# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2 _audit_update_record ; 2012-05-14 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common '[Co(bpy2py)OTf)OTf*0.75CH3CN' _chemical_melting_point ? _chemical_formula_moiety 'C29 H21 Co F6 N5 O6 S2' _chemical_formula_sum 'C30.50 H23.25 Co F6 N5.75 O6 S2' _chemical_formula_weight 803.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.8107(3) _cell_length_b 12.2952(3) _cell_length_c 13.4212(4) _cell_angle_alpha 93.2350(10) _cell_angle_beta 91.8140(10) _cell_angle_gamma 91.3500(10) _cell_volume 1615.01(8) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9935 _cell_measurement_theta_min 2.5340 _cell_measurement_theta_max 25.3391 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.652 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 815 _exptl_absorpt_coefficient_mu 0.750 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8008 _exptl_absorpt_correction_T_max 0.9023 _exptl_absorpt_process_details SADABS _exptl_special_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'microfocus sealed tube' _diffrn_radiation_monochromator 'QUAZAR multilayer mirrors' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_reflns_number 16243 _diffrn_reflns_av_R_equivalents 0.0230 _diffrn_reflns_av_sigmaI/netI 0.0271 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 25.36 _reflns_number_total 5814 _reflns_number_gt 5030 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v. 2009.1' _computing_cell_refinement 'Bruker APEX2 v. 2009.1' _computing_data_reduction 'Bruker APEX2 v. 2009.1' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics DIAMOND _computing_publication_material CIFTAB _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^)+(0.0438P)^2^+2.2413P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5814 _refine_ls_number_parameters 471 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0445 _refine_ls_R_factor_gt 0.0361 _refine_ls_wR_factor_ref 0.0990 _refine_ls_wR_factor_gt 0.0925 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.01394(3) 0.70473(3) 0.24254(2) 0.01536(10) Uani 1 1 d . . . S1 S -0.25287(6) 0.75521(5) 0.37338(5) 0.01862(15) Uani 1 1 d . . . S2 S 0.54448(7) 0.26979(7) 0.22415(6) 0.03271(19) Uani 1 1 d . . . F1 F -0.48344(17) 0.81126(14) 0.28955(14) 0.0376(4) Uani 1 1 d . . . F2 F -0.32545(17) 0.93731(13) 0.29735(12) 0.0300(4) Uani 1 1 d . . . F3 F -0.43111(17) 0.89851(14) 0.42955(13) 0.0339(4) Uani 1 1 d . . . F4 F 0.29066(19) 0.25606(18) 0.27915(15) 0.0476(5) Uani 1 1 d . . . F5 F 0.3588(3) 0.11227(19) 0.20047(19) 0.0698(7) Uani 1 1 d . . . F6 F 0.4247(2) 0.1487(2) 0.35283(17) 0.0659(7) Uani 1 1 d . . . O1 O -0.19985(18) 0.72662(15) 0.27470(13) 0.0214(4) Uani 1 1 d . . . O2 O -0.15536(18) 0.81367(15) 0.44033(14) 0.0237(4) Uani 1 1 d . . . O3 O -0.32973(19) 0.66859(15) 0.41436(14) 0.0260(4) Uani 1 1 d . . . O4 O 0.4948(2) 0.3076(2) 0.13121(16) 0.0451(6) Uani 1 1 d . . . O5 O 0.5657(2) 0.3535(2) 0.30347(17) 0.0429(6) Uani 1 1 d . . . O6 O 0.6500(3) 0.1916(2) 0.2187(2) 0.0576(7) Uani 1 1 d . . . N1 N 0.1906(2) 0.63150(16) 0.18952(15) 0.0163(4) Uani 1 1 d . . . N1S N 0.2647(5) 0.8901(4) 0.0614(3) 0.0574(11) Uani 0.75 1 d P . . N2 N -0.0306(2) 0.67137(17) 0.08882(15) 0.0199(5) Uani 1 1 d . . . N3 N 0.1476(2) 0.77255(17) 0.35277(15) 0.0164(4) Uani 1 1 d . . . N4 N 0.0064(2) 0.87987(18) 0.22457(16) 0.0208(5) Uani 1 1 d . . . N5 N 0.0073(2) 0.56046(17) 0.32065(15) 0.0160(4) Uani 1 1 d . . . C1 C 0.2909(2) 0.5996(2) 0.25137(18) 0.0172(5) Uani 1 1 d . . . C1S C 0.3806(5) 0.8900(4) 0.0603(4) 0.0472(12) Uani 0.75 1 d P . . C2 C 0.4163(3) 0.5717(2) 0.2145(2) 0.0224(6) Uani 1 1 d . . . H2 H 0.4868 0.5478 0.2575 0.027 Uiso 1 1 calc R . . C2S C 0.5280(6) 0.8863(5) 0.0649(4) 0.0605(14) Uani 0.75 1 d P . . H2SA H 0.5619 0.8770 -0.0029 0.091 Uiso 0.75 1 calc PR . . H2SB H 0.5563 0.8250 0.1036 0.091 Uiso 0.75 1 calc PR . . H2SC H 0.5657 0.9545 0.0971 0.091 Uiso 0.75 1 calc PR . . C3 C 0.4369(3) 0.5792(2) 0.1132(2) 0.0266(6) Uani 1 1 d . . . H3 H 0.5241 0.5650 0.0873 0.032 Uiso 1 1 calc R . . C4 C 0.3314(3) 0.6074(2) 0.0499(2) 0.0253(6) Uani 1 1 d . . . H4 H 0.3438 0.6105 -0.0198 0.030 Uiso 1 1 calc R . . C5 C 0.2066(3) 0.6310(2) 0.09110(19) 0.0197(5) Uani 1 1 d . . . C6 C 0.0786(3) 0.6503(2) 0.03265(19) 0.0201(5) Uani 1 1 d . . . C7 C 0.0676(3) 0.6401(2) -0.0708(2) 0.0266(6) Uani 1 1 d . . . H7 H 0.1459 0.6278 -0.1092 0.032 Uiso 1 1 calc R . . C8 C -0.0599(3) 0.6481(2) -0.1169(2) 0.0296(7) Uani 1 1 d . . . H8 H -0.0696 0.6415 -0.1876 0.035 Uiso 1 1 calc R . . C9 C -0.1728(3) 0.6658(2) -0.0596(2) 0.0270(6) Uani 1 1 d . . . H9 H -0.2613 0.6692 -0.0899 0.032 Uiso 1 1 calc R . . C10 C -0.1534(3) 0.6785(2) 0.0430(2) 0.0229(6) Uani 1 1 d . . . H10 H -0.2301 0.6928 0.0827 0.027 Uiso 1 1 calc R . . C11 C 0.2325(2) 0.7115(2) 0.40518(18) 0.0165(5) Uani 1 1 d . . . C12 C 0.2998(3) 0.7548(2) 0.49162(19) 0.0206(5) Uani 1 1 d . . . H12 H 0.3605 0.7117 0.5282 0.025 Uiso 1 1 calc R . . C13 C 0.2769(3) 0.8620(2) 0.5238(2) 0.0241(6) Uani 1 1 d . . . H13 H 0.3172 0.8914 0.5850 0.029 Uiso 1 1 calc R . . C14 C 0.1952(3) 0.9258(2) 0.4661(2) 0.0231(6) Uani 1 1 d . . . H14 H 0.1818 1.0001 0.4856 0.028 Uiso 1 1 calc R . . C15 C 0.1334(2) 0.8790(2) 0.37948(19) 0.0184(5) Uani 1 1 d . . . C16 C 0.0529(3) 0.9393(2) 0.30662(19) 0.0196(5) Uani 1 1 d . . . C17 C 0.0298(3) 1.0506(2) 0.3195(2) 0.0262(6) Uani 1 1 d . . . H17 H 0.0637 1.0912 0.3777 0.031 Uiso 1 1 calc R . . C18 C -0.0433(3) 1.1007(2) 0.2461(2) 0.0313(7) Uani 1 1 d . . . H18 H -0.0626 1.1760 0.2544 0.038 Uiso 1 1 calc R . . C19 C -0.0879(3) 1.0409(2) 0.1610(2) 0.0313(7) Uani 1 1 d . . . H19 H -0.1365 1.0743 0.1090 0.038 Uiso 1 1 calc R . . C20 C -0.0602(3) 0.9314(2) 0.1532(2) 0.0266(6) Uani 1 1 d . . . H20 H -0.0899 0.8903 0.0941 0.032 Uiso 1 1 calc R . . C21 C 0.1210(2) 0.5242(2) 0.36615(17) 0.0150(5) Uani 1 1 d . . . C22 C 0.1197(3) 0.4257(2) 0.41193(18) 0.0172(5) Uani 1 1 d . . . H22 H 0.1996 0.4023 0.4454 0.021 Uiso 1 1 calc R . . C23 C 0.0013(3) 0.3618(2) 0.40870(18) 0.0199(5) Uani 1 1 d . . . H23 H -0.0009 0.2944 0.4400 0.024 Uiso 1 1 calc R . . C24 C -0.1140(3) 0.3975(2) 0.35917(19) 0.0201(5) Uani 1 1 d . . . H24 H -0.1957 0.3541 0.3540 0.024 Uiso 1 1 calc R . . C25 C -0.1072(3) 0.4970(2) 0.31778(18) 0.0173(5) Uani 1 1 d . . . H25 H -0.1869 0.5225 0.2856 0.021 Uiso 1 1 calc R . . C26 C 0.2541(2) 0.5944(2) 0.36231(18) 0.0166(5) Uani 1 1 d . . . C27 C 0.3699(2) 0.5426(2) 0.42111(19) 0.0198(5) Uani 1 1 d . . . H27A H 0.3882 0.4706 0.3901 0.030 Uiso 1 1 calc R . . H27B H 0.3431 0.5350 0.4901 0.030 Uiso 1 1 calc R . . H27C H 0.4523 0.5891 0.4207 0.030 Uiso 1 1 calc R . . C28 C -0.3804(3) 0.8561(2) 0.3458(2) 0.0247(6) Uani 1 1 d . . . C29 C 0.3978(3) 0.1921(3) 0.2666(2) 0.0394(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.01738(18) 0.01424(19) 0.01435(17) 0.00056(13) -0.00167(13) 0.00149(13) S1 0.0161(3) 0.0174(3) 0.0224(3) 0.0014(2) -0.0005(2) 0.0010(2) S2 0.0252(4) 0.0438(5) 0.0302(4) 0.0080(3) 0.0011(3) 0.0098(3) F1 0.0259(9) 0.0289(10) 0.0563(11) -0.0017(8) -0.0173(8) 0.0028(7) F2 0.0332(9) 0.0198(8) 0.0376(9) 0.0062(7) 0.0008(7) 0.0045(7) F3 0.0288(9) 0.0288(9) 0.0446(10) -0.0031(8) 0.0119(8) 0.0053(7) F4 0.0302(10) 0.0679(14) 0.0458(11) 0.0083(10) 0.0042(8) 0.0078(9) F5 0.0795(17) 0.0525(14) 0.0752(17) -0.0123(12) 0.0070(13) -0.0170(12) F6 0.0573(14) 0.0849(18) 0.0600(14) 0.0452(13) -0.0017(11) 0.0021(12) O1 0.0215(9) 0.0194(10) 0.0235(9) 0.0011(7) -0.0003(7) 0.0036(7) O2 0.0212(9) 0.0237(10) 0.0257(10) -0.0015(8) -0.0024(8) 0.0000(8) O3 0.0226(10) 0.0239(10) 0.0321(11) 0.0067(8) 0.0020(8) -0.0008(8) O4 0.0362(13) 0.0693(17) 0.0319(12) 0.0175(11) 0.0052(10) 0.0051(12) O5 0.0339(12) 0.0487(15) 0.0459(14) 0.0043(11) -0.0075(10) 0.0048(10) O6 0.0424(14) 0.0684(19) 0.0641(17) 0.0072(14) 0.0101(13) 0.0274(13) N1 0.0197(11) 0.0119(10) 0.0173(10) 0.0001(8) 0.0009(8) -0.0009(8) N1S 0.061(3) 0.046(3) 0.065(3) 0.009(2) 0.003(2) -0.001(2) N2 0.0246(11) 0.0175(11) 0.0175(11) 0.0013(9) -0.0017(9) 0.0025(9) N3 0.0158(10) 0.0152(11) 0.0183(10) 0.0001(8) 0.0022(8) -0.0014(8) N4 0.0229(11) 0.0177(12) 0.0219(11) 0.0034(9) 0.0002(9) 0.0004(9) N5 0.0183(10) 0.0151(11) 0.0143(10) -0.0017(8) -0.0004(8) 0.0010(8) C1 0.0188(12) 0.0143(13) 0.0182(12) -0.0005(10) 0.0009(10) -0.0014(10) C1S 0.048(3) 0.047(3) 0.044(3) -0.009(2) -0.004(2) -0.003(2) C2 0.0187(13) 0.0218(14) 0.0269(14) 0.0018(11) 0.0008(11) 0.0016(11) C2S 0.060(3) 0.077(4) 0.046(3) 0.010(3) 0.003(3) 0.005(3) C3 0.0232(14) 0.0264(15) 0.0305(15) -0.0006(12) 0.0088(11) 0.0033(11) C4 0.0305(15) 0.0252(15) 0.0205(13) 0.0011(11) 0.0077(11) 0.0009(12) C5 0.0252(14) 0.0158(13) 0.0182(13) 0.0010(10) 0.0038(10) 0.0000(10) C6 0.0267(14) 0.0140(13) 0.0196(13) 0.0011(10) 0.0008(11) 0.0005(10) C7 0.0350(16) 0.0269(16) 0.0179(13) 0.0006(11) 0.0014(11) 0.0029(12) C8 0.0413(17) 0.0279(16) 0.0191(14) 0.0008(11) -0.0048(12) 0.0019(13) C9 0.0313(15) 0.0260(15) 0.0233(14) 0.0025(11) -0.0089(12) 0.0020(12) C10 0.0256(14) 0.0209(14) 0.0219(13) 0.0009(11) -0.0025(11) 0.0014(11) C11 0.0147(12) 0.0170(13) 0.0179(12) 0.0011(10) 0.0020(9) -0.0021(10) C12 0.0180(13) 0.0227(14) 0.0209(13) 0.0022(11) -0.0009(10) -0.0024(10) C13 0.0247(14) 0.0244(15) 0.0222(13) -0.0028(11) -0.0014(11) -0.0043(11) C14 0.0253(14) 0.0171(14) 0.0263(14) -0.0033(11) 0.0013(11) -0.0020(11) C15 0.0153(12) 0.0153(13) 0.0245(13) 0.0002(10) 0.0031(10) -0.0012(10) C16 0.0190(13) 0.0164(13) 0.0235(13) 0.0025(10) 0.0031(10) -0.0012(10) C17 0.0279(15) 0.0187(14) 0.0316(15) -0.0009(11) 0.0002(12) 0.0014(11) C18 0.0358(16) 0.0168(15) 0.0418(17) 0.0041(12) -0.0001(13) 0.0038(12) C19 0.0384(17) 0.0222(15) 0.0342(16) 0.0107(12) -0.0034(13) 0.0054(13) C20 0.0307(15) 0.0221(15) 0.0270(14) 0.0036(11) -0.0032(12) 0.0011(12) C21 0.0163(12) 0.0160(13) 0.0121(11) -0.0026(9) -0.0001(9) 0.0011(10) C22 0.0190(12) 0.0176(13) 0.0147(12) -0.0009(10) -0.0002(9) 0.0025(10) C23 0.0272(14) 0.0154(13) 0.0174(12) 0.0016(10) 0.0020(10) 0.0002(11) C24 0.0205(13) 0.0181(14) 0.0212(13) -0.0022(10) 0.0016(10) -0.0021(10) C25 0.0184(12) 0.0162(13) 0.0168(12) -0.0029(10) 0.0003(10) 0.0012(10) C26 0.0161(12) 0.0163(13) 0.0172(12) 0.0003(10) -0.0004(10) 0.0007(10) C27 0.0147(12) 0.0217(14) 0.0230(13) 0.0023(11) -0.0027(10) 0.0020(10) C28 0.0207(13) 0.0192(14) 0.0338(15) -0.0004(12) -0.0004(11) 0.0009(11) C29 0.0403(18) 0.045(2) 0.0333(17) 0.0067(15) -0.0014(14) 0.0077(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N3 2.071(2) . ? Co1 N1 2.098(2) . ? Co1 N2 2.111(2) . ? Co1 N5 2.112(2) . ? Co1 O1 2.1746(18) . ? Co1 N4 2.183(2) . ? S1 O3 1.435(2) . ? S1 O2 1.4421(19) . ? S1 O1 1.4655(19) . ? S1 C28 1.827(3) . ? S2 O6 1.430(2) . ? S2 O4 1.431(2) . ? S2 O5 1.445(3) . ? S2 C29 1.832(4) . ? F1 C28 1.332(3) . ? F2 C28 1.334(3) . ? F3 C28 1.328(3) . ? F4 C29 1.337(4) . ? F5 C29 1.327(4) . ? F6 C29 1.323(4) . ? N1 C5 1.335(3) . ? N1 C1 1.347(3) . ? N1S C1S 1.138(6) . ? N2 C10 1.341(3) . ? N2 C6 1.351(3) . ? N3 C11 1.344(3) . ? N3 C15 1.349(3) . ? N4 C20 1.339(3) . ? N4 C16 1.348(3) . ? N5 C25 1.350(3) . ? N5 C21 1.352(3) . ? C1 C2 1.384(4) . ? C1 C26 1.548(3) . ? C1S C2S 1.448(7) . ? C2 C3 1.388(4) . ? C2 H2 0.9500 . ? C2S H2SA 0.9800 . ? C2S H2SB 0.9800 . ? C2S H2SC 0.9800 . ? C3 C4 1.381(4) . ? C3 H3 0.9500 . ? C4 C5 1.389(4) . ? C4 H4 0.9500 . ? C5 C6 1.491(4) . ? C6 C7 1.387(4) . ? C7 C8 1.386(4) . ? C7 H7 0.9500 . ? C8 C9 1.383(4) . ? C8 H8 0.9500 . ? C9 C10 1.384(4) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.389(3) . ? C11 C26 1.542(3) . ? C12 C13 1.389(4) . ? C12 H12 0.9500 . ? C13 C14 1.383(4) . ? C13 H13 0.9500 . ? C14 C15 1.384(4) . ? C14 H14 0.9500 . ? C15 C16 1.480(4) . ? C16 C17 1.393(4) . ? C17 C18 1.381(4) . ? C17 H17 0.9500 . ? C18 C19 1.377(4) . ? C18 H18 0.9500 . ? C19 C20 1.380(4) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C22 1.388(4) . ? C21 C26 1.552(3) . ? C22 C23 1.385(4) . ? C22 H22 0.9500 . ? C23 C24 1.386(4) . ? C23 H23 0.9500 . ? C24 C25 1.374(4) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C27 1.534(3) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? 