# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Chao Qin' _publ_contact_author_email QINC703@HOTMAIL.COM _publ_section_title ; Two unusual self-threading frameworks self-assembled from mixed ligands and transition metal ions ; loop_ _publ_author_name 'Chao Qin' 'Jie Qin' 'Zhong-Min Su' 'Cui-Xia Wang' 'Xin-Long Wang' ; Shuang Wang ; # Attachment 'com-11.cif' data_www _database_code_depnum_ccdc_archive 'CCDC 768676' #TrackingRef 'com-11.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H62 Co3 F2 N6 O26' _chemical_formula_weight 1545.99 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 21/c' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.853(3) _cell_length_b 13.391(3) _cell_length_c 18.438(7) _cell_angle_alpha 90.00 _cell_angle_beta 119.54(2) _cell_angle_gamma 90.00 _cell_volume 2975.7(15) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 22996 _cell_measurement_theta_min 3.04 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.725 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1590 _exptl_absorpt_coefficient_mu 0.932 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7423 _exptl_absorpt_correction_T_max 0.8004 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22996 _diffrn_reflns_av_R_equivalents 0.0302 _diffrn_reflns_av_sigmaI/netI 0.0223 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5229 _reflns_number_gt 4537 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material SHELXL-97 _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^)+(0.0470P)^2^+2.0190P] 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 5229 _refine_ls_number_parameters 465 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0365 _refine_ls_R_factor_gt 0.0305 _refine_ls_wR_factor_ref 0.0799 _refine_ls_wR_factor_gt 0.0773 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.21879(2) 0.47919(2) 0.726584(17) 0.01424(9) Uani 1 1 d . . . Co2 Co 0.5000 0.5000 1.0000 0.01068(10) Uani 1 2 d S . . F1 F 0.67898(13) 0.47955(13) 0.68824(11) 0.0409(4) Uani 1 1 d . . . C1 C -0.12294(18) 0.51494(17) 0.90981(13) 0.0188(5) Uani 1 1 d . . . C2 C -0.06174(19) 0.58607(18) 0.89415(14) 0.0214(5) Uani 1 1 d . . . H2A H -0.0608 0.6522 0.9100 0.026 Uiso 1 1 calc R . . C3 C -0.00283(19) 0.55830(18) 0.85518(14) 0.0222(5) Uani 1 1 d . . . H3A H 0.0380 0.6059 0.8451 0.027 Uiso 1 1 calc R . . C4 C -0.00380(18) 0.45998(18) 0.83078(13) 0.0184(5) Uani 1 1 d . . . C5 C -0.06655(19) 0.38975(18) 0.84486(13) 0.0199(5) Uani 1 1 d . . . H5A H -0.0690 0.3241 0.8275 0.024 Uiso 1 1 calc R . . C6 C -0.12537(19) 0.41655(18) 0.88446(13) 0.0205(5) Uani 1 1 d . . . H6A H -0.1665 0.3689 0.8942 0.025 Uiso 1 1 calc R . . C7 C -0.18061(18) 0.54554(18) 0.95619(13) 0.0195(5) Uani 1 1 d . . . C8 C 0.06440(19) 0.42744(18) 0.79115(13) 0.0203(5) Uani 1 1 d . . . C9 C 0.45888(18) 0.69287(15) 0.79702(12) 0.0138(4) Uani 1 1 d . . . C10 C 0.56953(18) 0.69294(16) 0.81683(13) 0.0181(5) Uani 1 1 d . . . H10A H 0.6207 0.6548 0.8615 0.022 Uiso 1 1 calc R . . C11 C 0.60462(18) 0.74908(16) 0.77094(12) 0.0166(4) Uani 1 1 d . . . H11A H 0.6788 0.7479 0.7845 0.020 Uiso 1 1 calc R . . C12 C 0.52880(17) 0.80717(15) 0.70454(12) 0.0129(4) Uani 1 1 d . . . C13 C 0.41873(18) 0.80909(16) 0.68573(12) 0.0151(4) Uani 1 1 d . . . H13A H 0.3680 0.8488 0.6422 0.018 Uiso 1 1 calc R . . C14 C 0.38366(18) 0.75226(16) 0.73145(12) 0.0149(4) Uani 1 1 d . . . H14A H 0.3096 0.7539 0.7182 0.018 Uiso 1 1 calc R . . C15 C 0.42259(18) 0.62927(15) 0.84677(12) 0.0137(4) Uani 1 1 d . . . C16 C 0.56566(18) 0.86557(15) 0.65239(12) 0.0129(4) Uani 1 1 d . . . C17 C 0.10461(17) 0.61012(16) 0.57418(12) 0.0154(4) Uani 1 1 d . . . C18 C 0.21001(18) 0.67634(17) 0.51143(13) 0.0189(5) Uani 1 1 d . . . H18A H 0.1460 0.7131 0.4788 0.023 Uiso 1 1 calc R . . C19 C 0.20781(18) 0.61094(16) 0.56796(13) 0.0156(4) Uani 1 1 d . . . C20 C 0.30518(18) 0.55338(15) 0.61883(12) 0.0144(4) Uani 1 1 d . . . C21 C 0.39790(18) 0.56912(16) 0.60436(12) 0.0146(4) Uani 1 1 d . . . C22 C 0.39382(17) 0.63725(16) 0.54481(12) 0.0143(4) Uani 1 1 d . . . C23 C 0.2792(2) 0.76473(18) 0.43356(14) 0.0242(5) Uani 1 1 d . . . H23A H 0.2404 0.8227 0.4378 0.029 Uiso 1 1 calc R . . H23B H 0.3509 0.7866 0.4422 0.029 Uiso 1 1 calc R . . C24 C 0.2148(3) 0.7211(2) 