102 0.066(3) 0.037(3) 0.040(2) -0.0169(19) 0.033(2) -0.018(2) O103 0.071(3) 0.049(3) 0.032(2) 0.017(2) 0.037(2) 0.025(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C10 1.361(7) . ? N1 C7 1.378(7) . ? N2 C15 1.367(6) . ? N2 C12 1.371(7) . ? N2 H2 0.9214 . ? N3 C17 1.366(6) . ? N3 C20 1.367(6) . ? N4 C5 1.386(6) . ? N4 C22 1.384(6) . ? N4 H4 0.8856 . ? C5 C6 1.392(7) . ? C5 C24 1.429(7) . ? C6 C7 1.421(7) . ? C6 C25 1.506(7) . ? C7 C8 1.436(8) . ? C8 C9 1.335(8) . ? C8 H8 0.9300 . ? C9 C10 1.465(7) . ? C9 H9 0.9298 . ? C10 C11 1.420(7) . ? C11 C12 1.388(7) . ? C11 C34 1.517(7) . ? C12 C13 1.428(7) . ? C13 C14 1.351(7) . ? C13 H13 0.9301 . ? C14 C15 1.426(7) . ? C14 H14 0.9298 . ? C15 C16 1.405(8) . ? C16 C17 1.406(7) . ? C16 C43 1.497(7) . ? C17 C18 1.451(7) . ? C18 C19 1.351(8) . ? C18 H18 0.9301 . ? C19 C20 1.458(7) . ? C19 H19 0.9301 . ? C20 C21 1.393(7) . ? C21 C22 1.408(7) . ? C21 C52 1.475(7) . ? C22 C23 1.431(7) . ? C23 C24 1.352(7) . ? C23 H23 0.9299 . ? C24 H24 0.9302 . ? C26 C25 1.372(8) . ? C26 C27 1.403(8) . ? C26 H26 0.9300 . ? C25 C30 1.390(7) . ? C27 C28 1.396(7) . ? C27 H27 0.9296 . ? C28 C29 1.390(8) . ? C28 C31 1.506(8) . ? C29 C30 1.372(7) . ? C29 H29 0.9301 . ? C30 H30 0.9301 . ? C31 O32 1.191(6) . ? C31 O33 1.329(7) . ? O32 Na61 2.360(4) . ? O33 H33 1.00(10) . ? C34 C39 1.387(8) . ? C34 C35 1.398(8) . ? C35 C36 1.397(8) . ? C35 H35 0.9300 . ? C36 C37 1.386(8) . ? C36 H36 0.9299 . ? C37 C38 1.392(8) . ? C37 C40 1.484(8) . ? C38 C39 1.368(7) . ? C38 H38 0.9299 . ? C39 H39 0.9300 . ? C40 O41 1.228(7) . ? C40 O42 1.319(8) . ? O41 Na61 2.318(4) 1_654 ? O42 H42 1.07(7) . ? C43 C44 1.394(8) . ? C43 C48 1.402(7) . ? C44 C45 1.389(8) . ? C44 H44 0.9301 . ? C45 C46 1.396(7) . ? C45 H45 0.9301 . ? C46 C47 1.360(8) . ? C46 C49 1.511(7) . ? C47 C48 1.404(7) . ? C47 H47 0.9299 . ? C48 H48 0.9301 . ? C49 O50 1.223(7) . ? C49 O51 1.315(6) . ? O50 Na61 2.345(4) 2_455 ? O51 H51 0.90(6) . ? C52 C53 1.386(8) . ? C52 C57 1.407(7) . ? C53 C54 1.399(8) . ? C53 H53 0.9299 . ? C54 C55 1.384(8) . ? C54 H54 0.9303 . ? C55 C56 1.384(8) . ? C55 C58 1.499(8) . ? C56 C57 1.365(8) . ? C56 H56 0.9298 . ? C57 H57 0.9298 . ? C58 O59 1.214(7) . ? C58 O60 1.329(7) . ? O59 Na61 2.358(4) 2_356 ? O60 H60 1.1(2) . ? Na61 O91 2.261(5) 2_346 ? Na61 O41 2.318(4) 1_456 ? Na61 O50 2.345(4) 2_445 ? Na61 O59 2.358(4) 2_346 ? Na61 O103 2.903(5) 2_447 ? C62 C63 1.359(9) . ? C62 C67 1.390(8) . ? C62 H62 0.9301 . ? C63 C64 1.371(9) . ? C63 H63 0.9301 . ? C64 C65 1.373(8) . ? C64 H64 0.9301 . ? C65 C66 1.397(8) . ? C65 H65 0.9300 . ? C66 C67 1.384(8) . ? C66 H66 0.9296 . ? C67 C68 1.498(8) . ? C68 O69 1.211(7) . ? C68 O70 1.336(7) . ? O70 C71 1.456(7) . ? C71 C72 1.496(10) . ? C71 H71A 0.9697 . ? C71 H71B 0.9700 . ? C72 H72A 0.9607 . ? C72 H72B 0.9601 . ? C72 H72C 0.9596 . ? C73 C74 1.371(8) . ? C73 C78 1.400(8) . ? C73 H73 0.9301 . ? C74 C75 1.395(9) . ? C74 H74 0.9302 . ? C75 C76 1.379(9) . ? C75 H75 0.9303 . ? C76 C77 1.382(8) . ? C76 H76 0.9303 . ? C77 C78 1.384(8) . ? C77 H77 0.9304 . ? C78 C79 1.491(8) . ? C79 O80 1.201(7) . ? C79 O81 1.352(6) . ? O81 C82 1.450(7) . ? C82 C83 1.474(9) . ? C82 H82A 0.9699 . ? C82 H82B 0.9704 . ? C83 H83A 0.9596 . ? C83 H83B 0.9601 . ? C83 H83C 0.9600 . ? C84 C89 1.341(9) . ? C84 C85 1.383(10) . ? C84 H84 0.9299 . ? C85 C86 1.318(11) . ? C85 H85 0.9300 . ? C86 C87 1.376(10) . ? C86 H86 0.9299 . ? C87 C88 1.398(9) . ? C87 H87 0.9302 . ? C88 C89 1.406(9) . ? C88 H88 0.9301 . ? C89 C90 1.488(8) . ? C90 O91 1.186(7) . ? C90 O92 1.320(8) . ? O91 Na61 2.261(5) 2_356 ? O92 C93 1.496(9) . ? C93 C94 1.492(10) . ? C93 H93A 0.9701 . ? C93 H93B 0.9704 . ? C94 H94A 0.9598 . ? C94 H94B 0.9602 . ? C94 H94C 0.9600 . ? C95 C100 1.370(9) . ? C95 C96 1.383(9) . ? C95 H95 0.9300 . ? C96 C97 1.363(10) . ? C96 H96 0.9296 . ? C97 C98 1.380(10) . ? C97 H97 0.9301 . ? C98 C99 1.372(9) . ? C98 H98 0.9301 . ? C99 C100 1.386(9) . ? C99 H99 0.9297 . ? C100 C101 1.500(5) . ? C101 O103 1.250(7) . ? C101 O102 1.262(7) . ? O103 Na61 2.903(5) 2_457 ? 