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 N3 Co1 N1 83.13(8) . . ? N3 Co1 N2 148.04(9) . . ? N1 Co1 N2 76.03(8) . . ? N3 Co1 N5 88.68(8) . . ? N1 Co1 N5 80.49(8) . . ? N2 Co1 N5 111.00(8) . . ? N3 Co1 O1 113.79(7) . . ? N1 Co1 O1 159.71(7) . . ? N2 Co1 O1 92.39(8) . . ? N5 Co1 O1 88.47(7) . . ? N3 Co1 N4 75.63(8) . . ? N1 Co1 N4 114.49(8) . . ? N2 Co1 N4 91.19(8) . . ? N5 Co1 N4 156.19(8) . . ? O1 Co1 N4 81.85(8) . . ? O3 S1 O2 116.37(11) . . ? O3 S1 O1 113.80(11) . . ? O2 S1 O1 113.69(11) . . ? O3 S1 C28 104.09(12) . . ? O2 S1 C28 104.20(12) . . ? O1 S1 C28 102.57(12) . . ? O6 S2 O4 116.37(16) . . ? O6 S2 O5 114.12(15) . . ? O4 S2 O5 114.94(15) . . ? O6 S2 C29 103.63(17) . . ? O4 S2 C29 102.78(14) . . ? O5 S2 C29 102.37(15) . . ? S1 O1 Co1 125.36(10) . . ? C5 N1 C1 121.1(2) . . ? C5 N1 Co1 116.06(17) . . ? C1 N1 Co1 122.26(16) . . ? C10 N2 C6 118.8(2) . . ? C10 N2 Co1 125.81(18) . . ? C6 N2 Co1 115.16(17) . . ? C11 N3 C15 120.4(2) . . ? C11 N3 Co1 122.01(16) . . ? C15 N3 Co1 116.96(16) . . ? C20 N4 C16 118.0(2) . . ? C20 N4 Co1 127.86(18) . . ? C16 N4 Co1 112.71(16) . . ? C25 N5 C21 118.5(2) . . ? C25 N5 Co1 120.51(16) . . ? C21 N5 Co1 120.67(16) . . ? N1 C1 C2 120.3(2) . . ? N1 C1 C26 115.7(2) . . ? C2 C1 C26 124.0(2) . . ? N1S C1S C2S 176.2(6) . . ? C1 C2 C3 118.6(2) . . ? C1 C2 H2 120.7 . . ? C3 C2 H2 120.7 . . ? C1S C2S H2SA 109.5 . . ? C1S C2S H2SB 109.5 . . ? H2SA C2S H2SB 109.5 . . ? C1S C2S H2SC 109.5 . . ? H2SA C2S H2SC 109.5 . . ? H2SB C2S H2SC 109.5 . . ? C4 C3 C2 120.4(3) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C3 C4 C5 118.1(2) . . ? C3 C4 H4 121.0 . . ? C5 C4 H4 121.0 . . ? N1 C5 C4 121.1(2) . . ? N1 C5 C6 113.9(2) . . ? C4 C5 C6 124.9(2) . . ? N2 C6 C7 121.7(2) . . ? N2 C6 C5 114.5(2) . . ? C7 C6 C5 123.7(2) . . ? C8 C7 C6 118.8(3) . . ? C8 C7 H7 120.6 . . ? C6 C7 H7 120.6 . . ? C9 C8 C7 119.8(3) . . ? C9 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? C8 C9 C10 118.2(3) . . ? C8 C9 H9 120.9 . . ? C10 C9 H9 120.9 . . ? N2 C10 C9 122.7(3) . . ? N2 C10 H10 118.6 . . ? C9 C10 H10 118.6 . . ? N3 C11 C12 120.6(2) . . ? N3 C11 C26 116.6(2) . . ? C12 C11 C26 122.8(2) . . ? C13 C12 C11 119.0(2) . . ? C13 C12 H12 120.5 . . ? C11 C12 H12 120.5 . . ? C14 C13 C12 119.7(2) . . ? C14 C13 H13 120.1 . . ? C12 C13 H13 120.1 . . ? C13 C14 C15 118.6(2) . . ? C13 C14 H14 120.7 . . ? C15 C14 H14 120.7 . . ? N3 C15 C14 121.3(2) . . ? N3 C15 C16 114.2(2) . . ? C14 C15 C16 124.4(2) . . ? N4 C16 C17 121.8(2) . . ? N4 C16 C15 115.3(2) . . ? C17 C16 C15 122.9(2) . . ? C18 C17 C16 118.8(3) . . ? C18 C17 H17 120.6 . . ? C16 C17 H17 120.6 . . ? C19 C18 C17 119.6(3) . . ? C19 C18 H18 120.2 . . ? C17 C18 H18 120.2 . . ? C18 C19 C20 118.2(3) . . ? C18 C19 H19 120.9 . . ? C20 C19 H19 120.9 . . ? N4 C20 C19 123.4(3) . . ? N4 C20 H20 118.3 . . ? C19 C20 H20 118.3 . . ? N5 C21 C22 121.0(2) . . ? N5 C21 C26 117.7(2) . . ? C22 C21 C26 121.2(2) . . ? C23 C22 C21 119.7(2) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C22 C23 C24 119.1(2) . . ? C22 C23 H23 120.4 . . ? C24 C23 H23 120.4 . . ? C25 C24 C23 118.3(2) . . ? C25 C24 H24 120.9 . . ? C23 C24 H24 120.9 . . ? N5 C25 C24 123.2(2) . . ? N5 C25 H25 118.4 . . ? C24 C25 H25 118.4 . . ? C27 C26 C11 109.9(2) . . ? C27 C26 C1 110.0(2) . . ? C11 C26 C1 108.3(2) . . ? C27 C26 C21 110.1(2) . . ? C11 C26 C21 110.8(2) . . ? C1 C26 C21 107.68(19) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? F3 C28 F1 108.0(2) . . ? F3 C28 F2 108.0(2) . . ? F1 C28 F2 108.4(2) . . ? F3 C28 S1 110.57(19) . . ? F1 C28 S1 111.03(18) . . ? F2 C28 S1 110.78(18) . . ? F6 C29 F5 108.1(3) . . ? F6 C29 F4 107.4(3) . . ? F5 C29 F4 106.9(3) . . ? F6 C29 S2 111.9(2) . . ? F5 C29 S2 111.5(2) . . ? F4 C29 S2 110.8(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 O3 S1 O1 Co1 -110.62(13) . . . . ? O2 S1 O1 Co1 25.75(17) . . . . ? C28 S1 O1 Co1 137.61(13) . . . . ? N3 Co1 O1 S1 -17.85(16) . . . . ? N1 Co1 O1 S1 126.7(2) . . . . ? N2 Co1 O1 S1 -179.01(13) . . . . ? N5 Co1 O1 S1 70.03(13) . . . . ? N4 Co1 O1 S1 -88.15(14) . . . . ? N3 Co1 N1 C5 -136.59(18) . . . . ? N2 Co1 N1 C5 19.00(17) . . . . ? N5 Co1 N1 C5 133.60(18) . . . . ? O1 Co1 N1 C5 75.7(3) . . . . ? N4 Co1 N1 C5 -65.84(19) . . . . ? N3 Co1 N1 C1 34.99(19) . . . . ? N2 Co1 N1 C1 -169.4(2) . . . . ? N5 Co1 N1 C1 -54.82(19) . . . . ? O1 Co1 N1 C1 -112.7(2) . . . . ? N4 Co1 N1 C1 105.74(19) . . . . ? N3 Co1 N2 C10 -139.9(2) . . . . ? N1 Co1 N2 C10 169.3(2) . . . . ? N5 Co1 N2 C10 95.5(2) . . . . ? O1 Co1 N2 C10 6.2(2) . . . . ? N4 Co1 N2 C10 -75.7(2) . . . . ? N3 Co1 N2 C6 34.2(3) . . . . ? N1 Co1 N2 C6 -16.61(17) . . . . ? N5 Co1 N2 C6 -90.47(19) . . . . ? O1 Co1 N2 C6 -179.75(18) . . . . ? N4 Co1 N2 C6 98.36(18) . . . . ? N1 Co1 N3 C11 -51.55(19) . . . . ? N2 Co1 N3 C11 -100.8(2) . . . . ? N5 Co1 N3 C11 29.02(19) . . . . ? O1 Co1 N3 C11 116.77(19) . . . . ? N4 Co1 N3 C11 -169.1(2) . . . . ? N1 Co1 N3 C15 137.20(19) . . . . ? N2 Co1 N3 C15 87.9(2) . . . . ? N5 Co1 N3 C15 -142.23(18) . . . . ? O1 Co1 N3 C15 -54.48(19) . . . . ? N4 Co1 N3 C15 19.69(17) . . . . ? N3 Co1 N4 C20 174.8(2) . . . . ? N1 Co1 N4 C20 99.5(2) . . . . ? N2 Co1 N4 C20 24.3(2) . . . . ? N5 Co1 N4 C20 -134.9(2) . . . . ? O1 Co1 N4 C20 -68.0(2) . . . . ? N3 Co1 N4 C16 -19.08(17) . . . . ? N1 Co1 N4 C16 -94.45(18) . . . . ? N2 Co1 N4 C16 -169.62(18) . . . . ? N5 Co1 N4 C16 31.2(3) . . . . ? O1 Co1 N4 C16 98.13(18) . . . . ? N3 Co1 N5 C25 148.10(19) . . . . ? N1 Co1 N5 C25 -128.65(19) . . . . ? N2 Co1 N5 C25 -57.7(2) . . . . ? O1 Co1 N5 C25 34.26(18) . . . . ? N4 Co1 N5 C25 99.9(2) . . . . ? N3 Co1 N5 C21 -38.50(18) . . . . ? N1 Co1 N5 C21 44.76(18) . . . . ? N2 Co1 N5 C21 115.69(18) . . . . ? O1 Co1 N5 C21 -152.34(18) . . . . ? N4 Co1 N5 C21 -86.6(3) . . . . ? C5 N1 C1 C2 3.9(4) . . . . ? Co1 N1 C1 C2 -167.28(19) . . . . ? C5 N1 C1 C26 -174.7(2) . . . . ? Co1 N1 C1 C26 14.1(3) . . . . ? N1 C1 C2 C3 1.2(4) . . . . ? C26 C1 C2 C3 179.7(2) . . . . ? C1 C2 C3 C4 -4.1(4) . . . . ? C2 C3 C4 C5 2.0(4) . . . . ? C1 N1 C5 C4 -6.1(4) . . . . ? Co1 N1 C5 C4 165.6(2) . . . . ? C1 N1 C5 C6 170.1(2) . . . . ? Co1 N1 C5 C6 -18.2(3) . . . . ? C3 C4 C5 N1 3.1(4) . . . . ? C3 C4 C5 C6 -172.7(3) . . . . ? C10 N2 C6 C7 2.5(4) . . . . ? Co1 N2 C6 C7 -172.0(2) . . . . ? C10 N2 C6 C5 -173.1(2) . . . . ? Co1 N2 C6 C5 12.4(3) . . . . ? N1 C5 C6 N2 3.6(3) . . . . ? C4 C5 C6 N2 179.7(2) . . . . ? N1 C5 C6 C7 -171.8(2) . . . . ? C4 C5 C6 C7 4.2(4) . . . . ? N2 C6 C7 C8 -2.2(4) . . . . ? C5 C6 C7 C8 172.9(3) . . . . ? C6 C7 C8 C9 -0.1(4) . . . . ? C7 C8 C9 C10 2.0(4) . . . . ? C6 N2 C10 C9 -0.4(4) . . . . ? Co1 N2 C10 C9 173.4(2) . . . . ? C8 C9 C10 N2 -1.8(4) . . . . ? C15 N3 C11 C12 4.5(4) . . . . ? Co1 N3 C11 C12 -166.45(18) . . . . ? C15 N3 C11 C26 -173.4(2) . . . . ? Co1 N3 C11 C26 15.6(3) . . . . ? N3 C11 C12 C13 0.7(4) . . . . ? C26 C11 C12 C13 178.4(2) . . . . ? C11 C12 C13 C14 -4.2(4) . . . . ? C12 C13 C14 C15 2.8(4) . . . . ? C11 N3 C15 C14 -6.1(4) . . . . ? Co1 N3 C15 C14 165.3(2) . . . . ? C11 N3 C15 C16 171.3(2) . . . . ? Co1 N3 C15 C16 -17.3(3) . . . . ? C13 C14 C15 N3 2.4(4) . . . . ? C13 C14 C15 C16 -174.7(2) . . . . ? C20 N4 C16 C17 1.9(4) . . . . ? Co1 N4 C16 C17 -165.7(2) . . . . ? C20 N4 C16 C15 -176.2(2) . . . . ? Co1 N4 C16 C15 16.3(3) . . . . ? N3 C15 C16 N4 -0.3(3) . . . . ? C14 C15 C16 N4 177.0(2) . . . . ? N3 C15 C16 C17 -178.3(2) . . . . ? C14 C15 C16 C17 -1.0(4) . . . . ? N4 C16 C17 C18 0.3(4) . . . . ? C15 C16 C17 C18 178.2(3) . . . . ? C16 C17 C18 C19 -2.0(4) . . . . ? C17 C18 C19 C20 1.4(5) . . . . ? C16 N4 C20 C19 -2.5(4) . . . . ? Co1 N4 C20 C19 163.0(2) . . . . ? C18 C19 C20 N4 0.8(5) . . . . ? C25 N5 C21 C22 -2.1(3) . . . . ? Co1 N5 C21 C22 -175.66(17) . . . . ? C25 N5 C21 C26 175.9(2) . . . . ? Co1 N5 C21 C26 2.3(3) . . . . ? N5 C21 C22 C23 1.9(4) . . . . ? C26 C21 C22 C23 -176.0(2) . . . . ? C21 C22 C23 C24 0.2(4) . . . . ? C22 C23 C24 C25 -2.0(4) . . . . ? C21 N5 C25 C24 0.2(4) . . . . ? Co1 N5 C25 C24 173.78(19) . . . . ? C23 C24 C25 N5 1.9(4) . . . . ? N3 C11 C26 C27 171.0(2) . . . . ? C12 C11 C26 C27 -6.9(3) . . . . ? N3 C11 C26 C1 50.7(3) . . . . ? C12 C11 C26 C1 -127.1(2) . . . . ? N3 C11 C26 C21 -67.2(3) . . . . ? C12 C11 C26 C21 115.0(3) . . . . ? N1 C1 C26 C27 172.4(2) . . . . ? C2 C1 C26 C27 -6.2(3) . . . . ? N1 C1 C26 C11 -67.5(3) . . . . ? C2 C1 C26 C11 114.0(3) . . . . ? N1 C1 C26 C21 52.4(3) . . . . ? C2 C1 C26 C21 -126.2(3) . . . . ? N5 C21 C26 C27 177.8(2) . . . . ? C22 C21 C26 C27 -4.2(3) . . . . ? N5 C21 C26 C11 56.1(3) . . . . ? C22 C21 C26 C11 -125.9(2) . . . . ? N5 C21 C26 C1 -62.2(3) . . . . ? C22 C21 C26 C1 115.8(2) . . . . ? O3 S1 C28 F3 66.7(2) . . . . ? O2 S1 C28 F3 -55.7(2) . . . . ? O1 S1 C28 F3 -174.47(17) . . . . ? O3 S1 C28 F1 -53.2(2) . . . . ? O2 S1 C28 F1 -175.57(19) . . . . ? O1 S1 C28 F1 65.7(2) . . . . ? O3 S1 C28 F2 -173.63(18) . . . . ? O2 S1 C28 F2 64.0(2) . . . . ? O1 S1 C28 F2 -54.8(2) . . . . ? O6 S2 C29 F6 57.7(3) . . . . ? O4 S2 C29 F6 179.3(3) . . . . ? O5 S2 C29 F6 -61.2(3) . . . . ? O6 S2 C29 F5 -63.5(3) . . . . ? O4 S2 C29 F5 58.1(3) . . . . ? O5 S2 C29 F5 177.6(2) . . . . ? O6 S2 C29 F4 177.6(2) . . . . ? O4 S2 C29 F4 -60.8(2) . . . . ? O5 S2 C29 F4 58.7(2) . . . