# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 1350 loop_ _publ_author_name 'Ma, Jian-Fang' _publ_contact_author_name 'Ma, Jian-Fang' _publ_contact_author_email jianfangma@yahoo.com.cn _publ_section_title ; Four novel topological networks based on 4,4\^a -(hexafluoroisopropylidene)diphthalic acid and 1,1\^a -(1,4-butanediyl)bis(imidazole) ligand ; # Attachment '- crystals.cif' data_Compound-1 _database_code_depnum_ccdc_archive 'CCDC 780167' #TrackingRef '- crystals.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H31 Cd F6 N6 O9, 2(H2 O)' _chemical_formula_sum 'C34 H35 Cd F6 N6 O11' _chemical_formula_weight 930.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_hall '-P 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.590(4) _cell_length_b 11.460(6) _cell_length_c 17.775(9) _cell_angle_alpha 77.232(19) _cell_angle_beta 75.175(16) _cell_angle_gamma 63.319(15) _cell_volume 1849.2(15) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8303 _cell_measurement_theta_min 3.3 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.219 _exptl_crystal_size_mid 0.190 _exptl_crystal_size_min 0.183 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.670 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 942 _exptl_absorpt_coefficient_mu 0.690 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.853 _exptl_absorpt_correction_T_max 0.874 _exptl_absorpt_process_details ; Higashi,T (1995) Program for absorption correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17692 _diffrn_reflns_av_R_equivalents 0.0304 _diffrn_reflns_av_sigmaI/netI 0.0388 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.30 _diffrn_reflns_theta_max 27.48 _reflns_number_total 8303 _reflns_number_gt 7208 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction PROCESS-AUTO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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^)+(0.0653P)^2^+0.6072P] 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 8303 _refine_ls_number_parameters 544 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0395 _refine_ls_R_factor_gt 0.0330 _refine_ls_wR_factor_ref 0.1117 _refine_ls_wR_factor_gt 0.0944 _refine_ls_goodness_of_fit_ref 1.152 _refine_ls_restrained_S_all 1.165 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.348001(19) 0.367798(19) 0.068503(11) 0.02248(8) Uani 1 1 d . . . C1 C 0.1227(3) 0.4353(3) 0.23789(18) 0.0314(6) Uani 1 1 d . . . H1 H 0.1802 0.3595 0.2661 0.038 Uiso 1 1 calc R . . C2 C 0.0414(3) 0.5849(3) 0.14476(19) 0.0365(7) Uani 1 1 d . . . H2 H 0.0332 0.6324 0.0952 0.044 Uiso 1 1 calc R . . C3 C -0.0553(3) 0.6209(3) 0.2102(2) 0.0395(7) Uani 1 1 d . . . H3 H -0.1412 0.6960 0.2143 0.047 Uiso 1 1 calc R . . C4 C -0.0754(4) 0.5220(4) 0.35168(19) 0.0431(8) Uani 1 1 d . . . H4A H -0.1099 0.6075 0.3689 0.052 Uiso 1 1 calc R . . H4B H -0.0075 0.4579 0.3841 0.052 Uiso 1 1 calc R . . C5 C -0.2011(4) 0.4861(4) 0.36191(19) 0.0401(8) Uani 1 1 d . . . H5A H -0.1651 0.3977 0.3486 0.048 Uiso 1 1 calc R . . H5B H -0.2641 0.5457 0.3258 0.048 Uiso 1 1 calc R . . C6 C -0.2879(4) 0.4927(4) 0.4457(2) 0.0456(9) Uani 1 1 d . . . H6A H -0.3128 0.5774 0.4613 0.055 Uiso 1 1 calc R . . H6B H -0.3767 0.4872 0.4459 0.055 Uiso 1 1 calc R . . C7 C -0.2107(3) 0.3864(3) 0.50499(18) 0.0387(8) Uani 1 1 d . . . H7A H -0.1919 0.3015 0.4921 0.046 Uiso 1 1 calc R . . H7B H -0.1191 0.3879 0.5032 0.046 Uiso 1 1 calc R . . C8 C -0.3690(3) 0.3352(3) 0.62512(19) 0.0335(6) Uani 1 1 d . . . H8 H -0.3779 0.2692 0.6074 0.040 Uiso 1 1 calc R . . C9 C -0.3074(4) 0.4904(4) 0.6308(2) 0.0470(9) Uani 1 1 d . . . H9 H -0.2661 0.5505 0.6169 0.056 Uiso 1 1 calc R . . C10 C -0.3896(5) 0.4726(4) 0.6995(2) 0.0538(10) Uani 1 1 d . . . H10 H -0.4160 0.5176 0.7425 0.065 Uiso 1 1 calc R . . C11 C 0.2410(3) 0.1883(3) 0.01020(19) 0.0320(6) Uani 1 1 d . . . H11 H 0.1949 0.2583 -0.0254 0.038 Uiso 1 1 calc R . . C12 C 0.3613(4) 0.0713(4) 0.1017(2) 0.0453(9) Uani 1 1 d . . . H12 H 0.4148 0.0463 0.1412 0.054 Uiso 1 1 calc R . . C13 C 0.3213(4) -0.0081(4) 0.0765(3) 0.0465(9) Uani 1 1 d . . . H13 H 0.3410 -0.0959 0.0951 0.056 Uiso 1 1 calc R . . C14 C 0.1751(4) 0.0263(4) -0.0255(2) 0.0391(8) Uani 1 1 d . . . H14A H 0.2402 -0.0600 -0.0410 0.047 Uiso 1 1 calc R . . H14B H 0.1543 0.0874 -0.0728 0.047 Uiso 1 1 calc R . . C15 C 0.0362(4) 0.0209(4) 0.02261(19) 0.0413(8) Uani 1 1 d . . . H15A H 0.0570 -0.0407 0.0697 0.050 Uiso 1 1 calc R . . H15B H -0.0288 0.1070 0.0385 0.050 Uiso 1 1 calc R . . C16 C 0.5743(3) 0.2941(3) 0.14698(15) 0.0227(5) Uani 1 1 d . . . C17 C 0.7142(3) 0.2677(2) 0.16991(15) 0.0197(5) Uani 1 1 d . . . C18 C 0.7642(3) 0.1696(3) 0.23071(15) 0.0216(5) Uani 1 1 d . . . H18 H 0.7120 0.1205 0.2561 0.026 Uiso 1 1 calc R . . C19 C 0.8916(3) 0.1433(3) 0.25440(16) 0.0233(5) Uani 1 1 d . . . C20 C 0.9692(3) 0.2157(3) 0.21547(17) 0.0282(6) Uani 1 1 d . . . H20 H 1.0558 0.1973 0.2293 0.034 Uiso 1 1 calc R . . C21 C 0.9182(3) 0.3158(3) 0.15575(17) 0.0281(6) Uani 1 1 d . . . H21 H 0.9696 0.3660 0.1312 0.034 Uiso 1 1 calc R . . C22 C 0.7924(3) 0.3418(3) 0.13240(15) 0.0225(5) Uani 1 1 d . . . C23 C 0.7503(3) 0.4472(3) 0.06329(17) 0.0288(6) Uani 1 1 d . . . C24 C 0.9429(3) 0.0275(3) 0.32034(16) 0.0239(5) Uani 1 1 d . . . C25 C 1.0032(3) -0.1003(3) 0.28198(18) 0.0331(7) Uani 1 1 d . . . C26 C 1.0639(3) 0.0301(3) 0.35342(18) 0.0320(6) Uani 1 1 d . . . C27 C 0.8210(3) 0.0334(3) 0.39130(15) 0.0229(5) Uani 1 1 d . . . C28 C 0.8222(3) -0.0777(3) 0.44062(17) 0.0268(6) Uani 1 1 d . . . H28 H 0.8928 -0.1590 0.4272 0.032 Uiso 1 1 calc R . . C29 C 0.7224(3) -0.0747(3) 0.51002(17) 0.0259(6) Uani 1 1 d D . . C30 C 0.7496(3) -0.2105(3) 0.5553(2) 0.0349(7) Uani 1 1 d D . . C31 C 0.6154(3) 0.0491(3) 0.53098(16) 0.0257(6) Uani 1 1 d D . . C32 C 0.5027(3) 0.0792(4) 0.60463(18) 0.0362(7) Uani 1 1 d D . . C33 C 0.6129(3) 0.1593(3) 0.47922(17) 0.0293(6) Uani 1 1 d . . . H33 H 0.5403 0.2408 0.4908 0.035 Uiso 1 1 calc R . . C34 C 0.7131(3) 0.1545(3) 0.41093(17) 0.0272(6) Uani 1 1 d . . . H34 H 0.7083 0.2315 0.3784 0.033 Uiso 1 1 calc R . . N1 N 0.1549(3) 0.4674(3) 0.16164(15) 0.0297(5) Uani 1 1 d . . . N2 N -0.0030(3) 0.5254(3) 0.26960(15) 0.0332(6) Uani 1 1 d . . . N3 N -0.2958(3) 0.4034(2) 0.58500(14) 0.0294(5) Uani 1 1 d . . . N5 N 0.3106(3) 0.1948(3) 0.06010(15) 0.0301(5) Uani 1 1 d . . . N6 N 0.2455(3) 0.0676(3) 0.01774(16) 0.0328(6) Uani 1 1 d . . . O1 O 0.5465(3) 0.2004(2) 0.14640(15) 0.0408(5) Uani 1 1 d . . . O2 O 0.4937(2) 0.4136(2) 0.12816(12) 0.0283(4) Uani 1 1 d . . . O3 O 0.7346(2) 0.4152(2) 0.00464(12) 0.0370(5) Uani 1 1 d . . . O4 O 0.7406(3) 0.5576(2) 0.06612(17) 0.0512(7) Uani 1 1 d . . . O5 O 0.8450(3) -0.3075(2) 0.52681(18) 0.0536(7) Uani 1 1 d . . . O6 O 0.6727(3) -0.2213(3) 0.62305(16) 0.0565(7) Uani 1 1 d . . . H6 H 0.6143 -0.1479 0.6342 0.085 Uiso 1 1 calc R . . O7 O 0.4778(3) -0.0150(3) 0.65035(15) 0.0513(7) Uani 1 1 d . . . O8 O 0.4372(3) 0.1915(3) 0.61976(17) 0.0582(8) Uani 1 1 d . . . F1 F 1.0244(2) 0.1467(2) 0.37612(12) 0.0422(5) Uani 1 1 d . . . F2 F 1.18771(19) 0.0029(2) 0.30300(12) 0.0475(5) Uani 1 1 d . . . F3 F 1.0943(2) -0.0585(2) 0.41692(11) 0.0425(5) Uani 1 1 d . . . F4 F 1.0911(3) -0.0954(2) 0.21427(12) 0.0545(6) Uani 1 1 d . . . F5 F 1.0794(2) -0.20785(18) 0.32624(12) 0.0426(5) Uani 1 1 d . . . F6 F 0.8976(2) -0.1198(2) 0.26839(14) 0.0492(5) Uani 1 1 d . . . O1W O 0.3559(3) 0.0813(3) 0.79947(15) 0.0452(6) Uani 1 1 d D . . H1A H 0.381(5) 0.000(3) 0.826(2) 0.068 Uiso 1 1 d D . . H1B H 0.381(5) 0.068(4) 0.7497(12) 0.068 Uiso 1 1 d D . . O2W O -0.5764(4) 0.2816(4) 0.81484(19) 0.0713(9) Uani 1 1 d D . . H2A H -0.589(6) 0.210(4) 0.813(4) 0.107 Uiso 1 1 d D . . H2B H -0.639(5) 0.321(5) 0.854(3) 0.107 Uiso 1 1 d D . . O3W O 0.5591(3) 0.3275(2) -0.03336(14) 0.0393(5) Uani 1 1 d D . . H3A H 0.623(4) 0.352(4) -0.022(2) 0.059 Uiso 1 1 d D . . H3B H 0.530(4) 0.392(3) -0.0746(19) 0.059 Uiso 1 1 d D . . N4 N -0.4272(3) 0.3764(3) 0.69430(17) 0.0425(7) Uani 1 1 d D . . H4N H -0.476(4) 0.346(4) 0.7344(18) 0.051 Uiso 1 1 d 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 Cd1 0.02371(11) 0.02370(11) 0.02289(11) 0.00058(7) -0.00659(7) -0.01264(8) C1 0.0280(14) 0.0372(16) 0.0275(14) 0.0010(12) -0.0044(11) -0.0149(12) C2 0.0336(15) 0.0335(16) 0.0307(16) 0.0033(13) -0.0049(12) -0.0076(13) C3 0.0321(16) 0.0354(17) 0.0401(18) -0.0051(14) -0.0038(13) -0.0058(13) C4 0.0421(18) 0.060(2) 0.0248(15) -0.0087(15) 0.0040(13) -0.0226(16) C5 0.0374(17) 0.0434(19) 0.0287(16) 0.0040(14) -0.0032(13) -0.0127(14) C6 0.0300(15) 0.047(2) 0.0335(17) 0.0052(15) 0.0011(13) -0.0012(14) C7 0.0313(15) 0.0381(18) 0.0288(16) 0.0012(13) 0.0014(12) -0.0051(13) C8 0.0333(15) 0.0363(16) 0.0337(16) -0.0022(13) -0.0071(13) -0.0172(13) C9 0.062(2) 0.0353(18) 0.049(2) -0.0089(16) -0.0039(18) -0.0266(17) C10 0.070(3) 0.045(2) 0.040(2) -0.0172(17) 0.0007(18) -0.0184(19) C11 0.0337(15) 0.0316(15) 0.0340(16) -0.0009(12) -0.0110(13) -0.0152(12) C12 0.0491(19) 0.0413(19) 0.058(2) 0.0143(16) -0.0329(18) -0.0266(16) C13 0.0450(19) 0.0330(18) 0.068(3) 0.0098(17) -0.0250(18) -0.0216(15) C14 0.0421(17) 0.053(2) 0.0381(17) -0.0176(15) 0.0009(14) -0.0320(16) C15 0.0476(19) 0.062(2) 0.0316(16) -0.0173(16) -0.0018(14) -0.0359(18) C16 0.0212(12) 0.0288(14) 0.0168(12) 0.0004(10) -0.0062(10) -0.0094(10) C17 0.0201(11) 0.0198(12) 0.0180(11) 0.0001(9) -0.0059(9) -0.0071(9) C18 0.0227(12) 0.0213(12) 0.0215(12) 0.0021(10) -0.0071(10) -0.0103(10) C19 0.0257(13) 0.0227(13) 0.0205(12) 0.0020(10) -0.0088(10) -0.0089(10) C20 0.0234(13) 0.0351(15) 0.0302(14) 0.0073(12) -0.0115(11) -0.0174(12) C21 0.0303(14) 0.0292(14) 0.0290(14) 0.0055(11) -0.0077(11) -0.0189(12) C22 0.0282(13) 0.0195(12) 0.0193(12) 0.0025(10) -0.0065(10) -0.0106(10) C23 0.0253(13) 0.0321(15) 0.0290(14) 0.0084(12) -0.0075(11) -0.0161(11) C24 0.0243(12) 0.0224(13) 0.0233(13) 0.0019(10) -0.0100(10) -0.0072(10) C25 0.0383(16) 0.0272(15) 0.0285(15) 0.0001(12) -0.0110(12) -0.0079(12) C26 0.0285(14) 0.0345(16) 0.0316(15) 0.0054(12) -0.0149(12) -0.0113(12) C27 0.0274(13) 0.0228(13) 0.0210(12) 0.0037(10) -0.0105(10) -0.0121(10) C28 0.0291(13) 0.0207(13) 0.0299(14) 0.0032(11) -0.0101(11) -0.0102(11) C29 0.0301(13) 0.0235(13) 0.0280(14) 0.0064(11) -0.0139(11) -0.0141(11) C30 0.0372(16) 0.0282(15) 0.0397(17) 0.0088(13) -0.0118(13) -0.0172(13) C31 0.0287(13) 0.0297(14) 0.0229(13) 0.0021(11) -0.0087(11) -0.0160(11) C32 0.0383(16) 0.0449(19) 0.0288(15) -0.0069(14) -0.0051(13) -0.0197(14) C33 0.0312(14) 0.0253(14) 