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 C10 N1 C7 104.5(4) . . ? C15 N2 C12 110.0(4) . . ? C15 N2 H2 122.5 . . ? C12 N2 H2 124.0 . . ? C17 N3 C20 106.1(4) . . ? C5 N4 C22 109.6(4) . . ? C5 N4 H4 114.9 . . ? C22 N4 H4 133.6 . . ? N4 C5 C6 126.6(4) . . ? N4 C5 C24 106.0(4) . . ? C6 C5 C24 127.4(5) . . ? C5 C6 C7 124.8(5) . . ? C5 C6 C25 117.5(4) . . ? C7 C6 C25 117.7(5) . . ? N1 C7 C6 123.7(5) . . ? N1 C7 C8 111.2(4) . . ? C6 C7 C8 125.1(5) . . ? C9 C8 C7 107.3(5) . . ? C9 C8 H8 126.3 . . ? C7 C8 H8 126.4 . . ? C8 C9 C10 105.9(5) . . ? C8 C9 H9 127.0 . . ? C10 C9 H9 127.1 . . ? N1 C10 C11 126.2(5) . . ? N1 C10 C9 111.1(4) . . ? C11 C10 C9 122.7(5) . . ? C12 C11 C10 125.9(5) . . ? C12 C11 C34 116.8(5) . . ? C10 C11 C34 117.3(5) . . ? N2 C12 C11 128.0(5) . . ? N2 C12 C13 106.3(4) . . ? C11 C12 C13 125.7(5) . . ? C14 C13 C12 108.7(4) . . ? C14 C13 H13 125.6 . . ? C12 C13 H13 125.6 . . ? C13 C14 C15 107.7(4) . . ? C13 C14 H14 126.2 . . ? C15 C14 H14 126.2 . . ? N2 C15 C16 125.4(4) . . ? N2 C15 C14 107.2(4) . . ? C16 C15 C14 127.3(5) . . ? C17 C16 C15 124.9(5) . . ? C17 C16 C43 118.8(5) . . ? C15 C16 C43 116.2(4) . . ? N3 C17 C16 125.7(5) . . ? N3 C17 C18 110.1(4) . . ? C16 C17 C18 124.1(4) . . ? C19 C18 C17 107.2(4) . . ? C19 C18 H18 126.4 . . ? C17 C18 H18 126.4 . . ? C18 C19 C20 106.0(5) . . ? C18 C19 H19 127.0 . . ? C20 C19 H19 127.0 . . ? N3 C20 C21 126.3(5) . . ? N3 C20 C19 110.5(4) . . ? C21 C20 C19 123.1(5) . . ? C20 C21 C22 126.7(5) . . ? C20 C21 C52 117.9(5) . . ? C22 C21 C52 115.3(4) . . ? N4 C22 C21 126.3(4) . . ? N4 C22 C23 107.2(4) . . ? C21 C22 C23 126.3(5) . . ? C24 C23 C22 107.5(4) . . ? C24 C23 H23 126.2 . . ? C22 C23 H23 126.3 . . ? C23 C24 C5 109.6(4) . . ? C23 C24 H24 125.2 . . ? C5 C24 H24 125.2 . . ? C25 C26 C27 120.1(5) . . ? C25 C26 H26 119.9 . . ? C27 C26 H26 119.9 . . ? C26 C25 C30 120.0(5) . . ? C26 C25 C6 120.6(5) . . ? C30 C25 C6 119.4(4) . . ? C28 C27 C26 119.6(5) . . ? C28 C27 H27 120.2 . . ? C26 C27 H27 120.2 . . ? C29 C28 C27 119.3(5) . . ? C29 C28 C31 122.6(4) . . ? C27 C28 C31 118.1(5) . . ? C30 C29 C28 120.6(5) . . ? C30 C29 H29 119.7 . . ? C28 C29 H29 119.7 . . ? C29 C30 C25 120.3(5) . . ? C29 C30 H30 119.8 . . ? C25 C30 H30 119.8 . . ? O32 C31 O33 124.3(5) . . ? O32 C31 C28 123.1(5) . . ? O33 C31 C28 112.6(5) . . ? C31 O32 Na61 145.5(4) . . ? C31 O33 H33 112(5) . . ? C39 C34 C35 120.5(5) . . ? C39 C34 C11 120.8(5) . . ? C35 C34 C11 118.6(5) . . ? C34 C35 C36 119.4(5) . . ? C34 C35 H35 120.4 . . ? C36 C35 H35 120.3 . . ? C37 C36 C35 119.8(5) . . ? C37 C36 H36 120.1 . . ? C35 C36 H36 120.1 . . ? C36 C37 C38 119.5(5) . . ? C36 C37 C40 119.0(5) . . ? C38 C37 C40 121.5(5) . . ? C39 C38 C37 121.4(5) . . ? C39 C38 H38 119.3 . . ? C37 C38 H38 119.2 . . ? C38 C39 C34 119.3(5) . . ? C38 C39 H39 120.3 . . ? C34 C39 H39 120.4 . . ? O41 C40 O42 122.9(6) . . ? O41 C40 C37 122.1(6) . . ? O42 C40 C37 114.9(6) . . ? C40 O41 Na61 145.0(4) . 1_654 ? C40 O42 H42 104(3) . . ? C44 C43 C48 118.2(5) . . ? C44 C43 C16 122.1(5) . . ? C48 C43 C16 119.6(5) . . ? C43 C44 C45 120.7(5) . . ? C43 C44 H44 119.7 . . ? C45 C44 H44 119.7 . . ? C44 C45 C46 120.1(5) . . ? C44 C45 H45 120.0 . . ? C46 C45 H45 120.0 . . ? C47 C46 C45 120.3(5) . . ? C47 C46 C49 121.8(5) . . ? C45 C46 C49 117.9(5) . . ? C46 C47 C48 120.0(5) . . ? C46 C47 H47 120.0 . . ? C48 C47 H47 120.0 . . ? C47 C48 C43 120.7(5) . . ? C47 C48 H48 119.7 . . ? C43 C48 H48 119.7 . . ? O50 C49 O51 123.9(5) . . ? O50 C49 C46 122.9(5) . . ? O51 C49 C46 113.2(5) . . ? C49 O50 Na61 135.7(4) . 2_455 ? C49 O51 H51 108(3) . . ? C53 C52 C57 117.2(5) . . ? C53 C52 C21 122.5(5) . . ? C57 C52 C21 120.3(5) . . ? C52 C53 C54 121.8(5) . . ? C52 C53 H53 119.1 . . ? C54 C53 H53 119.1 . . ? C55 C54 C53 119.5(5) . . ? C55 C54 H54 120.3 . . ? C53 C54 H54 120.2 . . ? C56 C55 C54 119.1(5) . . ? C56 C55 C58 119.0(5) . . ? C54 C55 C58 121.8(5) . . ? C57 C56 C55 121.3(5) . . ? C57 C56 H56 119.4 . . ? C55 C56 H56 119.4 . . ? C56 C57 C52 121.1(5) . . ? C56 C57 H57 119.5 . . ? C52 C57 H57 119.4 . . ? O59 C58 O60 123.1(5) . . ? O59 C58 C55 123.2(6) . . ? O60 C58 C55 113.7(5) . . ? C58 O59 Na61 137.0(4) . 