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.36 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.714 _refine_diff_density_min -0.419 _refine_diff_density_rms 0.071 _database_code_depnum_ccdc_archive 'CCDC 943488' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Ni(bpy2py)(CH3CN)]*1.5PF6*0.5BF4*Et2O' _chemical_melting_point ? _chemical_formula_moiety 'C27 H21 B0.50 Ni F11 P1.5' _chemical_formula_sum 'C33 H30.50 B0.50 F11 N7 Ni O0.50 P1.50' _chemical_formula_weight 852.71 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 '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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.605(3) _cell_length_b 26.456(6) _cell_length_c 12.584(3) _cell_angle_alpha 90.00 _cell_angle_beta 114.443(3) _cell_angle_gamma 90.00 _cell_volume 3517.3(14) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9783 _cell_measurement_theta_min 2.3518 _cell_measurement_theta_max 25.4128 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.610 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1734 _exptl_absorpt_coefficient_mu 0.717 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8467 _exptl_absorpt_correction_T_max 0.9253 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'microfocus sealed tube' _diffrn_radiation_monochromator 'QUAZAR multilayer mirrors' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_reflns_number 38001 _diffrn_reflns_av_R_equivalents 0.0220 _diffrn_reflns_av_sigmaI/netI 0.0152 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 25.41 _reflns_number_total 6459 _reflns_number_gt 5933 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v. 2009.1' _computing_cell_refinement 'Bruker APEX2 v. 2009.1' _computing_data_reduction 'Bruker APEX2 v. 2009.1' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics DIAMOND _computing_publication_material CIFTAB _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^)+(0.0736P)^2^+9.2270P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6459 _refine_ls_number_parameters 510 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0550 _refine_ls_R_factor_gt 0.0515 _refine_ls_wR_factor_ref 0.1423 _refine_ls_wR_factor_gt 0.1394 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.002 _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 Ni1 Ni 0.83918(3) 0.593649(14) 0.64657(3) 0.01676(13) Uani 1 1 d . . . P1 P 0.39997(9) 0.38808(4) 0.85197(8) 0.0287(2) Uani 1 1 d . . . P2 P 1.1209(7) 0.1791(2) 0.8524(5) 0.0190(7) Uani 0.50 1 d P A 1 F1 F 0.5417(2) 0.39286(9) 0.86313(19) 0.0406(5) Uani 1 1 d . . . F2 F 0.4485(2) 0.35476(9) 0.96693(19) 0.0396(5) Uani 1 1 d . . . F3 F 0.25746(19) 0.38421(8) 0.8383(2) 0.0369(5) Uani 1 1 d . . . F4 F 0.3529(2) 0.42164(8) 0.73628(17) 0.0347(5) Uani 1 1 d . . . F5 F 0.42052(19) 0.43816(8) 0.92776(17) 0.0327(5) Uani 1 1 d . . . F6 F 0.3813(2) 0.33845(8) 0.77493(19) 0.0399(5) Uani 1 1 d . . . F7 F 1.2243(2) 0.17726(9) 0.97496(18) 0.0377(5) Uani 1 1 d . . . F8 F 1.0155(4) 0.17627(15) 0.7186(3) 0.0330(9) Uani 0.50 1 d P A 1 F9 F 1.1607(2) 0.23051(7) 0.82093(19) 0.0326(5) Uani 1 1 d . . . F10 F 1.2212(6) 0.1501(3) 0.8140(6) 0.0383(13) Uani 0.50 1 d P A 1 F11 F 1.0207(4) 0.20510(18) 0.8899(4) 0.0342(7) Uani 0.50 1 d P A 1 F12 F 1.0710(4) 0.12426(14) 0.8757(3) 0.0258(8) Uani 0.50 1 d P A 1 F13 F 1.0160(4) 0.17704(18) 0.8482(4) 0.0342(7) Uani 0.50 1 d P A 2 F14 F 1.1625(6) 0.1448(3) 0.7840(6) 0.0383(13) Uani 0.50 1 d P A 2 O1S O 0.9725 0.4924 0.9742 0.119(2) Uiso 0.50 1 d P . 1 N1 N 0.8540(2) 0.63925(10) 0.7813(2) 0.0209(5) Uani 1 1 d . . . N1S N 0.7502(5) 0.2677(3) 0.8446(4) 0.099(2) Uani 1 1 d . . . N2 N 0.7319(2) 0.55373(10) 0.7240(2) 0.0228(6) Uani 1 1 d . . . N3 N 1.0248(2) 0.57991(10) 0.7404(2) 0.0188(5) Uani 1 1 d . . . N4 N 0.8648(2) 0.52661(10) 0.5718(2) 0.0182(5) Uani 1 1 d . . . N5 N 0.9093(2) 0.65101(10) 0.5794(2) 0.0185(5) Uani 1 1 d . . . N6 N 0.6586(2) 0.61240(10) 0.5241(2) 0.0215(6) Uani 1 1 d . . . C1 C 0.9463(3) 0.67325(12) 0.8269(3) 0.0227(6) Uani 1 1 d . . . C1S C 0.8133(5) 0.2789(3) 0.7983(4) 0.0720(18) Uani 1 1 d . . . C2 C 0.9485(3) 0.70557(13) 0.9148(3) 0.0279(7) Uani 1 1 d . . . H2 H 1.0135 0.7301 0.9468 0.033 Uiso 1 1 calc R . . C2S C 0.8918(5) 0.2929(3) 0.7386(5) 0.0763(18) Uani 1 1 d . . . H2SA H 0.8378 0.3020 0.6576 0.114 Uiso 1 1 calc R . . H2SB H 0.9460 0.2644 0.7397 0.114 Uiso 1 1 calc R . . H2SC H 0.9447 0.3219 0.7781 0.114 Uiso 1 1 calc R . . C3 C 0.8540(3) 0.70133(14) 0.9549(3) 0.0304(8) Uani 1 1 d . . . H3 H 0.8504 0.7247 1.0106 0.037 Uiso 1 1 calc R . . C3S C 0.9739(7) 0.4353(4) 0.9430(7) 0.104(3) Uani 1 1 d U . . H3SC H 1.0420 0.4314 0.9156 0.125 Uiso 0.50 1 calc PR . 1 H3SD H 1.0016 0.4165 1.0174 0.125 Uiso 0.50 1 calc PR . 1 H3SA H 1.0420 0.4314 0.9156 0.125 Uiso 0.50 1 calc PR . -1 H3SB H 1.0016 0.4165 1.0174 0.125 Uiso 0.50 1 calc PR . -1 C4 C 0.7659(4) 0.66340(14) 0.9141(3) 0.0303(7) Uani 1 1 d . . . H4 H 0.7039 0.6589 0.9442 0.036 Uiso 1 1 calc R . . C4S C 0.8775(13) 0.4118(5) 0.8695(11) 0.074(3) Uani 0.50 1 d PU . . H4SA H 0.8091 0.4125 0.8960 0.111 Uiso 0.50 1 calc PR . . H4SB H 0.9007 0.3766 0.8633 0.111 Uiso 0.50 1 calc PR . . H4SC H 0.8490 0.4281 0.7930 0.111 Uiso 0.50 1 calc PR . . C5 C 0.7696(3) 0.63177(13) 0.8277(3) 0.0238(7) Uani 1 1 d . . . C5S C 0.9725 0.4924 0.9742 0.119(2) Uiso 0.50 1 d P . -1 C6 C 0.6961(3) 0.58431(13) 0.7906(3) 0.0247(7) Uani 1 1 d . . . C7 C 0.6038(4) 0.57033(15) 0.8282(3) 0.0352(8) Uani 1 1 d . . . H7 H 0.5791 0.5928 0.8739 0.042 Uiso 1 1 calc R . . C8 C 0.5484(4) 0.52323(15) 0.7982(4) 0.0376(9) Uani 1 1 d . . . H8 H 0.4859 0.5127 0.8240 0.045 Uiso 1 1 calc R . . C9 C 0.5848(3) 0.49186(14) 0.7305(3) 0.0327(8) Uani 1 1 d . . . H9 H 0.5482 0.4593 0.7089 0.039 Uiso 1 1 calc R . . C10 C 0.6756(3) 0.50861(13) 0.6947(3) 0.0284(7) Uani 1 1 d . . . H10 H 0.6993 0.4870 0.6468 0.034 Uiso 1 1 calc R . . C11 C 1.1053(3) 0.61593(12) 0.8043(3) 0.0211(6) Uani 1 1 d . . . C12 C 1.2276(3) 0.60259(13) 0.8801(3) 0.0256(7) Uani 1 1 d . . . H12 H 1.2852 0.6275 0.9269 0.031 Uiso 1 1 calc R . . C13 C 1.2644(3) 0.55245(14) 0.8865(3) 0.0286(7) Uani 1 1 d . . . H13 H 1.3458 0.5426 0.9419 0.034 Uiso 1 1 calc R . . C14 C 1.1837(3) 0.51669(13) 0.8132(3) 0.0249(7) Uani 1 1 d . . . H14 H 1.2099 0.4826 0.8139 0.030 Uiso 1 1 calc R . . C15 C 1.0630(3) 0.53230(12) 0.7384(3) 0.0205(6) Uani 1 1 d . . . C16 C 0.9692(3) 0.50111(12) 0.6439(3) 0.0201(6) Uani 1 1 d . . . C17 C 0.9876(3) 0.45078(13) 0.6251(3) 0.0254(7) Uani 1 1 d . . . H17 H 1.0611 0.4334 0.6768 0.030 Uiso 1 1 calc R . . C18 C 0.8974(3) 0.42594(13) 0.5300(3) 0.0273(7) Uani 1 1 d . . . H18 H 0.9076 0.3912 0.5166 0.033 Uiso 1 1 calc R . . C19 C 0.7923(3) 0.45243(13) 0.4549(3) 0.0257(7) Uani 1 1 d . . . H19 H 0.7303 0.4365 0.3880 0.031 Uiso 1 1 calc R . . C20 C 0.7795(3) 0.50261(12) 0.4793(3) 0.0209(6) Uani 1 1 d . . . H20 H 0.7071 0.5207 0.4281 0.025 Uiso 1 1 calc R . . C21 C 0.9985(3) 0.68262(12) 0.6521(3) 0.0210(6) Uani 1 1 d . . . C22 C 1.0375(3) 0.72399(12) 0.6083(3) 0.0256(7) Uani 1 1 d . . . H22 H 1.0992 0.7465 0.6599 0.031 Uiso 1 1 calc R . . C23 C 0.9867(3) 0.73256(12) 0.4896(3) 0.0270(7) Uani 1 1 d . . . H23 H 1.0124 0.7611 0.4591 0.032 Uiso 1 1 calc R . . C24 C 0.8987(3) 0.69949(12) 0.4157(3) 0.0245(7) Uani 1 1 d . . . H24 H 0.8640 0.7042 0.3336 0.029 Uiso 1 1 calc R . . C25 C 0.8622(3) 0.65932(12) 0.4644(3) 0.0196(6) Uani 1 1 d . . . H25 H 0.8007 0.6365 0.4139 0.024 Uiso 1 1 calc R . . C26 C 1.0527(3) 0.67058(12) 0.7843(3) 0.0226(7) Uani 1 1 d . . . C27 C 1.1593(3) 0.70746(14) 0.8528(3) 0.0286(7) Uani 1 1 d . . . H27A H 1.2275 0.7043 0.8264 0.043 Uiso 1 1 calc R . . H27B H 1.1923 0.6995 0.9362 0.043 Uiso 1 1 calc R . . H27C H 1.1264 0.7421 0.8396 0.043 Uiso 1 1 calc R . . C28 C 0.5638(3) 0.62785(12) 0.4617(3) 0.0214(6) Uani 1 1 d . . . C29 C 0.4423(3) 0.64782(15) 0.3796(3) 0.0341(8) Uani 1 1 d . . . H29A H 0.4443 0.6526 0.3032 0.051 Uiso 1 1 calc R . . H29B H 0.4261 0.6803 0.4083 0.051 Uiso 1 1 calc R . . H29C H 0.3748 0.6239 0.3723 0.051 Uiso 1 1 calc R . . B1 B 1.123(3) 0.1725(11) 0.838(3) 0.0190(7) Uani 0.50 1 d P A 2 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 Ni1 0.0153(2) 0.0173(2) 0.0180(2) -0.00138(14) 0.00718(16) -0.00117(14) P1 0.0307(5) 0.0286(5) 0.0261(5) 0.0029(4) 0.0109(4) 0.0006(4) P2 0.0289(8) 0.0147(18) 0.0152(18) -0.0036(11) 0.0111(11) 0.0020(12) F1 0.0349(12) 0.0505(14) 0.0369(12) 0.0009(10) 0.0153(10) 0.0005(10) F2 0.0450(13) 0.0379(12) 0.0374(12) 0.0084(10) 0.0186(10) 0.0075(10) F3 0.0277(11) 0.0379(12) 0.0453(13) 0.0029(10) 0.0153(10) -0.0013(9) F4 0.0426(12) 0.0316(11) 0.0243(10) 0.0039(8) 0.0081(9) -0.0045(9) F5 0.0353(11) 0.0324(11) 0.0271(10) -0.0019(8) 0.0095(9) 0.0008(9) F6 0.0467(13) 0.0312(12) 0.0372(12) 0.0003(9) 0.0126(10) 0.0025(10) F7 0.0314(11) 0.0437(13) 0.0325(11) 0.0092(9) 0.0077(9) -0.0014(9) F8 0.042(2) 0.030(2) 0.0184(18) -0.0002(16) 0.0032(17) -0.0049(18) F9 0.0420(12) 0.0232(10) 0.0416(11) 0.0072(9) 0.0261(10) 0.0033(9) F10 0.060(4) 0.0251(19) 0.038(3) -0.002(2) 0.029(3) 0.001(3) F11 0.0297(14) 0.037(2) 0.041(2) 0.0030(14) 0.0195(15) -0.0022(17) F12 0.030(2) 0.0183(18) 0.032(2) 0.0020(15) 0.0156(17) -0.0032(15) F13 0.0297(14) 0.037(2) 0.041(2) 0.0030(14) 0.0195(15) -0.0022(17) F14 0.060(4) 0.0251(19) 0.038(3) -0.002(2) 0.029(3) 0.001(3) N1 0.0221(13) 0.0208(13) 0.0211(13) -0.0013(10) 0.0102(11) -0.0004(10) N1S 0.054(3) 0.192(7) 0.046(3) -0.022(3) 0.016(2) 0.001(4) N2 0.0229(13) 0.0243(14) 0.0237(13) -0.0011(11) 0.0119(11) -0.0024(11) N3 0.0180(12) 0.0218(13) 0.0174(12) -0.0009(10) 0.0080(10) -0.0010(10) N4 0.0169(12) 0.0196(13) 0.0195(12) 0.0012(10) 0.0091(10) -0.0006(10) N5 0.0169(12) 0.0166(12) 0.0226(13) -0.0021(10) 0.0089(10) -0.0002(10) N6 0.0207(14) 0.0214(13) 0.0244(13) -0.0025(11) 0.0115(12) -0.0018(11) C1 0.0236(16) 0.0224(16) 0.0208(15) -0.0010(12) 0.0077(13) 0.0011(13) C1S 0.046(3) 0.127(5) 0.034(2) -0.008(3) 0.008(2) 0.027(3) C2 0.0305(17) 0.0252(17) 0.0246(16) -0.0052(13) 0.0082(14) -0.0011(14) C2S 0.064(3) 0.114(5) 0.050(3) 0.019(3) 0.023(3) 0.038(3) C3 0.039(2) 0.0295(18) 0.0258(17) -0.0054(14) 0.0160(15) 0.0037(15) C3S 0.081(5) 0.150(8) 0.092(5) 0.038(5) 0.046(4) 0.011(5) C4 0.0371(19) 0.0311(18) 0.0295(17) -0.0023(14) 0.0205(15) 0.0025(15) C4S 0.074(8) 0.082(8) 0.066(7) 0.029(6) 0.029(6) 0.016(7) C5 0.0252(16) 0.0255(17) 0.0235(16) 0.0009(13) 0.0128(13) 0.0025(13) C6 0.0252(16) 0.0272(17) 0.0252(16) 0.0009(13) 0.0139(14) -0.0001(13) C7 0.042(2) 0.033(2) 0.045(2) -0.0056(16) 0.0322(18) -0.0043(16) C8 0.040(2) 0.037(2) 0.049(2) -0.0002(17) 0.0326(19) -0.0076(17) C9 0.0345(19) 0.0279(18) 0.042(2) -0.0037(15) 0.0228(17) -0.0077(15) C10 0.0329(18) 0.0250(17) 0.0332(18) -0.0043(14) 0.0197(15) -0.0047(14) C11 0.0198(15) 0.0260(17) 0.0182(14) -0.0017(12) 0.0085(12) -0.0027(12) C12 0.0203(16) 0.0327(18) 0.0217(15) -0.0039(13) 0.0065(13) -0.0053(13) C13 0.0190(16) 0.041(2) 0.0221(16) 0.0049(14) 0.0043(13) 0.0038(14) C14 0.0236(16) 0.0280(17) 0.0218(15) 0.0030(13) 0.0083(13) 0.0033(13) C15 0.0194(15) 0.0240(16) 0.0205(15) 0.0021(12) 0.0107(12) 0.0005(12) C16 0.0192(15) 0.0232(16) 0.0208(15) 0.0018(12) 0.0112(12) -0.0004(12) C17 0.0235(16) 0.0239(17) 0.0296(17) 0.0014(13) 0.0118(14) 0.0039(13) C18 0.0287(17) 0.0222(16) 0.0348(18) -0.0056(14) 0.0170(15) 0.0006(13) C19 0.0251(16) 0.0280(17) 0.0260(16) -0.0067(13) 0.0126(14) -0.0042(13) C20 0.0192(15) 0.0233(16) 0.0208(15) -0.0011(12) 0.0090(12) -0.0007(12) C21 0.0182(14) 0.0200(15) 0.0261(16) -0.0032(12) 0.0103(13) 0.0004(12) C22 0.0236(16) 0.0192(16) 0.0355(18) -0.0030(13) 0.0138(14) -0.0042(12) C23 0.0282(17) 0.0194(16) 0.0374(19) 0.0057(14) 0.0176(15) 0.0003(13) C24 0.0221(15) 0.0253(17) 0.0283(17) 0.0054(13) 0.0125(13) 0.0055(13) C25 0.0176(14) 0.0187(15) 0.0229(15) 0.0007(12) 0.0086(12) 0.0023(11) C26 0.0211(15) 0.0228(16) 0.0226(15) -0.0043(12) 0.0076(13) -0.0052(13) C27 0.0265(17) 0.0287(18) 0.0283(17) -0.0086(14) 0.0089(14) -0.0088(14) C28 0.0214(16) 0.0217(16) 0.0229(15) -0.0046(12) 0.0110(14) -0.0002(13) C29 0.0244(17) 0.043(2) 0.0291(18) -0.0040(16) 0.0051(15) 0.0116(15) B1 0.0289(8) 0.0147(18) 0.0152(18) -0.0036(11) 0.0111(11) 0.0020(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 Ni1 N3 