0.0290(14) -0.0027(11) -0.0067(12) -0.0092(11) C34 0.0329(14) 0.0206(13) 0.0264(14) 0.0031(10) -0.0096(11) -0.0102(11) N1 0.0250(11) 0.0335(13) 0.0271(12) -0.0013(10) -0.0035(10) -0.0108(10) N2 0.0327(13) 0.0404(15) 0.0237(12) -0.0044(11) -0.0009(10) -0.0148(11) N3 0.0300(12) 0.0257(12) 0.0268(12) 0.0020(10) -0.0039(10) -0.0096(10) N5 0.0300(12) 0.0304(13) 0.0364(14) 0.0040(11) -0.0127(10) -0.0182(10) N6 0.0328(13) 0.0338(14) 0.0398(14) -0.0049(11) -0.0072(11) -0.0204(11) O1 0.0417(12) 0.0376(13) 0.0556(15) 0.0003(11) -0.0263(11) -0.0209(10) O2 0.0233(9) 0.0260(10) 0.0296(10) 0.0043(8) -0.0092(8) -0.0062(8) O3 0.0372(11) 0.0514(14) 0.0185(10) 0.0056(9) -0.0071(8) -0.0186(10) O4 0.0688(17) 0.0341(13) 0.0566(16) 0.0120(12) -0.0277(14) -0.0258(12) O5 0.0488(14) 0.0289(13) 0.0646(18) 0.0142(12) -0.0015(13) -0.0138(11) O6 0.0734(18) 0.0340(14) 0.0461(15) 0.0121(11) 0.0013(13) -0.0222(13) O7 0.0612(16) 0.0486(15) 0.0380(14) -0.0009(12) 0.0102(12) -0.0297(13) O8 0.0659(18) 0.0438(15) 0.0507(16) -0.0135(13) 0.0172(13) -0.0217(13) F1 0.0499(11) 0.0413(11) 0.0492(12) -0.0010(9) -0.0247(9) -0.0248(9) F2 0.0247(9) 0.0655(14) 0.0469(12) 0.0047(10) -0.0105(8) -0.0172(9) F3 0.0413(10) 0.0487(12) 0.0384(10) 0.0150(9) -0.0270(9) -0.0183(9) F4 0.0647(14) 0.0472(13) 0.0324(11) -0.0096(9) 0.0062(10) -0.0124(11) F5 0.0418(10) 0.0268(9) 0.0429(11) 0.0015(8) -0.0132(9) 0.0002(8) F6 0.0579(13) 0.0314(10) 0.0676(14) -0.0101(10) -0.0309(11) -0.0146(9) O1W 0.0452(14) 0.0490(15) 0.0367(13) -0.0070(11) -0.0068(11) -0.0151(12) O2W 0.093(2) 0.086(3) 0.0497(18) -0.0104(17) 0.0186(16) -0.066(2) O3W 0.0416(13) 0.0416(13) 0.0365(12) -0.0048(10) -0.0079(10) -0.0183(11) N4 0.0373(15) 0.0474(17) 0.0339(15) -0.0014(13) 0.0039(12) -0.0170(13) _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 Cd1 N5 2.230(3) . ? Cd1 N1 2.287(3) . ? Cd1 O2 2.365(2) . ? Cd1 O3 2.416(3) 2_665 ? Cd1 O3W 2.421(3) . ? Cd1 O1 2.591(2) . ? Cd1 O4 2.620(3) 2_665 ? C1 N1 1.321(4) . ? C1 N2 1.340(4) . ? C1 H1 0.9300 . ? C2 C3 1.339(5) . ? C2 N1 1.379(4) . ? C2 H2 0.9300 . ? C3 N2 1.365(4) . ? C3 H3 0.9300 . ? C4 N2 1.466(4) . ? C4 C5 1.518(5) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.535(5) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C7 1.497(4) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 N3 1.477(4) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 N4 1.312(4) . ? C8 N3 1.317(4) . ? C8 H8 0.9300 . ? C9 C10 1.340(6) . ? C9 N3 1.368(4) . ? C9 H9 0.9300 . ? C10 N4 1.356(5) . ? C10 H10 0.9300 . ? C11 N5 1.323(4) . ? C11 N6 1.340(4) . ? C11 H11 0.9300 . ? C12 C13 1.354(5) . ? C12 N5 1.377(4) . ? C12 H12 0.9300 . ? C13 N6 1.376(4) . ? C13 H13 0.9300 . ? C14 N6 1.463(4) . ? C14 C15 1.521(4) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C15 1.509(6) 2 ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 O1 1.237(4) . ? C16 O2 1.269(3) . ? C16 C17 1.518(4) . ? C17 C18 1.391(3) . ? C17 C22 1.396(4) . ? C18 C19 1.399(4) . ? C18 H18 0.9300 . ? C19 C20 1.382(4) . ? C19 C24 1.556(4) . ? C20 C21 1.390(4) . ? C20 H20 0.9300 . ? C21 C22 1.381(4) . ? C21 H21 0.9300 . ? C22 C23 1.519(4) . ? C23 O4 1.234(4) . ? C23 O3 1.249(4) . ? C24 C27 1.545(4) . ? C24 C25 1.548(4) . ? C24 C26 1.555(4) . ? C25 F6 1.320(4) . ? C25 F4 1.328(4) . ? C25 F5 1.339(3) . ? C26 F1 1.331(4) . ? C26 F2 1.332(4) . ? C26 F3 1.340(3) . ? C27 C28 1.374(4) . ? C27 C34 1.393(4) . ? C28 C29 1.399(4) . ? C28 H28 0.9300 . ? C29 C31 1.418(4) . ? C29 C30 1.521(4) . ? C30 O5 1.221(4) . ? C30 O6 1.285(4) . ? C31 C33 1.382(4) . ? C31 C32 1.513(4) . ? C32 O8 1.211(4) . ? C32 O7 1.286(4) . ? C33 C34 1.386(4) . ? C33 H33 0.9300 . ? C34 H34 0.9300 . ? O3 Cd1 2.416(3) 2_665 ? O4 Cd1 2.620(3) 2_665 ? O6 H6 0.8200 . ? O1W H1A 0.899(19) . ? O1W H1B 0.883(19) . ? O2W H2A 0.90(5) . ? O2W H2B 0.90(5) . ? O3W H3A 0.92(5) . ? O3W H3B 0.922(19) . ? N4 H4N 0.87(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Cd1 N1 100.56(10) . . ? N5 Cd1 O2 138.09(8) . . ? N1 Cd1 O2 89.30(9) . . ? N5 Cd1 O3 129.11(9) . 2_665 ? N1 Cd1 O3 83.40(9) . 2_665 ? O2 Cd1 O3 92.26(8) . 2_665 ? N5 Cd1 O3W 97.45(9) . . ? N1 Cd1 O3W 161.73(9) . . ? O2 Cd1 O3W 79.26(8) . . ? O3 Cd1 O3W 82.87(8) 2_665 . ? N5 Cd1 O1 85.34(9) . . ? N1 Cd1 O1 105.11(9) . . ? O2 Cd1 O1 52.85(8) . . ? O3 Cd1 O1 143.11(8) 2_665 . ? O3W Cd1 O1 79.33(9) . . ? N5 Cd1 O4 79.99(9) . 2_665 ? N1 Cd1 O4 107.17(10) . 2_665 ? O2 Cd1 O4 135.81(8) . 2_665 ? O3 Cd1 O4 51.25(8) 2_665 2_665 ? O3W Cd1 O4 72.93(9) . 2_665 ? O1 Cd1 O4 146.43(9) . 2_665 ? N1 C1 N2 111.6(3) . . ? N1 C1 H1 124.2 . . ? N2 C1 H1 124.2 . . ? C3 C2 N1 110.1(3) . . ? C3 C2 H2 124.9 . . ? N1 C2 H2 124.9 . . ? C2 C3 N2 106.5(3) . . ? C2 C3 H3 126.8 . . ? N2 C3 H3 126.8 . . ? N2 C4 C5 111.1(3) . . ? N2 C4 H4A 109.4 . . ? C5 C4 H4A 109.4 . . ? N2 C4 H4B 109.4 . . ? C5 C4 H4B 109.4 . . ? H4A C4 H4B 108.0 . . ? C4 C5 C6 112.9(3) . . ? C4 C5 H5A 109.0 . . ? C6 C5 H5A 109.0 . . ? C4 C5 H5B 109.0 . . ? C6 C5 H5B 109.0 . . ? H5A C5 H5B 107.8 . . ? C7 C6 C5 114.1(3) . . ? C7 C6 H6A 108.7 . . ? C5 C6 H6A 108.7 . . ? C7 C6 H6B 108.7 . . ? C5 C6 H6B 108.7 . . ? H6A C6 H6B 107.6 . . ? N3 C7 C6 111.4(3) . . ? N3 C7 H7A 109.3 . . ? C6 C7 H7A 109.3 . . ? N3 C7 H7B 109.3 . . ? C6 C7 H7B 109.3 . . ? H7A C7 H7B 108.0 . . ? N4 C8 N3 108.3(3) . . ? N4 C8 H8 125.8 . . ? N3 C8 H8 125.8 . . ? C10 C9 N3 106.8(3) . . ? C10 C9 H9 126.6 . . ? N3 C9 H9 126.6 . . ? C9 C10 N4 107.0(3) . . ? C9 C10 H10 126.5 . . ? N4 C10 H10 126.5 . . ? N5 C11 N6 111.1(3) . . ? N5 C11 H11 124.4 . . ? N6 C11 H11 124.4 . . ? C13 C12 N5 109.7(3) . . ? C13 C12 H12 125.1 . . ? N5 C12 H12 125.1 . . ? C12 C13 N6 105.9(3) . . ? C12 C13 H13 127.0 . . ? N6 C13 H13 127.0 . . ? N6 C14 C15 112.4(3) . . ? N6 C14 H14A 109.1 . . ? C15 C14 H14A 109.1 . . ? N6 C14 H14B 109.1 . . ? C15 C14 H14B 109.1 . . ? H14A C14 H14B 107.8 . . ? C15 C15 C14 112.1(3) 2 . ? C15 C15 H15A 109.2 2 . ? C14 C15 H15A 109.2 . . ? C15 C15 H15B 109.2 2 . ? C14 C15 H15B 109.2 . . ? H15A C15 H15B 107.9 . . ? O1 C16 O2 124.2(3) . . ? O1 C16 C17 119.3(2) . . ? O2 C16 C17 116.4(2) . . ? C18 C17 C22 119.1(2) . . ? C18 C17 C16 119.4(2) . . ? C22 C17 C16 121.5(2) . . ? C17 C18 C19 121.3(2) . . ? C17 C18 H18 119.4 . . ? C19 C18 H18 119.4 . . ? C20 C19 C18 118.8(2) . . ? C20 C19 C24 123.4(2) . . ? C18 C19 C24 117.7(2) . . ? C19 C20 C21 120.3(3) . . ? C19 C20 H20 119.9 . . ? C21 C20 H20 119.9 . . ? C22 C21 C20 120.9(3) . . ? C22 C21 H21 119.6 . . ? C20 C21 H21 119.6 . . ? C21 C22 C17 119.7(2) . . ? C21 C22 C23 117.1(2) . . ? C17 C22 C23 123.2(2) . . ? O4 C23 O3 123.3(3) . . ? O4 C23 C22 118.7(3) . . ? O3 C23 C22 117.9(3) . . ? C27 C24 C25 112.1(2) . . ? C27 C24 C26 105.8(2) . . ? C25 C24 C26 109.0(2) . . ? C27 C24 C19 112.2(2) . . ? C25 C24 C19 106.2(2) . . ? C26 C24 C19 111.6(2) . . ? F6 C25 F4 108.0(3) . . ? F6 C25 F5 107.4(3) . . ? F4 C25 F5 105.7(3) . . ? F6 C25 C24 110.5(2) . . ? F4 C25 C24 111.7(3) . . ? F5 C25 C24 113.3(2) . . ? F1 C26 F2 107.8(3) . . ? F1 C26 F3 106.2(3) . . ? F2 C26 F3 105.8(2) . . ? F1 C26 C24 111.3(2) . . ? F2 C26 C24 113.9(3) . . ? F3 C26 C24 111.4(3) . . ? C28 C27 C34 118.0(3) . . ? C28 C27 C24 121.7(2) . . ? C34 C27 C24 120.1(2) . . ? C27 C28 C29 123.3(3) . . ? C27 C28 H28 118.4 . . ? C29 C28 H28 118.4 . . ? C28 C29 C31 118.5(2) . . ? C28 C29 C30 113.0(3) . . ? C31 C29 C30 128.4(3) . . ? O5 C30 O6 121.1(3) . . ? O5 C30 C29 119.3(3) . . ? O6 C30 C29 119.6(3) . . ? C33 C31 C29 117.3(3) . . ? C33 C31 C32 114.0(3) . . ? C29 C31 C32 128.6(3) . . ? O8 C32 O7 120.9(3) . . ? O8 C32 C31 119.6(3) . . ? O7 C32 C31 119.5(3) . . ? C31 C33 C34 123.3(3) . . ? C31 C33 H33 118.4 . . ? C34 C33 H33 118.4 . . ? C33 C34 C27 119.5(3) . . ? C33 C34 H34 120.2 . . ? C27 C34 H34 120.2 . . ? C1 N1 C2 104.7(3) . . ? C1 N1 Cd1 132.4(2) . . ? C2 N1 Cd1 122.9(2) . . ? C1 N2 C3 107.0(3) . . ? C1 N2 C4 127.3(3) . . ? C3 N2 C4 125.6(3) . . ? C8 N3 C9 108.6(3) . . ? C8 N3 C7 126.2(3) . . ? C9 N3 C7 125.2(3) . . ? C11 N5 C12 105.6(3) . . ? C11 N5 Cd1 126.4(2) . . ? C12 N5 Cd1 127.8(2) . . ? C11 N6 C13 107.6(3) . . ? C11 N6 C14 126.1(3) . . ? C13 N6 C14 126.2(3) . . ? C16 O1 Cd1 85.81(17) . . ? C16 O2 Cd1 95.44(17) . . ? C23 O3 Cd1 97.0(2) . 2_665 ? C23 O4 Cd1 87.80(19) . 2_665 ? C30 O6 H6 109.5 . . ? H1A O1W H1B 104(3) . . ? H2A O2W H2B 107(3) . . ? Cd1 O3W H3A 112(3) . . ? Cd1 O3W H3B 106(3) . . ? H3A O3W H3B 98(2) . . ? C8 N4 C10 109.3(3) . . ? C8 N4 H4N 129(3) . . ? C10 N4 H4N 121(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C2 C3 N2 0.1(4) . . . . ? N2 C4 C5 C6 -175.2(3) . . . . ? C4 C5 C6 C7 -70.3(5) . . . . ? C5 C6 C7 N3 176.2(3) . . . . ? N3 C9 C10 N4 -0.3(5) . . . . ? N5 C12 C13 N6 0.5(5) . . . . ? N6 C14 C15 C15 179.6(4) . . . 2 ? O1 C16 C17 C18 -39.3(4) . . . . ? O2 C16 C17 C18 141.9(3) . . . . ? O1 C16 C17 C22 142.1(3) . . . . ? O2 C16 C17 C22 -36.8(4) . . . . ? C22 C17 C18 C19 -0.5(4) . . . . ? C16 C17 C18 C19 -179.1(2) . . . . ? C17 C18 C19 C20 -0.9(4) . . . . ? C17 C18 C19 C24 -177.3(2) . . . . ? C18 C19 C20 C21 2.3(4) . . . . ? C24 C19 C20 C21 178.4(3) . . . . ? C19 C20 C21 C22 -2.3(5) . . . . ? C20 C21 C22 C17 0.9(4) . . . . ? C20 C21 C22 C23 -176.2(3) . . . . ? C18 C17 C22 C21 0.5(4) . . . . ? C16 C17 C22 C21 179.1(3) . . . . ? C18 C17 C22 C23 177.4(3) . . . . ? C16 C17 C22 C23 -4.0(4) . . . . ? C21 C22 C23 O4 -54.6(4) . . . . ? C17 C22 C23 O4 128.4(3) . . . . ? C21 C22 C23 O3 121.6(3) . . . . ? C17 C22 C23 O3 -55.4(4) . . . . ? C20 C19 C24 C27 135.4(3) . . . . ? C18 C19 C24 C27 -48.4(3) . . . . ? C20 C19 C24 C25 -101.8(3) . . . . ? C18 C19 C24 C25 74.4(3) . . . . ? C20 C19 C24 C26 16.9(4) . . . . ? C18 C19 C24 C26 -167.0(3) . . . . ? C27 C24 C25 F6 49.8(3) . . . . ? C26 C24 C25 F6 166.6(2) . . . . ? C19 C24 C25 F6 -73.0(3) . . . . ? C27 C24 C25 F4 170.1(2) . . . . ? C26 C24 C25 F4 -73.2(3) . . . . ? C19 C24 C25 F4 47.2(3) . . . . ? C27 C24 C25 F5 -70.7(3) . . . . ? C26 C24 C25 F5 46.1(3) . . . . ? C19 C24 C25 F5 166.4(3) . . . . ? C27 C24 C26 F1 -68.9(3) . . . . ? C25 C24 C26 F1 170.3(2) . . . . ? C19 C24 C26 F1 53.4(3) . . . . ? C27 C24 C26 F2 169.0(2) . . . . ? C25 C24 C26 F2 48.3(3) . . . . ? C19 C24 C26 F2 -68.7(3) . . . . ? C27 C24 C26 F3 49.4(3) . . . . ? C25 C24 C26 F3 -71.4(3) . . . . ? C19 C24 C26 F3 171.7(2) . . . . ? C25 C24 C27 C28 35.1(3) . . . . ? C26 C24 C27 C28 -83.6(3) . . . . ? C19 C24 C27 C28 154.5(3) . . . . ? C25 C24 C27 C34 -150.8(3) . . . . ? C26 C24 C27 C34 90.5(3) . . . . ? C19 C24 C27 C34 -31.4(3) . . . . ? C34 C27 C28 C29 -1.3(4) . . . . ? C24 C27 C28 C29 