2_356 ? C58 O60 H60 113(10) . . ? O91 Na61 O41 108.9(2) 2_346 1_456 ? O91 Na61 O50 80.89(19) 2_346 2_445 ? O41 Na61 O50 168.09(18) 1_456 2_445 ? O91 Na61 O32 83.21(18) 2_346 . ? O41 Na61 O32 92.54(18) 1_456 . ? O50 Na61 O32 95.46(14) 2_445 . ? O91 Na61 O59 101.86(19) 2_346 2_346 ? O41 Na61 O59 83.39(12) 1_456 2_346 ? O50 Na61 O59 87.97(17) 2_445 2_346 ? O32 Na61 O59 174.30(17) . 2_346 ? O91 Na61 O103 155.0(2) 2_346 2_447 ? O41 Na61 O103 95.84(15) 1_456 2_447 ? O50 Na61 O103 74.12(14) 2_445 2_447 ? O32 Na61 O103 99.84(14) . 2_447 ? O59 Na61 O103 76.69(15) 2_346 2_447 ? C63 C62 C67 120.0(5) . . ? C63 C62 H62 120.0 . . ? C67 C62 H62 120.0 . . ? C62 C63 C64 120.9(6) . . ? C62 C63 H63 119.6 . . ? C64 C63 H63 119.5 . . ? C65 C64 C63 120.7(6) . . ? C65 C64 H64 119.6 . . ? C63 C64 H64 119.6 . . ? C64 C65 C66 118.7(5) . . ? C64 C65 H65 120.6 . . ? C66 C65 H65 120.7 . . ? C67 C66 C65 120.4(5) . . ? C67 C66 H66 119.8 . . ? C65 C66 H66 119.8 . . ? C62 C67 C66 119.3(5) . . ? C62 C67 C68 118.2(5) . . ? C66 C67 C68 122.5(5) . . ? O69 C68 O70 123.8(6) . . ? O69 C68 C67 123.6(5) . . ? O70 C68 C67 112.6(5) . . ? C68 O70 C71 114.6(5) . . ? O70 C71 C72 107.2(5) . . ? O70 C71 H71A 110.3 . . ? C72 C71 H71A 110.3 . . ? O70 C71 H71B 110.3 . . ? C72 C71 H71B 110.3 . . ? H71A C71 H71B 108.6 . . ? C71 C72 H72A 109.5 . . ? C71 C72 H72B 109.5 . . ? H72A C72 H72B 109.4 . . ? C71 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C74 C73 C78 120.3(5) . . ? C74 C73 H73 119.8 . . ? C78 C73 H73 119.9 . . ? C73 C74 C75 119.8(5) . . ? C73 C74 H74 120.1 . . ? C75 C74 H74 120.1 . . ? C76 C75 C74 119.7(6) . . ? C76 C75 H75 120.2 . . ? C74 C75 H75 120.1 . . ? C75 C76 C77 120.9(6) . . ? C75 C76 H76 119.6 . . ? C77 C76 H76 119.5 . . ? C76 C77 C78 119.4(6) . . ? C76 C77 H77 120.3 . . ? C78 C77 H77 120.3 . . ? C77 C78 C73 119.9(5) . . ? C77 C78 C79 122.5(5) . . ? C73 C78 C79 117.5(5) . . ? O80 C79 O81 122.2(5) . . ? O80 C79 C78 124.8(5) . . ? O81 C79 C78 113.0(5) . . ? C79 O81 C82 115.8(4) . . ? O81 C82 C83 108.4(5) . . ? O81 C82 H82A 110.0 . . ? C83 C82 H82A 110.1 . . ? O81 C82 H82B 110.0 . . ? C83 C82 H82B 110.0 . . ? H82A C82 H82B 108.3 . . ? C82 C83 H83A 109.5 . . ? C82 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? C82 C83 H83C 109.4 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? C89 C84 C85 119.9(7) . . ? C89 C84 H84 120.1 . . ? C85 C84 H84 120.0 . . ? C86 C85 C84 122.9(7) . . ? C86 C85 H85 118.6 . . ? C84 C85 H85 118.5 . . ? C85 C86 C87 118.0(7) . . ? C85 C86 H86 121.0 . . ? C87 C86 H86 121.0 . . ? C86 C87 C88 120.8(7) . . ? C86 C87 H87 119.6 . . ? C88 C87 H87 119.6 . . ? C87 C88 C89 118.2(7) . . ? C87 C88 H88 120.9 . . ? C89 C88 H88 120.9 . . ? C84 C89 C88 118.8(6) . . ? C84 C89 C90 120.0(6) . . ? C88 C89 C90 120.2(6) . . ? O91 C90 O92 120.7(6) . . ? O91 C90 C89 123.9(6) . . ? O92 C90 C89 114.8(6) . . ? C90 O91 Na61 163.4(6) . 2_356 ? C90 O92 C93 118.3(5) . . ? C94 C93 O92 110.6(7) . . ? C94 C93 H93A 109.6 . . ? O92 C93 H93A 109.5 . . ? C94 C93 H93B 109.5 . . ? O92 C93 H93B 109.5 . . ? H93A C93 H93B 108.0 . . ? C93 C94 H94A 109.5 . . ? C93 C94 H94B 109.4 . . ? H94A C94 H94B 109.5 . . ? C93 C94 H94C 109.5 . . ? H94A C94 H94C 109.5 . . ? H94B C94 H94C 109.5 . . ? C100 C95 C96 121.2(6) . . ? C100 C95 H95 119.4 . . ? C96 C95 H95 119.4 . . ? C97 C96 C95 120.1(6) . . ? C97 C96 H96 119.9 . . ? C95 C96 H96 119.9 . . ? C96 C97 C98 119.1(4) . . ? C96 C97 H97 120.4 . . ? C98 C97 H97 120.5 . . ? C99 C98 C97 120.9(6) . . ? C99 C98 H98 119.5 . . ? C97 C98 H98 119.6 . . ? C98 C99 C100 120.1(6) . . ? C98 C99 H99 120.0 . . ? C100 C99 H99 119.9 . . ? C95 C100 C99 118.4(4) . . ? C95 C100 C101 120.5(6) . . ? C99 C100 C101 121.0(6) . . ? O103 C101 O102 123.4(4) . . ? O103 C101 C100 119.6(6) . . ? O102 C101 C100 117.0(6) . . ? C101 O103 Na61 90.3(3) . 2_457 ? _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 25.74 _diffrn_measured_fraction_theta_full 0.952 _refine_diff_density_max 0.745 _refine_diff_density_min -0.264 _refine_diff_density_rms 0.064 #==== END #=================================================================== data_Compound(2) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C48 H26 N4 O8 Zn2).13(C2 H6 O2)' _chemical_formula_sum 'C74 H104 N4 O34 Zn2' _chemical_formula_weight 1724.