2.015(3) . ? Ni1 N1 2.029(3) . ? Ni1 N5 2.061(3) . ? Ni1 N6 2.083(3) . ? Ni1 N4 2.086(3) . ? Ni1 N2 2.149(3) . ? P1 F2 1.585(2) . ? P1 F5 1.592(2) . ? P1 F6 1.593(2) . ? P1 F3 1.594(2) . ? P1 F4 1.596(2) . ? P1 F1 1.597(2) . ? P2 F7 1.513(7) . ? P2 F9 1.540(7) . ? P2 F11 1.582(6) . ? P2 F8 1.622(7) . ? P2 F10 1.625(9) . ? P2 F12 1.633(7) . ? F7 B1 1.64(3) . ? F9 B1 1.63(3) . ? F13 B1 1.31(3) . ? F14 B1 1.21(3) . ? O1S O1S 0.80398(11) 3_767 ? O1S C3S 1.562(10) . ? N1 C1 1.333(4) . ? N1 C5 1.346(4) . ? N1S C1S 1.148(8) . ? N2 C10 1.337(4) . ? N2 C6 1.348(4) . ? N3 C15 1.339(4) . ? N3 C11 1.344(4) . ? N4 C20 1.336(4) . ? N4 C16 1.356(4) . ? N5 C25 1.337(4) . ? N5 C21 1.351(4) . ? N6 C28 1.132(4) . ? C1 C2 1.389(5) . ? C1 C26 1.538(4) . ? C1S C2S 1.448(8) . ? C2 C3 1.388(5) . ? C2 H2 0.9500 . ? C2S H2SA 0.9800 . ? C2S H2SB 0.9800 . ? C2S H2SC 0.9800 . ? C3 C4 1.372(5) . ? C3 H3 0.9500 . ? C3S C4S 1.280(15) . ? C3S C5S 1.562(10) . ? C3S H3SC 0.9900 . ? C3S H3SD 0.9900 . ? C3S H3SA 0.9900 . ? C3S H3SB 0.9900 . ? C4 C5 1.386(5) . ? C4 H4 0.9500 . ? C4S H4SA 0.9800 . ? C4S H4SB 0.9800 . ? C4S H4SC 0.9800 . ? C5 C6 1.481(5) . ? C6 C7 1.389(5) . ? C7 C8 1.381(5) . ? C7 H7 0.9500 . ? C8 C9 1.376(5) . ? C8 H8 0.9500 . ? C9 C10 1.379(5) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.389(5) . ? C11 C26 1.549(5) . ? C12 C13 1.386(5) . ? C12 H12 0.9500 . ? C13 C14 1.381(5) . ? C13 H13 0.9500 . ? C14 C15 1.388(4) . ? C14 H14 0.9500 . ? C15 C16 1.486(4) . ? C16 C17 1.384(5) . ? C17 C18 1.386(5) . ? C17 H17 0.9500 . ? C18 C19 1.385(5) . ? C18 H18 0.9500 . ? C19 C20 1.384(5) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C22 1.383(5) . ? C21 C26 1.548(4) . ? C22 C23 1.379(5) . ? C22 H22 0.9500 . ? C23 C24 1.373(5) . ? C23 H23 0.9500 . ? C24 C25 1.378(5) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C27 1.531(4) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.459(5) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? 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 N3 Ni1 N1 85.26(10) . . ? N3 Ni1 N5 82.27(10) . . ? N1 Ni1 N5 89.63(10) . . ? N3 Ni1 N6 168.67(10) . . ? N1 Ni1 N6 100.83(11) . . ? N5 Ni1 N6 88.19(10) . . ? N3 Ni1 N4 78.09(10) . . ? N1 Ni1 N4 154.67(10) . . ? N5 Ni1 N4 106.66(10) . . ? N6 Ni1 N4 98.99(10) . . ? N3 Ni1 N2 108.97(10) . . ? N1 Ni1 N2 77.18(10) . . ? N5 Ni1 N2 161.59(10) . . ? N6 Ni1 N2 81.85(10) . . ? N4 Ni1 N2 90.24(10) . . ? F2 P1 F5 90.43(12) . . ? F2 P1 F6 90.26(13) . . ? F5 P1 F6 178.79(14) . . ? F2 P1 F3 91.33(13) . . ? F5 P1 F3 90.55(12) . . ? F6 P1 F3 90.43(13) . . ? F2 P1 F4 179.28(14) . . ? F5 P1 F4 89.62(12) . . ? F6 P1 F4 89.68(12) . . ? F3 P1 F4 89.39(12) . . ? F2 P1 F1 90.00(13) . . ? F5 P1 F1 89.31(12) . . ? F6 P1 F1 89.70(13) . . ? F3 P1 F1 178.66(14) . . ? F4 P1 F1 89.28(12) . . ? F7 P2 F9 95.4(4) . . ? F7 P2 F11 94.6(3) . . ? F9 P2 F11 91.6(3) . . ? F7 P2 F8 174.7(4) . . ? F9 P2 F8 87.2(4) . . ? F11 P2 F8 89.9(4) . . ? F7 P2 F10 85.6(4) . . ? F9 P2 F10 90.8(4) . . ? F11 P2 F10 177.6(5) . . ? F8 P2 F10 89.7(3) . . ? F7 P2 F12 88.8(4) . . ? F9 P2 F12 175.8(5) . . ? F11 P2 F12 88.5(4) . . ? F8 P2 F12 88.6(4) . . ? F10 P2 F12 89.1(4) . . ? P2 F7 B1 8.3(11) . . ? P2 F9 B1 8.9(10) . . ? O1S O1S C3S 126.7(3) 3_767 . ? C1 N1 C5 120.7(3) . . ? C1 N1 Ni1 122.4(2) . . ? C5 N1 Ni1 116.7(2) . . ? C10 N2 C6 117.8(3) . . ? C10 N2 Ni1 128.5(2) . . ? C6 N2 Ni1 111.9(2) . . ? C15 N3 C11 121.6(3) . . ? C15 N3 Ni1 116.2(2) . . ? C11 N3 Ni1 122.2(2) . . ? C20 N4 C16 118.8(3) . . ? C20 N4 Ni1 127.2(2) . . ? C16 N4 Ni1 112.1(2) . . ? C25 N5 C21 119.2(3) . . ? C25 N5 Ni1 120.7(2) . . ? C21 N5 Ni1 120.0(2) . . ? C28 N6 Ni1 172.5(3) . . ? N1 C1 C2 120.3(3) . . ? N1 C1 C26 115.9(3) . . ? C2 C1 C26 123.6(3) . . ? N1S C1S C2S 179.3(7) . . ? C3 C2 C1 118.9(3) . . ? C3 C2 H2 120.6 . . ? C1 C2 H2 120.6 . . ? C1S C2S H2SA 109.5 . . ? C1S C2S H2SB 109.5 . . ? H2SA C2S H2SB 109.5 . . ? C1S C2S H2SC 109.5 . . ? H2SA C2S H2SC 109.5 . . ? H2SB C2S H2SC 109.5 . . ? C4 C3 C2 120.1(3) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C4S C3S C5S 123.7(8) . . ? C4S C3S O1S 123.7(8) . . ? C5S C3S O1S 0.0 . . ? C4S C3S H3SC 106.4 . . ? C5S C3S H3SC 106.4 . . ? O1S C3S H3SC 106.4 . . ? C4S C3S H3SD 106.4 . . ? C5S C3S H3SD 106.4 . . ? O1S C3S H3SD 106.4 . . ? H3SC C3S H3SD 106.5 . . ? C4S C3S H3SA 106.4 . . ? C5S C3S H3SA 106.4 . . ? O1S C3S H3SA 106.4 . . ? H3SC C3S H3SA 0.0 . . ? H3SD C3S H3SA 106.5 . . ? C4S C3S H3SB 106.4 . . ? C5S C3S H3SB 106.4 . . ? O1S C3S H3SB 106.4 . . ? H3SC C3S H3SB 106.5 . . ? H3SD C3S H3SB 0.0 . . ? H3SA C3S H3SB 106.5 . . ? C3 C4 C5 118.4(3) . . ? C3 C4 H4 120.8 . . ? C5 C4 H4 120.8 . . ? C3S C4S H4SA 109.5 . . ? C3S C4S H4SB 109.5 . . ? H4SA C4S H4SB 109.5 . . ? C3S C4S H4SC 109.5 . . ? H4SA C4S H4SC 109.5 . . ? H4SB C4S H4SC 109.5 . . ? N1 C5 C4 121.0(3) . . ? N1 C5 C6 114.6(3) . . ? C4 C5 C6 123.9(3) . . ? N2 C6 C7 122.1(3) . . ? N2 C6 C5 114.8(3) . . ? C7 C6 C5 122.9(3) . . ? C8 C7 C6 119.0(3) . . ? C8 C7 H7 120.5 . . ? C6 C7 H7 120.5 . . ? C9 C8 C7 119.0(3) . . ? C9 C8 H8 120.5 . . ? C7 C8 H8 120.5 . . ? C8 C9 C10 118.8(3) . . ? C8 C9 H9 120.6 . . ? C10 C9 H9 120.6 . . ? N2 C10 C9 123.2(3) . . ? N2 C10 H10 118.4 . . ? C9 C10 H10 118.4 . . ? N3 C11 C12 119.4(3) . . ? N3 C11 C26 115.8(3) . . ? C12 C11 C26 124.8(3) . . ? C13 C12 C11 119.1(3) . . ? C13 C12 H12 120.5 . . ? C11 C12 H12 120.5 . . ? C14 C13 C12 120.6(3) . . ? C14 C13 H13 119.7 . . ? C12 C13 H13 119.7 . . ? C13 C14 C15 117.7(3) . . ? C13 C14 H14 121.2 . . ? C15 C14 H14 121.2 . . ? N3 C15 C14 121.1(3) . . ? N3 C15 C16 113.5(3) . . ? C14 C15 C16 125.2(3) . . ? N4 C16 C17 121.5(3) . . ? N4 C16 C15 114.5(3) . . ? C17 C16 C15 123.9(3) . . ? C16 C17 C18 119.3(3) . . ? C16 C17 H17 120.4 . . ? C18 C17 H17 120.4 . . ? C19 C18 C17 119.1(3) . . ? C19 C18 H18 120.5 . . ? C17 C18 H18 120.5 . . ? C20 C19 C18 118.6(3) . . ? C20 C19 H19 120.7 . . ? C18 C19 H19 120.7 . . ? N4 C20 C19 122.7(3) . . ? N4 C20 H20 118.6 . . ? C19 C20 H20 118.6 . . ? N5 C21 C22 120.3(3) . . ? N5 C21 C26 117.2(3) . . ? C22 C21 C26 122.4(3) . . ? C23 C22 C21 119.9(3) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C24 C23 C22 119.5(3) . . ? C24 C23 H23 120.2 . . ? C22 C23 H23 120.2 . . ? C23 C24 C25 118.1(3) . . ? C23 C24 H24 121.0 . . ? C25 C24 H24 121.0 . . ? N5 C25 C24 123.0(3) . . ? N5 C25 H25 118.5 . . ? C24 C25 H25 118.5 . . ? C27 C26 C1 110.7(3) . . ? C27 C26 C21 110.4(3) . . ? C1 C26 C21 109.7(3) . . ? C27 C26 C11 109.3(3) . . ? C1 C26 C11 107.8(3) . . ? C21 C26 C11 108.9(2) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N6 C28 C29 179.0(4) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? F14 B1 F13 135(3) . . ? F14 B1 F9 109(2) . . ? F13 B1 F9 104.0(18) . . ? F14 B1 F7 111(2) . . ? F13 B1 F7 100.5(16) . . ? F9 B1 F7 87.3(15) . . ? 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 F9 P2 F7 B1 -110(10) . . . . ? F11 P2 F7 B1 158(10) . . . . ? F8 P2 F7 B1 10(5) . . . . ? F10 P2 F7 B1 -20(10) . . . . ? F12 P2 F7 B1 70(10) . . . . ? F7 P2 F9 B1 118(10) . . . . ? F11 P2 F9 B1 -148(10) . . . . ? F8 P2 F9 B1 -58(10) . . . . ? F10 P2 F9 B1 32(9) . . . . ? F12 P2 F9 B1 -56(7) . . . . ? N3 Ni1 N1 C1 48.3(3) . . . . ? N5 Ni1 N1 C1 -34.0(3) . . . . ? N6 Ni1 N1 C1 -122.1(2) . . . . ? N4 Ni1 N1 C1 97.0(3) . . . . ? N2 Ni1 N1 C1 159.0(3) . . . . ? N3 Ni1 N1 C5 -128.1(2) . . . . ? N5 Ni1 N1 C5 149.6(2) . . . . ? N6 Ni1 N1 C5 61.5(2) . . . . ? N4 Ni1 N1 C5 -79.3(3) . . . . ? N2 Ni1 N1 C5 -17.4(2) . . . . ? N3 Ni1 N2 C10 -96.2(3) . . . . ? N1 Ni1 N2 C10 -176.6(3) . . . . ? N5 Ni1 N2 C10 138.2(3) . . . . ? N6 Ni1 N2 C10 80.3(3) . . . . ? N4 Ni1 N2 C10 -18.7(3) . . . . ? N3 Ni1 N2 C6 100.0(2) . . . . ? N1 Ni1 N2 C6 19.7(2) . . . . ? N5 Ni1 N2 C6 -25.6(4) . . . . ? N6 Ni1 N2 C6 -83.5(2) . . . . ? N4 Ni1 N2 C6 177.5(2) . . . . ? N1 Ni1 N3 C15 141.2(2) . . . . ? N5 Ni1 N3 C15 -128.5(2) . . . . ? N6 Ni1 N3 C15 -95.7(6) . . . . ? N4 Ni1 N3 C15 -19.6(2) . . . . ? N2 Ni1 N3 C15 66.5(2) . . . . ? N1 Ni1 N3 C11 -36.8(2) . . . . ? N5 Ni1 N3 C11 53.5(2) . . . . ? N6 Ni1 N3 C11 86.3(6) . . . . ? N4 Ni1 N3 C11 162.4(2) . . . . ? N2 Ni1 N3 C11 -111.5(2) . . . . ? N3 Ni1 N4 C20 -175.2(3) . . . . ? N1 Ni1 N4 C20 134.8(3) . . . . ? N5 Ni1 N4 C20 -97.1(3) . . . . ? N6 Ni1 N4 C20 -6.3(3) . . . . ? N2 Ni1 N4 C20 75.4(3) . . . . ? N3 Ni1 N4 C16 20.8(2) . . . . ? N1 Ni1 N4 C16 -29.2(3) . . . . ? N5 Ni1 N4 C16 98.9(2) . . . . ? N6 Ni1 N4 C16 -170.3(2) . . . . ? N2 Ni1 N4 C16 -88.5(2) . . . . ? N3 Ni1 N5 C25 134.0(2) . . . . ? N1 Ni1 N5 C25 -140.7(2) . . . . ? N6 Ni1 N5 C25 -39.9(2) . . . . ? N4 Ni1 N5 C25 59.0(2) . . . . ? N2 Ni1 N5 C25 -96.9(4) . . . . ? N3 Ni1 N5 C21 -50.0(2) . . . . ? N1 Ni1 N5 C21 35.3(2) . . . . ? N6 Ni1 N5 C21 136.1(2) . . . . ? N4 Ni1 N5 C21 -125.0(2) . . . . ? N2 Ni1 N5 C21 79.1(4) . . . . ? N3 Ni1 N6 C28 -83(2) . . . . ? N1 Ni1 N6 C28 39(2) . . . . ? N5 Ni1 N6 C28 -50(2) . . . . ? N4 Ni1 N6 C28 -157(2) . . . . ? N2 Ni1 N6 C28 114(2) . . . . ? C5 N1 C1 C2 -7.4(5) . . . . ? Ni1 N1 C1 C2 176.4(2) . . . . ? C5 N1 C1 C26 167.3(3) . . . . ? Ni1 N1 C1 C26 -8.9(4) . . . . ? N1 C1 C2 C3 0.8(5) . . . . ? C26 C1 C2 C3 -173.5(3) . . . . ? C1 C2 C3 C4 4.7(5) . . . . ? O1S O1S C3S C4S 171.0(8) 3_767 . . . ? O1S O1S C3S C5S 0(100) 3_767 . . . ? C2 C3 C4 C5 -3.7(5) . . . . ? C1 N1 C5 C4 8.4(5) . . . . ? Ni1 N1 C5 C4 -175.1(3) . . . . ? C1 N1 C5 C6 -163.8(3) . . . . ? Ni1 N1 C5 C6 12.6(4) . . . . ? C3 C4 C5 N1 -2.8(5) . . . . ? C3 C4 C5 C6 168.8(3) . . . . ? C10 N2 C6 C7 -0.3(5) . . . . ? Ni1 N2 C6 C7 165.4(3) . . . . ? C10 N2 C6 C5 175.2(3) . . . . ? Ni1 N2 C6 C5 -19.1(3) . . . . ? N1 C5 C6 N2 5.3(4) . . . . ? C4 C5 C6 N2 -166.7(3) . . . . ? N1 C5 C6 C7 -179.2(3) . . . . ? C4 C5 C6 C7 8.7(5) . . . . ? N2 C6 C7 C8 1.2(6) . . . . ? C5 C6 C7 C8 -173.9(4) . . . . ? C6 C7 C8 C9 -1.0(6) . . . . ? C7 C8 C9 C10 -0.1(6) . . . . ? C6 N2 C10 C9 -0.9(5) . . . . ? Ni1 N2 C10 C9 -163.9(3) . . . . ? C8 C9 C10 N2 1.1(6) . . . . ? C15 N3 C11 C12 -7.2(4) . . . . ? Ni1 N3 C11 C12 170.7(2) . . . . ? C15 N3 C11 C26 171.4(3) . . . . ? Ni1 N3 C11 C26 -10.6(4) . . . . ? N3 C11 C12 C13 1.1(5) . . . . ? C26 C11 C12 C13 -177.5(3) . . . . ? C11 C12 C13 C14 4.3(5) . . . . ? C12 C13 C14 C15 -3.7(5) . . . . ? C11 N3 C15 C14 8.0(4) . . . . ? Ni1 N3 C15 C14 -170.1(2) . . . . ? C11 N3 C15 C16 -167.1(3) . . . . ? Ni1 N3 C15 C16 14.9(3) . . . . ? C13 C14 C15 N3 -2.4(5) . . . . ? C13 C14 C15 C16 172.1(3) . . . . ? C20 N4 C16 C17 -1.5(4) . . . . ? Ni1 N4 C16 C17 163.9(2) . . . . ? C20 N4 C16 C15 175.2(3) . . . . ? Ni1 N4 C16 C15 -19.3(3) . . . . ? N3 C15 C16 N4 3.7(4) . . . . ? C14 C15 C16 N4 -171.2(3) . . . . ? N3 C15 C16 C17 -179.6(3) . . . . ? C14 C15 C16 C17 5.5(5) . . . . ? N4 C16 C17 C18 0.4(5) . . . . ? C15 C16 C17 C18 -176.1(3) . . . . ? C16 C17 C18 C19 1.2(5) . . . . ? C17 C18 C19 C20 -1.6(5) . . . . ? C16 N4 C20 C19 1.1(4) . . . . ? Ni1 N4 C20 C19 -161.9(2) . . . . ? C18 C19 C20 N4 0.5(5) . . . . ? C25 N5 C21 C22 2.1(4) . . . . ? Ni1 N5 C21 C22 -173.9(2) . . . . ? C25 N5 C21 C26 -178.4(3) . . . . ? Ni1 N5 C21 C26 5.5(4) . . . . ? N5 C21 C22 C23 -1.1(5) . . . . ? C26 C21 C22 C23 179.4(3) . . . . ? C21 C22 C23 C24 -0.7(5) . . . . ? C22 C23 