0.34920(17) 0.0532(9) Uani 1 1 d . . . H24A H 0.2055 0.7702 0.3083 0.080 Uiso 1 1 calc R . . H24B H 0.1434 0.7004 0.3401 0.080 Uiso 1 1 calc R . . H24C H 0.2538 0.6645 0.3444 0.080 Uiso 1 1 calc R . . C25 C 0.49720(19) 0.51712(17) 0.65273(14) 0.0197(5) Uani 1 1 d . . . H25A H 0.5023 0.4711 0.6923 0.024 Uiso 1 1 calc R . . C26 C 0.58568(19) 0.53379(18) 0.64192(14) 0.0214(5) Uani 1 1 d . . . C27 C 0.58516(18) 0.60271(16) 0.58376(13) 0.0171(4) Uani 1 1 d . . . C28 C 0.48652(18) 0.65311(16) 0.53524(13) 0.0166(4) Uani 1 1 d . . . H28A H 0.4819 0.6985 0.4955 0.020 Uiso 1 1 calc R . . C29 C 0.78201(19) 0.6446(2) 0.65324(14) 0.0245(5) Uani 1 1 d . . . H29A H 0.7891 0.6053 0.6998 0.029 Uiso 1 1 calc R . . H29B H 0.7769 0.7144 0.6650 0.029 Uiso 1 1 calc R . . C30 C 0.88330(19) 0.62888(19) 0.64331(14) 0.0234(5) Uani 1 1 d . . . H30A H 0.9492 0.6511 0.6933 0.028 Uiso 1 1 calc R . . H30B H 0.8917 0.5584 0.6357 0.028 Uiso 1 1 calc R . . C31 C 0.66748(18) 0.67379(17) 0.50516(13) 0.0184(5) Uani 1 1 d . . . H31A H 0.6606 0.7440 0.5148 0.022 Uiso 1 1 calc R . . H31B H 0.6007 0.6535 0.4550 0.022 Uiso 1 1 calc R . . C32 C 0.76695(18) 0.65829(18) 0.49391(13) 0.0200(5) Uani 1 1 d . . . H32A H 0.7705 0.5888 0.4805 0.024 Uiso 1 1 calc R . . H32B H 0.7591 0.6987 0.4476 0.024 Uiso 1 1 calc R . . N1 N 0.87128(16) 0.68575(16) 0.57035(12) 0.0187(4) Uani 1 1 d . . . N2 N 0.68004(15) 0.61475(14) 0.57623(11) 0.0172(4) Uani 1 1 d . . . N3 N 0.29585(15) 0.69165(14) 0.49927(11) 0.0189(4) Uani 1 1 d . . . O1 O -0.24044(15) 0.47322(13) 0.96317(11) 0.0297(4) Uani 1 1 d . . . H1 H -0.2695 0.4932 0.9918 0.045 Uiso 1 1 d R . . O2 O -0.17360(14) 0.62797(13) 0.98506(10) 0.0261(4) Uani 1 1 d . . . O3 O 0.05907(17) 0.33848(14) 0.77075(13) 0.0384(5) Uani 1 1 d . . . O4 O 0.12314(13) 0.49365(12) 0.78301(9) 0.0202(3) Uani 1 1 d . . . O5 O 0.32462(12) 0.59783(11) 0.81311(9) 0.0162(3) Uani 1 1 d . . . O6 O 0.49451(12) 0.61429(11) 0.92218(9) 0.0167(3) Uani 1 1 d . . . O7 O 0.49168(12) 0.89745(11) 0.58325(8) 0.0163(3) Uani 1 1 d . . . O8 O 0.66916(12) 0.87644(11) 0.68010(9) 0.0147(3) Uani 1 1 d . . . O9 O 0.10466(13) 0.56984(13) 0.63576(9) 0.0236(4) Uani 1 1 d . . . O10 O 0.02042(13) 0.65368(13) 0.51787(9) 0.0228(4) Uani 1 1 d . . . O11 O 0.31527(13) 0.49020(11) 0.67306(9) 0.0174(3) Uani 1 1 d . . . O1W O 0.12951(13) 0.35017(12) 0.65826(9) 0.0219(4) Uani 1 1 d . . . H2 H 0.1016 0.3349 0.6888 0.033 Uiso 1 1 d R . . H3 H 0.0797 0.3552 0.6074 0.033 Uiso 1 1 d R . . O2W O 0.67497(12) 0.51273(11) 1.06130(9) 0.0159(3) Uani 1 1 d . . . H4 H 0.6919 0.4650 1.0959 0.024 Uiso 1 1 d R . . H5 H 0.6908 0.5578 1.0980 0.024 Uiso 1 1 d R . . H6 H 0.930(2) 0.671(2) 0.5585(16) 0.033(7) Uiso 1 1 d . . . H7 H 0.870(2) 0.747(2) 0.5761(15) 0.023(7) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.01187(16) 0.01985(16) 0.01375(16) 0.00184(11) 0.00843(12) 0.00097(11) Co2 0.0122(2) 0.0124(2) 0.01007(19) 0.00010(14) 0.00751(16) -0.00027(15) F1 0.0216(8) 0.0523(10) 0.0572(10) 0.0342(8) 0.0259(8) 0.0213(7) C1 0.0138(11) 0.0265(12) 0.0155(11) 0.0002(9) 0.0068(9) 0.0009(9) C2 0.0227(12) 0.0221(12) 0.0220(11) 0.0013(9) 0.0131(10) 0.0009(10) C3 0.0188(12) 0.0273(13) 0.0235(12) 0.0064(9) 0.0127(10) 0.0003(10) C4 0.0124(11) 0.0279(12) 0.0144(10) 0.0044(9) 0.0063(9) 0.0037(9) C5 0.0156(11) 0.0261(12) 0.0190(11) -0.0021(9) 0.0092(9) -0.0005(9) C6 0.0155(11) 0.0279(12) 0.0198(11) -0.0020(9) 0.0100(9) -0.0053(9) C7 0.0143(11) 0.0289(13) 0.0143(11) -0.0010(9) 0.0063(9) -0.0006(9) C8 0.0150(11) 0.0271(13) 0.0202(11) 0.0056(9) 0.0098(9) 0.0042(9) C9 0.0181(11) 0.0128(10) 0.0123(10) -0.0013(8) 0.0088(9) -0.0020(8) C10 0.0148(11) 0.0222(11) 0.0147(10) 0.0059(8) 0.0054(9) 0.0018(9) C11 0.0106(11) 0.0225(11) 0.0166(11) 0.0034(9) 0.0067(9) 0.0002(9) C12 0.0145(11) 0.0137(10) 0.0125(10) -0.0016(8) 0.0082(8) -0.0021(8) C13 0.0156(11) 0.0166(11) 0.0120(10) 0.0026(8) 0.0059(8) 0.0013(9) C14 0.0111(10) 0.0197(11) 0.0156(10) -0.0004(8) 0.0079(8) 0.0002(8) C15 0.0185(12) 0.0113(10) 0.0163(11) -0.0016(8) 0.0124(9) 0.0005(8) C16 0.0162(11) 0.0108(10) 0.0137(10) -0.0022(8) 0.0089(9) -0.0014(8) C17 0.0119(11) 0.0181(11) 0.0158(10) -0.0010(8) 0.0064(9) 0.0002(9) C18 0.0117(11) 0.0242(12) 0.0203(11) 0.0044(9) 0.0075(9) 0.0009(9) C19 0.0130(11) 