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'C2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 27.6940(8) _cell_length_b 19.5100(9) _cell_length_c 32.5980(13) _cell_angle_alpha 90.00 _cell_angle_beta 92.724(3) _cell_angle_gamma 90.00 _cell_volume 17593.1(12) _cell_formula_units_Z 8 _cell_measurement_temperature 115 _cell_measurement_reflns_used 13909 _cell_measurement_theta_min 1.25 _cell_measurement_theta_max 25.0 _exptl_crystal_description 'chunks' _exptl_crystal_colour 'purple' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.302 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7264 _exptl_absorpt_coefficient_mu 0.628 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; Poorly diffracting crystals with relatively large mosaicity. ; _diffrn_ambient_temperature 115 _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '0.7 degrees Phi scans' _diffrn_detector_area_resol_mean '56 microns' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13909 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0802 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 1.25 _diffrn_reflns_theta_max 25.02 _reflns_number_total 13909 _reflns_number_gt 5931 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement 'Denzo' _computing_data_reduction 'Denzo' _computing_structure_solution 'DIRDIF-96' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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. Only one molecule of the ethylene glycol solvent which coordinates to zinc could be located. The contribution of the other molecules of the solvent was subtracted from the diffraction data by the Squeeze procedure using PLATON. ; _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^)+(0.0726P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13909 _refine_ls_number_parameters 598 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1497 _refine_ls_R_factor_gt 0.0758 _refine_ls_wR_factor_ref 0.1652 _refine_ls_wR_factor_gt 0.1435 _refine_ls_goodness_of_fit_ref 0.910 _refine_ls_restrained_S_all 0.910 _refine_ls_shift/su_max 0.975 _refine_ls_shift/su_mean 0.084 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 N1 N 0.42224(14) 0.7588(2) 0.38293(11) 0.0530(12) Uani 1 1 d . . . N2 N 0.36219(13) 0.8025(2) 0.44826(12) 0.0521(11) Uani 1 1 d . . . N3 N 0.41893(14) 0.7202(2) 0.50547(11) 0.0539(12) Uani 1 1 d . . . N4 N 0.48136(13) 0.6816(2) 0.44140(11) 0.0526(11) Uani 1 1 d . . . C5 C 0.50734(18) 0.6687(3) 0.40680(15) 0.0570(15) Uani 1 1 d . . . C6 C 0.49549(18) 0.6945(3) 0.36784(14) 0.0540(15) Uani 1 1 d . . . C7 C 0.4570(2) 0.7362(3) 0.35672(15) 0.0616(16) Uani 1 1 d . . . C8 C 0.4450(2) 0.7630(3) 0.31635(14) 0.079(2) Uani 1 1 d . . . H8 H 0.4620 0.7548 0.2929 0.095 Uiso 1 1 calc R . . C9 C 0.4058(2) 0.8014(3) 0.31820(14) 0.0676(17) Uani 1 1 d . . . H9 H 0.3907 0.8251 0.2964 0.081 Uiso 1 1 calc R . . C10 C 0.39060(18) 0.8002(3) 0.36017(14) 0.0550(15) Uani 1 1 d . . . C11 C 0.35192(18) 0.8361(3) 0.37437(14) 0.0519(14) Uani 1 1 d . . . C12 C 0.33864(18) 0.8386(3) 0.41644(15) 0.0600(15) Uani 1 1 d . . . C13 C 0.29755(17) 0.8741(3) 0.43258(16) 0.0618(15) Uani 1 1 d . . . H13 H 0.2754 0.9009 0.4174 0.074 Uiso 1 1 calc R . . C14 C 0.2969(2) 0.8617(3) 0.47321(16) 0.0628(16) Uani 1 1 d . . . H14 H 0.2749 0.8788 0.4913 0.075 Uiso 1 1 calc R . . C15 C 0.33667(19) 0.8172(3) 0.48306(14) 0.0576(15) Uani 1 1 d . . . C16 C 0.34857(19) 0.7900(3) 0.52207(14) 0.0557(15) Uani 1 1 d . . . C17 C 0.38673(19) 0.7465(3) 0.53181(14) 0.0573(16) Uani 1 1 d . . . C18 C 0.4000(2) 0.7204(3) 0.57177(14) 0.0709(17) Uani 1 1 d . . . H18 H 0.3835 0.7297 0.5953 0.085 Uiso 1 1 calc R . . C19 C 0.4394(2) 0.6811(3) 0.57078(15) 0.0714(18) Uani 1 1 d . . . H19 H 0.4556 0.6587 0.5926 0.086 Uiso 1 1 calc R . . C20 C 0.45117(18) 0.6812(3) 0.52818(15) 0.0562(15) Uani 1 1 d . . . C21 C 0.49224(18) 