C24 C25 1.6(5) . . . . ? C21 N5 C25 C24 -1.2(4) . . . . ? Ni1 N5 C25 C24 174.8(2) . . . . ? C23 C24 C25 N5 -0.6(5) . . . . ? N1 C1 C26 C27 -173.7(3) . . . . ? C2 C1 C26 C27 0.8(4) . . . . ? N1 C1 C26 C21 64.2(4) . . . . ? C2 C1 C26 C21 -121.3(3) . . . . ? N1 C1 C26 C11 -54.2(4) . . . . ? C2 C1 C26 C11 120.3(3) . . . . ? N5 C21 C26 C27 175.6(3) . . . . ? C22 C21 C26 C27 -4.9(4) . . . . ? N5 C21 C26 C1 -62.2(3) . . . . ? C22 C21 C26 C1 117.3(3) . . . . ? N5 C21 C26 C11 55.5(3) . . . . ? C22 C21 C26 C11 -125.0(3) . . . . ? N3 C11 C26 C27 -173.8(3) . . . . ? C12 C11 C26 C27 4.8(4) . . . . ? N3 C11 C26 C1 65.8(3) . . . . ? C12 C11 C26 C1 -115.6(3) . . . . ? N3 C11 C26 C21 -53.2(3) . . . . ? C12 C11 C26 C21 125.4(3) . . . . ? Ni1 N6 C28 C29 96(20) . . . . ? P2 F9 B1 F14 -166(12) . . . . ? P2 F9 B1 F13 46(8) . . . . ? P2 F9 B1 F7 -55(9) . . . . ? P2 F7 B1 F14 171(12) . . . . ? P2 F7 B1 F13 -42(9) . . . . ? P2 F7 B1 F9 62(10) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.41 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.663 _refine_diff_density_min -1.717 _refine_diff_density_rms 0.091 _database_code_depnum_ccdc_archive 'CCDC 943489' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Cu(bpy2py))2OTf*2CH3CN' _chemical_melting_point ? _chemical_formula_moiety 'C29 H21 Cu F6 N5 O6 S2' _chemical_formula_sum 'C33 H27 Cu F6 N7 O6 S2' _chemical_formula_weight 859.28 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.9247(6) _cell_length_b 13.1783(8) _cell_length_c 14.8490(9) _cell_angle_alpha 66.577(2) _cell_angle_beta 80.638(2) _cell_angle_gamma 81.873(2) _cell_volume 1752.01(18) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9035 _cell_measurement_theta_min 2.4261 _cell_measurement_theta_max 25.3844 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.629 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 874 _exptl_absorpt_coefficient_mu 0.831 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8254 _exptl_absorpt_correction_T_max 0.9068 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'microfocus sealed tube' _diffrn_radiation_monochromator 'QUAZAR multilayer mirrors' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_reflns_number 22772 _diffrn_reflns_av_R_equivalents 0.0630 _diffrn_reflns_av_sigmaI/netI 0.0365 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 25.42 _reflns_number_total 6342 _reflns_number_gt 5760 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v. 2009.1' _computing_cell_refinement 'Bruker APEX2 v. 2009.1' _computing_data_reduction 'Bruker APEX2 v. 2009.1' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics DIAMOND _computing_publication_material CIFTAB _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^)+(0.0404P)^2^+1.3518P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6342 _refine_ls_number_parameters 544 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0348 _refine_ls_R_factor_gt 0.0317 _refine_ls_wR_factor_ref 0.0858 _refine_ls_wR_factor_gt 0.0838 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _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 Cu1 Cu 0.49918(2) 0.594928(18) 0.735682(16) 0.01208(8) Uani 1 1 d . . . S1 S 0.21266(5) 0.83068(4) 0.70070(3) 0.01448(11) Uani 1 1 d . . . S2 S 0.3424(3) 0.82288(19) 1.19499(14) 0.0228(4) Uani 0.50 1 d P A 2 S3 S 0.3552(3) 0.85033(18) 1.15854(14) 0.0226(4) Uani 0.50 1 d P A 1 F1 F 0.15420(14) 0.79710(12) 0.88938(9) 0.0309(3) Uani 1 1 d . . . F2 F 0.03737(17) 0.93583(12) 0.79281(11) 0.0437(4) Uani 1 1 d . . . F3 F -0.01022(14) 0.77009(13) 0.82560(10) 0.0370(4) Uani 1 1 d . . . F4 F 0.17635(17) 0.79921(19) 1.07976(16) 0.0673(6) Uani 1 1 d . A . F5 F 0.0844(5) 0.8880(6) 1.1704(5) 0.086(2) Uani 0.50 1 d P A 2 F5A F 0.0979(4) 0.8087(3) 1.2102(2) 0.0370(7) Uani 0.50 1 d P A 1 F6 F 0.2269(8) 0.9496(4) 1.0383(4) 0.110(2) Uani 0.50 1 d P A 2 F6A F 0.1327(4) 0.9663(3) 1.0903(3) 0.0474(9) Uani 0.50 1 d P A 1 O1 O 0.32424(16) 0.88848(12) 0.70245(11) 0.0233(3) Uani 1 1 d . . . O2 O 0.24350(15) 0.71307(11) 0.72344(10) 0.0190(3) Uani 1 1 d . . . O3 O 0.13320(15) 0.88797(12) 0.61857(10) 0.0199(3) Uani 1 1 d . . . O4 O 0.3461(2) 0.9048(2) 1.22602(17) 0.0602(6) Uani 1 1 d . . . O5 O 0.2887(4) 0.7357(3) 1.2823(2) 0.0405(9) Uani 0.50 1 d P A 2 O5A O 0.3948(4) 0.7323(3) 1.1858(4) 0.0444(11) Uani 0.50 1 d P A 1 O6 O 0.4497(5) 0.7839(5) 1.1388(4) 0.0538(12) Uani 0.50 1 d P A 2 O6A O 0.4281(4) 0.9195(3) 1.0687(2) 0.0315(8) Uani 0.50 1 d P A 1 N1 N 0.42688(17) 0.53109(13) 0.65125(12) 0.0143(3) Uani 1 1 d . . . N1S N 0.1824(3) 0.2412(2) 0.8670(2) 0.0481(6) Uani 1 1 d . . . N2 N 0.53108(16) 0.71722(13) 0.60367(11) 0.0119(3) Uani 1 1 d . . . N2S N 0.0999(3) 1.2701(2) 0.5746(2) 0.0564(7) Uani 1 1 d . . . N3 N 0.38913(17) 0.51960(13) 0.86972(11) 0.0152(3) Uani 1 1 d . . . N4 N 0.53360(16) 0.69146(13) 0.80219(11) 0.0126(3) Uani 1 1 d . . . N5 N 0.73049(17) 0.57616(13) 0.71297(11) 0.0144(3) Uani 1 1 d . . . C1 C 0.3926(2) 0.42726(17) 0.67524(15) 0.0186(4) Uani 1 1 d . . . H1 H 0.4204 0.3699 0.7339 0.022 Uiso 1 1 calc R . . C1A C 0.6287(2) 0.84289(17) 0.80924(15) 0.0183(4) Uani 1 1 d . . . H1A H 0.6871 0.9016 0.7798 0.022 Uiso 1 1 calc R . . C1S C 0.2249(3) 0.1644(2) 0.8521(2) 0.0353(6) Uani 1 1 d . . . C2 C 0.3182(2) 0.40163(18) 0.61716(16) 0.0227(5) Uani 1 1 d . . . H2 H 0.2942 0.3280 0.6364 0.027 Uiso 1 1 calc R . . C2S C 0.2803(4) 0.0680(3) 0.8305(4) 0.0761(13) Uani 1 1 d . . . H2SA H 0.2627 0.0795 0.7639 0.114 Uiso 1 1 calc R . . H2SB H 0.2364 0.0025 0.8788 0.114 Uiso 1 1 calc R . . H2SC H 0.3793 0.0565 0.8342 0.114 Uiso 1 1 calc R . . C3 C 0.2793(2) 0.48385(19) 0.53120(16) 0.0249(5) Uani 1 1 d . . . H3 H 0.2249 0.4682 0.4919 0.030 Uiso 1 1 calc R . . C3S C -0.0684(2) 1.12969(18) 0.58885(16) 0.0226(5) Uani 1 1 d . . . H3SA H -0.1123 1.1560 0.5281 0.034 Uiso 1 1 calc R . . H3SB H -0.1386 1.1216 0.6453 0.034 Uiso 1 1 calc R . . H3SC H -0.0169 1.0577 0.5983 0.034 Uiso 1 1 calc R . . C4 C 0.0243(3) 1.2089(2) 0.58127(17) 0.0299(5) Uani 1 1 d . . . C5 C 0.3202(2) 0.59003(18) 0.50242(16) 0.0208(4) Uani 1 1 d . . . H5 H 0.2978 0.6472 0.4420 0.025 Uiso 1 1 calc R . . C6 C 0.3947(2) 0.61076(16) 0.56402(14) 0.0151(4) Uani 1 1 d . . . C7 C 0.4566(2) 0.71667(16) 0.53594(14) 0.0142(4) Uani 1 1 d . . . C8 C 0.4518(2) 0.80477(17) 0.44544(14) 0.0175(4) Uani 1 1 d . . . H8 H 0.3967 0.8053 0.3985 0.021 Uiso 1 1 calc R . . C9 C 0.5299(2) 0.89201(16) 0.42574(14) 0.0185(4) Uani 1 1 d . . . H9 H 0.5263 0.9548 0.3653 0.022 Uiso 1 1 calc R . . C10 C 0.6131(2) 0.88836(16) 0.49355(15) 0.0162(4) Uani 1 1 d . . . H10 H 0.6701 0.9465 0.4788 0.019 Uiso 1 1 calc R . . C11 C 0.6119(2) 0.79794(15) 0.58394(14) 0.0133(4) Uani 1 1 d . . . C12 C 0.3109(2) 0.43445(17) 0.89824(15) 0.0215(4) Uani 1 1 d . . . H12 H 0.3212 0.3911 0.8591 0.026 Uiso 1 1 calc R . . C13 C 0.2158(2) 0.40666(18) 0.98187(16) 0.0239(5) Uani 1 1 d . . . H13 H 0.1620 0.3460 0.9992 0.029 Uiso 1 1 calc R . . C14 C 0.2008(2) 0.46871(18) 1.03936(15) 0.0237(5) Uani 1 1 d . . . H14 H 0.1361 0.4519 1.0969 0.028 Uiso 1 1 calc R . . C15 C 0.2818(2) 0.55586(17) 1.01184(15) 0.0209(4) Uani 1 1 d . . . H15 H 0.2743 0.5989 1.0511 0.025 Uiso 1 1 calc R . . C16 C 0.3739(2) 0.58019(16) 0.92683(14) 0.0153(4) Uani 1 1 d . . . C17 C 0.4606(2) 0.67415(16) 0.89078(14) 0.0144(4) Uani 1 1 d . . . C18 C 0.4689(2) 0.73994(17) 0.94226(15) 0.0192(4) Uani 1 1 d . . . H18 H 0.4179 0.7262 1.0053 0.023 Uiso 1 1 calc R . . C19 C 0.5530(2) 0.82605(17) 0.90019(16) 0.0211(4) Uani 1 1 d . . . H19 H 0.5589 0.8734 0.9335 0.025 Uiso 1 1 calc R . . C20 C 0.6184(2) 0.77303(15) 0.76131(14) 0.0134(4) Uani 1 1 d . . . C21 C 0.8059(2) 0.47840(16) 0.73214(14) 0.0174(4) Uani 1 1 d . . . H21 H 0.7597 0.4134 0.7505 0.021 Uiso 1 1 calc R . . C22 C 0.9473(2) 0.46776(18) 0.72644(16) 0.0220(5) Uani 1 1 d . . . H22 H 0.9974 0.3972 0.7412 0.026 Uiso 1 1 calc R . . C23 C 1.0137(2) 0.56291(18) 0.69864(15) 0.0212(4) Uani 1 1 d . . . H23 H 1.1107 0.5585 0.6951 0.025 Uiso 1 1 calc R . . C24 C 0.9376(2) 0.66498(17) 0.67585(14) 0.0168(4) Uani 1 1 d . . . H24 H 0.9821 0.7312 0.6551 0.020 Uiso 1 1 calc R . . C25 C 0.7957(2) 0.66932(16) 0.68372(13) 0.0136(4) Uani 1 1 d . . . C26 C 0.7051(2) 0.78143(15) 0.66302(14) 0.0135(4) Uani 1 1 d . . . C27 C 0.7941(2) 0.87932(16) 0.62640(15) 0.0171(4) Uani 1 1 d . . . H27A H 0.8535 0.8693 0.6765 0.026 Uiso 1 1 calc R . . H27B H 0.7351 0.9485 0.6144 0.026 Uiso 1 1 calc R . . H27C H 0.8508 0.8827 0.5649 0.026 Uiso 1 1 calc R . . C28 C 0.0925(2) 0.83358(19) 0.80769(16) 0.0235(5) Uani 1 1 d . . . C29 C 0.1894(3) 0.8628(2) 1.12521(19) 0.0365(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.01427(14) 0.01075(13) 0.01165(13) -0.00423(9) -0.00125(9) -0.00290(9) S1 0.0136(2) 0.0138(2) 0.0161(2) -0.00574(19) -0.00297(18) 0.00012(18) S2 0.0325(9) 0.0203(11) 0.0192(10) -0.0103(8) -0.0077(9) -0.0001(8) S3 0.0302(9) 0.0180(10) 0.0230(11) -0.0095(9) -0.0109(10) 0.0007(7) F1 0.0332(8) 0.0423(8) 0.0192(6) -0.0142(6) -0.0101(6) 0.0056(6) F2 0.0550(10) 0.0410(9) 0.0346(8) -0.0227(7) -0.0085(7) 0.0268(8) F3 0.0220(7) 0.0650(10) 0.0263(7) -0.0207(7) 0.0063(6) -0.0123(7) F4 0.0358(10) 0.1180(17) 0.0976(15) -0.0957(14) -0.0189(9) 0.0135(10) F5 0.045(3) 0.141(5) 0.130(5) -0.120(5) -0.041(3) 0.049(4) F5A 0.0318(19) 0.053(2) 0.0361(17) -0.0271(17) -0.0003(14) -0.0074(17) F6 0.193(7) 0.058(3) 0.062(3) 0.026(2) -0.079(4) -0.027(4) F6A 0.046(2) 0.046(2) 0.0358(19) -0.0116(17) -0.0034(16) 0.0284(17) O1 0.0221(8) 0.0176(7) 0.0300(8) -0.0060(6) -0.0086(6) -0.0042(6) O2 0.0179(8) 0.0153(7) 0.0237(7) -0.0076(6) -0.0012(6) -0.0018(6) O3 0.0187(8) 0.0225(8) 0.0179(7) -0.0071(6) -0.0043(6) 0.0010(6) O4 0.0664(15) 0.0789(16) 0.0669(14) -0.0575(13) -0.0278(12) 0.0066(12) O5 0.070(3) 0.0282(18) 0.0266(18) -0.0044(15) -0.0184(18) -0.0174(18) O5A 0.027(2) 0.0155(19) 0.083(3) -0.0054(19) -0.021(2) -0.0016(15) O6 0.036(3) 0.094(4) 0.058(3) -0.060(3) -0.016(2) 0.012(3) O6A 0.036(2) 0.0390(19) 0.0239(17) -0.0193(15) 0.0036(14) -0.0047(16) N1 0.0135(8) 0.0143(8) 0.0170(8) -0.0089(7) 0.0011(6) -0.0019(7) N1S 0.0465(15) 0.0331(13) 0.0721(18) -0.0242(12) -0.0128(13) -0.0079(11) N2 0.0117(8) 0.0117(8) 0.0122(7) -0.0054(6) 0.0000(6) 0.0001(6) N2S 0.0633(18) 0.0696(18) 0.0541(16) -0.0362(14) 0.0047(13) -0.0384(15) N3 0.0167(9) 0.0149(8) 0.0118(8) -0.0025(6) -0.0017(6) -0.0024(7) N4 0.0117(8) 0.0130(8) 0.0126(8) -0.0048(6) -0.0022(6) 0.0006(6) N5 0.0171(9) 0.0135(8) 0.0136(8) -0.0060(6) -0.0024(6) -0.0008(7) C1 0.0190(11) 0.0162(10) 0.0222(10) -0.0111(8) 0.0041(8) -0.0024(8) C1A 0.0185(11) 0.0151(10) 0.0234(10) -0.0087(8) -0.0043(8) -0.0016(8) C1S 0.0345(15) 0.0266(13) 0.0441(15) -0.0099(11) -0.0040(12) -0.0118(11) C2 0.0219(11) 0.0223(11) 0.0306(12) -0.0189(9) 0.0064(9) -0.0083(9) C2S 0.059(2) 0.049(2) 0.131(4) -0.056(2) 0.023(2) -0.0144(17) C3 0.0226(12) 0.0350(13) 0.0279(12) -0.0229(10) 0.0016(9) -0.0093(10) C3S 0.0232(12) 0.0240(11) 0.0233(11) -0.0115(9) -0.0029(9) -0.0033(9) C4 0.0324(14) 0.0364(13) 0.0261(12) -0.0168(10) -0.0018(10) -0.0074(11) C5 0.0192(11) 0.0267(11) 0.0210(10) -0.0138(9) -0.0020(8) -0.0025(9) C6 0.0126(10) 0.0186(10) 0.0167(9) -0.0109(8) 0.0006(8) -0.0001(8) C7 0.0117(9) 0.0167(10) 