0.0184(11) 0.0156(10) -0.0006(8) 0.0074(9) -0.0009(9) C20 0.0151(11) 0.0154(11) 0.0131(10) -0.0034(8) 0.0072(9) -0.0031(8) C21 0.0137(11) 0.0166(11) 0.0154(10) -0.0016(8) 0.0086(9) 0.0001(8) C22 0.0122(11) 0.0170(11) 0.0137(10) -0.0019(8) 0.0064(8) -0.0015(8) C23 0.0174(12) 0.0299(13) 0.0236(12) 0.0124(10) 0.0088(10) -0.0009(10) C24 0.077(2) 0.0496(19) 0.0300(16) 0.0008(13) 0.0240(16) -0.0297(18) C25 0.0201(12) 0.0213(12) 0.0217(12) 0.0040(9) 0.0133(10) 0.0024(9) C26 0.0140(11) 0.0261(12) 0.0257(12) 0.0068(9) 0.0110(10) 0.0064(9) C27 0.0155(11) 0.0197(11) 0.0201(11) -0.0039(9) 0.0119(9) -0.0026(9) C28 0.0160(11) 0.0195(11) 0.0161(10) 0.0001(8) 0.0094(9) -0.0019(9) C29 0.0136(12) 0.0414(15) 0.0184(11) -0.0022(10) 0.0079(9) -0.0026(10) C30 0.0135(12) 0.0354(14) 0.0221(12) 0.0037(10) 0.0096(10) 0.0010(10) C31 0.0134(11) 0.0241(12) 0.0189(11) 0.0024(9) 0.0089(9) 0.0001(9) C32 0.0153(12) 0.0275(12) 0.0191(11) 0.0002(9) 0.0100(9) -0.0022(9) N1 0.0138(10) 0.0185(11) 0.0262(10) -0.0004(8) 0.0116(8) 0.0003(8) N2 0.0126(9) 0.0236(10) 0.0173(9) 0.0017(7) 0.0090(8) 0.0004(8) N3 0.0125(9) 0.0255(10) 0.0190(9) 0.0066(8) 0.0079(8) 0.0013(8) O1 0.0307(10) 0.0372(10) 0.0370(10) -0.0161(8) 0.0288(9) -0.0133(8) O2 0.0261(9) 0.0274(10) 0.0289(9) -0.0043(7) 0.0167(8) 0.0024(7) O3 0.0469(12) 0.0270(10) 0.0685(13) -0.0038(9) 0.0492(11) -0.0021(9) O4 0.0167(8) 0.0287(9) 0.0199(8) 0.0023(6) 0.0126(7) -0.0007(7) O5 0.0159(8) 0.0170(8) 0.0185(8) -0.0003(6) 0.0105(6) -0.0028(6) O6 0.0170(8) 0.0197(8) 0.0133(7) 0.0037(6) 0.0073(6) -0.0026(6) O7 0.0145(8) 0.0213(8) 0.0128(7) 0.0048(6) 0.0066(6) -0.0013(6) O8 0.0116(8) 0.0181(8) 0.0169(7) 0.0003(6) 0.0089(6) -0.0012(6) O9 0.0158(8) 0.0371(10) 0.0223(8) 0.0116(7) 0.0127(7) 0.0087(7) O10 0.0135(8) 0.0347(9) 0.0216(8) 0.0086(7) 0.0098(7) 0.0062(7) O11 0.0168(8) 0.0212(8) 0.0184(8) 0.0041(6) 0.0119(7) 0.0025(6) O1W 0.0182(8) 0.0302(9) 0.0171(8) -0.0018(6) 0.0085(7) -0.0012(7) O2W 0.0140(8) 0.0220(8) 0.0141(7) -0.0012(6) 0.0088(6) -0.0001(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O11 2.0205(16) . ? Co1 O9 2.0412(16) . ? Co1 O4 2.0579(16) . ? Co1 O1W 2.1367(17) . ? Co1 O8 2.1516(15) 2_646 ? Co1 O5 2.2164(15) . ? Co2 O6 2.0734(14) . ? Co2 O6 2.0734(15) 3_667 ? Co2 O7 2.1046(14) 2_646 ? Co2 O7 2.1046(14) 4_576 ? Co2 O2W 2.1166(16) 3_667 ? Co2 O2W 2.1166(16) . ? F1 C26 1.356(3) . ? C1 C6 1.393(3) . ? C1 C2 1.397(3) . ? C1 C7 1.487(3) . ? C2 C3 1.378(3) . ? C2 H2A 0.9300 . ? C3 C4 1.389(3) . ? C3 H3A 0.9300 . ? C4 C5 1.389(3) . ? C4 C8 1.516(3) . ? C5 C6 1.383(3) . ? C5 H5A 0.9300 . ? C6 H6A 0.9300 . ? C7 O2 1.208(3) . ? C7 O1 1.322(3) . ? C8 O3 1.240(3) . ? C8 O4 1.261(3) . ? C9 C10 1.390(3) . ? C9 C14 1.392(3) . ? C9 C15 1.508(3) . ? C10 C11 1.387(3) . ? C10 H10A 0.9300 . ? C11 C12 1.393(3) . ? C11 H11A 0.9300 . ? C12 C13 1.387(3) . ? C12 C16 1.510(3) . ? C13 C14 1.389(3) . ? C13 H13A 0.9300 . ? C14 H14A 0.9300 . ? C15 O5 1.254(3) . ? C15 O6 1.265(3) . ? C16 O7 1.253(3) . ? C16 O8 1.271(3) . ? C17 O9 1.257(3) . ? C17 O10 1.259(3) . ? C17 C19 1.490(3) . ? C18 N3 1.330(3) . ? C18 C19 1.373(3) . ? C18 H18A 0.9300 . ? C19 C20 1.430(3) . ? C20 O11 1.264(3) . ? C20 C21 1.450(3) . ? C21 C25 1.401(3) . ? C21 C22 1.407(3) . ? C22 C28 1.396(3) . ? C22 N3 1.398(3) . ? C23 C24 1.479(4) . ? C23 N3 1.484(3) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C26 1.354(3) . ? C25 H25A 0.9300 . ? C26 C27 1.412(3) . ? C27 C28 1.385(3) . ? C27 N2 1.397(3) . ? C28 H28A 0.9300 . ? C29 N2 1.481(3) . ? C29 C30 1.517(3) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 N1 1.482(3) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 N2 1.465(3) . ? C31 C32 1.506(3) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 N1 1.484(3) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? N1 H6 0.96(3) . ? N1 H7 0.83(3) . ? O1 H1 0.8496 . ? O7 Co2 2.1046(14) 2_656 ? O8 Co1 2.1516(15) 2_656 ? O1W H2 0.8500 . ? O1W H3 0.8499 . ? O2W H4 0.8500 . ? O2W H5 0.8501 . ? 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 O11 Co1 O9 89.26(6) . . ? O11 Co1 O4 170.36(6) . . ? O9 Co1 O4 85.84(7) . . ? O11 Co1 O1W 95.80(6) . . ? O9 Co1 O1W 90.46(7) . . ? O4 Co1 O1W 92.54(6) . . ? O11 Co1 O8 92.70(6) . 2_646 ? O9 Co1 O8 176.30(6) . 2_646 ? O4 Co1 O8 92.66(6) . 