0.6481(3) 0.51408(14) 0.0546(15) Uani 1 1 d . . . C22 C 0.50646(18) 0.6481(3) 0.47362(15) 0.0568(15) Uani 1 1 d . . . C23 C 0.54866(18) 0.6158(3) 0.45996(15) 0.0622(16) Uani 1 1 d . . . H23 H 0.5710 0.5900 0.4756 0.075 Uiso 1 1 calc R . . C24 C 0.54944(18) 0.6305(3) 0.41886(16) 0.0622(16) Uani 1 1 d . . . H24 H 0.5736 0.6176 0.4016 0.075 Uiso 1 1 calc R . . C25 C 0.52957(19) 0.6755(3) 0.33456(15) 0.0611(16) Uani 1 1 d . . . C26 C 0.5282(2) 0.6157(4) 0.31532(18) 0.096(2) Uani 1 1 d . . . H26 H 0.5051 0.5831 0.3216 0.116 Uiso 1 1 calc R . . C27 C 0.5617(2) 0.6015(4) 0.28526(18) 0.097(2) Uani 1 1 d . . . H27 H 0.5620 0.5584 0.2731 0.116 Uiso 1 1 calc R . . C28 C 0.59355(19) 0.6498(4) 0.27384(15) 0.0604(17) Uani 1 1 d . . . C29 C 0.5949(3) 0.7112(4) 0.2931(2) 0.122(3) Uani 1 1 d . . . H29 H 0.6176 0.7438 0.2860 0.146 Uiso 1 1 calc R . . C30 C 0.5628(2) 0.7263(4) 0.3233(2) 0.111(3) Uani 1 1 d . . . H30 H 0.5632 0.7691 0.3359 0.133 Uiso 1 1 calc R . . C31 C 0.6286(2) 0.6296(4) 0.24136(16) 0.0673(19) Uani 1 1 d . . . O32 O 0.65803(16) 0.6782(2) 0.23243(12) 0.0912(14) Uani 1 1 d . . . H32 H 0.6645 0.6631 0.2046 0.40(8) Uiso 1 1 d R . . O33 O 0.62690(13) 0.5721(2) 0.22627(10) 0.0688(12) Uani 1 1 d . . . C34 C 0.3225(2) 0.8762(4) 0.34513(16) 0.0573(15) Uani 1 1 d . . . C35 C 0.2950(2) 0.8469(3) 0.31460(17) 0.0709(17) Uani 1 1 d . . . H35 H 0.2944 0.7994 0.3123 0.085 Uiso 1 1 calc R . . C36 C 0.2678(2) 0.8862(4) 0.28674(16) 0.0688(17) Uani 1 1 d . . . H36 H 0.2502 0.8644 0.2655 0.083 Uiso 1 1 calc R . . C37 C 0.26604(19) 0.9548(4) 0.28953(16) 0.0615(17) Uani 1 1 d . . . C38 C 0.2926(2) 0.9874(3) 0.31992(17) 0.0700(17) Uani 1 1 d . . . H38 H 0.2920 1.0349 0.3222 0.084 Uiso 1 1 calc R . . C39 C 0.3209(2) 0.9473(4) 0.34782(16) 0.0742(18) Uani 1 1 d . . . H39 H 0.3392 0.9690 0.3687 0.089 Uiso 1 1 calc R . . C40 C 0.2361(2) 1.0002(4) 0.25995(18) 0.0705(19) Uani 1 1 d . . . O41 O 0.23639(17) 1.0624(3) 0.26108(13) 0.0912(15) Uani 1 1 d . . . O42 O 0.20958(13) 0.9633(3) 0.23240(11) 0.0746(12) Uani 1 1 d . . . H42 H 0.2071 0.9148 0.2362 0.45(9) Uiso 1 1 d R . . C43 C 0.31678(18) 0.8137(3) 0.55622(14) 0.0585(16) Uani 1 1 d . . . C44 C 0.2855(2) 0.7660(3) 0.57161(17) 0.0778(18) Uani 1 1 d . . . H44 H 0.2831 0.7222 0.5604 0.093 Uiso 1 1 calc R . . C45 C 0.25685(19) 0.7854(4) 0.60514(17) 0.081(2) Uani 1 1 d . . . H45 H 0.2366 0.7536 0.6169 0.097 Uiso 1 1 calc R . . C46 C 0.2595(2) 0.8523(3) 0.62007(15) 0.0592(15) Uani 1 1 d . . . C47 C 0.2909(2) 0.8965(3) 0.60312(16) 0.0757(19) Uani 1 1 d . . . H47 H 0.2935 0.9410 0.6133 0.091 Uiso 1 1 calc R . . C48 C 0.3192(2) 0.8771(3) 0.57094(17) 0.0733(18) Uani 1 1 d . . . H48 H 0.3399 0.9087 0.5597 0.088 Uiso 1 1 calc R . . C49 C 0.2277(2) 0.8715(4) 0.65337(16) 0.0634(17) Uani 1 1 d . . . O50 O 0.22505(12) 0.9328(2) 0.66137(10) 0.0654(11) Uani 1 1 d . . . O51 O 0.20520(16) 0.8249(2) 0.67102(13) 0.1048(16) Uani 1 1 d . . . C52 C 0.52364(19) 0.6088(4) 0.54452(15) 0.0571(15) Uani 1 1 d . . . C53 C 0.5180(2) 0.5417(3) 0.55283(16) 0.0619(16) Uani 1 1 d . . . H53 H 0.4933 0.5176 0.5389 0.074 Uiso 1 1 calc R . . C54 C 0.5476(2) 0.5075(3) 0.58115(16) 0.0666(17) Uani 1 1 d . . . H54 H 0.5432 0.4608 0.5853 0.080 Uiso 1 1 calc R . . C55 C 0.58283(19) 0.5412(3) 0.60302(15) 0.0552(15) Uani 1 1 d . . . C56 C 0.5889(2) 0.6092(4) 0.59598(19) 0.085(2) Uani 1 1 d . . . H56 H 0.6129 0.6326 0.6112 0.102 Uiso 1 1 calc R . . C57 C 0.5604(2) 0.6455(4) 0.56658(18) 0.089(2) Uani 1 1 d . . . H57 H 0.5655 0.6919 0.5618 0.106 Uiso 1 1 calc R . . C58 C 0.6150(2) 0.5072(4) 0.63455(19) 0.0679(18) Uani 1 1 d . . . O59 O 0.63893(13) 0.5401(2) 0.66098(11) 0.0720(12) Uani 1 1 d . . . O60 O 0.61872(13) 0.4415(2) 0.63240(9) 0.0719(11) Uani 1 1 d . . . Zn61 Zn 0.41524(2) 0.72883(3) 0.442892(16) 0.0538(2) Uani 1 1 d . . . Zn62 Zn 0.17584(2) 1.02710(3) 0.194731(16) 0.0538(2) Uani 1 1 d . . . O63 O 0.37163(12) 0.64165(19) 0.43178(9) 0.0687(11) Uani 1 1 d . . . H63 H 0.3836 0.6240 0.4023 0.082 Uiso 1 1 d R . . C64 C 0.3340(2) 0.6144(4) 0.4580(2) 0.109(2) Uani 1 1 d . . . H64A H 0.3092 0.5918 0.4409 