172.8(2) . . . . ? C27 C28 C29 C31 -0.6(4) . . . . ? C27 C28 C29 C30 -178.3(3) . . . . ? C28 C29 C30 O5 -4.7(4) . . . . ? C31 C29 C30 O5 177.9(3) . . . . ? C28 C29 C30 O6 174.8(3) . . . . ? C31 C29 C30 O6 -2.7(5) . . . . ? C28 C29 C31 C33 2.8(4) . . . . ? C30 C29 C31 C33 -179.9(3) . . . . ? C28 C29 C31 C32 -175.6(3) . . . . ? C30 C29 C31 C32 1.7(5) . . . . ? C33 C31 C32 O8 -12.2(4) . . . . ? C29 C31 C32 O8 166.3(3) . . . . ? C33 C31 C32 O7 167.8(3) . . . . ? C29 C31 C32 O7 -13.7(5) . . . . ? C29 C31 C33 C34 -3.3(4) . . . . ? C32 C31 C33 C34 175.4(3) . . . . ? C31 C33 C34 C27 1.4(4) . . . . ? C28 C27 C34 C33 0.9(4) . . . . ? C24 C27 C34 C33 -173.3(2) . . . . ? N2 C1 N1 C2 -0.2(4) . . . . ? N2 C1 N1 Cd1 179.1(2) . . . . ? C3 C2 N1 C1 0.1(4) . . . . ? C3 C2 N1 Cd1 -179.3(2) . . . . ? N5 Cd1 N1 C1 71.2(3) . . . . ? O2 Cd1 N1 C1 -67.8(3) . . . . ? O3 Cd1 N1 C1 -160.1(3) 2_665 . . . ? O3W Cd1 N1 C1 -118.6(3) . . . . ? O1 Cd1 N1 C1 -16.7(3) . . . . ? O4 Cd1 N1 C1 153.9(3) 2_665 . . . ? N5 Cd1 N1 C2 -109.6(3) . . . . ? O2 Cd1 N1 C2 111.4(3) . . . . ? O3 Cd1 N1 C2 19.1(3) 2_665 . . . ? O3W Cd1 N1 C2 60.6(4) . . . . ? O1 Cd1 N1 C2 162.5(2) . . . . ? O4 Cd1 N1 C2 -26.9(3) 2_665 . . . ? N1 C1 N2 C3 0.3(4) . . . . ? N1 C1 N2 C4 178.2(3) . . . . ? C2 C3 N2 C1 -0.3(4) . . . . ? C2 C3 N2 C4 -178.2(3) . . . . ? C5 C4 N2 C1 -104.2(4) . . . . ? C5 C4 N2 C3 73.3(5) . . . . ? N4 C8 N3 C9 0.4(4) . . . . ? N4 C8 N3 C7 178.4(3) . . . . ? C10 C9 N3 C8 0.0(4) . . . . ? C10 C9 N3 C7 -178.1(3) . . . . ? C6 C7 N3 C8 103.6(4) . . . . ? C6 C7 N3 C9 -78.7(4) . . . . ? N6 C11 N5 C12 -0.3(4) . . . . ? N6 C11 N5 Cd1 176.3(2) . . . . ? C13 C12 N5 C11 -0.1(4) . . . . ? C13 C12 N5 Cd1 -176.6(3) . . . . ? N1 Cd1 N5 C11 93.0(3) . . . . ? O2 Cd1 N5 C11 -166.1(2) . . . . ? O3 Cd1 N5 C11 2.9(3) 2_665 . . . ? O3W Cd1 N5 C11 -83.9(3) . . . . ? O1 Cd1 N5 C11 -162.5(3) . . . . ? O4 Cd1 N5 C11 -12.8(3) 2_665 . . . ? N1 Cd1 N5 C12 -91.2(3) . . . . ? O2 Cd1 N5 C12 9.7(4) . . . . ? O3 Cd1 N5 C12 178.8(3) 2_665 . . . ? O3W Cd1 N5 C12 91.9(3) . . . . ? O1 Cd1 N5 C12 13.4(3) . . . . ? O4 Cd1 N5 C12 163.0(3) 2_665 . . . ? N5 C11 N6 C13 0.6(4) . . . . ? N5 C11 N6 C14 177.3(3) . . . . ? C12 C13 N6 C11 -0.7(4) . . . . ? C12 C13 N6 C14 -177.3(3) . . . . ? C15 C14 N6 C11 -100.7(4) . . . . ? C15 C14 N6 C13 75.4(5) . . . . ? O2 C16 O1 Cd1 12.8(3) . . . . ? C17 C16 O1 Cd1 -165.9(2) . . . . ? N5 Cd1 O1 C16 175.94(19) . . . . ? N1 Cd1 O1 C16 -84.36(19) . . . . ? O2 Cd1 O1 C16 -7.10(16) . . . . ? O3 Cd1 O1 C16 14.9(3) 2_665 . . . ? O3W Cd1 O1 C16 77.44(18) . . . . ? O4 Cd1 O1 C16 111.9(2) 2_665 . . . ? O1 C16 O2 Cd1 -14.1(3) . . . . ? C17 C16 O2 Cd1 164.69(19) . . . . ? N5 Cd1 O2 C16 11.5(2) . . . . ? N1 Cd1 O2 C16 116.58(17) . . . . ? O3 Cd1 O2 C16 -160.06(16) 2_665 . . . ? O3W Cd1 O2 C16 -77.75(17) . . . . ? O1 Cd1 O2 C16 6.93(16) . . . . ? O4 Cd1 O2 C16 -129.16(17) 2_665 . . . ? O4 C23 O3 Cd1 -8.5(3) . . . 2_665 ? C22 C23 O3 Cd1 175.5(2) . . . 2_665 ? O3 C23 O4 Cd1 7.8(3) . . . 2_665 ? C22 C23 O4 Cd1 -176.2(2) . . . 2_665 ? N3 C8 N4 C10 -0.6(4) . . . . ? C9 C10 N4 C8 0.6(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O6 H6 O7 0.82 1.58 2.387(4) 167.3 . O1W H1A O1 0.899(19) 2.05(2) 2.925(4) 163(4) 2_656 O1W H1B O7 0.883(19) 2.00(2) 2.859(4) 163(4) . O1W H1B O8 0.883(19) 2.51(3) 3.214(4) 137(4) . O2W H2B O4 0.87(5) 1.96(5) 2.804(5) 161(5) 2_566 O2W H2A O1W 0.90(5) 1.89(6) 2.777(5) 169(6) 1_455 O3W H3A O3 0.92(5) 1.83(5) 2.747(4) 174(4) . O3W H3B O2 0.922(19) 2.15(3) 2.956(3) 145(3) 2_665 N4 H4N O2W 0.87(4) 1.78(2) 2.655(4) 179(4) . _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.767 _refine_diff_density_min -0.454 _refine_diff_density_rms 0.121 #=========================END data_Compound-2 _database_code_depnum_ccdc_archive 'CCDC 780168' #TrackingRef '- crystals.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H18 Cd2 F6 N2 O10 0.5(H2 O)' _chemical_formula_sum 'C24 H19 Cd2 F6 N2 O10.50' _chemical_formula_weight 842.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_hall '-P 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.838(5) _cell_length_b 11.043(5) _cell_length_c 16.485(5) _cell_angle_alpha 73.063(5) _cell_angle_beta 80.033(5) _cell_angle_gamma 85.796(5) _cell_volume 1344.0(11) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6575 _cell_measurement_theta_min 4.4 _cell_measurement_theta_max 29.7 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.226 _exptl_crystal_size_mid 0.214 _exptl_crystal_size_min 0.197 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.081 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 822 _exptl_absorpt_coefficient_mu 1.687 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.685 _exptl_absorpt_correction_T_max 0.721 _exptl_absorpt_process_details ; Higashi,T (1995) Program for absorption correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10870 _diffrn_reflns_av_R_equivalents 0.0340 _diffrn_reflns_av_sigmaI/netI 0.0821 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 4.37 _diffrn_reflns_theta_max 29.74 _reflns_number_total 6575 _reflns_number_gt 4300 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction PROCESS-AUTO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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^)+(0.0252P)^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 6575 _refine_ls_number_parameters 422 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0713 _refine_ls_R_factor_gt 0.0366 _refine_ls_wR_factor_ref 0.0682 _refine_ls_wR_factor_gt 0.0618 _refine_ls_goodness_of_fit_ref 0.885 _refine_ls_restrained_S_all 0.886 _refine_ls_shift/su_max 0.008 _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 Cd1 Cd -0.07865(3) 0.65816(2) 0.389412(16) 0.02115(8) Uani 1 1 d . . . Cd2 Cd -0.51092(4) 0.75857(3) 0.468650(18) 0.02599(9) Uani 1 1 d . . . C1 C -0.0014(6) 0.7463(4) 0.1840(3) 0.0378(10) Uani 1 1 d . . . H1 H -0.1167 0.7308 0.1845 0.045 Uiso 1 1 calc R . . C2 C 0.2364(6) 0.7620(4) 0.2249(3) 0.0369(11) Uani 1 1 d . . . H2 H 0.3187 0.7594 0.2598 0.044 Uiso 1 1 calc R . . C3 C 0.2649(6) 0.8021(4) 0.1385(3) 0.0425(11) Uani 1 1 d . . . H3 H 0.3684 0.8309 0.1033 0.051 Uiso 1 1 calc R . . C4 C 0.0759(7) 0.8235(4) 0.0239(2) 0.0426(12) Uani 1 1 d . . . H4A H -0.0351 0.7898 0.0241 0.051 Uiso 1 1 calc R . . H4B H 0.1642 0.7827 -0.0089 0.051 Uiso 1 1 calc R . . C5 C 0.0736(6) 0.9644(4) -0.0204(2) 0.0420(12) Uani 1 1 d . . . H5A H 0.0633 0.9778 -0.0802 0.050 Uiso 1 1 calc R . . H5B H 0.1829 0.9988 -0.0187 0.050 Uiso 1 1 calc R . . C6 C -0.2248(6) 0.9271(4) 0.3768(3) 0.0423(13) Uani 1 1 d . . . C7 C -0.0917(5) 1.0138(3) 0.3161(2) 0.0237(8) Uani 1 1 d . . . C8 C -0.1531(5) 1.1125(3) 0.2530(2) 0.0290(9) Uani 1 1 d . . . H8 H -0.2697 1.1160 0.2476 0.035 Uiso 1 1 calc R . . C9 C -0.0455(5) 1.2052(3) 0.1985(2) 0.0249(9) Uani 1 1 d . . . H9 H -0.0898 1.2698 0.1567 0.030 Uiso 1 1 calc R . . C10 C 0.1285(4) 1.2026(3) 0.2056(2) 0.0168(7) Uani 1 1 d . . . C11 C 0.1917(5) 1.1023(3) 0.2684(2) 0.0201(8) Uani 1 1 d . . . H11 H 0.3081 1.0997 0.2741 0.024 Uiso 1 1 calc R . . C12 C 0.0849(5) 1.0075(3) 0.3221(2) 0.0197(8) Uani 1 1 d . . . C13 C 0.1628(5) 0.8986(3) 0.3854(2) 0.0226(8) Uani 1 1 d . . . C14 C 0.2563(4) 1.3052(3) 0.1499(2) 0.0187(8) Uani 1 1 d . . . C15 C 0.3481(5) 1.3620(3) 0.2052(2) 0.0182(8) Uani 1 1 d . . . C16 C 0.2538(5) 1.3744(3) 0.2827(2) 0.0194(8) Uani 1 1 d . . . H16 H 0.1426 1.3425 0.3007 0.023 Uiso 1 1 calc R . . C17 C 0.3224(4) 1.4331(3) 0.3331(2) 0.0152(7) Uani 1 1 d . . . C18 C 0.4874(4) 1.4834(3) 0.3060(2) 0.0186(8) Uani 1 1 d . . . C19 C 0.5810(5) 1.4701(4) 0.2294(2) 0.0254(8) Uani 1 1 d . . . H19 H 0.6920 1.5022 0.2111 0.030 Uiso 1 1 calc R . . C20 C 0.5134(5) 1.4104(4) 0.1798(2) 0.0259(9) Uani 1 1 d . . . H20 H 0.5792 1.4025 0.1289 0.031 Uiso 1 1 calc R . . C21 C 0.5595(5) 1.5615(3) 0.3533(2) 0.0195(8) Uani 1 1 d . . . C22 C 0.2124(5) 1.4282(3) 0.4187(2) 0.0185(8) Uani 1 1 d . . . C23 C 0.3861(5) 1.2422(4) 0.0909(2) 0.0277(9) Uani 1 1 d . . . C24 C 0.1652(5) 1.4181(4) 0.0918(2) 0.0286(9) Uani 1 1 d . . . N1 N 0.0690(5) 0.7258(3) 0.2535(2) 0.0330(8) Uani 1 1 d . . . N2 N 0.1102(5) 0.7917(3) 0.11291(19) 0.0323(8) Uani 1 1 d . . . O1 O -0.2719(4) 0.8340(3) 0.3584(2) 0.0582(10) Uani 1 1 d DU . . O2 O -0.2557(16) 0.9724(11) 0.4561(8) 0.051(3) Uani 0.40 1 d P . . O2' O -0.3129(9) 0.9496(7) 0.4327(5) 0.0424(18) Uani 0.60 1 d P . . O3 O 0.0719(3) 0.8040(2) 0.42535(15) 0.0270(6) Uani 1 1 d . . . O4 O 0.3167(3) 0.9096(2) 0.39323(18) 0.0363(7) Uani 1 1 d . . . O5 O 0.0600(3) 1.4669(2) 0.42075(15) 0.0264(6) Uani 1 1 d . . . O6 O 0.2766(3) 1.3728(2) 0.48598(14) 0.0226(6) Uani 1 1 d . . . O7 O 0.4539(3) 1.6201(2) 0.39516(16) 0.0268(6) Uani 1 1 d . . . O8 O 0.7236(3) 1.5611(2) 0.34459(16) 0.0291(6) Uani 1 1 d . . . F1 F 0.4759(3) 1.3241(2) 0.02356(14) 0.0423(6) Uani 1 1 d . . . F2 F 0.3053(3) 1.1686(2) 0.05838(15) 0.0414(6) Uani 1 1 d . . . F3 F 0.5029(3) 1.1671(2) 0.13379(15) 0.0411(6) Uani 1 1 d . . . F4 F 0.0980(3) 1.3851(2) 0.03186(13) 0.0396(6) Uani 1 1 d . . . F5 F 0.2723(3) 1.5122(2) 0.04939(14) 0.0409(6) Uani 1 1 d . . . F6 F 0.0361(3) 1.4675(2) 0.13703(14) 0.0349(6) Uani 1 1 d . . . O1W O -0.7614(4) 0.6991(3) 0.56408(18) 0.0406(8) Uani 1 1 d D . . H1A H -0.777(6) 0.620(2) 0.591(3) 0.061 Uiso 1 1 d D . . H1B H -0.830(5) 0.727(4) 0.527(2) 0.061 Uiso 1 1 d D . . O2W O -0.4873(4) 0.8326(3) 0.5878(2) 0.0476(8) Uani 1 1 d D . . H2A H -0.579(3) 0.883(3) 0.574(3) 0.071 Uiso 1 1 d D . . H2B H -0.396(3) 0.883(3) 0.572(3) 0.071 Uiso 1 1 d D . . O3W O -0.392(2) 0.8823(16) 0.1970(9) 0.212(7) Uiso 0.50 1 d PD . . 