2_646 ? O1W Co1 O8 86.22(6) . 2_646 ? O11 Co1 O5 86.39(6) . . ? O9 Co1 O5 97.71(7) . . ? O4 Co1 O5 86.04(6) . . ? O1W Co1 O5 171.58(6) . . ? O8 Co1 O5 85.55(6) 2_646 . ? O6 Co2 O6 180.0 . 3_667 ? O6 Co2 O7 88.48(6) . 2_646 ? O6 Co2 O7 91.52(6) 3_667 2_646 ? O6 Co2 O7 91.52(6) . 4_576 ? O6 Co2 O7 88.48(6) 3_667 4_576 ? O7 Co2 O7 180.000(1) 2_646 4_576 ? O6 Co2 O2W 92.76(6) . 3_667 ? O6 Co2 O2W 87.24(6) 3_667 3_667 ? O7 Co2 O2W 91.03(6) 2_646 3_667 ? O7 Co2 O2W 88.97(6) 4_576 3_667 ? O6 Co2 O2W 87.24(6) . . ? O6 Co2 O2W 92.76(6) 3_667 . ? O7 Co2 O2W 88.97(6) 2_646 . ? O7 Co2 O2W 91.03(6) 4_576 . ? O2W Co2 O2W 180.00(4) 3_667 . ? C6 C1 C2 119.5(2) . . ? C6 C1 C7 121.5(2) . . ? C2 C1 C7 118.9(2) . . ? C3 C2 C1 120.0(2) . . ? C3 C2 H2A 120.0 . . ? C1 C2 H2A 120.0 . . ? C2 C3 C4 120.7(2) . . ? C2 C3 H3A 119.6 . . ? C4 C3 H3A 119.6 . . ? C3 C4 C5 119.2(2) . . ? C3 C4 C8 121.3(2) . . ? C5 C4 C8 119.5(2) . . ? C6 C5 C4 120.6(2) . . ? C6 C5 H5A 119.7 . . ? C4 C5 H5A 119.7 . . ? C5 C6 C1 120.0(2) . . ? C5 C6 H6A 120.0 . . ? C1 C6 H6A 120.0 . . ? O2 C7 O1 123.0(2) . . ? O2 C7 C1 123.8(2) . . ? O1 C7 C1 113.3(2) . . ? O3 C8 O4 125.8(2) . . ? O3 C8 C4 117.7(2) . . ? O4 C8 C4 116.6(2) . . ? C10 C9 C14 118.96(19) . . ? C10 C9 C15 119.72(19) . . ? C14 C9 C15 121.3(2) . . ? C11 C10 C9 120.9(2) . . ? C11 C10 H10A 119.6 . . ? C9 C10 H10A 119.6 . . ? C10 C11 C12 120.0(2) . . ? C10 C11 H11A 120.0 . . ? C12 C11 H11A 120.0 . . ? C13 C12 C11 119.33(19) . . ? C13 C12 C16 120.41(19) . . ? C11 C12 C16 120.24(19) . . ? C12 C13 C14 120.5(2) . . ? C12 C13 H13A 119.7 . . ? C14 C13 H13A 119.7 . . ? C13 C14 C9 120.3(2) . . ? C13 C14 H14A 119.9 . . ? C9 C14 H14A 119.9 . . ? O5 C15 O6 124.36(19) . . ? O5 C15 C9 119.49(18) . . ? O6 C15 C9 116.11(19) . . ? O7 C16 O8 124.39(19) . . ? O7 C16 C12 117.42(19) . . ? O8 C16 C12 118.15(18) . . ? O9 C17 O10 122.1(2) . . ? O9 C17 C19 119.98(18) . . ? O10 C17 C19 117.85(18) . . ? N3 C18 C19 125.6(2) . . ? N3 C18 H18A 117.2 . . ? C19 C18 H18A 117.2 . . ? C18 C19 C20 118.3(2) . . ? C18 C19 C17 116.39(19) . . ? C20 C19 C17 125.18(19) . . ? O11 C20 C19 125.5(2) . . ? O11 C20 C21 118.71(19) . . ? C19 C20 C21 115.81(18) . . ? C25 C21 C22 117.9(2) . . ? C25 C21 C20 119.43(19) . . ? C22 C21 C20 122.64(19) . . ? C28 C22 N3 121.74(19) . . ? C28 C22 C21 120.8(2) . . ? N3 C22 C21 117.39(19) . . ? C24 C23 N3 111.6(2) . . ? C24 C23 H23A 109.3 . . ? N3 C23 H23A 109.3 . . ? C24 C23 H23B 109.3 . . ? N3 C23 H23B 109.3 . . ? H23A C23 H23B 108.0 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 C21 120.0(2) . . ? C26 C25 H25A 120.0 . . ? C21 C25 H25A 120.0 . . ? C25 C26 F1 118.0(2) . . ? C25 C26 C27 123.6(2) . . ? F1 C26 C27 118.3(2) . . ? C28 C27 N2 123.8(2) . . ? C28 C27 C26 116.3(2) . . ? N2 C27 C26 119.9(2) . . ? C27 C28 C22 121.4(2) . . ? C27 C28 H28A 119.3 . . ? C22 C28 H28A 119.3 . . ? N2 C29 C30 110.40(18) . . ? N2 C29 H29A 109.6 . . ? C30 C29 H29A 109.6 . . ? N2 C29 H29B 109.6 . . ? C30 C29 H29B 109.6 . . ? H29A C29 H29B 108.1 . . ? N1 C30 C29 109.97(19) . . ? N1 C30 H30A 109.7 . . ? C29 C30 H30A 109.7 . . ? N1 C30 H30B 109.7 . . ? C29 C30 H30B 109.7 . . ? H30A C30 H30B 108.2 . . ? N2 C31 C32 109.60(18) . . ? N2 C31 H31A 109.7 . . ? C32 C31 H31A 109.7 . . ? N2 C31 H31B 109.7 . . ? C32 C31 H31B 109.7 . . ? H31A C31 H31B 108.2 . . ? N1 C32 C31 111.35(18) . . ? N1 C32 H32A 109.4 . . ? C31 C32 H32A 109.4 . . ? N1 C32 H32B 109.4 . . ? C31 C32 H32B 109.4 . . ? H32A C32 H32B 108.0 . . ? C30 N1 C32 110.84(18) . . ? C30 N1 H6 111.7(16) . . ? C32 N1 H6 105.5(16) . . ? C30 N1 H7 113.1(17) . . ? C32 N1 H7 107.1(18) . . ? H6 N1 H7 108(2) . . ? C27 N2 C31 116.63(17) . . ? C27 N2 C29 115.79(17) . . ? C31 N2 C29 110.37(18) . . ? C18 N3 C22 120.16(18) . . ? C18 N3 C23 116.57(19) . . ? C22 N3 C23 123.21(18) . . ? C7 O1 H1 110.0 . . ? C8 O4 Co1 127.44(15) . . ? C15 O5 Co1 140.09(13) . . ? C15 O6 Co2 128.17(14) . . ? C16 O7 Co2 130.77(14) . 2_656 ? C16 O8 Co1 128.38(13) . 2_656 ? C17 O9 Co1 130.67(14) . . ? C20 O11 Co1 126.41(14) . . ? Co1 O1W H2 97.1 . . ? Co1 O1W H3 120.3 . . ? H2 O1W H3 111.4 . . ? Co2 O2W H4 99.2 . . ? Co2 O2W H5 105.1 . . ? H4 O2W H5 94.0 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.360 _refine_diff_density_min -0.395 _refine_diff_density_rms 0.058 # Attachment 'com-21.cif' data_www2 _database_code_depnum_ccdc_archive 'CCDC 768677' #TrackingRef 'com-21.