0.131 Uiso 1 1 calc R . . H64B H 0.3190 0.6521 0.4720 0.131 Uiso 1 1 calc R . . C65 C 0.3548(3) 0.5641(4) 0.4895(2) 0.125(3) Uani 1 1 d . . . H65A H 0.3696 0.5255 0.4761 0.150 Uiso 1 1 calc R . . H65B H 0.3788 0.5860 0.5076 0.150 Uiso 1 1 calc R . . O66 O 0.3139(2) 0.5419(3) 0.51196(19) 0.159(2) Uani 1 1 d . . . H66 H 0.2912 0.5094 0.4927 0.56(14) Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.049(3) 0.073(3) 0.037(2) 0.005(2) 0.006(2) 0.012(2) N2 0.046(3) 0.063(3) 0.048(3) -0.002(2) 0.011(2) 0.011(2) N3 0.042(2) 0.092(4) 0.028(2) -0.001(2) 0.003(2) 0.013(3) N4 0.044(2) 0.080(3) 0.034(2) 0.004(2) 0.001(2) 0.006(2) C5 0.047(3) 0.078(4) 0.047(4) 0.007(3) 0.015(3) 0.003(3) C6 0.055(3) 0.077(4) 0.031(3) 0.005(3) 0.020(3) 0.012(3) C7 0.068(4) 0.079(4) 0.039(3) -0.004(3) 0.014(3) 0.025(3) C8 0.079(4) 0.138(6) 0.021(3) 0.010(3) 0.012(3) 0.028(4) C9 0.074(4) 0.098(5) 0.031(3) 0.004(3) 0.003(3) 0.019(4) C10 0.051(3) 0.075(4) 0.039(3) 0.001(3) -0.002(3) 0.012(3) C11 0.051(3) 0.072(4) 0.032(3) 0.003(3) -0.006(3) 0.022(3) C12 0.050(3) 0.077(5) 0.051(4) 0.009(3) -0.015(3) 0.008(3) C13 0.043(3) 0.074(4) 0.067(4) -0.006(3) -0.010(3) 0.021(3) C14 0.069(4) 0.073(4) 0.047(4) 0.001(3) 0.005(3) 0.016(3) C15 0.054(3) 0.085(5) 0.035(3) -0.007(3) 0.014(3) 0.002(3) C16 0.061(4) 0.078(5) 0.028(3) 0.002(3) -0.001(3) 0.004(3) C17 0.067(4) 0.083(5) 0.023(3) 0.008(3) 0.010(3) 0.014(3) C18 0.083(4) 0.099(5) 0.033(3) 0.004(3) 0.022(3) 0.012(4) C19 0.069(4) 0.100(5) 0.046(4) 0.013(3) 0.008(3) 0.039(4) C20 0.040(3) 0.091(5) 0.038(3) 0.000(3) 0.009(3) 0.012(3) C21 0.052(3) 0.085(5) 0.026(3) 0.007(3) -0.004(3) -0.001(3) C22 0.044(3) 0.084(5) 0.042(3) -0.005(3) 0.001(3) 0.012(3) C23 0.056(4) 0.092(5) 0.039(3) 0.013(3) 0.010(3) 0.011(3) C24 0.044(3) 0.077(4) 0.066(4) 0.004(3) 0.013(3) 0.011(3) C25 0.056(4) 0.088(5) 0.039(3) -0.002(3) 0.005(3) 0.004(4) C26 0.105(5) 0.116(6) 0.072(4) -0.039(4) 0.050(4) -0.033(5) C27 0.105(5) 0.102(6) 0.086(5) -0.035(4) 0.031(5) -0.004(5) C28 0.056(4) 0.088(5) 0.039(3) 0.025(3) 0.022(3) 0.011(4) C29 0.147(7) 0.085(6) 0.142(7) -0.036(5) 0.089(6) -0.027(5) C30 0.137(6) 0.103(6) 0.102(5) -0.013(4) 0.087(5) 0.002(5) C31 0.067(4) 0.101(7) 0.034(4) 0.021(4) 0.006(3) 0.014(5) O32 0.125(4) 0.082(3) 0.071(3) 0.011(2) 0.060(3) 0.016(3) O33 0.065(3) 0.095(4) 0.047(2) -0.018(2) 0.0116(19) 0.005(3) C34 0.066(4) 0.066(5) 0.040(3) 0.006(3) 0.003(3) 0.015(4) C35 0.092(5) 0.072(5) 0.048(4) 0.008(3) -0.003(3) 0.012(4) C36 0.078(4) 0.079(5) 0.047(4) -0.003(4) -0.019(3) 0.022(4) C37 0.052(4) 0.090(6) 0.041(3) 0.011(4) -0.017(3) 0.015(4) C38 0.076(4) 0.072(5) 0.060(4) 0.003(3) -0.020(3) 0.002(4) C39 0.081(4) 0.095(6) 0.045(3) 0.000(4) -0.015(3) 0.010(4) C40 0.056(4) 0.108(6) 0.048(4) 0.007(4) 0.005(3) 0.000(5) O41 0.115(4) 0.066(3) 0.091(3) 0.008(3) -0.014(3) 0.019(3) O42 0.072(3) 0.097(4) 0.053(2) 0.023(2) -0.005(2) 0.002(2) C43 0.053(3) 0.085(5) 0.039(3) 0.002(3) 0.012(3) 0.012(4) C44 0.076(4) 0.078(5) 0.081(4) -0.007(4) 0.019(4) -0.012(4) C45 0.066(4) 0.116(6) 0.064(4) -0.006(4) 0.035(3) 0.009(4) C46 0.071(4) 0.069(5) 0.038(3) -0.012(3) 0.007(3) 0.008(4) C47 0.090(4) 0.089(5) 0.051(4) -0.022(3) 0.028(4) -0.022(4) C48 0.079(4) 0.067(5) 0.077(4) -0.013(4) 0.035(4) -0.005(4) C49 0.059(4) 0.089(6) 0.044(4) -0.009(4) 0.024(3) 0.008(4) O50 0.058(2) 0.078(3) 0.062(2) -0.024(2) 0.0187(19) 0.006(2) O51 0.127(4) 0.096(4) 0.100(3) 0.001(3) 0.087(3) 0.014(3) C52 0.051(4) 0.078(5) 0.041(3) 0.000(3) 0.003(3) 0.019(4) C53 0.068(4) 0.062(5) 0.055(4) -0.013(3) -0.008(3) -0.009(4) C54 0.065(4) 0.082(5) 0.050(3) 0.006(3) -0.020(3) 0.006(4) C55 0.054(4) 0.067(5) 0.042(3) 0.008(3) -0.019(3) 0.010(4) C56 0.082(5) 0.086(6) 0.084(5) 0.016(4) -0.029(4) -0.006(4) C57 0.090(5) 0.095(6) 0.077(4) 0.022(4) -0.043(4) -0.014(4) C58 0.075(5) 0.063(5) 0.067(4) 0.016(4) 0.013(4) 0.024(4) O59 0.076(3) 0.085(3) 0.053(2) -0.012(2) -0.023(2) -0.012(2) O60 0.083(3) 0.092(3) 0.038(2) -0.001(2) -0.0176(19) 0.009(3) Zn61 0.0516(4) 0.0797(5) 0.0307(3) 0.0022(3) 0.0078(3) 0.0090(4) Zn62 0.0534(4) 0.0732(5) 0.0352(3) 0.0027(3) 0.0052(3) 