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 Cd1 0.01804(15) 0.02212(15) 0.02254(15) -0.00407(12) -0.00357(12) -0.00428(12) Cd2 0.02180(16) 0.02321(16) 0.03445(17) -0.00941(13) -0.00776(13) 0.00290(13) C1 0.039(3) 0.041(3) 0.036(2) -0.009(2) -0.013(2) -0.009(2) C2 0.028(2) 0.050(3) 0.029(2) -0.005(2) -0.0074(19) 0.001(2) C3 0.029(2) 0.066(3) 0.027(2) -0.007(2) -0.0010(19) -0.005(2) C4 0.067(3) 0.037(3) 0.028(2) -0.0117(19) -0.018(2) 0.000(2) C5 0.064(3) 0.040(3) 0.020(2) -0.0056(18) -0.006(2) -0.003(2) C6 0.018(2) 0.023(2) 0.064(3) 0.013(2) 0.003(2) 0.011(2) C7 0.023(2) 0.0164(18) 0.031(2) -0.0049(16) -0.0018(17) -0.0069(16) C8 0.019(2) 0.026(2) 0.038(2) -0.0005(18) -0.0068(18) -0.0076(17) C9 0.022(2) 0.022(2) 0.026(2) 0.0051(16) -0.0101(17) -0.0034(17) C10 0.0197(18) 0.0151(17) 0.0148(17) -0.0035(14) -0.0002(15) -0.0045(15) C11 0.0194(19) 0.0201(19) 0.0205(18) -0.0038(15) -0.0048(16) -0.0033(16) C12 0.024(2) 0.0131(17) 0.0211(18) -0.0044(15) -0.0028(16) -0.0007(16) C13 0.024(2) 0.0170(19) 0.026(2) -0.0044(16) -0.0058(17) 0.0011(17) C14 0.0179(18) 0.0227(19) 0.0172(17) -0.0062(15) -0.0034(15) -0.0073(16) C15 0.0218(19) 0.0181(18) 0.0159(17) -0.0060(14) -0.0010(15) -0.0087(16) C16 0.0171(18) 0.0193(18) 0.0192(18) -0.0018(15) -0.0007(15) -0.0052(15) C17 0.0194(18) 0.0107(16) 0.0168(17) -0.0031(13) -0.0079(15) 0.0003(14) C18 0.0135(17) 0.0205(19) 0.0216(18) -0.0052(15) -0.0032(15) -0.0020(15) C19 0.0170(19) 0.034(2) 0.027(2) -0.0127(17) 0.0044(16) -0.0122(17) C20 0.021(2) 0.037(2) 0.022(2) -0.0134(17) 0.0048(16) -0.0104(18) C21 0.0214(19) 0.0160(18) 0.0206(18) -0.0006(15) -0.0078(16) -0.0048(16) C22 0.0197(19) 0.0155(18) 0.0224(19) -0.0080(15) -0.0031(16) -0.0034(16) C23 0.032(2) 0.029(2) 0.027(2) -0.0149(18) -0.0033(19) -0.0087(19) C24 0.038(2) 0.022(2) 0.024(2) 0.0032(17) -0.0114(19) -0.0100(19) N1 0.035(2) 0.037(2) 0.0240(18) -0.0034(15) -0.0048(16) -0.0075(17) N2 0.045(2) 0.0307(19) 0.0204(17) -0.0036(14) -0.0073(16) -0.0036(17) O1 0.0268(17) 0.0195(16) 0.109(3) 0.0245(17) -0.0281(19) -0.0130(14) O2 0.058(8) 0.043(6) 0.047(7) -0.013(5) 0.023(6) -0.037(5) O2' 0.037(4) 0.032(4) 0.050(5) -0.008(3) 0.007(3) 0.006(3) O3 0.0316(15) 0.0190(13) 0.0280(14) 0.0019(11) -0.0095(12) -0.0097(12) O4 0.0205(15) 0.0274(15) 0.0523(18) 0.0055(13) -0.0106(14) -0.0021(13) O5 0.0155(13) 0.0318(15) 0.0305(14) -0.0091(12) -0.0009(11) 0.0029(12) O6 0.0232(14) 0.0303(14) 0.0149(12) -0.0078(11) -0.0044(11) 0.0038(12) O7 0.0258(15) 0.0285(14) 0.0329(15) -0.0177(12) -0.0073(12) 0.0000(12) O8 0.0200(14) 0.0385(16) 0.0359(15) -0.0180(13) -0.0079(12) -0.0074(12) F1 0.0495(16) 0.0442(15) 0.0297(13) -0.0129(11) 0.0150(12) -0.0191(13) F2 0.0485(16) 0.0451(15) 0.0421(14) -0.0307(12) 0.0001(12) -0.0162(12) F3 0.0332(14) 0.0459(15) 0.0456(14) -0.0190(12) -0.0031(12) 0.0076(12) F4 0.0570(17) 0.0370(13) 0.0278(12) -0.0018(10) -0.0243(12) -0.0083(12) F5 0.0511(16) 0.0286(13) 0.0344(13) 0.0096(11) -0.0071(12) -0.0213(12) F6 0.0361(14) 0.0258(12) 0.0421(13) -0.0069(10) -0.0108(12) 0.0020(11) O1W 0.0333(17) 0.0461(19) 0.0357(17) 0.0008(15) -0.0084(14) -0.0017(16) O2W 0.046(2) 0.0416(19) 0.057(2) -0.0160(17) -0.0087(18) -0.0027(16) _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 Cd1 O5 2.265(2) 1_545 ? Cd1 N1 2.274(3) . ? Cd1 O8 2.280(3) 1_445 ? Cd1 O6 2.304(2) 2_576 ? Cd1 O3 2.327(3) . ? Cd1 O1 2.363(3) . ? Cd2 O7 2.266(3) 1_445 ? Cd2 O4 2.279(2) 1_455 ? Cd2 O1W 2.298(3) . ? Cd2 O6 2.343(2) 2_576 ? Cd2 O2W 2.376(3) . ? Cd2 O1 2.382(4) . ? Cd2 O2' 2.578(8) . ? C1 N1 1.310(5) . ? C1 N2 1.326(5) . ? C1 H1 0.9300 . ? C2 C3 1.345(6) . ? C2 N1 1.363(5) . ? C2 H2 0.9300 . ? C3 N2 1.373(5) . ? C3 H3 0.9300 . ? C4 N2 1.474(5) . ? C4 C5 1.513(6) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C5 1.519(8) 2_575 ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 O2' 1.130(8) . ? C6 O1 1.249(6) . ? C6 C7 1.494(6) . ? C6 O2 1.508(12) . ? C7 C8 1.392(5) . ? C7 C12 1.400(5) . ? C8 C9 1.376(5) . ? C8 H8 0.9300 . ? C9 C10 1.387(5) . ? C9 H9 0.9300 . ? C10 C11 1.405(4) . ? C10 C14 1.541(5) . ? C11 C12 1.383(5) . ? C11 H11 0.9300 . ? C12 C13 1.513(5) . ? C13 O4 1.254(5) . ? C13 O3 1.256(4) . ? C14 C15 1.538(5) . ? C14 C24 1.547(5) . ? C14 C23 1.555(5) . ? C15 C20 1.387(5) . ? C15 C16 1.399(5) . ? C16 C17 1.386(5) . ? C16 H16 0.9300 . ? C17 C18 1.394(5) . ? C17 C22 1.509(5) . ? C18 C19 1.388(5) . ? C18 C21 1.512(5) . ? C19 C20 1.378(5) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 O7 1.251(4) . ? C21 O8 1.269(4) . ? C22 O5 1.237(4) . ? C22 O6 1.269(4) . ? C23 F1 1.335(4) . ? C23 F2 1.340(4) . ? C23 F3 1.340(4) . ? C24 F6 1.331(5) . ? C24 F5 1.332(4) . ? C24 F4 1.344(4) . ? O2 O2' 0.739(10) . ? O4 Cd2 2.279(2) 1_655 ? O5 Cd1 2.265(2) 1_565 ? O6 Cd1 2.304(2) 2_576 ? O6 Cd2 2.343(2) 2_576 ? O7 Cd2 2.266(3) 1_665 ? O8 Cd1 2.280(3) 1_665 ? O1W H1A 0.864(18) . ? O1W H1B 0.86(4) . ? O2W H2A 0.90(3) . ? O2W H2B 0.89(3) . ? 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 O5 Cd1 N1 94.72(10) 1_545 . ? O5 Cd1 O8 85.93(10) 1_545 1_445 ? N1 Cd1 O8 91.34(11) . 1_445 ? O5 Cd1 O6 98.36(9) 1_545 2_576 ? N1 Cd1 O6 165.99(10) . 2_576 ? O8 Cd1 O6 84.61(10) 1_445 2_576 ? O5 Cd1 O3 109.64(10) 1_545 . ? N1 Cd1 O3 88.05(11) . . ? O8 Cd1 O3 164.42(8) 1_445 . ? O6 Cd1 O3 92.26(10) 2_576 . ? O5 Cd1 O1 168.59(10) 1_545 . ? N1 Cd1 O1 89.68(12) . . ? O8 Cd1 O1 83.44(11) 1_445 . ? O6 Cd1 O1 76.55(11) 2_576 . ? O3 Cd1 O1 80.99(11) . . ? O7 Cd2 O4 92.72(10) 1_445 1_455 ? O7 Cd2 O1W 92.85(11) 1_445 . ? O4 Cd2 O1W 84.71(10) 1_455 . ? O7 Cd2 O6 85.83(9) 1_445 2_576 ? O4 Cd2 O6 164.39(10) 1_455 2_576 ? O1W Cd2 O6 110.87(10) . 2_576 ? O7 Cd2 O2W 158.60(10) 1_445 . ? O4 Cd2 O2W 103.10(11) 1_455 . ? O1W Cd2 O2W 74.65(12) . . ? O6 Cd2 O2W 82.67(9) 2_576 . ? O7 Cd2 O1 85.81(12) 1_445 . ? O4 Cd2 O1 88.92(10) 1_455 . ? O1W Cd2 O1 173.43(9) . . ? O6 Cd2 O1 75.47(9) 2_576 . ? O2W Cd2 O1 108.50(13) . . ? O7 Cd2 O2' 132.3(2) 1_445 . ? O4 Cd2 O2' 81.27(17) 1_455 . ? O1W Cd2 O2' 132.99(19) . . ? O6 Cd2 O2' 88.20(17) 2_576 . ? O2W Cd2 O2' 65.4(2) . . ? O1 Cd2 O2' 47.0(2) . . ? N1 C1 N2 112.4(4) . . ? N1 C1 H1 123.8 . . ? N2 C1 H1 123.8 . . ? C3 C2 N1 109.8(4) . . ? C3 C2 H2 125.1 . . ? N1 C2 H2 125.1 . . ? C2 C3 N2 106.2(4) . . ? C2 C3 H3 126.9 . . ? N2 C3 H3 126.9 . . ? N2 C4 C5 113.5(3) . . ? N2 C4 H4A 108.9 . . ? C5 C4 H4A 108.9 . . ? N2 C4 H4B 108.9 . . ? C5 C4 H4B 108.9 . . ? H4A C4 H4B 107.7 . . ? C4 C5 C5 113.1(5) . 2_575 ? C4 C5 H5A 109.0 . . ? C5 C5 H5A 109.0 2_575 . ? C4 C5 H5B 109.0 . . ? C5 C5 H5B 109.0 2_575 . ? H5A C5 H5B 107.8 . . ? O2' C6 O1 113.2(6) . . ? O2' C6 C7 124.8(6) . . ? O1 C6 C7 120.5(5) . . ? O2' C6 O2 28.2(5) . . ? O1 C6 O2 134.6(6) . . ? C7 C6 O2 104.5(6) . . ? C8 C7 C12 118.7(3) . . ? C8 C7 C6 116.3(3) . . ? C12 C7 C6 124.9(3) . . ? C9 C8 C7 121.6(4) . . ? C9 C8 H8 119.2 . . ? C7 C8 H8 119.2 . . ? C8 C9 C10 120.3(3) . . ? C8 C9 H9 119.8 . . ? C10 C9 H9 119.8 . . ? C9 C10 C11 118.4(3) . . ? C9 C10 C14 123.8(3) . . ? C11 C10 C14 117.8(3) . . ? C12 C11 C10 121.5(3) . . ? C12 C11 H11 119.3 . . ? C10 C11 H11 119.3 . . ? C11 C12 C7 119.4(3) . . ? C11 C12 C13 118.9(3) . . ? C7 C12 C13 121.6(3) . . ? O4 C13 O3 124.6(3) . . ? O4 C13 C12 116.6(3) . . ? O3 C13 C12 118.8(3) . . ? C15 C14 C10 111.7(3) . . ? C15 C14 C24 105.8(3) . . ? C10 C14 C24 112.4(3) . . ? C15 C14 C23 112.2(3) . . ? C10 C14 C23 106.8(3) . . ? C24 C14 C23 107.9(3) . . ? C20 C15 C16 118.1(3) . . ? C20 C15 C14 123.9(3) . . ? C16 C15 C14 117.8(3) . . ? C17 C16 C15 121.4(3) . . ? C17 C16 H16 119.3 . . ? C15 C16 H16 119.3 . . ? C16 C17 C18 119.9(3) . . ? C16 C17 C22 115.3(3) . . ? C18 C17 C22 124.7(3) . . ? C19 C18 C17 118.5(3) . . ? C19 C18 C21 119.4(3) . . ? C17 C18 C21 121.8(3) . . ? C20 C19 C18 121.5(4) . . ? C20 C19 H19 119.2 . . ? C18 C19 H19 119.2 . . ? C19 C20 C15 120.6(3) . . ? C19 C20 H20 119.7 . . ? C15 C20 H20 119.7 . . ? O7 C21 O8 127.1(3) . . ? O7 C21 C18 117.7(3) . . ? O8 C21 C18 115.1(3) . . ? O5 C22 O6 122.8(3) . . ? O5 C22 C17 119.2(3) . . ? O6 C22 C17 117.6(3) . . ? F1 C23 F2 106.0(3) . . ? F1 C23 F3 106.5(3) . . ? F2 C23 F3 106.2(3) . . ? F1 C23 C14 114.2(3) . . ? F2 C23 C14 111.6(3) . . ? F3 C23 C14 111.8(3) . . ? F6 C24 F5 106.4(3) . . ? F6 C24 F4 107.2(3) . . ? F5 C24 F4 106.1(3) . . ? F6 C24 C14 111.7(3) . . ? F5 C24 C14 112.6(3) . . ? F4 C24 C14 112.4(3) . . ? C1 N1 C2 105.2(3) . . ? C1 N1 Cd1 124.2(3) . . ? C2 N1 Cd1 130.5(3) . . ? C1 N2 C3 106.4(3) . . ? C1 N2 C4 126.9(4) . . ? C3 N2 C4 126.7(4) . . ? C6 O1 Cd1 112.4(2) . . ? C6 O1 Cd2 103.1(3) . . ? Cd1 O1 Cd2 99.81(11) . . ? O2' O2 C6 46.2(12) . . ? O2 O2' C6 105.6(16) . . ? O2 O2' Cd2 135.0(16) . . ? C6 O2' Cd2 96.5(5) . . ? C13 O3 Cd1 136.4(2) . . ? C13 O4 Cd2 127.1(2) . 1_655 ? C22 O5 Cd1 136.2(2) . 1_565 ? C22 O6 Cd1 113.5(2) . 2_576 ? C22 O6 Cd2 141.4(2) . 2_576 ? Cd1 O6 Cd2 102.72(9) 2_576 2_576 ? C21 O7 Cd2 132.5(2) . 1_665 ? C21 O8 Cd1 135.5(2) . 1_665 ? Cd2 O1W H1A 119(3) . . ? Cd2 O1W H1B 96(3) . . ? H1A O1W H1B 112(3) . . ? Cd2 O2W H2A 86(3) . . ? Cd2 O2W H2B 107(4) . . ? H2A O2W H2B 106(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C2 C3 N2 0.7(5) . . . . ? N2 C4 C5 C5 -64.9(6) . . . 2_575 ? O2' C6 C7 C8 -77.9(7) . . . . ? O1 C6 C7 C8 86.8(4) . . . . ? O2 C6 C7 C8 -99.6(6) . . . . ? O2' C6 C7 C12 97.5(6) . . . . ? O1 C6 C7 C12 -97.9(5) . . . . ? O2 C6 C7 C12 75.8(7) . . . . ? C12 C7 C8 C9 -1.8(6) . . . . ? C6 C7 C8 C9 173.9(4) . . . . ? C7 C8 C9 C10 -0.4(6) . . . . ? C8 C9 C10 C11 1.1(5) . . . . ? C8 C9 C10 C14 -177.4(3) . . . . ? C9 C10 C11 C12 0.3(5) . . . . ? C14 C10 C11 C12 178.9(3) . . . . ? C10 C11 C12 C7 -2.5(5) . . . . ? C10 C11 C12 C13 176.9(3) . . . . ? C8 C7 C12 C11 3.1(5) . . . . ? C6 C7 C12 C11 -172.1(4) . . . . ? C8 C7 C12 C13 -176.2(3) . . . . ? C6 C7 C12 C13 8.6(6) . . . . ? C11 C12 C13 O4 9.2(5) . . . . ? C7 C12 C13 O4 -171.4(3) . . . . ? C11 C12 C13 O3 -170.0(3) . . . . ? C7 C12 C13 O3 9.4(5) . . . . ? C9 C10 C14 C15 124.6(4) . . . . ? C11 C10 C14 C15 -53.9(4) . . . . ? C9 C10 C14 C24 5.8(5) . . . . ? C11 C10 C14 C24 -172.6(3) . . . . ? C9 C10 C14 C23 -112.3(4) . . . . ? C11 C10 C14 C23 69.2(4) . . . . ? C10 C14 C15 C20 150.6(3) . . . . ? C24 C14 C15 C20 -86.8(4) . . . . ? C23 C14 C15 C20 30.7(5) . . . . ? C10 C14 C15 C16 -34.6(4) . . . . ? C24 C14 C15 C16 88.0(4) . . . . ? C23 C14 C15 C16 -154.6(3) . . . . ? C20 C15 C16 C17 -0.1(5) . . . . ? C14 C15 C16 C17 -175.2(3) . . . . ? C15 C16 C17 C18 1.3(5) . . . . ? C15 C16 C17 C22 -174.4(3) . . . . ? C16 C17 C18 C19 -1.7(5) . . . . ? C22 C17 C18 C19 173.5(3) . . . . ? C16 C17 C18 C21 172.7(3) . . . . ? C22 C17 C18 C21 -12.0(5) . . . . ? C17 C18 C19 C20 1.0(5) . . . . ? C21 C18 C19 C20 -173.6(3) . . . . ? C18 C19 C20 C15 0.3(5) . . . . ? C16 C15 C20 C19 -0.7(5) . . . . ? C14 C15 C20 C19 174.1(3) . . . . ? C19 C18 C21 O7 147.8(3) . . . . ? C17 C18 C21 O7 -26.6(5) . . . . ? C19 C18 C21 O8 -31.2(4) . . . . ? C17 C18 C21 O8 154.4(3) . . . . ? C16 C17 C22 O5 -54.2(4) . . . . ? C18 C17 C22 O5 130.4(4) . . . . ? C16 C17 C22 O6 119.1(3) . . . . ? C18 C17 C22 O6 -56.4(5) . . . . ? C15 C14 C23 F1 -74.2(4) . . . . ? C10 C14 C23 F1 163.0(3) . . . . ? C24 C14 C23 F1 42.0(4) . . . . ? C15 C14 C23 F2 165.6(3) . . . . ? C10 C14 C23 F2 42.8(4) . . . . ? C24 C14 C23 F2 -78.2(4) . . . . ? C15 C14 C23 F3 46.8(4) . . . . ? C10 C14 C23 F3 -76.0(4) . . . . ? C24 C14 C23 F3 163.0(3) . . . . ? C15 C14 C24 F6 -67.7(4) . . . . ? C10 C14 C24 F6 54.5(4) . . . . ? C23 C14 C24 F6 172.0(3) . . . . ? C15 C14 C24 F5 52.1(4) . . . . ? C10 C14 C24 F5 174.3(3) . . . . ? C23 C14 C24 F5 -68.3(4) . . . . ? C15 C14 C24 F4 171.8(3) . . . . ? C10 C14 C24 F4 -66.0(4) . . . . ? C23 C14 C24 F4 51.5(4) . . . . ? N2 C1 N1 C2 0.8(5) . . . . ? N2 C1 N1 Cd1 176.6(3) . . . . ? C3 C2 N1 C1 -0.9(5) . . . . ? C3 C2 N1 Cd1 -176.3(3) . . . . ? O5 Cd1 N1 C1 113.0(3) 1_545 . . . ? O8 Cd1 N1 C1 27.0(3) 1_445 . . . ? O6 Cd1 N1 C1 -45.9(6) 2_576 . . . ? O3 Cd1 N1 C1 -137.4(3) . . . . ? O1 Cd1 N1 C1 -56.5(3) . . . . ? O5 Cd1 N1 C2 -72.3(4) 1_545 . . . ? O8 Cd1 N1 C2 -158.3(4) 1_445 . . . ? O6 Cd1 N1 C2 128.8(4) 2_576 . . . ? O3 Cd1 N1 C2 37.2(4) . . . . ? O1 Cd1 N1 C2 118.2(4) . . . . ? N1 C1 N2 C3 -0.4(5) . . . . ? N1 C1 N2 C4 179.0(3) . . . . ? C2 C3 N2 C1 -0.2(5) . . . . ? C2 C3 N2 C4 -179.6(4) . . . . ? C5 C4 N2 C1 109.6(5) . . . . ? C5 C4 N2 C3 -71.1(6) . . . . ? O2' C6 O1 Cd1 -111.6(5) . . . . ? C7 C6 O1 Cd1 82.1(4) . . . . ? O2 C6 O1 Cd1 -89.3(9) . . . . ? O2' C6 O1 Cd2 -5.0(5) . . . . ? C7 C6 O1 Cd2 -171.4(3) . . . . ? O2 C6 O1 Cd2 17.3(9) . . . . ? O5 Cd1 O1 C6 155.7(5) 1_545 . . . ? N1 Cd1 O1 C6 -91.5(3) . . . . ? O8 Cd1 O1 C6 177.1(3) 1_445 . . . ? O6 Cd1 O1 C6 91.1(3) 2_576 . . . ? O3 Cd1 O1 C6 -3.4(3) . . . . ? O5 Cd1 O1 Cd2 47.0(6) 1_545 . . . ? N1 Cd1 O1 Cd2 159.83(14) . . . . ? O8 Cd1 O1 Cd2 68.44(13) 1_445 . . . ? O6 Cd1 O1 Cd2 -17.56(11) 2_576 . . . ? O3 Cd1 O1 Cd2 -112.09(14) . . . . ? O7 Cd2 O1 C6 174.6(2) 1_445 . . . ? O4 Cd2 O1 C6 81.8(2) 1_455 . . . ? O1W Cd2 O1 C6 96.1(11) . . . . ? O6 Cd2 O1 C6 -98.6(2) 2_576 . . . ? O2W Cd2 O1 C6 -21.6(3) . . . . ? O2' Cd2 O1 C6 2.8(3) . . . . ? O7 Cd2 O1 Cd1 -69.43(13) 1_445 . . . ? O4 Cd2 O1 Cd1 -162.23(13) 1_455 . . . ? O1W Cd2 O1 Cd1 -147.9(10) . . . . ? O6 Cd2 O1 Cd1 17.35(10) 2_576 . . . ? O2W Cd2 O1 Cd1 94.30(14) . . . . ? O2' Cd2 O1 Cd1 118.7(3) . . . . ? O1 C6 O2 O2' -48(2) . . . . ? C7 C6 O2 O2' 140.0(15) . . . . ? C6 O2 O2' Cd2 117(2) . . . . ? O1 C6 O2' O2 145.0(15) . . . . ? C7 C6 O2' O2 -49.3(18) . . . . ? O1 C6 O2' Cd2 4.6(5) . . . . ? C7 C6 O2' Cd2 170.2(4) . . . . ? O2 C6 O2' Cd2 -140.5(17) . . . . ? O7 Cd2 O2' O2 -134(2) 1_445 . . . ? O4 Cd2 O2' O2 140(2) 1_455 . . . ? O1W Cd2 O2' O2 66(2) . . . . ? O6 Cd2 O2' O2 -51(2) 2_576 . . . ? O2W Cd2 O2' O2 32(2) . . . . ? O1 Cd2 O2' O2 -123(2) . . . . ? O7 Cd2 O2' C6 -14.0(6) 1_445 . . . ? O4 Cd2 O2' C6 -99.7(4) 1_455 . . . ? O1W Cd2 O2' C6 -174.0(3) . . . . ? O6 Cd2 O2' C6 68.7(4) 2_576 . . . ? O2W Cd2 O2' C6 151.5(5) . . . . ? O1 Cd2 O2' C6 -3.0(3) . . . . ? O4 C13 O3 Cd1 -122.1(4) . . . . ? C12 C13 O3 Cd1 57.0(5) . . . . ? O5 Cd1 O3 C13 109.1(3) 1_545 . . . ? N1 Cd1 O3 C13 14.8(3) . . . . ? O8 Cd1 O3 C13 -73.2(5) 1_445 . . . ? O6 Cd1 O3 C13 -151.2(3) 2_576 . . . ? O1 Cd1 O3 C13 -75.2(3) . . . . ? O3 C13 O4 Cd2 7.1(6) . . . 1_655 ? C12 C13 O4 Cd2 -172.1(2) . . . 1_655 ? O6 C22 O5 Cd1 112.6(4) . . . 1_565 ? C17 C22 O5 Cd1 -74.6(4) . . . 1_565 ? O5 C22 O6 Cd1 3.2(4) . . . 2_576 ? C17 C22 O6 Cd1 -169.7(2) . . . 2_576 ? O5 C22 O6 Cd2 161.5(3) . . . 2_576 ? C17 C22 O6 Cd2 -11.5(6) . . . 2_576 ? O8 C21 O7 Cd2 3.8(6) . . . 1_665 ? C18 C21 O7 Cd2 -175.2(2) . . . 1_665 ? O7 C21 O8 Cd1 -2.0(6) . . . 1_665 ? C18 C21 O8 Cd1 177.0(2) . . . 1_665 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2W H2B O2 0.89(3) 2.05(4) 2.736(12) 133(5) . O1W H1A O8 0.864(18) 2.02(2) 2.850(4) 160(4) 2_576 O1W H1B O3 0.86(4) 1.90(2) 2.747(3) 165(5) 1_455 O2W H2A O2 0.90(3) 1.98(2) 2.860(14) 166(4) 2_476 O2W H2B O4 0.89(3) 2.65(4) 3.348(5) 135(4) 2_576 _diffrn_measured_fraction_theta_max 0.859 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.860 _refine_diff_density_min -1.040 _refine_diff_density_rms 0.121 #=========================END data_Compound-3 _database_code_depnum_ccdc_archive 'CCDC 780169' #TrackingRef '- crystals.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H17 F6 Mn2 N2 O10 0.5(H2 O)' _chemical_formula_sum 'C24 H18 F6 Mn2 N2 O10.50' _chemical_formula_weight 726.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_hall '-P 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.7343(4) _cell_length_b 10.9887(8) _cell_length_c 16.5426(10) _cell_angle_alpha 73.026(6) _cell_angle_beta 80.561(5) _cell_angle_gamma 85.382(5) _cell_volume 1325.71(14) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6040 _cell_measurement_theta_min 2.8 _cell_measurement_theta_max 29.2 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.232 _exptl_crystal_size_mid 0.221 _exptl_crystal_size_min 0.201 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.819 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 728 _exptl_absorpt_coefficient_mu 1.059 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.791 _exptl_absorpt_correction_T_max 0.812 _exptl_absorpt_process_details ; Higashi,T (1995) Program for absorption correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Rigaku RAXIS-RAPID' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9703 _diffrn_reflns_av_R_equivalents 0.0354 _diffrn_reflns_av_sigmaI/netI 0.0627 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.79 _diffrn_reflns_theta_max 29.21 _reflns_number_total 6040 _reflns_number_gt 4129 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction PROCESS-AUTO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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^)+(0.0726P)^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 6040 _refine_ls_number_parameters 413 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0697 _refine_ls_R_factor_gt 0.0479 _refine_ls_wR_factor_ref 0.1216 _refine_ls_wR_factor_gt 0.1160 _refine_ls_goodness_of_fit_ref 0.935 _refine_ls_restrained_S_all 0.935 _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 Mn1 Mn 0.91683(5) 0.16843(4) 0.38762(3) 0.02359(13) Uani 1 1 d . . . Mn2 Mn 0.49554(6) 0.24459(4) 0.47123(3) 0.02755(14) Uani 1 1 d . . . C1 C 1.2023(4) 0.5956(3) 0.27272(19) 0.0239(6) Uani 1 1 d . . . H1 H 1.3209 0.5912 0.2775 0.029 Uiso 1 1 calc R . . C2 C 1.0951(4) 0.5011(3) 0.32676(19) 0.0234(6) Uani 1 1 d . . . C3 C 0.9150(4) 0.5117(3) 0.32218(19) 0.0245(6) Uani 1 1 d . . . C4 C 0.8512(4) 0.6101(3) 0.2604(2) 0.0326(7) Uani 1 1 d . . . H4 H 0.7323 0.6154 0.2560 0.039 Uiso 1 1 calc R . . C5 C 0.9610(4) 0.7015(3) 0.2047(2) 0.0304(7) Uani 1 1 d . . . H5 H 0.9157 0.7661 0.1625 0.036 Uiso 1 1 calc R . . C6 C 1.1373(4) 0.6973(3) 0.21136(18) 0.0222(6) Uani 1 1 d . . . C7 C 1.2659(4) 0.8008(3) 0.15504(19) 0.0235(6) Uani 1 1 d . . . C8 C 1.3571(4) 0.8594(3) 0.20994(18) 0.0233(6) Uani 1 1 d . . . C9 C 1.5268(4) 0.9075(3) 0.1834(2) 0.0304(7) Uani 1 1 d . . . H9 H 1.5934 0.8974 0.1334 0.037 Uiso 1 1 calc R . . C10 C 1.5935(4) 0.9700(3) 0.2324(2) 0.0296(7) Uani 1 1 d . . . H10 H 1.7058 1.0012 0.2148 0.035 Uiso 1 1 calc R . . C11 C 1.4986(4) 0.9876(3) 0.30669(18) 0.0225(6) Uani 1 1 d . . . C12 C 1.3303(4) 0.9373(3) 0.33504(18) 0.0213(6) Uani 1 1 d . . . C13 C 1.2637(4) 0.8748(3) 0.28516(18) 0.0235(6) Uani 1 1 d . . . H13 H 1.1521 0.8422 0.3033 0.028 Uiso 1 1 calc R . . C14 C 1.1734(4) 0.3887(3) 0.38765(19) 0.0243(6) Uani 1 1 d . . . C15 C 0.7838(4) 0.4312(3) 0.3898(2) 0.0348(8) Uani 1 1 d . . . C16 C 1.1707(4) 0.9135(3) 0.0967(2) 0.0324(8) Uani 1 1 d . . . C17 C 1.3956(4) 0.7360(3) 0.0966(2) 0.0326(7) Uani 1 1 d . . . C18 C 1.5713(4) 1.0678(3) 0.35264(19) 0.0229(6) Uani 1 1 d . . . C19 C 1.2173(4) 0.9422(3) 0.41674(18) 0.0211(6) Uani 1 1 d . . . C20 C 0.9855(5) 0.2550(3) 0.1847(2) 0.0395(8) Uani 1 1 d . . . H20 H 0.8676 0.2444 0.1843 0.047 Uiso 1 1 calc R . . C21 C 1.2297(5) 0.2621(4) 0.2267(2) 0.0414(8) Uani 1 1 d . . . H21 H 1.3141 0.2569 0.2618 0.050 Uiso 1 1 calc R . . C22 C 1.2600(5) 0.2949(4) 0.1409(2) 0.0468(9) Uani 1 1 d . . . H22 H 1.3670 0.3166 0.1064 0.056 Uiso 1 1 calc R . . C23 C 1.0687(6) 0.3192(4) 0.0261(2) 0.0475(9) Uani 1 1 d . . . H23A H 0.9551 0.2875 0.0262 0.057 Uiso 1 1 calc R . . H23B H 1.1566 0.2753 -0.0052 0.057 Uiso 1 1 calc R . . C24 C 1.0707(5) 0.4617(4) -0.0194(2) 0.0471(9) Uani 1 1 d . . . H24A H 1.1838 0.4932 -0.0184 0.057 Uiso 1 1 calc R . . H24B H 1.0578 0.4747 -0.0787 0.057 Uiso 1 1 calc R . . N1 N 1.0548(4) 0.2372(3) 0.25488(17) 0.0352(6) Uani 1 1 d . . . N2 N 1.1033(4) 0.2903(3) 0.11414(17) 0.0378(7) Uani 1 1 d . . . O1 O 1.0760(3) 0.29422(19) 0.42432(14) 0.0297(5) Uani 1 1 d . . . O2 O 1.3282(3) 0.3931(2) 0.39823(15) 0.0344(5) Uani 1 1 d . . . O3 O 0.7244(3) 0.3352(2) 0.37733(17) 0.0420(6) Uani 1 1 d . . . O4 O 0.7381(4) 0.4712(3) 0.4536(2) 0.0677(9) Uani 1 1 d . . . O5 O 1.4629(3) 1.1210(2) 0.39709(14) 0.0305(5) Uani 1 1 d . . . O6 O 1.7352(3) 1.0771(2) 0.34035(14) 0.0308(5) Uani 1 1 d . . . O7 O 1.0717(3) 0.9979(2) 0.41251(14) 0.0309(5) Uani 1 1 d . . . O8 O 1.2683(3) 0.87787(19) 0.48675(13) 0.0265(5) Uani 1 1 d . . . F1 F 1.0421(3) 0.96603(18) 0.14176(13) 0.0403(5) Uani 1 1 d . . . F2 F 1.2794(3) 1.00767(18) 0.05421(13) 0.0461(5) Uani 1 1 d . . . F3 F 1.1001(3) 0.88126(19) 0.03775(12) 0.0460(5) Uani 1 1 d . . . F4 F 1.4841(3) 0.8180(2) 0.02940(12) 0.0480(5) Uani 1 1 d . . . F5 F 1.5146(3) 0.6609(2) 0.13888(13) 0.0451(5) Uani 1 1 d . . . F6 F 1.3122(3) 0.6625(2) 0.06420(13) 0.0467(5) Uani 1 1 d . . . O3W O 0.6026(17) 0.3807(14) 0.2090(9) 0.175(5) Uiso 0.50 1 d P . . O1W O 0.2468(3) 0.1805(3) 0.55739(17) 0.0453(6) Uani 1 1 d D . . H1B H 0.167(4) 0.211(4) 0.523(2) 0.068 Uiso 1 1 d D . . H1A H 0.222(5) 0.104(2) 0.591(2) 0.068 Uiso 1 1 d D . . O2W O 0.5086(3) 0.3307(2) 0.57476(17) 0.0454(6) Uani 1 1 d D . . H2B H 0.400(3) 0.369(3) 0.580(3) 0.068 Uiso 1 1 d D . . H2A H 0.585(4) 0.393(3) 0.547(3) 0.068 Uiso 1 1 d 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 Mn1 0.0207(2) 0.0249(2) 0.0272(2) -0.00711(19) -0.00753(18) -0.00595(18) Mn2 0.0236(2) 0.0249(2) 0.0389(3) -0.0134(2) -0.0102(2) -0.00066(19) C1 0.0193(14) 0.0256(15) 0.0288(16) -0.0091(12) -0.0052(12) -0.0041(12) C2 0.0235(14) 0.0202(14) 0.0280(15) -0.0068(12) -0.0069(12) -0.0038(12) C3 0.0236(14) 0.0194(14) 0.0307(16) -0.0062(12) -0.0040(12) -0.0058(12) C4 0.0206(15) 0.0323(17) 0.044(2) -0.0051(15) -0.0114(14) -0.0072(13) C5 0.0303(16) 0.0252(15) 0.0350(17) -0.0004(13) -0.0157(14) -0.0054(13) C6 0.0250(14) 0.0205(14) 0.0229(14) -0.0062(12) -0.0051(12) -0.0086(12) C7 0.0250(14) 0.0233(14) 0.0253(15) -0.0081(12) -0.0059(12) -0.0102(12) C8 0.0257(14) 0.0251(14) 0.0221(15) -0.0082(12) -0.0059(12) -0.0085(12) C9 0.0246(15) 0.0394(18) 0.0325(17) -0.0187(14) 