0.0159(9) -0.0096(8) -0.0007(7) 0.0021(8) C8 0.0170(10) 0.0201(10) 0.0160(10) -0.0084(8) -0.0039(8) 0.0035(8) C9 0.0204(11) 0.0155(10) 0.0146(9) -0.0029(8) -0.0005(8) 0.0035(8) C10 0.0154(10) 0.0126(9) 0.0186(10) -0.0052(8) 0.0010(8) -0.0008(8) C11 0.0126(10) 0.0127(9) 0.0148(9) -0.0067(7) 0.0001(7) 0.0008(7) C12 0.0262(12) 0.0190(10) 0.0190(10) -0.0060(8) -0.0010(9) -0.0072(9) C13 0.0243(12) 0.0226(11) 0.0208(10) -0.0028(9) -0.0003(9) -0.0091(9) C14 0.0204(11) 0.0279(12) 0.0164(10) -0.0032(9) 0.0021(8) -0.0029(9) C15 0.0221(11) 0.0219(11) 0.0168(10) -0.0065(8) -0.0019(8) 0.0006(9) C16 0.0153(10) 0.0157(10) 0.0136(9) -0.0041(8) -0.0049(8) 0.0020(8) C17 0.0113(10) 0.0157(9) 0.0146(9) -0.0045(7) -0.0039(7) 0.0030(8) C18 0.0205(11) 0.0229(11) 0.0154(9) -0.0096(8) -0.0020(8) 0.0012(9) C19 0.0241(11) 0.0206(10) 0.0247(11) -0.0151(9) -0.0059(9) 0.0013(9) C20 0.0125(9) 0.0121(9) 0.0154(9) -0.0046(7) -0.0044(7) 0.0011(7) C21 0.0210(11) 0.0142(10) 0.0181(10) -0.0078(8) -0.0015(8) -0.0008(8) C22 0.0208(11) 0.0180(10) 0.0266(11) -0.0100(9) -0.0029(9) 0.0045(9) C23 0.0140(10) 0.0249(11) 0.0242(11) -0.0106(9) -0.0005(8) 0.0019(9) C24 0.0165(10) 0.0188(10) 0.0154(9) -0.0068(8) 0.0001(8) -0.0040(8) C25 0.0166(10) 0.0149(9) 0.0098(9) -0.0052(7) -0.0020(7) -0.0015(8) C26 0.0128(10) 0.0119(9) 0.0154(9) -0.0050(7) -0.0012(7) -0.0014(8) C27 0.0164(10) 0.0134(9) 0.0213(10) -0.0055(8) -0.0025(8) -0.0037(8) C28 0.0229(12) 0.0283(12) 0.0204(10) -0.0120(9) -0.0050(9) 0.0050(9) C29 0.0491(17) 0.0323(13) 0.0334(13) -0.0181(11) -0.0192(12) 0.0131(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 Cu1 N4 1.9853(16) . ? Cu1 N2 1.9927(15) . ? Cu1 N1 2.0239(16) . ? Cu1 N3 2.0416(16) . ? Cu1 N5 2.2581(17) . ? S1 O1 1.4391(15) . ? S1 O3 1.4462(15) . ? S1 O2 1.4468(15) . ? S1 C28 1.835(2) . ? S2 O4 1.338(3) . ? S2 O6 1.412(5) . ? S2 O5 1.432(4) . ? S2 C29 1.873(4) . ? S3 O6A 1.428(4) . ? S3 O4 1.432(3) . ? S3 O5A 1.455(4) . ? S3 C29 1.761(4) . ? F1 C28 1.331(2) . ? F2 C28 1.326(3) . ? F3 C28 1.336(3) . ? F4 C29 1.297(3) . ? F5 C29 1.224(5) . ? F5A C29 1.421(4) . ? F6 C29 1.380(5) . ? F6A C29 1.327(4) . ? N1 C1 1.349(3) . ? N1 C6 1.357(3) . ? N1S C1S 1.129(3) . ? N2 C11 1.333(2) . ? N2 C7 1.344(2) . ? N2S C4 1.143(3) . ? N3 C12 1.343(3) . ? N3 C16 1.357(3) . ? N4 C20 1.343(2) . ? N4 C17 1.344(3) . ? N5 C21 1.344(3) . ? N5 C25 1.350(2) . ? C1 C2 1.383(3) . ? C1 H1 0.9500 . ? C1A C19 1.384(3) . ? C1A C20 1.391(3) . ? C1A H1A 0.9500 . ? C1S C2S 1.446(4) . ? C2 C3 1.377(3) . ? C2 H2 0.9500 . ? C2S H2SA 0.9800 . ? C2S H2SB 0.9800 . ? C2S H2SC 0.9800 . ? C3 C5 1.391(3) . ? C3 H3 0.9500 . ? C3S C4 1.447(3) . ? C3S H3SA 0.9800 . ? C3S H3SB 0.9800 . ? C3S H3SC 0.9800 . ? C5 C6 1.390(3) . ? C5 H5 0.9500 . ? C6 C7 1.482(3) . ? C7 C8 1.386(3) . ? C8 C9 1.385(3) . ? C8 H8 0.9500 . ? C9 C10 1.385(3) . ? C9 H9 0.9500 . ? C10 C11 1.396(3) . ? C10 H10 0.9500 . ? C11 C26 1.541(3) . ? C12 C13 1.386(3) . ? C12 H12 0.9500 . ? C13 C14 1.378(3) . ? C13 H13 0.9500 . ? C14 C15 1.383(3) . ? C14 H14 0.9500 . ? C15 C16 1.385(3) . ? C15 H15 0.9500 . ? C16 C17 1.478(3) . ? C17 C18 1.382(3) . ? C18 C19 1.382(3) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C26 1.540(3) . ? C21 C22 1.383(3) . ? C21 H21 0.9500 . ? C22 C23 1.382(3) . ? C22 H22 0.9500 . ? C23 C24 1.389(3) . ? C23 H23 0.9500 . ? C24 C25 1.389(3) . ? C24 H24 0.9500 . ? C25 C26 1.562(3) . ? C26 C27 1.533(3) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? 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 N4 Cu1 N2 90.86(6) . . ? N4 Cu1 N1 164.51(7) . . ? N2 Cu1 N1 80.15(6) . . ? N4 Cu1 N3 80.95(7) . . ? N2 Cu1 N3 153.51(7) . . ? N1 Cu1 N3 101.54(7) . . ? N4 Cu1 N5 82.06(6) . . ? N2 Cu1 N5 80.68(6) . . ? N1 Cu1 N5 108.59(6) . . ? N3 Cu1 N5 122.49(6) . . ? O1 S1 O3 115.05(9) . . ? O1 S1 O2 115.44(9) . . ? O3 S1 O2 114.54(9) . . ? O1 S1 C28 103.36(10) . . ? O3 S1 C28 103.26(9) . . ? O2 S1 C28 102.72(9) . . ? O4 S2 O6 126.3(3) . . ? O4 S2 O5 103.1(2) . . ? O6 S2 O5 112.7(3) . . ? O4 S2 C29 105.34(19) . . ? O6 S2 C29 106.9(2) . . ? O5 S2 C29 99.0(2) . . ? O6A S3 O4 106.1(2) . . ? O6A S3 O5A 114.1(3) . . ? O4 S3 O5A 122.9(3) . . ? O6A S3 C29 102.5(2) . . ? O4 S3 C29 106.9(2) . . ? O5A S3 C29 102.1(2) . . ? S2 O4 S3 21.48(9) . . ? C1 N1 C6 118.44(17) . . ? C1 N1 Cu1 129.01(14) . . ? C6 N1 Cu1 111.98(12) . . ? C11 N2 C7 121.57(16) . . ? C11 N2 Cu1 123.99(13) . . ? C7 N2 Cu1 114.30(13) . . ? C12 N3 C16 117.60(17) . . ? C12 N3 Cu1 128.47(14) . . ? C16 N3 Cu1 112.40(13) . . ? C20 N4 C17 120.72(16) . . ? C20 N4 Cu1 123.60(13) . . ? C17 N4 Cu1 115.60(13) . . ? C21 N5 C25 118.68(17) . . ? C21 N5 Cu1 124.21(13) . . ? C25 N5 Cu1 116.99(13) . . ? N1 C1 C2 122.1(2) . . ? N1 C1 H1 118.9 . . ? C2 C1 H1 118.9 . . ? C19 C1A C20 119.44(19) . . ? C19 C1A H1A 120.3 . . ? C20 C1A H1A 120.3 . . ? N1S C1S C2S 178.5(3) . . ? C3 C2 C1 119.3(2) . . ? C3 C2 H2 120.3 . . ? C1 C2 H2 120.3 . . ? C1S C2S H2SA 109.5 . . ? C1S C2S H2SB 109.5 . . ? H2SA C2S H2SB 109.5 . . ? C1S C2S H2SC 109.5 . . ? H2SA C2S H2SC 109.5 . . ? H2SB C2S H2SC 109.5 . . ? C2 C3 C5 119.4(2) . . ? C2 C3 H3 120.3 . . ? C5 C3 H3 120.3 . . ? C4 C3S H3SA 109.5 . . ? C4 C3S H3SB 109.5 . . ? H3SA C3S H3SB 109.5 . . ? C4 C3S H3SC 109.5 . . ? H3SA C3S H3SC 109.5 . . ? H3SB C3S H3SC 109.5 . . ? N2S C4 C3S 178.4(3) . . ? C6 C5 C3 118.6(2) . . ? C6 C5 H5 120.7 . . ? C3 C5 H5 120.7 . . ? N1 C6 C5 121.97(18) . . ? N1 C6 C7 114.61(17) . . ? C5 C6 C7 123.16(18) . . ? N2 C7 C8 121.25(18) . . ? N2 C7 C6 113.63(17) . . ? C8 C7 C6 124.85(18) . . ? C9 C8 C7 117.74(18) . . ? C9 C8 H8 121.1 . . ? C7 C8 H8 121.1 . . ? C8 C9 C10 120.45(18) . . ? C8 C9 H9 119.8 . . ? C10 C9 H9 119.8 . . ? C9 C10 C11 118.93(19) . . ? C9 C10 H10 120.5 . . ? C11 C10 H10 120.5 . . ? N2 C11 C10 119.81(18) . . ? N2 C11 C26 116.34(16) . . ? C10 C11 C26 123.78(17) . . ? N3 C12 C13 123.3(2) . . ? N3 C12 H12 118.3 . . ? C13 C12 H12 118.3 . . ? C14 C13 C12 118.7(2) . . ? C14 C13 H13 120.6 . . ? C12 C13 H13 120.6 . . ? C13 C14 C15 118.8(2) . . ? C13 C14 H14 120.6 . . ? C15 C14 H14 120.6 . . ? C14 C15 C16 119.7(2) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? N3 C16 C15 121.87(18) . . ? N3 C16 C17 115.21(17) . . ? C15 C16 C17 122.92(18) . . ? N4 C17 C18 121.41(18) . . ? N4 C17 C16 114.43(17) . . ? C18 C17 C16 124.16(18) . . ? C19 C18 C17 118.66(19) . . ? C19 C18 H18 120.7 . . ? C17 C18 H18 120.7 . . ? C18 C19 C1A 119.60(19) . . ? C18 C19 H19 120.2 . . ? C1A C19 H19 120.2 . . ? N4 C20 C1A 120.14(18) . . ? N4 C20 C26 116.96(16) . . ? C1A C20 C26 122.87(18) . . ? N5 C21 C22 123.23(19) . . ? N5 C21 H21 118.4 . . ? C22 C21 H21 118.4 . . ? C23 C22 C21 117.99(19) . . ? C23 C22 H22 121.0 . . ? C21 C22 H22 121.0 . . ? C22 C23 C24 119.5(2) . . ? C22 C23 H23 120.3 . . ? C24 C23 H23 120.3 . . ? C23 C24 C25 119.35(19) . . ? C23 C24 H24 120.3 . . ? C25 C24 H24 120.3 . . ? N5 C25 C24 121.21(18) . . ? N5 C25 C26 117.41(17) . . ? C24 C25 C26 121.35(17) . . ? C27 C26 C20 110.05(16) . . ? C27 C26 C11 109.18(15) . . ? C20 C26 C11 110.52(15) . . ? C27 C26 C25 110.97(16) . . ? C20 C26 C25 106.82(15) . . ? C11 C26 C25 109.28(15) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? F2 C28 F1 107.64(18) . . ? F2 C28 F3 107.37(19) . . ? F1 C28 F3 107.38(18) . . ? F2 C28 S1 111.00(15) . . ? F1 C28 S1 111.63(15) . . ? F3 C28 S1 111.60(15) . . ? F5 C29 F4 115.8(3) . . ? F5 C29 F6A 61.0(4) . . ? F4 C29 F6A 117.6(3) . . ? F5 C29 F6 111.9(5) . . ? F4 C29 F6 92.9(3) . . ? F6A C29 F6 51.0(3) . . ? F5 C29 F5A 42.5(3) . . ? F4 C29 F5A 95.4(2) . . ? F6A C29 F5A 103.5(3) . . ? F6 C29 F5A 153.8(4) . . ? F5 C29 S3 124.4(3) . . ? F4 C29 S3 113.6(2) . . ? F6A C29 S3 114.2(3) . . ? F6 C29 S3 89.2(3) . . ? F5A C29 S3 110.0(2) . . ? F5 C29 S2 113.8(3) . . ? F4 C29 S2 114.8(2) . . ? F6A C29 S2 122.3(3) . . ? F6 C29 S2 105.1(3) . . ? F5A C29 S2 93.9(2) . . ? S3 C29 S2 16.22(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O6 S2 O4 S3 56.4(5) . . . . ? O5 S2 O4 S3 -172.1(7) . . . . ? C29 S2 O4 S3 -68.8(5) . . . . ? O6A S3 O4 S2 -163.3(7) . . . . ? O5A S3 O4 S2 -29.5(5) . . . . ? C29 S3 O4 S2 87.9(6) . . . . ? N4 Cu1 N1 C1 -136.0(2) . . . . ? N2 Cu1 N1 C1 168.73(18) . . . . ? N3 Cu1 N1 C1 -38.18(18) . . . . ? N5 Cu1 N1 C1 92.14(17) . . . . ? N4 Cu1 N1 C6 35.1(3) . . . . ? N2 Cu1 N1 C6 -20.18(13) . . . . ? N3 Cu1 N1 C6 132.90(13) . . . . ? N5 Cu1 N1 C6 -96.78(13) . . . . ? N4 Cu1 N2 C11 27.98(15) . . . . ? N1 Cu1 N2 C11 -164.70(16) . . . . ? N3 Cu1 N2 C11 99.2(2) . . . . ? N5 Cu1 N2 C11 -53.83(15) . . . . ? N4 Cu1 N2 C7 -147.78(14) . . . . ? N1 Cu1 N2 C7 19.54(13) . . . . ? N3 Cu1 N2 C7 -76.6(2) . . . . ? N5 Cu1 N2 C7 130.41(14) . . . . ? N4 Cu1 N3 C12 176.20(19) . . . . ? N2 Cu1 N3 C12 102.8(2) . . . . ? N1 Cu1 N3 C12 11.75(19) . . . . ? N5 Cu1 N3 C12 -109.30(18) . . . . ? N4 Cu1 N3 C16 10.82(13) . . . . ? N2 Cu1 N3 C16 -62.6(2) . . . . ? N1 Cu1 N3 C16 -153.63(13) . . . . ? N5 Cu1 N3 C16 85.32(14) . . . . ? N2 Cu1 N4 C20 -30.27(15) . . . . ? N1 Cu1 N4 C20 -84.4(3) . . . . ? N3 Cu1 N4 C20 175.05(16) . . . . ? N5 Cu1 N4 C20 50.20(15) . . . . ? N2 Cu1 N4 C17 146.54(14) . . . . ? N1 Cu1 N4 C17 92.5(3) . . . . ? N3 Cu1 N4 C17 -8.14(13) . . . . ? N5 Cu1 N4 C17 -132.99(14) . . . . ? N4 Cu1 N5 C21 132.02(16) . . . . ? N2 Cu1 N5 C21 -135.78(16) . . . . ? N1 Cu1 N5 C21 -59.56(16) . . . . ? N3 Cu1 N5 C21 58.11(17) . . . . ? N4 Cu1 N5 C25 -43.95(13) . . . . ? N2 Cu1 N5 C25 48.25(13) . . . . ? N1 Cu1 N5 C25 124.47(13) . . . . ? N3 Cu1 N5 C25 -117.86(13) . . . . ? C6 N1 C1 C2 -4.4(3) . . . . ? Cu1 N1 C1 C2 166.20(15) . . . . ? N1 C1 C2 C3 1.0(3) . . . . ? C1 C2 C3 C5 2.6(3) . . . . ? C2 C3 C5 C6 -2.7(3) . . . . ? C1 N1 C6 C5 4.3(3) . . . . ? Cu1 N1 C6 C5 -167.88(15) . . . . ? C1 N1 C6 C7 -170.03(17) . . . . ? Cu1 N1 C6 C7 17.8(2) . . . . ? C3 C5 C6 N1 -0.7(3) . . . . ? C3 C5 C6 C7 173.05(19) . . . . ? C11 N2 C7 C8 -5.4(3) . . . . ? Cu1 N2 C7 C8 170.44(15) . . . . ? C11 N2 C7 C6 168.86(17) . . . . ? Cu1 N2 C7 C6 -15.3(2) . . . . ? N1 C6 C7 N2 -2.1(2) . . . . ? C5 C6 C7 N2 -176.28(18) . . . . ? N1 C6 C7 C8 171.99(19) . . . . ? C5 C6 C7 C8 -2.2(3) . . . . ? N2 C7 C8 C9 2.0(3) . . . . ? C6 C7 C8 C9 -171.59(18) . . . . ? C7 C8 C9 C10 2.2(3) . . . . ? C8 C9 C10 C11 -3.1(3) . . . . ? C7 N2 C11 C10 4.4(3) . . . . ? Cu1 N2 C11 C10 -171.04(14) . . . . ? C7 N2 C11 C26 -172.70(17) . . . . ? Cu1 N2 C11 C26 11.8(2) . . . . ? C9 C10 C11 N2 -0.2(3) . . . . ? C9 C10 C11 C26 176.73(18) . . . . ? C16 N3 C12 C13 0.5(3) . . . . ? Cu1 N3 C12 C13 -164.22(17) . . . . ? N3 C12 C13 C14 -0.4(3) . . . . ? C12 C13 C14 C15 -0.4(3) . . . . ? C13 C14 C15 C16 1.1(3) . . . . ? C12 N3 C16 C15 0.2(3) . . . . ? Cu1 N3 C16 C15 167.36(15) . . . . ? C12 N3 C16 C17 -178.84(17) . . . . ? Cu1 N3 C16 C17 -11.7(2) . . . . ? C14 C15 C16 N3 -1.1(3) . . . . ? C14 C15 C16 C17 177.94(19) . . . . ? C20 N4 C17 C18 0.7(3) . . . . ? Cu1 N4 C17 C18 -176.21(15) . . . . ? C20 N4 C17 C16 -178.95(16) . . . . ? Cu1 N4 C17 C16 4.1(2) . . . . ? N3 C16 C17 N4 5.3(2) . . . . ? C15 C16 C17 N4 -173.75(18) . . . . ? N3 C16 C17 C18 -174.31(18) . . . . ? C15 C16 C17 C18 6.6(3) . . . . ? N4 C17 C18 C19 0.9(3) . . . . ? C16 C17 C18 C19 -179.45(18) . . . . ? C17 C18 C19 C1A -1.4(3) . . . . ? C20 