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H62 F2 N6 O26 Zn3' _chemical_formula_weight 1565.31 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 21/c' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.859(3) _cell_length_b 13.313(3) _cell_length_c 18.894(7) _cell_angle_alpha 90.00 _cell_angle_beta 119.31(2) _cell_angle_gamma 90.00 _cell_volume 3039.8(15) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 22452 _cell_measurement_theta_min 3.05 _cell_measurement_theta_max 24.99 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.710 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1608 _exptl_absorpt_coefficient_mu 1.278 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7323 _exptl_absorpt_correction_T_max 0.7842 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22452 _diffrn_reflns_av_R_equivalents 0.0689 _diffrn_reflns_av_sigmaI/netI 0.0530 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 24.99 _reflns_number_total 5213 _reflns_number_gt 4000 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material SHELXL-97 _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^)+(0.1600P)^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 5213 _refine_ls_number_parameters 473 _refine_ls_number_restraints 123 _refine_ls_R_factor_all 0.0928 _refine_ls_R_factor_gt 0.0736 _refine_ls_wR_factor_ref 0.2126 _refine_ls_wR_factor_gt 0.1943 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.21750(5) -0.51758(6) -0.27415(4) 0.0221(3) Uani 1 1 d . . . Zn2 Zn 0.5000 -0.5000 0.0000 0.0192(3) Uani 1 2 d S . . F1 F 0.6883(3) -0.5059(3) -0.3042(3) 0.0382(11) Uani 1 1 d U . . O1 O 0.3265(3) -0.3997(3) -0.18644(18) 0.0077(7) Uani 1 1 d U . . O2W O 0.3176(3) -0.5105(3) -0.0658(2) 0.0096(7) Uani 1 1 d . . . H4 H 0.2788 -0.5387 -0.1115 0.014 Uiso 1 1 d R . . H5 H 0.2864 -0.4552 -0.0664 0.014 Uiso 1 1 d R . . O2 O 0.4959(3) -0.3819(3) -0.07967(18) 0.0090(7) Uani 1 1 d U . . O1W O 0.1220(3) -0.6510(3) -0.3442(2) 0.0138(8) Uani 1 1 d U . . H2 H 0.1328 -0.7118 -0.3286 0.021 Uiso 1 1 d R . . H3 H 0.0640 -0.6490 -0.3905 0.021 Uiso 1 1 d R . . O5 O 0.0456(4) -0.6566(4) -0.2386(3) 0.0399(12) Uani 1 1 d . . . O6 O 0.1133(3) -0.5030(3) -0.2210(2) 0.0160(8) Uani 1 1 d U . . O7 O -0.2321(3) -0.5354(4) -0.0298(3) 0.0264(10) Uani 1 1 d DU . . O8 O -0.1751(3) -0.3769(3) -0.0145(2) 0.0205(9) Uani 1 1 d . . . O9 O 0.1074(3) -0.4188(3) -0.3673(2) 0.0173(9) Uani 1 1 d . . . O10 O 0.0220(3) -0.3443(3) -0.4859(2) 0.0134(8) Uani 1 1 d U . . O11 O 0.3164(3) -0.5059(3) -0.3303(2) 0.0092(7) Uani 1 1 d U . . N3 N 0.2985(3) -0.3110(4) -0.5050(3) 0.0148(10) Uani 1 1 d . B . N2 N 0.6860(3) -0.3829(3) -0.4229(2) 0.0099(9) Uani 1 1 d . . . N1 N 0.8741(3) -0.3102(3) -0.4324(2) 0.0100(9) Uani 1 1 d D . . C1 C 0.4605(4) -0.3052(4) -0.2034(3) 0.0065(9) Uiso 1 1 d . . . C2 C 0.3848(4) -0.2498(4) -0.2693(3) 0.0079(10) Uani 1 1 d . . . H2A H 0.3105 -0.2500 -0.2832 0.010 Uiso 1 1 calc R . . C3 C 0.4200(4) -0.1936(4) -0.3150(3) 0.0071(9) Uani 1 1 d U . . H3A H 0.3689 -0.1558 -0.3587 0.009 Uiso 1 1 calc R . . C4 C 0.5308(4) -0.1939(4) -0.2956(3) 0.0076(9) Uani 1 1 d . . . C5 C 0.6068(4) -0.2484(4) -0.2283(3) 0.0071(9) Uani 1 1 d . . . H5A H 0.6812 -0.2478 -0.2141 0.009 Uiso 1 1 calc R . . C6 C 0.5731(4) -0.3033(4) -0.1824(3) 0.0103(10) Uani 1 1 d . . . H6A H 0.6247 -0.3392 -0.1376 0.012 Uiso 1 1 calc R . . C7 C 0.4259(4) -0.3677(4) -0.1534(3) 0.0063(9) Uani 1 1 d . . . C9 C -0.0115(4) -0.5407(4) -0.1718(3) 0.0123(11) Uani 1 1 d U . . C10 C -0.0696(4) -0.6143(4) -0.1551(3) 0.0140(11) Uani 1 1 d . . . H10A H -0.0714 -0.6801 -0.1722 0.017 Uiso 1 1 calc R . . C11 C -0.1242(4) -0.5891(4) -0.1130(3) 0.0119(10) Uani 1 1 d . . . H11A H -0.1616 -0.6380 -0.1008 0.014 Uiso 1 1 calc R . . C12 C -0.1231(4) -0.4890(4) -0.0889(3) 0.0109(10) Uani 1 1 d . . . C13 C -0.0686(4) -0.4160(4) -0.1077(3) 0.0161(11) Uani 1 1 d . . . H13A H -0.0699 -0.3496 -0.0930 0.019 Uiso 1 1 calc R . . C14 C -0.0119(4) -0.4417(5) -0.1484(3) 0.0205(12) Uani 1 1 d . . . H14A H 0.0260 -0.3926 -0.1602 0.025 Uiso 1 1 calc R . . C15 C 0.0536(4) -0.5703(4) -0.2144(3) 0.0154(12) Uani 