0.0021(13) -0.0117(14) C10 0.0217(14) 0.0377(17) 0.0351(18) -0.0174(14) -0.0023(13) -0.0124(13) C11 0.0204(14) 0.0245(14) 0.0256(15) -0.0088(12) -0.0068(12) -0.0045(12) C12 0.0211(13) 0.0216(14) 0.0250(15) -0.0091(12) -0.0092(12) -0.0013(11) C13 0.0212(14) 0.0263(15) 0.0259(15) -0.0094(12) -0.0041(12) -0.0088(12) C14 0.0234(15) 0.0219(14) 0.0309(16) -0.0099(12) -0.0080(12) -0.0019(12) C15 0.0253(16) 0.0222(16) 0.048(2) 0.0010(15) -0.0021(15) 0.0016(13) C16 0.0400(19) 0.0295(16) 0.0285(17) -0.0024(14) -0.0098(15) -0.0180(15) C17 0.0369(18) 0.0361(18) 0.0299(17) -0.0156(15) -0.0013(14) -0.0149(15) C18 0.0246(15) 0.0210(14) 0.0262(15) -0.0070(12) -0.0092(12) -0.0054(12) C19 0.0245(14) 0.0191(13) 0.0240(15) -0.0092(11) -0.0084(12) -0.0041(12) C20 0.0417(19) 0.042(2) 0.0355(19) -0.0078(16) -0.0088(16) -0.0122(16) C21 0.0354(18) 0.054(2) 0.037(2) -0.0132(17) -0.0138(16) 0.0019(17) C22 0.0358(19) 0.066(3) 0.040(2) -0.0163(19) -0.0027(16) -0.0061(18) C23 0.073(3) 0.042(2) 0.0314(19) -0.0122(16) -0.0170(19) -0.0026(19) C24 0.066(3) 0.052(2) 0.0254(18) -0.0110(16) -0.0069(18) -0.009(2) N1 0.0398(16) 0.0356(15) 0.0297(15) -0.0046(12) -0.0074(12) -0.0110(13) N2 0.0489(17) 0.0385(16) 0.0283(15) -0.0086(13) -0.0117(13) -0.0065(14) O1 0.0314(11) 0.0237(10) 0.0353(12) -0.0034(9) -0.0144(10) -0.0082(9) O2 0.0252(11) 0.0247(11) 0.0514(15) -0.0037(10) -0.0124(10) -0.0039(9) O3 0.0241(11) 0.0234(11) 0.0707(18) 0.0057(11) -0.0171(11) -0.0069(9) O4 0.080(2) 0.0456(17) 0.062(2) -0.0114(15) 0.0294(17) -0.0032(15) O5 0.0265(11) 0.0349(12) 0.0394(13) -0.0218(10) -0.0091(10) -0.0052(9) O6 0.0228(11) 0.0415(13) 0.0346(12) -0.0171(10) -0.0055(9) -0.0115(9) O7 0.0238(11) 0.0380(12) 0.0316(12) -0.0111(10) -0.0082(9) 0.0074(10) O8 0.0259(10) 0.0311(11) 0.0246(11) -0.0098(9) -0.0063(9) -0.0010(9) F1 0.0427(11) 0.0314(10) 0.0475(12) -0.0095(9) -0.0128(9) 0.0008(9) F2 0.0519(12) 0.0345(11) 0.0449(12) 0.0060(9) -0.0094(10) -0.0206(10) F3 0.0631(13) 0.0441(11) 0.0368(11) -0.0066(9) -0.0291(10) -0.0118(10) F4 0.0577(13) 0.0528(13) 0.0330(11) -0.0161(10) 0.0126(10) -0.0233(11) F5 0.0371(10) 0.0542(13) 0.0486(12) -0.0242(11) -0.0057(10) 0.0069(10) F6 0.0537(12) 0.0536(13) 0.0476(12) -0.0352(11) -0.0034(10) -0.0177(10) O1W 0.0379(14) 0.0461(15) 0.0452(15) 0.0013(12) -0.0110(12) -0.0061(12) O2W 0.0498(15) 0.0390(14) 0.0496(16) -0.0155(12) -0.0075(13) -0.0036(12) _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 Mn1 O7 2.113(2) 1_545 ? Mn1 O6 2.1541(19) 1_445 ? Mn1 O1 2.192(2) . ? Mn1 N1 2.219(3) . ? Mn1 O3 2.250(2) . ? Mn1 O8 2.270(2) 2_766 ? Mn2 O5 2.131(2) 1_445 ? Mn2 O2 2.195(2) 1_455 ? Mn2 O2W 2.204(3) . ? Mn2 O1W 2.228(3) . ? Mn2 O3 2.240(2) . ? Mn2 O8 2.259(2) 2_766 ? C1 C2 1.385(4) . ? C1 C6 1.395(4) . ? C1 H1 0.9300 . ? C2 C3 1.401(4) . ? C2 C14 1.503(4) . ? C3 C4 1.376(4) . ? C3 C15 1.502(4) . ? C4 C5 1.385(4) . ? C4 H4 0.9300 . ? C5 C6 1.382(4) . ? C5 H5 0.9300 . ? C6 C7 1.553(4) . ? C7 C8 1.536(4) . ? C7 C16 1.548(4) . ? C7 C17 1.554(4) . ? C8 C13 1.381(4) . ? C8 C9 1.408(4) . ? C9 C10 1.384(4) . ? C9 H9 0.9300 . ? C10 C11 1.380(4) . ? C10 H10 0.9300 . ? C11 C12 1.408(4) . ? C11 C18 1.511(4) . ? C12 C13 1.395(4) . ? C12 C19 1.497(4) . ? C13 H13 0.9300 . ? C14 O2 1.245(3) . ? C14 O1 1.274(3) . ? C15 O4 1.248(5) . ? C15 O3 1.266(4) . ? C16 F3 1.335(4) . ? C16 F2 1.339(3) . ? C16 F1 1.339(4) . ? C17 F5 1.330(4) . ? C17 F4 1.335(4) . ? C17 F6 1.344(3) . ? C18 O5 1.247(4) . ? C18 O6 1.258(3) . ? C19 O7 1.240(3) . ? C19 O8 1.274(3) . ? C20 N1 1.314(4) . ? C20 N2 1.337(4) . ? C20 H20 0.9300 . ? C21 C22 1.343(5) . ? C21 N1 1.379(4) . ? C21 H21 0.9300 . ? C22 N2 1.366(4) . ? C22 H22 0.9300 . ? C23 N2 1.462(4) . ? C23 C24 1.527(5) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C24 1.501(8) 2_765 ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? O2 Mn2 2.195(2) 1_655 ? O5 Mn2 2.131(2) 1_665 ? O6 Mn1 2.1541(19) 1_665 ? O7 Mn1 2.113(2) 1_565 ? O8 Mn2 2.259(2) 2_766 ? O8 Mn1 2.270(2) 2_766 ? O1W H1B 0.884(18) . ? O1W H1A 0.881(18) . ? O2W H2B 0.914(18) . ? O2W H2A 0.91(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Mn1 O6 89.38(9) 1_545 1_445 ? O7 Mn1 O1 100.97(8) 1_545 . ? O6 Mn1 O1 169.33(8) 1_445 . ? O7 Mn1 N1 92.40(10) 1_545 . ? O6 Mn1 N1 88.47(9) 1_445 . ? O1 Mn1 N1 88.48(9) . . ? O7 Mn1 O3 171.74(8) 1_545 . ? O6 Mn1 O3 88.11(9) 1_445 . ? O1 Mn1 O3 82.00(8) . . ? N1 Mn1 O3 95.39(10) . . ? O7 Mn1 O8 97.50(8) 1_545 2_766 ? O6 Mn1 O8 86.68(8) 1_445 2_766 ? O1 Mn1 O8 94.48(8) . 2_766 ? N1 Mn1 O8 168.92(9) . 2_766 ? O3 Mn1 O8 74.50(8) . 2_766 ? O5 Mn2 O2 91.18(9) 1_445 1_455 ? O5 Mn2 O2W 165.65(9) 1_445 . ? O2 Mn2 O2W 97.62(9) 1_455 . ? O5 Mn2 O1W 90.80(9) 1_445 . ? O2 Mn2 O1W 84.76(9) 1_455 . ? O2W Mn2 O1W 78.80(10) . . ? O5 Mn2 O3 91.67(9) 1_445 . ? O2 Mn2 O3 87.37(8) 1_455 . ? O2W Mn2 O3 100.01(10) . . ? O1W Mn2 O3 171.80(9) . . ? O5 Mn2 O8 88.19(8) 1_445 2_766 ? O2 Mn2 O8 162.24(8) 1_455 2_766 ? O2W Mn2 O8 86.85(9) . 2_766 ? O1W Mn2 O8 112.99(8) . 2_766 ? O3 Mn2 O8 74.91(8) . 2_766 ? C2 C1 C6 121.9(3) . . ? C2 C1 H1 119.1 . . ? C6 C1 H1 119.1 . . ? C1 C2 C3 118.8(3) . . ? C1 C2 C14 119.9(2) . . ? C3 C2 C14 121.3(2) . . ? C4 C3 C2 119.4(3) . . ? C4 C3 C15 117.5(3) . . ? C2 C3 C15 122.5(3) . . ? C3 C4 C5 121.1(3) . . ? C3 C4 H4 119.5 . . ? C5 C4 H4 119.5 . . ? C6 C5 C4 120.5(3) . . ? C6 C5 H5 119.7 . . ? C4 C5 H5 119.7 . . ? C5 C6 C1 118.2(3) . . ? C5 C6 C7 123.4(3) . . ? C1 C6 C7 118.4(2) . . ? C8 C7 C16 105.6(2) . . ? C8 C7 C6 111.4(2) . . ? C16 C7 C6 112.1(2) . . ? C8 C7 C17 113.4(2) . . ? C16 C7 C17 107.8(3) . . ? C6 C7 C17 106.5(2) . . ? C13 C8 C9 118.5(3) . . ? C13 C8 C7 118.6(2) . . ? C9 C8 C7 122.7(3) . . ? C10 C9 C8 119.3(3) . . ? C10 C9 H9 120.4 . . ? C8 C9 H9 120.4 . . ? C11 C10 C9 122.2(3) . . ? C11 C10 H10 118.9 . . ? C9 C10 H10 118.9 . . ? C10 C11 C12 119.2(3) . . ? C10 C11 C18 119.6(2) . . ? C12 C11 C18 121.1(3) . . ? C13 C12 C11 118.4(3) . . ? C13 C12 C19 116.6(2) . . ? C11 C12 C19 125.0(2) . . ? C8 C13 C12 122.5(3) . . ? C8 C13 H13 118.7 . . ? C12 C13 H13 118.7 . . ? O2 C14 O1 124.4(3) . . ? O2 C14 C2 118.4(3) . . ? O1 C14 C2 117.1(2) . . ? O4 C15 O3 125.8(3) . . ? O4 C15 C3 114.3(3) . . ? O3 C15 C3 119.9(3) . . ? F3 C16 F2 106.3(2) . . ? F3 C16 F1 107.4(3) . . ? F2 C16 F1 105.6(3) . . ? F3 C16 C7 113.4(3) . . ? F2 C16 C7 111.8(2) . . ? F1 C16 C7 111.8(3) . . ? F5 C17 F4 106.6(3) . . ? F5 C17 F6 106.5(3) . . ? F4 C17 F6 105.7(2) . . ? F5 C17 C7 111.9(3) . . ? F4 C17 C7 113.9(3) . . ? F6 C17 C7 111.7(2) . . ? O5 C18 O6 126.4(3) . . ? O5 C18 C11 116.9(2) . . ? O6 C18 C11 116.6(3) . . ? O7 C19 O8 123.5(3) . . ? O7 C19 C12 118.1(2) . . ? O8 C19 C12 118.0(2) . . ? N1 C20 N2 112.5(3) . . ? N1 C20 H20 123.8 . . ? N2 C20 H20 123.8 . . ? C22 C21 N1 109.8(3) . . ? C22 C21 H21 125.1 . . ? N1 C21 H21 125.1 . . ? C21 C22 N2 106.8(3) . . ? C21 C22 H22 126.6 . . ? N2 C22 H22 126.6 . . ? N2 C23 C24 112.4(3) . . ? N2 C23 H23A 109.1 . . ? C24 C23 H23A 109.1 . . ? N2 C23 H23B 109.1 . . ? C24 C23 H23B 109.1 . . ? H23A C23 H23B 107.9 . . ? C24 C24 C23 113.8(4) 2_765 . ? C24 C24 H24A 108.8 2_765 . ? C23 C24 H24A 108.8 . . ? C24 C24 H24B 108.8 2_765 . ? C23 C24 H24B 108.8 . . ? H24A C24 H24B 107.7 . . ? C20 N1 C21 104.6(3) . . ? C20 N1 Mn1 126.1(2) . . ? C21 N1 Mn1 129.2(2) . . ? C20 N2 C22 106.4(3) . . ? C20 N2 C23 126.2(3) . . ? C22 N2 C23 127.4(3) . . ? C14 O1 Mn1 138.0(2) . . ? C14 O2 Mn2 129.50(19) . 1_655 ? C15 O3 Mn2 116.3(2) . . ? C15 O3 Mn1 113.83(18) . . ? Mn2 O3 Mn1 100.93(8) . . ? C18 O5 Mn2 131.68(18) . 1_665 ? C18 O6 Mn1 135.1(2) . 1_665 ? C19 O7 Mn1 150.2(2) . 1_565 ? C19 O8 Mn2 137.55(19) . 2_766 ? C19 O8 Mn1 121.88(18) . 2_766 ? Mn2 O8 Mn1 99.73(8) 2_766 2_766 ? Mn2 O1W H1B 103(3) . . ? Mn2 O1W H1A 128(3) . . ? H1B O1W H1A 111(3) . . ? Mn2 O2W H2B 101(3) . . ? Mn2 O2W H2A 100(3) . . ? H2B O2W H2A 106(3) . . ? _diffrn_measured_fraction_theta_max 0.839 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.030 _refine_diff_density_min -0.566 _refine_diff_density_rms 0.092 #=========================END data_Compound-4 _database_code_depnum_ccdc_archive 'CCDC 780170' #TrackingRef '- crystals.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H27 F6 N6 O8 Zn2, (C H3 C H2 OH)' _chemical_formula_sum 'C36 H33 F6 N6 O9 Zn2' _chemical_formula_weight 938.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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 'P 21/c ' _symmetry_space_group_name_hall '-P 2ybc ' 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 11.021(3) _cell_length_b 20.571(6) _cell_length_c 18.561(6) _cell_angle_alpha 90.00 _cell_angle_beta 105.822(10) _cell_angle_gamma 90.00 _cell_volume 4048.6(19) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9237 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.252 _exptl_crystal_size_mid 0.213 _exptl_crystal_size_min 0.191 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.540 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1908 _exptl_absorpt_coefficient_mu 1.272 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.743 _exptl_absorpt_correction_T_max 0.776 _exptl_absorpt_process_details ; Higashi,T (1995) Program for absorption correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38079 _diffrn_reflns_av_R_equivalents 0.0779 _diffrn_reflns_av_sigmaI/netI 0.0670 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.18 _diffrn_reflns_theta_max 27.48 _reflns_number_total 9237 _reflns_number_gt 5839 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction PROCESS-AUTO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.1206P)^2^+3.4688P] 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 9237 _refine_ls_number_parameters 532 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.1152 _refine_ls_R_factor_gt 0.0702 _refine_ls_wR_factor_ref 0.2198 _refine_ls_wR_factor_gt 0.1912 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.04540(5) 0.10399(3) 0.42202(3) 0.03381(18) Uani 1 1 d . . . Zn2 Zn 0.04949(6) 0.14773(3) 0.66619(3) 0.0407(2) Uani 1 1 d . . . C1 C 0.0295(6) 0.2386(3) 0.4787(4) 0.0601(16) Uani 1 1 d . . . H1 H 0.0712 0.2286 0.5281 0.072 Uiso 1 1 calc R . . C2 C -0.0561(8) 0.2315(3) 0.3622(4) 0.077(2) Uani 1 1 d . . . H2 H -0.0862 0.2136 0.3146 0.092 Uiso 1 1 calc R . . C3 C -0.0594(8) 0.2948(4) 0.3802(5) 0.076(2) Uani 1 1 d . . . H3 H -0.0924 0.3286 0.3475 0.091 Uiso 1 1 calc R . . C4 C 0.0116(8) 0.3593(3) 0.4979(4) 0.072(2) Uani 1 1 d . . . H4A H -0.0075 0.3957 0.4636 0.086 Uiso 1 1 calc R . . H4B H 0.0994 0.3628 0.5263 0.086 