0.0004(4) O63 0.063(2) 0.101(3) 0.045(2) -0.002(2) 0.0231(19) -0.002(2) C64 0.113(6) 0.124(7) 0.090(5) -0.001(5) -0.003(5) -0.007(5) C65 0.131(7) 0.141(8) 0.104(6) 0.026(5) 0.018(6) -0.011(6) O66 0.159(5) 0.167(6) 0.153(5) 0.031(4) 0.038(5) -0.005(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C10 1.382(6) . ? N1 C7 1.388(5) . ? N1 Zn61 2.058(4) . ? N2 C12 1.389(6) . ? N2 C15 1.394(5) . ? N2 Zn61 2.069(4) . ? N3 C20 1.364(6) . ? N3 C17 1.367(6) . ? N3 Zn61 2.044(3) . ? N4 C5 1.389(5) . ? N4 C22 1.394(6) . ? N4 Zn61 2.053(4) . ? C5 C6 1.391(6) . ? C5 C24 1.423(7) . ? C6 C7 1.377(6) . ? C6 C25 1.517(7) . ? C7 C8 1.440(7) . ? C8 C9 1.323(7) . ? C8 H8 0.9300 . ? C9 C10 1.451(6) . ? C9 H9 0.9300 . ? C10 C11 1.378(6) . ? C11 C12 1.437(6) . ? C11 C34 1.453(7) . ? C12 C13 1.452(6) . ? C13 C14 1.347(6) . ? C13 H13 0.9300 . ? C14 C15 1.427(7) . ? C14 H14 0.9300 . ? C15 C16 1.403(6) . ? C16 C17 1.381(6) . ? C16 C43 1.524(7) . ? C17 C18 1.430(6) . ? C18 C19 1.336(6) . ? C18 H18 0.9300 . ? C19 C20 1.441(6) . ? C19 H19 0.9300 . ? C20 C21 1.405(6) . ? C21 C22 1.394(6) . ? C21 C52 1.499(7) . ? C22 C23 1.418(6) . ? C23 C24 1.372(6) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 C26 1.324(7) . ? C25 C30 1.413(8) . ? C26 C27 1.409(7) . ? C26 H26 0.9300 . ? C27 C28 1.354(7) . ? C27 H27 0.9300 . ? C28 C29 1.352(8) . ? C28 C31 1.521(7) . ? C29 C30 1.390(7) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 O33 1.225(7) . ? C31 O32 1.293(7) . ? O32 H32 0.9773 . ? O33 Zn62 1.949(4) 3_545 ? C34 C35 1.350(7) . ? C34 C39 1.391(7) . ? C35 C36 1.384(7) . ? C35 H35 0.9300 . ? C36 C37 1.344(7) . ? C36 H36 0.9300 . ? C37 C38 1.362(7) . ? C37 C40 1.525(8) . ? C38 C39 1.411(7) . ? C38 H38 0.9300 . ? C39 H39 0.9300 . ? C40 O41 1.214(7) . ? C40 O42 1.343(7) . ? O42 Zn62 1.954(4) . ? O42 H42 0.9591 . ? C43 C48 1.327(7) . ? C43 C44 1.382(7) . ? C44 C45 1.432(7) . ? C44 H44 0.9300 . ? C45 C46 1.394(7) . ? C45 H45 0.9300 . ? C46 C47 1.361(7) . ? C46 C49 1.479(7) . ? C47 C48 1.392(7) . ? C47 H47 0.9300 . ? C48 H48 0.9300 . ? C49 O50 1.226(6) . ? C49 O51 1.257(6) . ? O50 Zn62 1.948(3) 6_576 ? C52 C53 1.347(7) . ? C52 C57 1.413(7) . ? C53 C54 1.376(7) . ? C53 H53 0.9300 . ? C54 C55 1.352(7) . ? C54 H54 0.9300 . ? C55 C56 1.358(7) . ? C55 C58 1.485(8) . ? C56 C57 1.405(7) . ? C56 H56 0.9300 . ? C57 H57 0.9300 . ? C58 O59 1.240(7) . ? C58 O60 1.288(6) . ? O59 Zn62 1.967(4) 8_566 ? Zn61 O63 2.108(4) . ? Zn62 O50 1.948(3) 6_575 ? Zn62 O33 1.949(4) 3_455 ? Zn62 O59 1.967(4) 8_465 ? O63 C64 1.478(7) . ? O63 H63 1.0871 . ? C64 C65 1.514(8) . ? C64 H64A 0.9700 . ? C64 H64B 0.9700 . ? C65 O66 1.444(7) . ? C65 H65A 0.9700 . ? C65 H65B 0.9700 . ? O66 H66 1.0738 . ? 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 C10 N1 C7 107.2(4) . . ? C10 N1 Zn61 126.2(3) . . ? C7 N1 Zn61 126.4(4) . . ? C12 N2 C15 105.4(4) . . ? C12 N2 Zn61 126.7(3) . . ? C15 N2 Zn61 126.9(4) . . ? C20 N3 C17 107.3(4) . . ? C20 N3 Zn61 126.0(3) . . ? C17 N3 Zn61 126.4(3) . . ? C5 N4 C22 105.6(4) . . ? C5 N4 Zn61 126.7(3) . . ? C22 N4 Zn61 127.3(3) . . ? N4 C5 C6 124.6(5) . . ? N4 C5 C24 108.6(4) . . ? C6 C5 C24 126.6(5) . . ? C7 C6 C5 126.9(4) . . ? C7 C6 C25 117.2(4) . . ? C5 C6 C25 115.9(5) . . ? C6 C7 N1 125.2(5) . . ? C6 C7 C8 126.7(5) . . ? N1 C7 C8 108.2(5) . . ? C9 C8 C7 108.5(5) . . ? C9 C8 H8 125.8 . . ? C7 C8 H8 125.7 . . ? C8 C9 C10 108.0(5) . . ? C8 C9 H9 126.0 . . ? C10 C9 H9 126.0 . . ? N1 C10 C11 126.9(4) . . ? N1 C10 C9 108.1(4) . . ? C11 C10 C9 125.0(5) . . ? C10 C11 C12 125.1(5) . . ? C10 C11 C34 118.3(4) . . ? C12 C11 C34 116.6(4) . . ? N2 C12 C11 124.3(5) . . ? N2 C12 C13 108.6(4) . . ? C11 C12 C13 127.0(5) . . ? C14 C13 C12 108.5(5) . . ? C14 C13 H13 125.7 . . ? C12 C13 H13 125.8 . . ? C13 C14 C15 106.5(5) . . ? C13 C14 H14 126.7 . . ? C15 C14 H14 126.7 . . ? N2 C15 C16 123.6(5) . . ? N2 C15 C14 110.9(4) . . ? C16 C15 C14 125.5(5) . . ? C17 C16 C15 125.8(4) . . ? C17 C16 C43 118.8(4) . . ? C15 C16 C43 115.4(5) . . ? N3 C17 C16 127.0(4) . . ? N3 C17 C18 107.0(5) . . ? C16 C17 C18 126.1(5) . . ? C19 C18 C17 110.9(5) . . ? C19 