C1A C19 C18 0.3(3) . . . . ? C17 N4 C20 C1A -1.8(3) . . . . ? Cu1 N4 C20 C1A 174.81(14) . . . . ? C17 N4 C20 C26 175.95(16) . . . . ? Cu1 N4 C20 C26 -7.4(2) . . . . ? C19 C1A C20 N4 1.3(3) . . . . ? C19 C1A C20 C26 -176.30(18) . . . . ? C25 N5 C21 C22 2.1(3) . . . . ? Cu1 N5 C21 C22 -173.81(15) . . . . ? N5 C21 C22 C23 -0.7(3) . . . . ? C21 C22 C23 C24 -1.2(3) . . . . ? C22 C23 C24 C25 1.5(3) . . . . ? C21 N5 C25 C24 -1.7(3) . . . . ? Cu1 N5 C25 C24 174.51(14) . . . . ? C21 N5 C25 C26 -179.41(16) . . . . ? Cu1 N5 C25 C26 -3.2(2) . . . . ? C23 C24 C25 N5 -0.1(3) . . . . ? C23 C24 C25 C26 177.54(17) . . . . ? N4 C20 C26 C27 179.31(16) . . . . ? C1A C20 C26 C27 -3.0(3) . . . . ? N4 C20 C26 C11 58.6(2) . . . . ? C1A C20 C26 C11 -123.6(2) . . . . ? N4 C20 C26 C25 -60.1(2) . . . . ? C1A C20 C26 C25 117.6(2) . . . . ? N2 C11 C26 C27 177.79(16) . . . . ? C10 C11 C26 C27 0.8(3) . . . . ? N2 C11 C26 C20 -61.0(2) . . . . ? C10 C11 C26 C20 122.0(2) . . . . ? N2 C11 C26 C25 56.2(2) . . . . ? C10 C11 C26 C25 -120.8(2) . . . . ? N5 C25 C26 C27 -177.57(16) . . . . ? C24 C25 C26 C27 4.7(2) . . . . ? N5 C25 C26 C20 62.5(2) . . . . ? C24 C25 C26 C20 -115.24(19) . . . . ? N5 C25 C26 C11 -57.1(2) . . . . ? C24 C25 C26 C11 125.17(18) . . . . ? O1 S1 C28 F2 68.69(17) . . . . ? O3 S1 C28 F2 -51.51(18) . . . . ? O2 S1 C28 F2 -170.90(15) . . . . ? O1 S1 C28 F1 -51.41(17) . . . . ? O3 S1 C28 F1 -171.61(15) . . . . ? O2 S1 C28 F1 69.01(17) . . . . ? O1 S1 C28 F3 -171.58(15) . . . . ? O3 S1 C28 F3 68.22(17) . . . . ? O2 S1 C28 F3 -51.17(17) . . . . ? O6A S3 C29 F5 -127.7(5) . . . . ? O4 S3 C29 F5 -16.3(6) . . . . ? O5A S3 C29 F5 114.0(6) . . . . ? O6A S3 C29 F4 81.4(3) . . . . ? O4 S3 C29 F4 -167.3(2) . . . . ? O5A S3 C29 F4 -37.0(3) . . . . ? O6A S3 C29 F6A -57.3(3) . . . . ? O4 S3 C29 F6A 54.1(3) . . . . ? O5A S3 C29 F6A -175.6(3) . . . . ? O6A S3 C29 F6 -11.4(4) . . . . ? O4 S3 C29 F6 99.9(3) . . . . ? O5A S3 C29 F6 -129.8(4) . . . . ? O6A S3 C29 F5A -173.1(3) . . . . ? O4 S3 C29 F5A -61.8(3) . . . . ? O5A S3 C29 F5A 68.5(3) . . . . ? O6A S3 C29 S2 179.3(7) . . . . ? O4 S3 C29 S2 -69.4(5) . . . . ? O5A S3 C29 S2 60.9(5) . . . . ? O4 S2 C29 F5 -50.3(5) . . . . ? O6 S2 C29 F5 173.2(5) . . . . ? O5 S2 C29 F5 56.0(5) . . . . ? O4 S2 C29 F4 172.9(2) . . . . ? O6 S2 C29 F4 36.5(4) . . . . ? O5 S2 C29 F4 -80.7(3) . . . . ? O4 S2 C29 F6A 19.3(4) . . . . ? O6 S2 C29 F6A -117.1(4) . . . . ? O5 S2 C29 F6A 125.7(3) . . . . ? O4 S2 C29 F6 72.4(4) . . . . ? O6 S2 C29 F6 -64.0(5) . . . . ? O5 S2 C29 F6 178.8(4) . . . . ? O4 S2 C29 F5A -89.3(2) . . . . ? O6 S2 C29 F5A 134.2(3) . . . . ? O5 S2 C29 F5A 17.1(3) . . . . ? O4 S2 C29 S3 83.5(5) . . . . ? O6 S2 C29 S3 -52.9(6) . . . . ? O5 S2 C29 S3 -170.1(7) . . . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.42 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.476 _refine_diff_density_min -0.512 _refine_diff_density_rms 0.063 _database_code_depnum_ccdc_archive 'CCDC 943490' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Zn(bpy2py)OTf)OTf*CH3CN' _chemical_melting_point ? _chemical_formula_moiety 'C29 H21 Zn F6 N5 O6 S2' _chemical_formula_sum 'C31 H24 F6 N6 O6 S2 Zn' _chemical_formula_weight 820.05 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' S S 0.1246 0.1234 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.8290(3) _cell_length_b 12.2969(3) _cell_length_c 13.4196(4) _cell_angle_alpha 92.8740(10) _cell_angle_beta 91.8050(10) _cell_angle_gamma 91.2320(10) _cell_volume 1618.70(8) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9956 _cell_measurement_theta_min 2.1923 _cell_measurement_theta_max 25.3584 _exptl_crystal_description block _exptl_crystal_colour white _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.682 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 832 _exptl_absorpt_coefficient_mu 0.978 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7646 _exptl_absorpt_correction_T_max 0.8592 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'microfocus sealed tube' _diffrn_radiation_monochromator 'QUAZAR multilayer mirrors' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_reflns_number 25512 _diffrn_reflns_av_R_equivalents 0.0223 _diffrn_reflns_av_sigmaI/netI 0.0181 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 25.36 _reflns_number_total 5878 _reflns_number_gt 5558 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v. 2009.1' _computing_cell_refinement 'Bruker APEX2 v. 2009.1' _computing_data_reduction 'Bruker APEX2 v. 2009.1' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics DIAMOND _computing_publication_material CIFTAB _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^)+(0.0387P)^2^+1.6198P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5878 _refine_ls_number_parameters 471 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0303 _refine_ls_R_factor_gt 0.0284 _refine_ls_wR_factor_ref 0.0798 _refine_ls_wR_factor_gt 0.0786 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.085 _refine_ls_shift/su_max 0.002 _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 0.01437(2) 0.709265(17) 0.240712(15) 0.01408(8) Uani 1 1 d . . . S1 S -0.25472(5) 0.75539(4) 0.37126(4) 0.01671(12) Uani 1 1 d . . . S2 S 0.45720(6) 0.73058(5) 0.77668(4) 0.02935(14) Uani 1 1 d . . . F1 F -0.43041(13) 0.89924(11) 0.43017(10) 0.0303(3) Uani 1 1 d . . . F2 F -0.48732(13) 0.81305(11) 0.29108(11) 0.0332(3) Uani 1 1 d . . . F3 F -0.32888(13) 0.93829(10) 0.29598(10) 0.0279(3) Uani 1 1 d . . . F4 F 0.6435(2) 0.88671(15) 0.80000(15) 0.0624(5) Uani 1 1 d . . . F5 F 0.70992(14) 0.74358(14) 0.72012(11) 0.0405(4) Uani 1 1 d . . . F6 F 0.57571(18) 0.85258(16) 0.64772(13) 0.0576(5) Uani 1 1 d . . . O1 O -0.20516(15) 0.72605(12) 0.27174(10) 0.0199(3) Uani 1 1 d . . . O2 O -0.15504(14) 0.81350(12) 0.43600(11) 0.0220(3) Uani 1 1 d . . . O3 O -0.33073(15) 0.66956(12) 0.41452(11) 0.0228(3) Uani 1 1 d . . . O4 O 0.50781(18) 0.69130(17) 0.86960(13) 0.0395(4) Uani 1 1 d . . . O5 O 0.3523(2) 0.80921(19) 0.78371(16) 0.0545(6) Uani 1 1 d . . . O6 O 0.43445(18) 0.64740(15) 0.69758(14) 0.0382(4) Uani 1 1 d . . . N1 N 0.19199(17) 0.62997(13) 0.18902(12) 0.0158(3) Uani 1 1 d . . . N1S N 0.2586(4) 0.8894(3) 0.0632(3) 0.0735(9) Uani 1 1 d . . . N2 N -0.02995(18) 0.67081(14) 0.08689(12) 0.0178(4) Uani 1 1 d . . . N3 N 0.14961(16) 0.77419(13) 0.35399(12) 0.0149(3) Uani 1 1 d . . . N4 N 0.00315(18) 0.88382(14) 0.22807(13) 0.0188(4) Uani 1 1 d . . . N5 N 0.00629(16) 0.56361(13) 0.32272(11) 0.0145(3) Uani 1 1 d . . . C1 C 0.2919(2) 0.60007(16) 0.25139(14) 0.0154(4) Uani 1 1 d . . . C1S C 0.3761(4) 0.8885(3) 0.0617(3) 0.0608(9) Uani 1 1 d . . . C2 C 0.4185(2) 0.57329(17) 0.21521(16) 0.0207(4) Uani 1 1 d . . . H2 H 0.4895 0.5509 0.2587 0.025 Uiso 1 1 calc R . . C2S C 0.5241(4) 0.8845(4) 0.0647(3) 0.0766(11) Uani 1 1 d . . . H2SA H 0.5567 0.8778 -0.0036 0.115 Uiso 1 1 calc R . . H2SB H 0.5530 0.8215 0.1013 0.115 Uiso 1 1 calc R . . H2SC H 0.5622 0.9514 0.0983 0.115 Uiso 1 1 calc R . . C3 C 0.4383(2) 0.58019(18) 0.11369(17) 0.0249(5) Uani 1 1 d . . . H3 H 0.5256 0.5662 0.0880 0.030 Uiso 1 1 calc R . . C4 C 0.3331(2) 0.60707(18) 0.04941(16) 0.0232(5) Uani 1 1 d . . . H4 H 0.3458 0.6099 -0.0203 0.028 Uiso 1 1 calc R . . C5 C 0.2081(2) 0.62982(16) 0.09027(15) 0.0182(4) Uani 1 1 d . . . C6 C 0.0800(2) 0.64836(16) 0.03204(15) 0.0182(4) Uani 1 1 d . . . C7 C 0.0689(2) 0.63651(18) -0.07157(16) 0.0242(5) Uani 1 1 d . . . H7 H 0.1472 0.6229 -0.1096 0.029 Uiso 1 1 calc R . . C8 C -0.0574(3) 0.64480(19) -0.11859(16) 0.0272(5) Uani 1 1 d . . . H8 H -0.0664 0.6371 -0.1893 0.033 Uiso 1 1 calc R . . C9 C -0.1706(2) 0.66435(18) -0.06222(16) 0.0253(5) Uani 1 1 d . . . H9 H -0.2587 0.6682 -0.0930 0.030 Uiso 1 1 calc R . . C10 C -0.1519(2) 0.67806(18) 0.04032(16) 0.0216(4) Uani 1 1 d . . . H10 H -0.2288 0.6933 0.0794 0.026 Uiso 1 1 calc R . . C11 C 0.23440(19) 0.71250(16) 0.40575(14) 0.0153(4) Uani 1 1 d . . . C12 C 0.3017(2) 0.75435(17) 0.49206(15) 0.0183(4) Uani 1 1 d . . . H12 H 0.3627 0.7108 0.5282 0.022 Uiso 1 1 calc R . . C13 C 0.2784(2) 0.86106(18) 0.52477(16) 0.0220(4) Uani 1 1 d . . . H13 H 0.3189 0.8896 0.5861 0.026 Uiso 1 1 calc R . . C14 C 0.1965(2) 0.92577(17) 0.46829(16) 0.0211(4) Uani 1 1 d . . . H14 H 0.1828 0.9998 0.4884 0.025 Uiso 1 1 calc R . . C15 C 0.1346(2) 0.87977(16) 0.38133(15) 0.0169(4) Uani 1 1 d . . . C16 C 0.0528(2) 0.94193(17) 0.30937(15) 0.0180(4) Uani 1 1 d . . . C17 C 0.0319(2) 1.05322(18) 0.32251(17) 0.0243(5) Uani 1 1 d . . . H17 H 0.0676 1.0931 0.3803 0.029 Uiso 1 1 calc R . . C18 C -0.0418(2) 1.10471(18) 0.24999(18) 0.0289(5) Uani 1 1 d . . . H18 H -0.0593 1.1802 0.2584 0.035 Uiso 1 1 calc R . . C19 C -0.0899(2) 1.04607(19) 0.16526(18) 0.0285(5) Uani 1 1 d . . . H19 H -0.1388 1.0804 0.1139 0.034 Uiso 1 1 calc R . . C20 C -0.0647(2) 0.93583(18) 0.15739(16) 0.0245(5) Uani 1 1 d . . . H20 H -0.0970 0.8951 0.0991 0.029 Uiso 1 1 calc R . . C21 C 0.12093(19) 0.52617(16) 0.36676(13) 0.0138(4) Uani 1 1 d . . . C22 C 0.1194(2) 0.42704(16) 0.41199(14) 0.0159(4) Uani 1 1 d . . . H22 H 0.1994 0.4028 0.4447 0.019 Uiso 1 1 calc R . . C23 C 0.0009(2) 0.36340(16) 0.40941(14) 0.0175(4) Uani 1 1 d . . . H23 H -0.0011 0.2958 0.4407 0.021 Uiso 1 1 calc R . . C24 C -0.1146(2) 0.39974(16) 0.36061(14) 0.0176(4) Uani 1 1 d . . . H24 H -0.1962 0.3567 0.3554 0.021 Uiso 1 1 calc R . . C25 C -0.1076(2) 0.50020(16) 0.31990(14) 0.0158(4) Uani 1 1 d . . . H25 H -0.1873 0.5263 0.2881 0.019 Uiso 1 1 calc R . . C26 C 0.25446(19) 0.59527(16) 0.36239(14) 0.0149(4) Uani 1 1 d . . . C27 C 0.3700(2) 0.54229(17) 0.42119(15) 0.0186(4) Uani 1 1 d . . . H27A H 0.3876 0.4703 0.3902 0.028 Uiso 1 1 calc R . . H27B H 0.3433 0.5345 0.4903 0.028 Uiso 1 1 calc R . . H27C H 0.4526 0.5882 0.4205 0.028 Uiso 1 1 calc R . . C28 C -0.3826(2) 0.85716(17) 0.34540(17) 0.0223(5) Uani 1 1 d . . . C29 C 0.6031(3) 0.8079(2) 0.73395(18) 0.0337(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.01511(13) 0.01442(13) 0.01265(12) 0.00007(9) -0.00029(9) 0.00125(9) S1 0.0142(2) 0.0163(2) 0.0197(2) 0.00079(19) 0.00106(19) 0.00101(19) S2 0.0212(3) 0.0401(3) 0.0279(3) 0.0087(2) 0.0039(2) 0.0087(2) F1 0.0248(7) 0.0272(7) 0.0392(8) -0.0036(6) 0.0113(6) 0.0051(5) F2 0.0223(7) 0.0275(7) 0.0487(8) -0.0013(6) -0.0131(6) 0.0019(5) F3 0.0302(7) 0.0193(6) 0.0348(7) 0.0060(5) 0.0034(6) 0.0032(5) F4 0.0731(13) 0.0476(11) 0.0646(12) -0.0114(9) 0.0079(10) -0.0164(9) F5 0.0247(7) 0.0589(10) 0.0389(8) 0.0078(7) 0.0052(6) 0.0058(7) F6 0.0501(10) 0.0751(13) 0.0511(10) 0.0396(9) 0.0013(8) 0.0016(9) O1 0.0207(7) 0.0188(7) 0.0205(7) 0.0008(6) 0.0021(6) 0.0035(6) O2 0.0175(7) 0.0243(8) 0.0239(8) -0.0008(6) 0.0003(6) -0.0010(6) O3 0.0193(7) 0.0217(8) 0.0279(8) 0.0055(6) 0.0025(6) -0.0010(6) O4 0.0319(9) 0.0604(13) 0.0280(9) 0.0155(8) 0.0052(7) 0.0033(9) O5 0.0391(11) 0.0666(14) 0.0608(13) 0.0107(11) 0.0144(10) 0.0288(10) O6 0.0293(9) 0.0446(11) 0.0406(10) 0.0055(8) -0.0073(8) 0.0014(8) N1 0.0179(8) 0.0139(8) 0.0156(8) -0.0001(6) 0.0019(7) -0.0006(7) N1S 0.072(2) 0.066(2) 0.083(2) 0.0048(17) 0.0045(18) -0.0001(17) N2 0.0216(9) 0.0159(9) 0.0158(8) 0.0007(7) 0.0001(7) 0.0013(7) N3 0.0140(8) 0.0146(8) 0.0159(8) 0.0002(6) 