1 1 d . . . C16 C -0.1786(4) -0.4610(4) -0.0405(3) 0.0133(11) Uani 1 1 d . . . C17 C 0.1064(3) -0.3856(4) -0.4292(3) 0.0077(10) Uani 1 1 d . . . C18 C 0.2102(4) -0.3870(4) -0.4358(3) 0.0083(10) Uani 1 1 d . . . C19 C 0.3083(4) -0.4441(4) -0.3837(3) 0.0064(9) Uani 1 1 d . . . C20 C 0.4020(4) -0.4284(4) -0.3966(3) 0.0064(9) Uani 1 1 d . . . C21 C 0.3964(3) -0.3633(4) -0.4572(3) 0.0068(9) Uani 1 1 d U . . C22 C 0.2101(4) -0.3252(4) -0.4933(3) 0.0136(11) Uani 1 1 d . . . H22A H 0.1453 -0.2904 -0.5268 0.016 Uiso 1 1 calc R . . C23 C 0.4918(4) -0.3472(4) -0.4655(3) 0.0101(10) Uani 1 1 d . . . H23A H 0.4873 -0.3042 -0.5058 0.012 Uiso 1 1 calc R . . C24 C 0.5908(4) -0.3940(4) -0.4149(3) 0.0083(10) Uani 1 1 d U . . C25 C 0.5925(4) -0.4580(4) -0.3550(3) 0.0155(11) Uani 1 1 d U . . C26 C 0.5030(4) -0.4756(4) -0.3450(3) 0.0119(11) Uani 1 1 d . . . H26A H 0.5088 -0.5186 -0.3042 0.014 Uiso 1 1 calc R . . C27 C 0.2833(4) -0.2456(5) -0.5719(3) 0.0230(13) Uani 1 1 d U . . H27A H 0.2294 -0.1941 -0.5796 0.028 Uiso 1 1 calc R A 1 H27B H 0.3527 -0.2123 -0.5575 0.028 Uiso 1 1 calc R A 1 C28 C 0.2463(11) -0.2996(9) -0.6474(5) 0.042(3) Uani 0.70 1 d PU B 1 H28A H 0.2374 -0.2534 -0.6892 0.063 Uiso 0.70 1 calc PR B 1 H28B H 0.1768 -0.3316 -0.6625 0.063 Uiso 0.70 1 calc PR B 1 H28C H 0.3002 -0.3495 -0.6405 0.063 Uiso 0.70 1 calc PR B 1 C28' C 0.188(3) -0.259(3) -0.6486(18) 0.058(8) Uani 0.30 1 d PU B 2 H28D H 0.1872 -0.2104 -0.6862 0.087 Uiso 0.30 1 calc PR B 2 H28E H 0.1226 -0.2508 -0.6432 0.087 Uiso 0.30 1 calc PR B 2 H28F H 0.1880 -0.3255 -0.6683 0.087 Uiso 0.30 1 calc PR B 2 C29 C 0.7869(4) -0.3460(5) -0.3498(3) 0.0160(11) Uani 1 1 d . . . H29A H 0.7954 -0.3811 -0.3021 0.019 Uiso 1 1 calc R . . H29B H 0.7792 -0.2748 -0.3425 0.019 Uiso 1 1 calc R . . C30 C 0.8885(4) -0.3631(4) -0.3588(3) 0.0144(11) Uani 1 1 d . . . H30A H 0.9537 -0.3377 -0.3113 0.017 Uiso 1 1 calc R . . H30B H 0.8986 -0.4344 -0.3634 0.017 Uiso 1 1 calc R . . C31 C 0.7711(4) -0.3450(4) -0.5059(3) 0.0116(10) Uani 1 1 d U . . H31A H 0.7778 -0.4158 -0.5149 0.014 Uiso 1 1 calc R . . H31B H 0.7618 -0.3082 -0.5531 0.014 Uiso 1 1 calc R . . C32 C 0.6707(4) -0.3288(4) -0.4951(3) 0.0097(10) Uani 1 1 d U . . H32A H 0.6612 -0.2576 -0.4892 0.012 Uiso 1 1 calc R . . H32B H 0.6048 -0.3531 -0.5426 0.012 Uiso 1 1 calc R . . H6 H 0.932(4) -0.310(7) -0.441(5) 0.06(3) Uiso 1 1 d D . . H7 H 0.866(5) -0.2434(8) -0.431(4) 0.026(17) Uiso 1 1 d D . . H1 H -0.243(6) -0.529(6) 0.010(3) 0.04(2) Uiso 1 1 d D . . O3 O 0.6704(2) -0.1244(3) -0.32015(19) 0.0070(7) Uani 1 1 d . . . O4 O 0.4935(3) -0.1078(3) -0.41574(18) 0.0092(7) Uani 1 1 d U . . C8 C 0.5661(4) -0.1373(4) -0.3479(3) 0.0060(9) Uani 1 1 d U . . 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 0.0208(4) 0.0267(4) 0.0208(4) 0.0022(3) 0.0118(3) 0.0009(3) Zn2 0.0230(5) 0.0196(5) 0.0178(5) -0.0001(4) 0.0120(4) 0.0000(4) F1 0.0141(16) 0.053(3) 0.053(2) 0.043(2) 0.0208(18) 0.0240(15) O1 0.0097(15) 0.0081(17) 0.0086(15) -0.0023(13) 0.0071(13) -0.0063(13) O2W 0.0050(15) 0.021(2) 0.0054(16) -0.0039(13) 0.0043(14) -0.0025(13) O2 0.0141(16) 0.0092(18) 0.0043(15) 0.0032(13) 0.0051(14) -0.0016(13) O1W 0.0125(16) 0.017(2) 0.0096(16) -0.0028(14) 0.0037(14) -0.0027(14) O5 0.063(3) 0.020(3) 0.078(3) 0.000(2) 0.066(3) 0.005(2) O6 0.0139(18) 0.026(2) 0.0168(18) 0.0043(15) 0.0144(16) 0.0052(15) O7 0.029(2) 0.039(3) 0.030(2) -0.018(2) 0.0291(19) -0.0141(19) O8 0.0216(19) 0.024(2) 0.0220(19) -0.0070(17) 0.0154(17) 0.0030(16) O9 0.0108(16) 0.032(2) 0.0141(18) 0.0150(16) 0.0099(15) 0.0124(16) O10 0.0028(15) 0.025(2) 0.0123(16) 0.0053(15) 0.0039(13) 0.0059(14) O11 0.0071(16) 0.0147(19) 0.0103(16) 0.0060(13) 0.0078(14) 0.0020(13) N3 0.0036(18) 0.025(3) 0.013(2) 0.0095(19) 0.0024(17) -0.0019(17) N2 0.0067(18) 0.013(2) 0.0117(19) -0.0008(17) 0.0060(17) -0.0008(16) N1 0.0053(19) 0.012(2) 0.015(2) -0.0003(17) 0.0064(17) 0.0007(16) C2 0.007(2) 0.011(3) 0.006(2) 0.0022(19) 0.0031(18) -0.0010(18) C3 0.009(2) 0.008(2) 0.0008(19) 0.0021(17) -0.0003(17) -0.0017(18) C4 0.010(2) 0.006(2) 0.007(2) 0.0017(18) 0.0044(18) -0.0021(18) C5 0.005(2) 0.011(3) 0.006(2) 0.0029(18) 0.0025(18) 0.0007(18) C6 0.008(2) 0.013(3) 0.005(2) 0.0054(19) 0.0005(18) 0.0000(19) C7 0.012(2) 0.002(2) 0.011(2) -0.0018(17) 