Uiso 1 1 calc R . . C5 C -0.0704(7) 0.3638(3) 0.5517(4) 0.071(2) Uani 1 1 d . . . H5A H -0.0475 0.3297 0.5891 0.085 Uiso 1 1 calc R . . H5B H -0.1584 0.3581 0.5245 0.085 Uiso 1 1 calc R . . C6 C -0.0514(7) 0.4305(4) 0.5899(4) 0.0703(19) Uani 1 1 d D . . H6A H 0.0380 0.4377 0.6119 0.084 Uiso 1 1 calc R . . H6B H -0.0820 0.4639 0.5525 0.084 Uiso 1 1 calc R . . C7 C -0.1167(10) 0.4358(4) 0.6474(5) 0.088(3) Uani 1 1 d D . . H7A H -0.0743 0.4091 0.6900 0.106 Uiso 1 1 calc R . . H7B H -0.2022 0.4197 0.6283 0.106 Uiso 1 1 calc R . . C8 C -0.0635(6) 0.5295(3) 0.7403(3) 0.0535(15) Uani 1 1 d . . . H8 H -0.0101 0.5061 0.7791 0.064 Uiso 1 1 calc R . . C9 C -0.1740(7) 0.6065(3) 0.6759(4) 0.0634(17) Uani 1 1 d . . . H9 H -0.2122 0.6468 0.6629 0.076 Uiso 1 1 calc R . . C10 C -0.1881(7) 0.5539(4) 0.6306(4) 0.0696(19) Uani 1 1 d . . . H10 H -0.2350 0.5516 0.5807 0.084 Uiso 1 1 calc R . . C11 C -0.1955(6) 0.1083(3) 0.5684(4) 0.0600(17) Uani 1 1 d . . . H11 H -0.1561 0.0774 0.5460 0.072 Uiso 1 1 calc R . . C12 C -0.2282(6) 0.1854(3) 0.6396(4) 0.0672(19) Uani 1 1 d . . . H12 H -0.2141 0.2179 0.6757 0.081 Uiso 1 1 calc RD . . C13 C -0.3411(6) 0.1668(4) 0.5969(5) 0.073(2) Uani 1 1 d . . . H13 H -0.4189 0.1838 0.5979 0.088 Uiso 1 1 calc R . . C14 C -0.4175(6) 0.0811(4) 0.4962(4) 0.073(2) Uani 1 1 d . . . H14A H -0.3870 0.0714 0.4530 0.088 Uiso 1 1 calc R . . H14B H -0.4931 0.1073 0.4793 0.088 Uiso 1 1 calc R . . C15 C -0.4489(5) 0.0184(3) 0.5296(4) 0.0596(17) Uani 1 1 d . . . H15A H -0.4792 0.0279 0.5729 0.072 Uiso 1 1 calc R . . H15B H -0.3738 -0.0082 0.5459 0.072 Uiso 1 1 calc R . . C16 C 0.1739(4) 0.0743(2) 0.5667(3) 0.0329(10) Uani 1 1 d . . . C17 C 0.2804(4) 0.0555(2) 0.6321(3) 0.0333(10) Uani 1 1 d . . . C18 C 0.3718(5) 0.1028(3) 0.6606(3) 0.0432(12) Uani 1 1 d . . . H18 H 0.3639 0.1438 0.6388 0.052 Uiso 1 1 calc R . . C19 C 0.4734(5) 0.0893(3) 0.7206(3) 0.0471(13) Uani 1 1 d . . . H19 H 0.5325 0.1216 0.7394 0.057 Uiso 1 1 calc R . . C20 C 0.4892(4) 0.0286(2) 0.7532(3) 0.0365(11) Uani 1 1 d . . . C21 C 0.3984(5) -0.0178(3) 0.7254(3) 0.0403(12) Uani 1 1 d . . . H21 H 0.4080 -0.0590 0.7467 0.048 Uiso 1 1 calc R . . C22 C 0.2924(4) -0.0048(2) 0.6661(3) 0.0381(11) Uani 1 1 d . . . C23 C 0.1908(5) -0.0550(3) 0.6460(4) 0.0522(15) Uani 1 1 d . . . C24 C 0.5987(5) 0.0103(3) 0.8224(3) 0.0394(12) Uani 1 1 d . . . C25 C 0.7101(6) 0.0584(3) 0.8358(4) 0.0631(19) Uani 1 1 d . . . C26 C 0.5426(7) 0.0130(4) 0.8909(3) 0.067(2) Uani 1 1 d . . . C27 C 0.6515(4) -0.0576(3) 0.8125(3) 0.0363(11) Uani 1 1 d . . . C28 C 0.6624(5) -0.1084(3) 0.8640(3) 0.0471(13) Uani 1 1 d . . . H28 H 0.6310 -0.1037 0.9054 0.057 Uiso 1 1 calc R . . C29 C 0.7198(6) -0.1654(3) 0.8529(3) 0.0473(13) Uani 1 1 d . . . H29 H 0.7246 -0.1994 0.8867 0.057 Uiso 1 1 calc R . . C30 C 0.7707(5) -0.1740(2) 0.7930(3) 0.0382(11) Uani 1 1 d . . . C31 C 0.8491(8) -0.2348(3) 0.7914(5) 0.0723(13) Uani 1 1 d U . . C32 C 0.7576(5) -0.1246(2) 0.7400(3) 0.0351(10) Uani 1 1 d . . . C33 C 0.8005(5) -0.1301(3) 0.6700(3) 0.0418(12) Uani 1 1 d . . . C34 C 0.6962(5) -0.0677(2) 0.7505(3) 0.0381(11) Uani 1 1 d . . . H34 H 0.6847 -0.0352 0.7144 0.046 Uiso 1 1 calc R . . C35 C 0.489(2) -0.3154(14) 0.4741(16) 0.160(10) Uiso 0.50 1 d PD . . H35A H 0.4789 -0.3535 0.5017 0.241 Uiso 0.50 1 calc PR . . H35B H 0.4958 -0.3279 0.4255 0.241 Uiso 0.50 1 calc PR . . H35C H 0.4180 -0.2872 0.4689 0.241 Uiso 0.50 1 calc PR . . C36 C 0.611(2) -0.2792(12) 0.5168(14) 0.133(8) Uiso 0.50 1 d PD . . H36A H 0.6030 -0.2675 0.5659 0.160 Uiso 0.50 1 calc PR . . H36B H 0.6812 -0.3093 0.5243 0.160 Uiso 0.50 1 calc PR . . C37 C 0.409(2) -0.2276(11) 0.7438(13) 0.113(6) Uiso 0.50 1 d P . . H37A H 0.4808 -0.2517 0.7742 0.135 Uiso 0.50 1 calc PR . . H37B H 0.3422 -0.2593 0.7280 0.135 Uiso 0.50 1 calc PR . . C38 C 0.3701(13) -0.1884(8) 0.7967(10) 0.117(7) Uiso 0.50 1 d PD . . H38A H 0.3641 -0.2148 0.8382 0.176 Uiso 0.50 1 calc PR . . H38B H 0.2892 -0.1697 0.7732 0.176 Uiso 0.50 1 calc PR . . H38C H 0.4306 -0.1544 0.8142 0.176 Uiso 0.50 1 calc PR . . N1 N 0.0016(5) 0.1970(2) 0.4290(3) 0.0478(11) Uani 1 1 d . . . N2 N -0.0053(6) 0.3002(2) 0.4555(3) 0.0669(16) Uani 1 1 d . . . N3 N -0.1201(5) 0.5051(3) 0.6723(3) 0.0584(13) Uani 1 1 d . . . N4 N -0.0938(4) 0.5906(2) 0.7447(3) 0.0439(10) Uani 1 1 d . . . N5 N -0.1365(4) 0.1491(2) 0.6217(3) 0.0498(12) Uani 1 1 d . . . N6 N -0.3207(5) 0.1181(3) 0.5515(3) 0.0611(14) Uani 1 1 d . . . O1 O 0.0805(3) 0.10432(19) 0.5762(2) 0.0451(9) Uani 1 1 d . . . O2 O 0.1844(3) 0.06307(19) 0.50220(19) 0.0428(9) Uani 1 1 d . . . O3 O 0.0962(3) -0.04262(19) 0.5931(2) 0.0453(9) Uani 1 1 d . . . O4 O 0.1973(5) -0.1024(3) 0.6879(4) 0.100(2) Uani 1 1 d D . . O5 O 0.8387(5) -0.2793(2) 0.8330(3) 0.0754(12) Uani 1 1 d U . . O6 O 0.9315(6) -0.2351(3) 0.7611(4) 0.0982(15) Uani 1 1 d U . . O7 O 0.7432(5) -0.1643(3) 0.6198(3) 0.0899(19) Uani 1 1 d . . . O8 O 0.8932(4) -0.0943(2) 0.6681(2) 0.0490(10) Uani 1 1 d . . . F1 F 0.7473(3) 0.06886(18) 0.7751(3) 0.0690(11) Uani 1 1 d . . . F2 F 0.8101(3) 0.0352(2) 0.8884(3) 0.0859(14) Uani 1 1 d . . . F3 F 0.6842(4) 0.11661(19) 0.8611(3) 0.0860(14) Uani 1 1 d . . . F4 F 0.4890(4) 0.0712(2) 0.8950(2) 0.0868(14) Uani 1 1 d . . . F5 F 0.6324(4) 0.0068(2) 0.9559(2) 0.0879(15) Uani 1 1 d . . . F6 F 0.4581(4) -0.0313(2) 0.8887(2) 0.0722(11) Uani 1 1 d . . . O9 O 0.6417(10) -0.2241(5) 0.4839(6) 0.077(3) Uiso 0.50 1 d PD . . H9A H 0.722(2) -0.237(5) 0.500(8) 0.115 Uiso 0.50 1 d PD . . O10 O 0.443(2) -0.2142(12) 0.6792(15) 0.209(9) Uiso 0.50 1 d PD . . H10A H 0.3824 -0.1998 0.6474 0.314 Uiso 0.50 1 calc PRD . . 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 0.0348(3) 0.0315(3) 0.0321(3) 0.0034(2) 0.0039(2) 0.0008(2) Zn2 0.0414(3) 0.0372(4) 0.0398(4) -0.0005(3) 0.0051(3) -0.0024(3) C1 0.075(4) 0.048(4) 0.045(3) 0.005(3) -0.004(3) 0.010(3) C2 0.113(6) 0.051(4) 0.057(4) 0.003(3) 0.007(4) 0.021(4) C3 0.096(5) 0.053(4) 0.074(5) 0.007(4) 0.012(4) 0.023(4) C4 0.086(5) 0.050(4) 0.069(5) -0.010(3) 0.004(4) 0.010(4) C5 0.080(5) 0.053(4) 0.068(5) -0.007(3) 0.001(4) 0.013(4) C6 0.083(5) 0.056(4) 0.066(5) -0.011(4) 0.010(4) 0.003(4) C7 0.141(8) 0.063(5) 0.070(5) -0.016(4) 0.044(5) -0.001(5) C8 0.061(4) 0.053(4) 0.045(3) 0.000(3) 0.011(3) 0.006(3) C9 0.078(4) 0.054(4) 0.050(4) -0.003(3) 0.003(3) 0.018(3) C10 0.086(5) 0.068(5) 0.043(4) -0.009(3) -0.002(3) 0.008(4) C11 0.042(3) 0.070(4) 0.063(4) -0.017(3) 0.006(3) -0.005(3) C12 0.046(3) 0.067(4) 0.086(5) -0.030(4) 0.014(3) 0.001(3) C13 0.045(3) 0.081(5) 0.093(6) -0.022(4) 0.019(4) 0.001(3) C14 0.045(3) 0.086(5) 0.081(5) -0.018(4) 0.002(3) -0.017(4) C15 0.034(3) 0.075(4) 0.066(4) -0.024(4) 0.007(3) -0.005(3) C16 0.030(2) 0.030(2) 0.035(3) 0.004(2) 0.002(2) 0.0005(19) C17 0.030(2) 0.038(3) 0.031(2) 0.003(2) 0.0057(19) 0.004(2) C18 0.045(3) 0.030(3) 0.045(3) 0.001(2) -0.004(2) 0.001(2) C19 0.043(3) 0.034(3) 0.053(3) -0.004(2) -0.007(2) -0.002(2) C20 0.031(2) 0.039(3) 0.032(3) -0.003(2) -0.003(2) 0.007(2) C21 0.038(3) 0.038(3) 0.040(3) 0.006(2) 0.003(2) 0.005(2) C22 0.033(2) 0.037(3) 0.039(3) 0.004(2) 0.001(2) 0.002(2) C23 0.044(3) 0.041(3) 0.063(4) 0.014(3) 0.000(3) -0.007(3) C24 0.034(2) 0.042(3) 0.033(3) -0.005(2) -0.006(2) 0.009(2) C25 0.056(4) 0.047(4) 0.066(4) -0.016(3) -0.019(3) 0.010(3) C26 0.076(5) 0.081(5) 0.037(3) -0.010(3) 0.002(3) 0.038(4) C27 0.033(2) 0.042(3) 0.028(2) 0.001(2) -0.0025(19) 0.006(2) C28 0.051(3) 0.056(4) 0.035(3) 0.003(3) 0.012(2) 0.015(3) C29 0.060(3) 0.045(3) 0.036(3) 0.011(2) 0.010(3) 0.007(3) C30 0.036(2) 0.035(3) 0.042(3) 0.002(2) 0.009(2) -0.001(2) C31 0.093(3) 0.051(2) 0.086(3) 0.022(2) 0.047(2) 0.026(2) C32 0.036(2) 0.033(2) 0.035(3) 0.003(2) 0.006(2) 0.001(2) C33 0.050(3) 0.039(3) 0.037(3) 0.001(2) 0.011(2) 0.010(2) C34 0.041(3) 0.034(3) 0.033(3) 0.007(2) -0.001(2) 0.002(2) N1 0.052(3) 0.039(3) 0.049(3) 0.004(2) 0.009(2) 0.006(2) N2 0.087(4) 0.037(3) 0.057(3) -0.014(2) -0.013(3) 0.014(3) N3 0.080(4) 0.045(3) 0.049(3) -0.008(2) 0.017(3) 0.001(3) N4 0.050(3) 0.043(3) 0.037(2) -0.002(2) 0.009(2) 0.006(2) N5 0.037(2) 0.051(3) 0.059(3) -0.010(2) 0.009(2) -0.002(2) N6 0.042(3) 0.065(3) 0.069(4) -0.007(3) 0.001(2) -0.007(2) O1 0.0398(19) 0.054(2) 0.0346(19) -0.0042(17) -0.0008(16) 0.0126(17) O2 0.0399(18) 0.052(2) 0.0342(19) 0.0078(17) 0.0065(15) 0.0108(17) O3 0.0379(18) 0.048(2) 0.040(2) 0.0081(17) -0.0069(16) -0.0069(16) O4 0.078(3) 0.073(4) 0.113(5) 0.043(3) -0.032(3) -0.027(3) O5 0.098(3) 0.049(2) 0.086(3) 0.022(2) 0.036(2) 0.027(2) O6 0.113(3) 0.079(3) 0.121(4) 0.027(3) 0.064(3) 0.036(3) O7 0.099(4) 0.109(4) 0.072(3) -0.051(3) 0.041(3) -0.054(3) O8 0.057(2) 0.052(2) 0.039(2) -0.0034(17) 0.0147(18) -0.0114(19) F1 0.050(2) 0.053(2) 0.094(3) -0.004(2) 0.003(2) -0.0101(17) F2 0.053(2) 0.076(3) 0.095(3) -0.021(2) -0.038(2) 0.0093(19) F3 0.076(3) 0.051(2) 0.104(3) -0.036(2) -0.022(2) 0.0100(19) F4 0.100(3) 0.091(3) 0.062(3) -0.018(2) 0.010(2) 0.050(3) F5 0.097(3) 0.120(4) 0.0320(19) -0.010(2) -0.0084(19) 0.047(3) F6 0.066(2) 0.101(3) 0.054(2) 0.008(2) 0.0254(19) 0.022(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 Zn1 O3 1.967(4) 3_556 ? Zn1 O8 1.977(4) 3_656 ? Zn1 N1 1.985(5) . ? Zn1 O2 2.006(3) . ? Zn2 O5 1.939(5) 2_656 ? Zn2 N4 1.979(5) 2_546 ? Zn2 N5 1.990(5) . ? Zn2 O1 2.004(4) . ? C1 N1 1.235(8) . ? C1 N2 1.359(8) . ? C1 H1 0.9300 . ? C2 C3 1.347(10) . ? C2 N1 1.420(8) . ? C2 H2 0.9300 . ? C3 N2 1.366(9) . ? C3 H3 0.9300 . ? C4 N2 1.433(8) . ? C4 C5 1.521(11) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.532(10) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C7 1.446(9) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 N3 1.502(9) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 N4 1.309(7) . ? C8 N3 1.344(8) . ? C8 H8 0.9300 . ? C9 C10 1.353(9) . ? C9 N4 1.379(8) . ? C9 H9 0.9300 . ? C10 N3 1.362(9) . ? C10 H10 0.9300 . ? C11 N5 1.325(8) . ? C11 N6 1.343(8) . ? C11 H11 0.9300 . ? C12 C13 1.337(9) . ? C12 N5 1.367(8) . ? C12 H12 0.9300 . ? C13 N6 1.368(9) . ? C13 H13 0.9300 . ? C14 N6 1.474(8) . ? C14 C15 1.511(10) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C15 1.542(11) 3_456 ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 O1 1.253(6) . ? C16 O2 1.255(6) . ? C16 C17 1.491(6) . ? C17 C22 1.381(7) . ? C17 C18 1.397(7) . ? C18 C19 1.375(7) . ? C18 H18 0.9300 . ? C19 C20 1.379(7) . ? C19 H19 0.9300 . ? C20 C21 1.376(7) . ? C20 C24 1.550(6) . ? C21 C22 1.395(7) . ? C21 H21 0.9300 . ? C22 C23 1.494(7) . ? C23 O4 1.238(7) . ? C23 O3 1.248(6) . ? C24 C25 1.543(9) . ? C24 C27 1.543(7) . ? C24 C26 1.560(9) . ? C25 F1 1.317(9) . ? C25 F2 1.344(7) . ? C25 F3 1.346(7) . ? C26 F6 1.294(9) . ? C26 F5 1.341(7) . ? C26 F4 1.347(7) . ? C27 C34 1.386(7) . ? C27 C28 1.398(7) . ? C28 C29 1.375(8) . ? C28 H28 0.9300 . ? C29 C30 1.386(8) . ? C29 H29 0.9300 . ? C30 C32 1.394(7) . ? C30 C31 1.526(8) . ? C31 O6 1.191(8) . ? C31 O5 1.223(8) . ? C32 C34 1.391(7) . ? C32 C33 1.503(7) . ? C33 O7 1.201(7) . ? C33 O8 1.268(7) . ? C34 H34 0.9300 . ? C35 C36 1.551(18) . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 O9 1.37(2) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 O10 1.38(3) . ? C37 C38 1.43(3) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? N4 Zn2 1.979(5) 2_556 ? O3 Zn1 1.967(4) 3_556 ? O5 Zn2 1.939(4) 2_646 ? O8 Zn1 1.977(4) 3_656 ? O9 H9A 0.888(10) . ? O10 H10A 0.8200 . ? 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 O3 Zn1 O8 104.79(16) 3_556 3_656 ? O3 Zn1 N1 115.46(18) 3_556 . ? O8 Zn1 N1 107.31(19) 3_656 . ? O3 Zn1 O2 104.60(15) 3_556 . ? O8 Zn1 O2 102.53(16) 3_656 . ? N1 Zn1 O2 120.40(18) . . ? O5 Zn2 N4 116.2(2) 2_656 2_546 ? O5 Zn2 N5 124.9(2) 2_656 . ? N4 Zn2 N5 110.3(2) 2_546 . ? O5 Zn2 O1 95.66(19) 2_656 . ? N4 Zn2 O1 111.93(18) 2_546 . ? N5 Zn2 O1 92.93(18) . . ? N1 C1 N2 114.8(6) . . ? N1 C1 H1 122.6 . . ? N2 C1 H1 122.6 . . ? C3 C2 N1 107.6(7) . . ? C3 C2 H2 126.2 . . ? N1 C2 H2 126.2 . . ? C2 C3 N2 107.4(6) . . ? C2 C3 H3 126.3 . . ? N2 C3 H3 126.3 . . ? N2 C4 C5 113.6(7) . . ? N2 C4 H4A 108.8 . . ? C5 C4 H4A 108.8 . . ? N2 C4 H4B 108.8 . . ? C5 C4 H4B 108.8 . . ? H4A C4 H4B 107.7 . . ? C4 C5 C6 109.1(6) . . ? C4 C5 H5A 109.9 . . ? C6 C5 H5A 109.9 . . ? C4 C5 H5B 109.9 . . ? C6 C5 H5B 109.9 . . ? H5A C5 H5B 108.3 . . ? C7 C6 C5 112.1(7) . . ? C7 C6 H6A 109.2 . . ? C5 C6 H6A 109.2 . . ? C7 C6 H6B 109.2 . . ? C5 C6 H6B 109.2 . . ? H6A C6 H6B 107.9 . . ? C6 C7 N3 111.0(6) . . ? C6 C7 H7A 109.4 . . ? N3 C7 H7A 109.4 . . ? C6 C7 H7B 109.4 . . ? N3 C7 H7B 109.4 . . ? H7A C7 H7B 108.0 . . ? N4 C8 N3 110.9(6) . . ? N4 C8 H8 124.6 . . ? N3 C8 H8 124.6 . . ? C10 C9 N4 108.8(6) . . ? C10 C9 H9 125.6 . . ? N4 C9 H9 125.6 . . ? C9 C10 N3 106.5(6) . . ? C9 C10 H10 126.7 . . ? N3 C10 H10 126.7 . . ? N5 C11 N6 110.2(6) . . ? N5 C11 H11 124.9 . . ? N6 C11 H11 124.9 . . ? C13 C12 N5 109.3(6) . . ? C13 C12 H12 125.3 . . ? N5 C12 H12 125.3 . . ? C12 C13 N6 107.0(6) . . ? C12 C13 H13 126.5 . . ? N6 C13 H13 126.5 . . ? N6 C14 C15 110.9(6) . . ? N6 C14 H14A 109.5 . . ? C15 C14 H14A 109.5 . . ? N6 C14 H14B 109.5 . . ? C15 C14 H14B 109.5 . . ? H14A C14 H14B 108.0 . . ? C14 C15 C15 109.3(7) . 3_456 ? C14 C15 H15A 109.8 . . ? C15 C15 H15A 109.8 3_456 . ? C14 C15 H15B 109.8 . . ? C15 C15 H15B 109.8 3_456 . ? H15A C15 H15B 108.3 . . ? O1 C16 O2 121.1(4) . . ? O1 C16 C17 120.5(4) . . ? O2 C16 C17 118.1(4) . . ? C22 C17 C18 118.9(4) . . ? C22 C17 C16 124.1(4) . . ? C18 C17 C16 117.1(4) . . ? C19 C18 C17 120.7(5) . . ? C19 C18 H18 119.7 . . ? C17 C18 H18 119.7 . . ? C18 C19 C20 121.1(5) . . ? C18 C19 H19 119.5 . . ? C20 C19 H19 119.5 . . ? C21 C20 C19 118.1(5) . . ? C21 C20 C24 117.8(5) . . ? C19 C20 C24 124.0(5) . . ? C20 C21 C22 122.0(5) . . ? C20 C21 H21 119.0 . . ? C22 C21 H21 119.0 . . ? C17 C22 C21 119.2(5) . . ? C17 C22 C23 122.4(4) . . ? C21 C22 C23 118.3(5) . . ? O4 C23 O3 123.2(5) . . ? O4 C23 C22 118.5(5) . . ? O3 C23 C22 117.6(5) . . ? C25 C24 C27 106.9(4) . . ? C25 C24 C20 112.6(5) . . ? C27 C24 C20 110.8(4) . . ? C25 C24 C26 108.7(5) . . ? C27 C24 C26 112.0(5) . . ? C20 C24 C26 106.0(4) . . ? F1 C25 F2 107.1(6) . . ? F1 C25 F3 107.3(6) . . ? F2 C25 F3 105.8(5) . . ? F1 C25 C24 112.7(5) . . ? F2 C25 C24 110.4(6) . . ? F3 C25 C24 113.0(6) . . ? F6 C26 F5 108.1(6) . . ? F6 C26 F4 107.7(6) . . ? F5 C26 F4 105.1(5) . . ? F6 C26 C24 113.0(5) . . ? F5 C26 C24 111.8(6) . . ? F4 C26 C24 110.8(6) . . ? C34 C27 C28 118.1(5) . . ? C34 C27 C24 117.7(4) . . ? C28 C27 C24 124.1(5) . . ? C29 C28 C27 119.5(5) . . ? C29 C28 H28 120.2 . . ? C27 C28 H28 120.2 . . ? C28 C29 C30 122.1(5) . . ? C28 C29 H29 119.0 . . ? C30 C29 H29 119.0 . . ? C29 C30 C32 119.1(5) . . ? C29 C30 C31 118.3(5) . . ? C32 C30 C31 122.3(5) . . ? O6 C31 O5 120.6(7) . . ? O6 C31 C30 121.4(6) . . ? O5 C31 C30 116.8(6) . . ? C34 C32 C30 118.4(5) . . ? C34 C32 C33 117.6(4) . . ? C30 C32 C33 123.9(5) . . ? O7 C33 O8 125.2(5) . . ? O7 C33 C32 119.4(5) . . ? O8 C33 C32 115.3(5) . . ? C27 C34 C32 122.6(5) . . ? C27 C34 H34 118.7 . . ? C32 C34 H34 118.7 . . ? C36 C35 H35A 109.5 . . ? C36 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C36 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? O9 C36 C35 117(2) . . ? O9 C36 H36A 108.1 . . ? C35 C36 H36A 108.1 . . ? O9 C36 H36B 108.1 . . ? C35 C36 H36B 108.1 . . ? H36A C36 H36B 107.3 . . ? O10 C37 C38 134(2) . . ? O10 C37 H37A 103.8 . . ? C38 C37 H37A 103.8 . . ? O10 C37 H37B 103.8 . . ? C38 C37 H37B 103.8 . . ? H37A C37 H37B 105.4 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C1 N1 C2 105.5(5) . . ? C1 N1 Zn1 134.5(4) . . ? C2 N1 Zn1 118.9(4) . . ? C1 N2 C3 104.7(5) . . ? C1 N2 C4 129.4(6) . . ? C3 N2 C4 125.9(6) . . ? C8 N3 C10 107.5(5) . . ? C8 N3 C7 126.8(6) . . ? C10 N3 C7 125.6(6) . . ? C8 N4 C9 106.3(5) . . ? C8 N4 Zn2 127.8(4) . 2_556 ? C9 N4 Zn2 125.6(4) . 2_556 ? C11 N5 C12 106.4(5) . . ? C11 N5 Zn2 122.8(4) . . ? C12 N5 Zn2 130.8(4) . . ? C11 N6 C13 107.2(5) . . ? C11 N6 C14 126.0(6) . . ? C13 N6 C14 126.7(6) . . ? C16 O1 Zn2 132.1(3) . . ? C16 O2 Zn1 112.3(3) . . ? C23 O3 Zn1 116.2(3) . 3_556 ? C31 O5 Zn2 114.5(5) . 2_646 ? C33 O8 Zn1 115.4(3) . 3_656 ? C36 O9 H9A 87(2) . . ? C37 O10 H10A 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C2 C3 N2 0.3(9) . . . . ? N2 C4 C5 C6 -176.2(6) . . . . ? C4 C5 C6 C7 -174.1(7) . . . . ? C5 C6 C7 N3 -167.8(7) . . . . ? N4 C9 C10 N3 2.1(9) . . . . ? N5 C12 C13 N6 0.0(9) . . . . ? N6 C14 C15 C15 179.5(6) . . . 3_456 ? O1 C16 C17 C22 95.9(6) . . . . ? O2 C16 C17 C22 -88.8(6) . . . . ? O1 C16 C17 C18 -83.0(6) . . . . ? O2 C16 C17 C18 92.2(6) . . . . ? C22 C17 C18 C19 1.3(8) . . . . ? C16 C17 C18 C19 -179.7(5) . . . . ? C17 C18 C19 C20 1.3(9) . . . . ? C18 C19 C20 C21 -1.8(8) . . . . ? C18 C19 C20 C24 -178.0(5) . . . . ? C19 C20 C21 C22 -0.2(8) . . . . ? C24 C20 C21 C22 176.2(5) . . . . ? C18 C17 C22 C21 -3.2(7) . . . . ? C16 C17 C22 C21 177.8(5) . . . . ? C18 C17 C22 C23 171.5(5) . . . . ? C16 C17 C22 C23 -7.4(8) . . . . ? C20 C21 C22 C17 2.8(8) . . . . ? C20 C21 C22 C23 -172.2(5) . . . . ? C17 C22 C23 O4 -166.4(6) . . . . ? C21 C22 C23 O4 8.4(9) . . . . ? C17 C22 C23 O3 4.8(9) . . . . ? C21 C22 C23 O3 179.6(5) . . . . ? C21 C20 C24 C25 165.4(5) . . . . ? C19 C20 C24 C25 -18.4(7) . . . . ? C21 C20 C24 C27 45.7(6) . . . . ? C19 C20 C24 C27 -138.1(5) . . . . ? C21 C20 C24 C26 -75.9(6) . . . . ? C19 C20 C24 C26 100.3(7) . . . . ? C27 C24 C25 F1 71.5(6) . . . . ? C20 C24 C25 F1 -50.4(6) . . . . ? C26 C24 C25 F1 -167.5(5) . . . . ? C27 C24 C25 F2 -48.3(7) . . . . ? C20 C24 C25 F2 -170.1(5) . . . . ? C26 C24 C25 F2 72.7(6) . . . . ? C27 C24 C25 F3 -166.6(5) . . . . ? C20 C24 C25 F3 71.6(7) . . . . ? C26 C24 C25 F3 -45.5(7) . . . . ? C25 C24 C26 F6 -172.4(5) . . . . ? C27 C24 C26 F6 -54.5(6) . . . . ? C20 C24 C26 F6 66.3(6) . . . . ? C25 C24 C26 F5 -50.2(7) . . . . ? C27 C24 C26 F5 67.7(7) . . . . ? C20 C24 C26 F5 -171.5(6) . . . . ? C25 C24 C26 F4 66.7(7) . . . . ? C27 C24 C26 F4 -175.5(5) . . . . ? C20 C24 C26 F4 -54.6(7) . . . . ? C25 C24 C27 C34 -65.4(6) . . . . ? C20 C24 C27 C34 57.6(6) . . . . ? C26 C24 C27 C34 175.6(5) . . . . ? C25 C24 C27 C28 111.4(6) . . . . ? C20 C24 C27 C28 -125.6(5) . . . . ? C26 C24 C27 C28 -7.5(7) . . . . ? C34 C27 C28 C29 2.0(8) . . . . ? C24 C27 C28 C29 -174.9(5) . . . . ? C27 C28 C29 C30 1.7(9) . . . . ? C28 C29 C30 C32 -3.5(9) . . . . ? C28 C29 C30 C31 171.2(6) . . . . ? C29 C30 C31 O6 -151.3(8) . . . . ? C32 C30 C31 O6 23.2(12) . . . . ? C29 C30 C31 O5 16.4(10) . . . . ? C32 C30 C31 O5 -169.1(7) . . . . ? C29 C30 C32 C34 1.6(8) . . . . ? C31 C30 C32 C34 -173.0(6) . . . . ? C29 C30 C32 C33 -175.5(5) . . . . ? C31 C30 C32 C33 10.0(9) . . . . ? C34 C32 C33 O7 -105.0(7) . . . . ? C30 C32 C33 O7 72.0(8) . . . . ? C34 C32 C33 O8 71.4(6) . . . . ? C30 C32 C33 O8 -111.6(6) . . . . ? C28 C27 C34 C32 -3.9(8) . . . . ? C24 C27 C34 C32 173.1(4) . . . . ? C30 C32 C34 C27 2.1(7) . . . . ? C33 C32 C34 C27 179.4(5) . . . . ? N2 C1 N1 C2 1.9(9) . . . . ? N2 C1 N1 Zn1 169.4(5) . . . . ? C3 C2 N1 C1 -1.3(9) . . . . ? C3 C2 N1 Zn1 -171.2(5) . . . . ? O3 Zn1 N1 C1 115.5(7) 3_556 . . . ? O8 Zn1 N1 C1 -128.1(7) 3_656 . . . ? O2 Zn1 N1 C1 -11.6(7) . . . . ? O3 Zn1 N1 C2 -78.3(5) 3_556 . . . ? O8 Zn1 N1 C2 38.1(5) 3_656 . . . ? O2 Zn1 N1 C2 154.6(5) . . . . ? N1 C1 N2 C3 -1.8(9) . . . . ? N1 C1 N2 C4 179.7(7) . . . . ? C2 C3 N2 C1 0.8(9) . . . . ? C2 C3 N2 C4 179.4(8) . . . . ? C5 C4 N2 C1 -70.4(10) . . . . ? C5 C4 N2 C3 111.3(9) . . . . ? N4 C8 N3 C10 1.3(8) . . . . ? N4 C8 N3 C7 -175.1(6) . . . . ? C9 C10 N3 C8 -2.1(8) . . . . ? C9 C10 N3 C7 174.4(7) . . . . ? C6 C7 N3 C8 -114.7(8) . . . . ? C6 C7 N3 C10 69.6(10) . . . . ? N3 C8 N4 C9 0.0(7) . . . . ? N3 C8 N4 Zn2 174.3(4) . . . 2_556 ? C10 C9 N4 C8 -1.3(8) . . . . ? C10 C9 N4 Zn2 -175.8(5) . . . 2_556 ? N6 C11 N5 C12 0.7(8) . . . . ? N6 C11 N5 Zn2 177.1(4) . . . . ? C13 C12 N5 C11 -0.5(9) . . . . ? C13 C12 N5 Zn2 -176.4(5) . . . . ? O5 Zn2 N5 C11 122.2(5) 2_656 . . . ? N4 Zn2 N5 C11 -91.4(6) 2_546 . . . ? O1 Zn2 N5 C11 23.3(5) . . . . ? O5 Zn2 N5 C12 -62.4(7) 2_656 . . . ? N4 Zn2 N5 C12 84.0(6) 2_546 . . . ? O1 Zn2 N5 C12 -161.3(6) . . . . ? N5 C11 N6 C13 -0.7(8) . . . . ? N5 C11 N6 C14 -178.6(7) . . . . ? C12 C13 N6 C11 0.4(9) . . . . ? C12 C13 N6 C14 178.2(7) . . . . ? C15 C14 N6 C11 82.5(9) . . . . ? C15 C14 N6 C13 -94.9(9) . . . . ? O2 C16 O1 Zn2 -164.2(4) . . . . ? C17 C16 O1 Zn2 10.9(7) . . . . ? O5 Zn2 O1 C16 72.1(5) 2_656 . . . ? N4 Zn2 O1 C16 -49.2(5) 2_546 . . . ? N5 Zn2 O1 C16 -162.4(5) . . . . ? O1 C16 O2 Zn1 4.3(6) . . . . ? C17 C16 O2 Zn1 -170.9(3) . . . . ? O3 Zn1 O2 C16 -82.5(4) 3_556 . . . ? O8 Zn1 O2 C16 168.4(3) 3_656 . . . ? N1 Zn1 O2 C16 49.4(4) . . . . ? O4 C23 O3 Zn1 -0.7(9) . . . 3_556 ? C22 C23 O3 Zn1 -171.5(4) . . . 3_556 ? O6 C31 O5 Zn2 -7.7(12) . . . 2_646 ? C30 C31 O5 Zn2 -175.5(5) . . . 2_646 ? O7 C33 O8 Zn1 -6.2(8) . . . 3_656 ? C32 C33 O8 Zn1 177.6(3) . . . 3_656 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.080 _refine_diff_density_min -1.083 _refine_diff_density_rms 0.112 #================END