C18 H18 124.5 . . ? C17 C18 H18 124.5 . . ? C18 C19 C20 104.1(5) . . ? C18 C19 H19 127.9 . . ? C20 C19 H19 128.0 . . ? N3 C20 C21 126.8(4) . . ? N3 C20 C19 110.6(4) . . ? C21 C20 C19 122.5(5) . . ? C22 C21 C20 125.4(5) . . ? C22 C21 C52 116.5(4) . . ? C20 C21 C52 118.2(4) . . ? N4 C22 C21 124.1(4) . . ? N4 C22 C23 111.1(4) . . ? C21 C22 C23 124.8(5) . . ? C24 C23 C22 105.4(5) . . ? C24 C23 H23 127.3 . . ? C22 C23 H23 127.3 . . ? C23 C24 C5 109.2(4) . . ? C23 C24 H24 125.4 . . ? C5 C24 H24 125.4 . . ? C26 C25 C30 120.0(5) . . ? C26 C25 C6 123.3(6) . . ? C30 C25 C6 116.6(6) . . ? C25 C26 C27 119.8(6) . . ? C25 C26 H26 120.1 . . ? C27 C26 H26 120.1 . . ? C28 C27 C26 120.9(6) . . ? C28 C27 H27 119.6 . . ? C26 C27 H27 119.5 . . ? C27 C28 C29 119.5(5) . . ? C27 C28 C31 117.1(6) . . ? C29 C28 C31 123.3(6) . . ? C28 C29 C30 120.8(6) . . ? C28 C29 H29 119.6 . . ? C30 C29 H29 119.6 . . ? C29 C30 C25 118.8(6) . . ? C29 C30 H30 120.6 . . ? C25 C30 H30 120.6 . . ? O33 C31 O32 126.3(6) . . ? O33 C31 C28 120.3(7) . . ? O32 C31 C28 113.4(7) . . ? C31 O32 H32 97.6 . . ? C31 O33 Zn62 127.6(4) . 3_545 ? C35 C34 C39 116.8(6) . . ? C35 C34 C11 122.3(6) . . ? C39 C34 C11 120.9(6) . . ? C34 C35 C36 121.3(6) . . ? C34 C35 H35 119.3 . . ? C36 C35 H35 119.3 . . ? C37 C36 C35 121.8(6) . . ? C37 C36 H36 119.1 . . ? C35 C36 H36 119.1 . . ? C36 C37 C38 119.6(6) . . ? C36 C37 C40 123.8(6) . . ? C38 C37 C40 116.5(7) . . ? C37 C38 C39 118.3(6) . . ? C37 C38 H38 120.8 . . ? C39 C38 H38 120.8 . . ? C34 C39 C38 122.1(6) . . ? C34 C39 H39 119.0 . . ? C38 C39 H39 119.0 . . ? O41 C40 O42 123.9(7) . . ? O41 C40 C37 124.0(7) . . ? O42 C40 C37 112.0(6) . . ? C40 O42 Zn62 108.0(4) . . ? C40 O42 H42 119.0 . . ? Zn62 O42 H42 132.4 . . ? C48 C43 C44 121.2(5) . . ? C48 C43 C16 121.7(5) . . ? C44 C43 C16 117.1(6) . . ? C43 C44 C45 118.6(6) . . ? C43 C44 H44 120.7 . . ? C45 C44 H44 120.7 . . ? C46 C45 C44 119.5(5) . . ? C46 C45 H45 120.3 . . ? C44 C45 H45 120.2 . . ? C47 C46 C45 118.5(5) . . ? C47 C46 C49 123.5(6) . . ? C45 C46 C49 118.0(6) . . ? C46 C47 C48 121.7(6) . . ? C46 C47 H47 119.1 . . ? C48 C47 H47 119.1 . . ? C43 C48 C47 120.4(5) . . ? C43 C48 H48 119.8 . . ? C47 C48 H48 119.8 . . ? O50 C49 O51 124.9(5) . . ? O50 C49 C46 116.5(6) . . ? O51 C49 C46 118.6(6) . . ? C49 O50 Zn62 124.1(4) . 6_576 ? C53 C52 C57 118.6(6) . . ? C53 C52 C21 124.1(6) . . ? C57 C52 C21 117.3(6) . . ? C52 C53 C54 122.3(6) . . ? C52 C53 H53 118.8 . . ? C54 C53 H53 118.8 . . ? C55 C54 C53 120.7(6) . . ? C55 C54 H54 119.7 . . ? C53 C54 H54 119.6 . . ? C54 C55 C56 118.5(6) . . ? C54 C55 C58 122.9(6) . . ? C56 C55 C58 118.6(6) . . ? C55 C56 C57 122.6(6) . . ? C55 C56 H56 118.7 . . ? C57 C56 H56 118.7 . . ? C56 C57 C52 117.3(6) . . ? C56 C57 H57 121.3 . . ? C52 C57 H57 121.4 . . ? O59 C58 O60 120.8(6) . . ? O59 C58 C55 122.2(6) . . ? O60 C58 C55 117.0(7) . . ? C58 O59 Zn62 106.8(4) . 8_566 ? N3 Zn61 N4 89.11(16) . . ? N3 Zn61 N1 165.57(17) . . ? N4 Zn61 N1 88.90(15) . . ? N3 Zn61 N2 88.55(16) . . ? N4 Zn61 N2 162.16(16) . . ? N1 Zn61 N2 88.98(16) . . ? N3 Zn61 O63 96.09(15) . . ? N4 Zn61 O63 97.93(15) . . ? N1 Zn61 O63 98.34(14) . . ? N2 Zn61 O63 99.90(14) . . ? O50 Zn62 O33 129.49(18) 6_575 3_455 ? O50 Zn62 O42 106.29(15) 6_575 . ? O33 Zn62 O42 106.20(15) 3_455 . ? O50 Zn62 O59 108.34(15) 6_575 8_465 ? O33 Zn62 O59 103.85(16) 3_455 8_465 ? O42 Zn62 O59 98.48(19) . 8_465 ? C64 O63 Zn61 127.2(3) . . ? C64 O63 H63 130.6 . . ? Zn61 O63 H63 102.2 . . ? O63 C64 C65 111.6(6) . . ? O63 C64 H64A 109.4 . . ? C65 C64 H64A 109.3 . . ? O63 C64 H64B 109.2 . . ? C65 C64 H64B 109.3 . . ? H64A C64 H64B 108.0 . . ? O66 C65 C64 104.9(6) . . ? O66 C65 H65A 110.8 . . ? C64 C65 H65A 110.8 . . ? O66 C65 H65B 110.8 . . ? C64 C65 H65B 110.7 . . ? H65A C65 H65B 108.9 . . ? C65 O66 H66 109.4 . . ? _diffrn_measured_fraction_theta_max 0.926 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.926 _refine_diff_density_max 0.265 _refine_diff_density_min -0.266 _refine_diff_density_rms 0.056 #=== END #====================================================================