0.010(2) -0.0003(17) C9 0.007(2) 0.023(3) 0.011(2) 0.013(2) 0.0074(19) 0.006(2) C10 0.007(2) 0.023(3) 0.013(2) 0.000(2) 0.0048(19) 0.004(2) C11 0.007(2) 0.024(3) 0.008(2) -0.002(2) 0.0062(19) -0.005(2) C12 0.011(2) 0.018(3) 0.007(2) -0.0015(19) 0.006(2) 0.0013(19) C13 0.017(2) 0.020(3) 0.015(2) 0.001(2) 0.011(2) 0.003(2) C14 0.016(3) 0.030(4) 0.021(3) 0.006(2) 0.013(2) 0.001(2) C15 0.010(2) 0.024(3) 0.016(2) 0.011(2) 0.010(2) 0.008(2) C16 0.006(2) 0.022(3) 0.011(2) -0.004(2) 0.003(2) -0.001(2) C17 0.002(2) 0.014(3) 0.009(2) -0.0015(19) 0.0037(18) -0.0012(18) C18 0.005(2) 0.008(2) 0.009(2) -0.0011(19) 0.0012(18) 0.0002(18) C19 0.008(2) 0.007(2) 0.005(2) -0.0030(18) 0.0035(18) -0.0034(18) C20 0.005(2) 0.008(2) 0.008(2) 0.0004(18) 0.0037(19) 0.0003(17) C21 0.0014(19) 0.013(2) 0.0059(19) -0.0001(17) 0.0021(16) -0.0022(16) C22 0.002(2) 0.023(3) 0.013(2) 0.009(2) 0.0021(19) -0.0004(19) C23 0.009(2) 0.017(3) 0.006(2) -0.0009(19) 0.0046(19) -0.004(2) C24 0.005(2) 0.011(2) 0.012(2) -0.0018(19) 0.0065(18) 0.0000(18) C25 0.006(2) 0.019(3) 0.021(3) 0.008(2) 0.006(2) 0.008(2) C26 0.008(2) 0.016(3) 0.013(2) 0.008(2) 0.006(2) 0.0021(19) C27 0.009(2) 0.036(3) 0.018(3) 0.022(2) 0.001(2) -0.003(2) C28 0.061(6) 0.048(6) 0.016(4) -0.009(4) 0.018(4) -0.037(5) C28' 0.062(11) 0.063(12) 0.046(10) 0.025(8) 0.024(8) -0.016(9) C29 0.008(2) 0.029(3) 0.010(2) -0.003(2) 0.003(2) 0.000(2) C30 0.006(2) 0.025(3) 0.012(2) 0.003(2) 0.004(2) -0.001(2) C31 0.003(2) 0.020(3) 0.013(2) -0.001(2) 0.0046(19) -0.0009(19) C32 0.004(2) 0.016(3) 0.012(2) -0.005(2) 0.0062(18) -0.0037(18) O3 0.0040(14) 0.0096(18) 0.0079(15) 0.0014(13) 0.0033(13) -0.0033(12) O4 0.0114(16) 0.0114(18) 0.0062(15) 0.0048(13) 0.0056(13) -0.0022(13) C8 0.011(2) 0.004(2) 0.006(2) -0.0039(17) 0.0064(19) -0.0038(17) _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 O11 2.110(3) . ? Zn1 O9 2.127(3) . ? Zn1 O6 2.134(4) . ? Zn1 O3 2.214(3) 2_644 ? Zn1 O1W 2.223(4) . ? Zn1 O1 2.245(3) . ? Zn2 O2 2.158(3) 3_645 ? Zn2 O2 2.158(3) . ? Zn2 O4 2.178(3) 2_644 ? Zn2 O4 2.178(3) 4_556 ? Zn2 O2W 2.209(3) 3_645 ? Zn2 O2W 2.209(3) . ? F1 C25 1.358(6) . ? O1 C7 1.276(6) . ? O2W H4 0.8498 . ? O2W H5 0.8499 . ? O2 C7 1.263(6) . ? O1W H2 0.8500 . ? O1W H3 0.8500 . ? O5 C15 1.221(8) . ? O6 C15 1.267(7) . ? O7 C16 1.312(7) . ? O7 H1 0.846(10) . ? O8 C16 1.214(7) . ? O9 C17 1.244(6) . ? O10 C17 1.262(6) . ? O11 C19 1.264(6) . ? N3 C22 1.361(6) . ? N3 C21 1.393(6) . ? N3 C27 1.463(7) . ? N2 C24 1.406(6) . ? N2 C32 1.464(6) . ? N2 C29 1.488(6) . ? N1 C30 1.483(7) . ? N1 C31 1.496(6) . ? N1 H6 0.9000(11) . ? N1 H7 0.9000(11) . ? C1 C2 1.385(7) . ? C1 C6 1.409(6) . ? C1 C7 1.503(7) . ? C2 C3 1.396(7) . ? C2 H2A 0.9300 . ? C3 C4 1.393(7) . ? C3 H3A 0.9300 . ? C4 C5 1.394(7) . ? C4 C8 1.503(6) . ? C5 C6 1.378(7) . ? C5 H5A 0.9300 . ? C6 H6A 0.9300 . ? C9 C14 1.391(9) . ? C9 C10 1.399(8) . ? C9 C15 1.525(7) . ? C10 C11 1.381(7) . ? C10 H10A 0.9300 . ? C11 C12 1.406(8) . ? C11 H11A 0.9300 . ? C12 C13 1.379(8) . ? C12 C16 1.502(7) . ? C13 C14 1.385(8) . ? C13 H13A 0.9300 . ? C14 H14A 0.9300 . ? C17 C18 1.504(6) . ? C18 C22 1.363(7) . ? C18 C19 1.443(7) . ? C19 C20 1.449(6) . ? C20 C26 1.403(7) . ? C20 C21 1.408(7) . ? C21 C23 1.422(6) . ? C22 H22A 0.9300 . ? C23 C24 1.379(7) . ? C23 H23A 0.9300 . ? C24 C25 1.408(7) . ? C25 C26 1.364(7) . ? C26 H26A 0.9300 . ? C27 C28' 1.42(3) . ? C27 C28 1.449(11) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C28' H28D 0.9600 . ? C28' H28E 0.9600 . ? C28' H28F 0.9600 . ? C29 C30 1.517(7) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C32 1.518(6) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? O3 C8 1.285(6) . ? O3 Zn1 2.214(3) 2_654 ? O4 C8 1.244(6) . ? O4 Zn2 2.178(3) 2_654 ? 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 O11 Zn1 O9 85.29(13) . . ? O11 Zn1 O6 170.40(15) . . ? O9 Zn1 O6 87.51(14) . . ? O11 Zn1 O3 94.57(13) . 2_644 ? O9 Zn1 O3 178.20(15) . 2_644 ? O6 Zn1 O3 92.83(13) . 2_644 ? O11 Zn1 O1W 95.90(13) . . ? O9 Zn1 O1W 91.41(15) . . ? O6 Zn1 O1W 90.61(14) . . ? O3 Zn1 O1W 86.82(13) 2_644 . ? O11 Zn1 O1 87.25(13) . . ? O9 Zn1 O1 97.41(15) . . ? O6 Zn1 O1 87.39(14) . . ? O3 Zn1 O1 84.37(13) 2_644 . ? O1W Zn1 O1 170.86(13) . . ? O2 Zn2 O2 180.0 3_645 . ? O2 Zn2 O4 91.91(14) 3_645 2_644 ? O2 Zn2 O4 88.09(14) . 2_644 ? O2 Zn2 O4 88.09(14) 3_645 4_556 ? O2 Zn2 O4 91.91(14) . 4_556 ? O4 Zn2 O4 180.00(12) 2_644 4_556 ? O2 Zn2 O2W 91.25(12) 3_645 3_645 ? O2 Zn2 O2W 88.75(12) . 3_645 ? O4 Zn2 O2W 90.41(12) 2_644 3_645 ? O4 Zn2 O2W 89.59(12) 4_556 3_645 ? O2 Zn2 O2W 88.75(12) 3_645 . ? O2 Zn2 O2W 91.25(12) . . ? O4 Zn2 O2W 89.59(12) 2_644 . ? O4 Zn2 O2W 90.41(12) 4_556 . ? O2W Zn2 O2W 180.0 3_645 . ? C7 O1 Zn1 140.3(3) . . ? Zn2 O2W H4 125.4 . . ? Zn2 O2W H5 112.7 . . ? H4 O2W H5 107.7 . . ? C7 O2 Zn2 128.5(3) . . ? Zn1 O1W H2 127.0 . . ? Zn1 O1W H3 125.1 . . ? H2 O1W H3 107.7 . . ? C15 O6 Zn1 127.4(4) . . ? C16 O7 H1 115(6) . . ? C17 O9 Zn1 132.1(3) . . ? C19 O11 Zn1 128.6(3) . . ? C22 N3 C21 119.6(4) . . ? C22 N3 C27 117.5(4) . . ? C21 N3 C27 122.7(4) . . ? C24 N2 C32 115.9(4) . . ? C24 N2 C29 116.1(4) . . ? C32 N2 C29 110.2(4) . . ? C30 N1 C31 110.6(4) . . ? C30 N1 H6 117(5) . . ? C31 N1 H6 111(5) . . ? C30 N1 H7 113(4) . . ? C31 N1 H7 105(4) . . ? H6 N1 H7 99(7) . . ? C2 C1 C6 119.3(4) . . ? C2 C1 C7 121.7(4) . . ? C6 C1 C7 118.9(4) . . ? C1 C2 C3 120.1(4) . . ? C1 C2 H2A 120.0 . . ? C3 C2 H2A 120.0 . . ? C4 C3 C2 120.6(4) . . ? C4 C3 H3A 119.7 . . ? C2 C3 H3A 119.7 . . ? C3 C4 C5 119.0(4) . . ? C3 C4 C8 119.9(4) . . ? C5 C4 C8 121.1(4) . . ? C6 C5 C4 120.8(4) . . ? C6 C5 H5A 119.6 . . ? C4 C5 H5A 119.6 . . ? C5 C6 C1 120.2(4) . . ? C5 C6 H6A 119.9 . . ? C1 C6 H6A 119.9 . . ? O2 C7 O1 123.5(4) . . ? O2 C7 C1 117.8(4) . . ? O1 C7 C1 118.6(4) . . ? C14 C9 C10 120.0(5) . . ? C14 C9 C15 120.5(5) . . ? C10 C9 C15 119.5(5) . . ? C11 C10 C9 119.9(5) . . ? C11 C10 H10A 120.1 . . ? C9 C10 H10A 120.1 . . ? C10 C11 C12 119.7(5) . . ? C10 C11 H11A 120.2 . . ? C12 C11 H11A 120.2 . . ? C13 C12 C11 120.3(5) . . ? C13 C12 C16 119.4(5) . . ? C11 C12 C16 120.3(5) . . ? C12 C13 C14 120.0(5) . . ? C12 C13 H13A 120.0 . . ? C14 C13 H13A 120.0 . . ? C13 C14 C9 120.1(5) . . ? C13 C14 H14A 119.9 . . ? C9 C14 H14A 119.9 . . ? O5 C15 O6 124.9(5) . . ? O5 C15 C9 118.2(5) . . ? O6 C15 C9 116.9(5) . . ? O8 C16 O7 123.2(5) . . ? O8 C16 C12 123.0(5) . . ? O7 C16 C12 113.8(5) . . ? O9 C17 O10 122.2(4) . . ? O9 C17 C18 120.2(4) . . ? O10 C17 C18 117.4(4) . . ? C22 C18 C19 119.6(4) . . ? C22 C18 C17 115.6(4) . . ? C19 C18 C17 124.7(4) . . ? O11 C19 C18 125.0(4) . . ? O11 C19 C20 119.4(4) . . ? C18 C19 C20 115.6(4) . . ? C26 C20 C21 118.7(4) . . ? C26 C20 C19 119.3(4) . . ? C21 C20 C19 121.9(4) . . ? N3 C21 C20 118.9(4) . . ? N3 C21 C23 121.1(4) . . ? C20 C21 C23 119.9(4) . . ? N3 C22 C18 124.3(5) . . ? N3 C22 H22A 117.8 . . ? C18 C22 H22A 117.8 . . ? C24 C23 C21 121.3(5) . . ? C24 C23 H23A 119.3 . . ? C21 C23 H23A 119.3 . . ? C23 C24 N2 123.1(4) . . ? C23 C24 C25 116.7(4) . . ? N2 C24 C25 120.2(4) . . ? F1 C25 C26 117.5(5) . . ? F1 C25 C24 118.6(4) . . ? C26 C25 C24 124.0(5) . . ? C25 C26 C20 119.4(5) . . ? C25 C26 H26A 120.3 . . ? C20 C26 H26A 120.3 . . ? C28' C27 C28 39.4(16) . . ? C28' C27 N3 118.3(12) . . ? C28 C27 N3 112.7(6) . . ? C28' C27 H27A 70.7 . . ? C28 C27 H27A 109.0 . . ? N3 C27 H27A 109.0 . . ? C28' C27 H27B 130.4 . . ? C28 C27 H27B 109.0 . . ? N3 C27 H27B 109.0 . . ? H27A C27 H27B 107.8 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C28' H28D 109.5 . . ? C27 C28' H28E 109.5 . . ? H28D C28' H28E 109.5 . . ? C27 C28' H28F 109.5 . . ? H28D C28' H28F 109.5 . . ? H28E C28' H28F 109.5 . . ? N2 C29 C30 110.4(4) . . ? N2 C29 H29A 109.6 . . ? C30 C29 H29A 109.6 . . ? N2 C29 H29B 109.6 . . ? C30 C29 H29B 109.6 . . ? H29A C29 H29B 108.1 . . ? N1 C30 C29 109.2(4) . . ? N1 C30 H30A 109.8 . . ? C29 C30 H30A 109.8 . . ? N1 C30 H30B 109.8 . . ? C29 C30 H30B 109.8 . . ? H30A C30 H30B 108.3 . . ? N1 C31 C32 110.7(4) . . ? N1 C31 H31A 109.5 . . ? C32 C31 H31A 109.5 . . ? N1 C31 H31B 109.5 . . ? C32 C31 H31B 109.5 . . ? H31A C31 H31B 108.1 . . ? N2 C32 C31 109.3(4) . . ? N2 C32 H32A 109.8 . . ? C31 C32 H32A 109.8 . . ? N2 C32 H32B 109.8 . . ? C31 C32 H32B 109.8 . . ? H32A C32 H32B 108.3 . . ? C8 O3 Zn1 128.3(3) . 2_654 ? C8 O4 Zn2 131.2(3) . 2_654 ? O4 C8 O3 124.0(4) . . ? O4 C8 C4 118.4(4) . . ? O3 C8 C4 117.5(4) . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 0.812 _refine_diff_density_min -2.274 _refine_diff_density_rms 0.163