0.0028(6) -0.0016(6) N4 0.0200(9) 0.0171(9) 0.0193(9) 0.0019(7) 0.0014(7) 0.0010(7) N5 0.0148(8) 0.0159(8) 0.0125(8) -0.0015(6) 0.0009(6) 0.0006(6) C1 0.0165(10) 0.0121(9) 0.0175(10) 0.0000(7) 0.0014(8) -0.0019(7) C1S 0.061(2) 0.060(2) 0.059(2) -0.0095(17) -0.0007(17) -0.0018(17) C2 0.0184(10) 0.0201(11) 0.0238(11) 0.0007(8) 0.0017(8) 0.0014(8) C2S 0.073(3) 0.097(3) 0.060(2) 0.008(2) 0.006(2) 0.005(2) C3 0.0210(11) 0.0257(12) 0.0284(11) 0.0001(9) 0.0090(9) 0.0028(9) C4 0.0272(11) 0.0237(11) 0.0191(10) 0.0012(8) 0.0077(9) 0.0019(9) C5 0.0237(11) 0.0141(10) 0.0168(10) -0.0001(8) 0.0030(8) 0.0000(8) C6 0.0240(11) 0.0133(10) 0.0175(10) 0.0018(8) 0.0016(8) 0.0001(8) C7 0.0318(12) 0.0248(12) 0.0164(10) 0.0010(9) 0.0043(9) 0.0017(9) C8 0.0388(13) 0.0269(12) 0.0154(10) 0.0006(9) -0.0031(9) 0.0014(10) C9 0.0295(12) 0.0237(12) 0.0222(11) 0.0015(9) -0.0072(9) 0.0010(9) C10 0.0222(11) 0.0224(11) 0.0199(10) 0.0009(8) -0.0021(8) 0.0013(8) C11 0.0140(9) 0.0163(10) 0.0158(9) 0.0013(8) 0.0035(7) -0.0022(8) C12 0.0165(10) 0.0207(11) 0.0175(10) 0.0023(8) 0.0006(8) -0.0022(8) C13 0.0213(11) 0.0244(11) 0.0194(10) -0.0032(8) -0.0007(8) -0.0050(9) C14 0.0208(10) 0.0177(10) 0.0242(11) -0.0045(8) 0.0020(9) -0.0022(8) C15 0.0148(9) 0.0171(10) 0.0187(10) -0.0007(8) 0.0045(8) -0.0022(8) C16 0.0156(10) 0.0172(10) 0.0214(10) 0.0010(8) 0.0053(8) -0.0006(8) C17 0.0260(11) 0.0187(11) 0.0279(11) -0.0010(9) 0.0017(9) -0.0001(9) C18 0.0328(13) 0.0168(11) 0.0376(13) 0.0034(10) 0.0033(10) 0.0043(9) C19 0.0318(12) 0.0241(12) 0.0304(12) 0.0083(10) -0.0005(10) 0.0056(10) C20 0.0285(12) 0.0218(11) 0.0232(11) 0.0030(9) -0.0018(9) 0.0012(9) C21 0.0151(9) 0.0154(10) 0.0106(9) -0.0025(7) 0.0016(7) 0.0011(8) C22 0.0174(10) 0.0171(10) 0.0129(9) -0.0008(8) 0.0006(7) 0.0027(8) C23 0.0229(10) 0.0142(10) 0.0153(9) 0.0001(8) 0.0029(8) -0.0002(8) C24 0.0183(10) 0.0171(10) 0.0171(10) -0.0024(8) 0.0034(8) -0.0027(8) C25 0.0147(9) 0.0181(10) 0.0142(9) -0.0028(8) 0.0006(7) 0.0010(8) C26 0.0131(9) 0.0156(10) 0.0163(9) 0.0012(8) 0.0010(7) -0.0002(7) C27 0.0143(10) 0.0211(11) 0.0204(10) 0.0030(8) -0.0017(8) 0.0012(8) C28 0.0188(10) 0.0186(11) 0.0293(11) 0.0003(9) -0.0002(9) 0.0002(8) C29 0.0337(13) 0.0388(14) 0.0293(12) 0.0072(11) 0.0019(10) 0.0045(11) _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 N3 2.1025(16) . ? Zn1 N2 2.1239(17) . ? Zn1 N1 2.1358(17) . ? Zn1 N5 2.1500(17) . ? Zn1 N4 2.1666(17) . ? Zn1 O1 2.2224(14) . ? S1 O3 1.4367(16) . ? S1 O2 1.4420(15) . ? S1 O1 1.4667(15) . ? S1 C28 1.830(2) . ? S2 O5 1.4307(19) . ? S2 O4 1.4378(18) . ? S2 O6 1.445(2) . ? S2 C29 1.827(3) . ? F1 C28 1.330(3) . ? F2 C28 1.332(3) . ? F3 C28 1.334(3) . ? F4 C29 1.325(3) . ? F5 C29 1.340(3) . ? F6 C29 1.328(3) . ? N1 C1 1.339(3) . ? N1 C5 1.340(3) . ? N1S C1S 1.156(5) . ? N2 C10 1.341(3) . ? N2 C6 1.352(3) . ? N3 C11 1.340(3) . ? N3 C15 1.344(3) . ? N4 C20 1.339(3) . ? N4 C16 1.346(3) . ? N5 C25 1.349(3) . ? N5 C21 1.356(3) . ? C1 C2 1.390(3) . ? C1 C26 1.549(3) . ? C1S C2S 1.456(5) . ? C2 C3 1.389(3) . ? C2 H2 0.9500 . ? C2S H2SA 0.9800 . ? C2S H2SB 0.9800 . ? C2S H2SC 0.9800 . ? C3 C4 1.382(3) . ? C3 H3 0.9500 . ? C4 C5 1.389(3) . ? C4 H4 0.9500 . ? C5 C6 1.489(3) . ? C6 C7 1.391(3) . ? C7 C8 1.383(3) . ? C7 H7 0.9500 . ? C8 C9 1.384(3) . ? C8 H8 0.9500 . ? C9 C10 1.384(3) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.386(3) . ? C11 C26 1.546(3) . ? C12 C13 1.389(3) . ? C12 H12 0.9500 . ? C13 C14 1.381(3) . ? C13 H13 0.9500 . ? C14 C15 1.388(3) . ? C14 H14 0.9500 . ? C15 C16 1.488(3) . ? C16 C17 1.392(3) . ? C17 C18 1.382(3) . ? C17 H17 0.9500 . ? C18 C19 1.380(3) . ? C18 H18 0.9500 . ? C19 C20 1.383(3) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C22 1.389(3) . ? C21 C26 1.552(3) . ? C22 C23 1.388(3) . ? C22 H22 0.9500 . ? C23 C24 1.386(3) . ? C23 H23 0.9500 . ? C24 C25 1.377(3) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C27 1.537(3) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? 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 N3 Zn1 N2 149.50(7) . . ? N3 Zn1 N1 83.18(6) . . ? N2 Zn1 N1 75.60(6) . . ? N3 Zn1 N5 86.96(6) . . ? N2 Zn1 N5 109.94(6) . . ? N1 Zn1 N5 79.47(6) . . ? N3 Zn1 N4 75.96(6) . . ? N2 Zn1 N4 94.85(6) . . ? N1 Zn1 N4 118.07(6) . . ? N5 Zn1 N4 153.08(6) . . ? N3 Zn1 O1 115.15(6) . . ? N2 Zn1 O1 91.71(6) . . ? N1 Zn1 O1 156.50(6) . . ? N5 Zn1 O1 86.65(6) . . ? N4 Zn1 O1 82.15(6) . . ? O3 S1 O2 116.38(9) . . ? O3 S1 O1 113.90(9) . . ? O2 S1 O1 113.68(9) . . ? O3 S1 C28 103.91(9) . . ? O2 S1 C28 104.08(9) . . ? O1 S1 C28 102.76(9) . . ? O5 S2 O4 116.03(12) . . ? O5 S2 O6 114.39(13) . . ? O4 S2 O6 114.70(12) . . ? O5 S2 C29 103.76(13) . . ? O4 S2 C29 102.68(11) . . ? O6 S2 C29 102.77(11) . . ? S1 O1 Zn1 123.02(8) . . ? C1 N1 C5 121.55(17) . . ? C1 N1 Zn1 122.32(13) . . ? C5 N1 Zn1 115.09(13) . . ? C10 N2 C6 119.06(17) . . ? C10 N2 Zn1 125.82(14) . . ? C6 N2 Zn1 114.74(13) . . ? C11 N3 C15 120.59(17) . . ? C11 N3 Zn1 122.80(13) . . ? C15 N3 Zn1 116.07(13) . . ? C20 N4 C16 118.62(18) . . ? C20 N4 Zn1 126.87(15) . . ? C16 N4 Zn1 113.63(13) . . ? C25 N5 C21 118.49(17) . . ? C25 N5 Zn1 120.64(13) . . ? C21 N5 Zn1 120.26(13) . . ? N1 C1 C2 120.33(18) . . ? N1 C1 C26 115.69(17) . . ? C2 C1 C26 123.96(18) . . ? N1S C1S C2S 177.0(4) . . ? C3 C2 C1 118.1(2) . . ? C3 C2 H2 120.9 . . ? C1 C2 H2 120.9 . . ? C1S C2S H2SA 109.5 . . ? C1S C2S H2SB 109.5 . . ? H2SA C2S H2SB 109.5 . . ? C1S C2S H2SC 109.5 . . ? H2SA C2S H2SC 109.5 . . ? H2SB C2S H2SC 109.5 . . ? C4 C3 C2 121.0(2) . . ? C4 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? C3 C4 C5 117.69(19) . . ? C3 C4 H4 121.2 . . ? C5 C4 H4 121.2 . . ? N1 C5 C4 121.01(19) . . ? N1 C5 C6 113.67(18) . . ? C4 C5 C6 125.19(18) . . ? N2 C6 C7 121.00(19) . . ? N2 C6 C5 115.49(17) . . ? C7 C6 C5 123.37(19) . . ? C8 C7 C6 119.2(2) . . ? C8 C7 H7 120.4 . . ? C6 C7 H7 120.4 . . ? C7 C8 C9 119.7(2) . . ? C7 C8 H8 120.1 . . ? C9 C8 H8 120.1 . . ? C8 C9 C10 118.0(2) . . ? C8 C9 H9 121.0 . . ? C10 C9 H9 121.0 . . ? N2 C10 C9 122.9(2) . . ? N2 C10 H10 118.6 . . ? C9 C10 H10 118.6 . . ? N3 C11 C12 120.70(18) . . ? N3 C11 C26 116.41(17) . . ? C12 C11 C26 122.88(18) . . ? C11 C12 C13 118.81(19) . . ? C11 C12 H12 120.6 . . ? C13 C12 H12 120.6 . . ? C14 C13 C12 120.08(19) . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C13 C14 C15 118.21(19) . . ? C13 C14 H14 120.9 . . ? C15 C14 H14 120.9 . . ? N3 C15 C14 121.33(19) . . ? N3 C15 C16 114.69(17) . . ? C14 C15 C16 123.93(19) . . ? N4 C16 C17 121.60(19) . . ? N4 C16 C15 115.43(17) . . ? C17 C16 C15 122.93(19) . . ? C18 C17 C16 118.8(2) . . ? C18 C17 H17 120.6 . . ? C16 C17 H17 120.6 . . ? C19 C18 C17 119.8(2) . . ? C19 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? C18 C19 C20 118.0(2) . . ? C18 C19 H19 121.0 . . ? C20 C19 H19 121.0 . . ? N4 C20 C19 123.1(2) . . ? N4 C20 H20 118.5 . . ? C19 C20 H20 118.5 . . ? N5 C21 C22 120.68(18) . . ? N5 C21 C26 118.26(17) . . ? C22 C21 C26 121.04(17) . . ? C23 C22 C21 120.02(18) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C24 C23 C22 119.15(19) . . ? C24 C23 H23 120.4 . . ? C22 C23 H23 120.4 . . ? C25 C24 C23 117.97(19) . . ? C25 C24 H24 121.0 . . ? C23 C24 H24 121.0 . . ? N5 C25 C24 123.60(18) . . ? N5 C25 H25 118.2 . . ? C24 C25 H25 118.2 . . ? C27 C26 C11 109.56(16) . . ? C27 C26 C1 109.61(16) . . ? C11 C26 C1 108.89(15) . . ? C27 C26 C21 110.15(16) . . ? C11 C26 C21 110.74(15) . . ? C1 C26 C21 107.86(15) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? F1 C28 F2 107.87(17) . . ? F1 C28 F3 108.08(17) . . ? F2 C28 F3 108.49(18) . . ? F1 C28 S1 110.39(15) . . ? F2 C28 S1 111.09(14) . . ? F3 C28 S1 110.81(14) . . ? F4 C29 F6 108.1(2) . . ? F4 C29 F5 106.8(2) . . ? F6 C29 F5 107.1(2) . . ? F4 C29 S2 111.75(18) . . ? F6 C29 S2 111.92(18) . . ? F5 C29 S2 110.96(18) . . ? 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 O3 S1 O1 Zn1 -112.85(10) . . . . ? O2 S1 O1 Zn1 23.61(13) . . . . ? C28 S1 O1 Zn1 135.43(10) . . . . ? N3 Zn1 O1 S1 -14.16(12) . . . . ? N2 Zn1 O1 S1 -179.23(10) . . . . ? N1 Zn1 O1 S1 124.49(14) . . . . ? N5 Zn1 O1 S1 70.89(10) . . . . ? N4 Zn1 O1 S1 -84.57(10) . . . . ? N3 Zn1 N1 C1 31.67(15) . . . . ? N2 Zn1 N1 C1 -170.42(16) . . . . ? N5 Zn1 N1 C1 -56.48(15) . . . . ? N4 Zn1 N1 C1 101.75(16) . . . . ? O1 Zn1 N1 C1 -111.30(18) . . . . ? N3 Zn1 N1 C5 -136.87(15) . . . . ? N2 Zn1 N1 C5 21.03(14) . . . . ? N5 Zn1 N1 C5 134.97(15) . . . . ? N4 Zn1 N1 C5 -66.79(15) . . . . ? O1 Zn1 N1 C5 80.2(2) . . . . ? N3 Zn1 N2 C10 -143.34(17) . . . . ? N1 Zn1 N2 C10 169.29(18) . . . . ? N5 Zn1 N2 C10 96.38(17) . . . . ? N4 Zn1 N2 C10 -72.95(17) . . . . ? O1 Zn1 N2 C10 9.32(17) . . . . ? N3 Zn1 N2 C6 29.5(2) . . . . ? N1 Zn1 N2 C6 -17.91(14) . . . . ? N5 Zn1 N2 C6 -90.82(15) . . . . ? N4 Zn1 N2 C6 99.85(14) . . . . ? O1 Zn1 N2 C6 -177.88(14) . . . . ? N2 Zn1 N3 C11 -95.03(18) . . . . ? N1 Zn1 N3 C11 -49.16(15) . . . . ? N5 Zn1 N3 C11 30.59(15) . . . . ? N4 Zn1 N3 C11 -170.39(16) . . . . ? O1 Zn1 N3 C11 115.45(14) . . . . ? N2 Zn1 N3 C15 93.40(17) . . . . ? N1 Zn1 N3 C15 139.27(14) . . . . ? N5 Zn1 N3 C15 -140.98(14) . . . . ? N4 Zn1 N3 C15 18.05(13) . . . . ? O1 Zn1 N3 C15 -56.12(15) . . . . ? N3 Zn1 N4 C20 174.10(19) . . . . ? N2 Zn1 N4 C20 23.63(18) . . . . ? N1 Zn1 N4 C20 99.89(18) . . . . ? N5 Zn1 N4 C20 -133.75(18) . . . . ? O1 Zn1 N4 C20 -67.43(18) . . . . ? N3 Zn1 N4 C16 -16.93(14) . . . . ? N2 Zn1 N4 C16 -167.40(14) . . . . ? N1 Zn1 N4 C16 -91.14(15) . . . . ? N5 Zn1 N4 C16 35.2(2) . . . . ? O1 Zn1 N4 C16 101.54(14) . . . . ? N3 Zn1 N5 C25 148.94(14) . . . . ? N2 Zn1 N5 C25 -57.10(15) . . . . ? N1 Zn1 N5 C25 -127.44(15) . . . . ? N4 Zn1 N5 C25 98.84(18) . . . . ? O1 Zn1 N5 C25 33.50(14) . . . . ? N3 Zn1 N5 C21 -40.17(14) . . . . ? N2 Zn1 N5 C21 113.79(14) . . . . ? N1 Zn1 N5 C21 43.45(14) . . . . ? N4 Zn1 N5 C21 -90.26(19) . . . . ? O1 Zn1 N5 C21 -155.60(14) . . . . ? C5 N1 C1 C2 3.4(3) . . . . ? Zn1 N1 C1 C2 -164.42(15) . . . . ? C5 N1 C1 C26 -175.17(17) . . . . ? Zn1 N1 C1 C26 17.0(2) . . . . ? N1 C1 C2 C3 1.0(3) . . . . ? C26 C1 C2 C3 179.43(19) . . . . ? C1 C2 C3 C4 -3.5(3) . . . . ? C2 C3 C4 C5 1.7(3) . . . . ? C1 N1 C5 C4 -5.3(3) . . . . ? Zn1 N1 C5 C4 163.35(16) . . . . ? C1 N1 C5 C6 170.83(17) . . . . ? Zn1 N1 C5 C6 -20.5(2) . . . . ? C3 C4 C5 N1 2.6(3) . . . . ? C3 C4 C5 C6 -173.0(2) . . . . ? C10 N2 C6 C7 2.2(3) . . . . ? Zn1 N2 C6 C7 -171.11(16) . . . . ? C10 N2 C6 C5 -173.58(18) . . . . ? Zn1 N2 C6 C5 13.1(2) . . . . ? N1 C5 C6 N2 4.9(3) . . . . ? C4 C5 C6 N2 -179.1(2) . . . . ? N1 C5 C6 C7 -170.77(19) . . . . ? C4 C5 C6 C7 5.2(3) . . . . ? N2 C6 C7 C8 -1.9(3) . . . . ? C5 C6 C7 C8 173.6(2) . . . . ? C6 C7 C8 C9 -0.2(3) . . . . ? C7 C8 C9 C10 1.8(3) . . . . ? C6 N2 C10 C9 -0.5(3) . . . . ? Zn1 N2 C10 C9 172.01(16) . . . . ? C8 C9 C10 N2 -1.5(3) . . . . ? C15 N3 C11 C12 4.1(3) . . . . ? Zn1 N3 C11 C12 -167.09(14) . . . . ? C15 N3 C11 C26 -174.44(17) . . . . ? Zn1 N3 C11 C26 14.4(2) . . . . ? N3 C11 C12 C13 0.8(3) . . . . ? C26 C11 C12 C13 179.28(18) . . . . ? C11 C12 C13 C14 -4.2(3) . . . . ? C12 C13 C14 C15 2.7(3) . . . . ? C11 N3 C15 C14 -5.7(3) . . . . ? Zn1 N3 C15 C14 166.05(15) . . . . ? C11 N3 C15 C16 171.78(17) . . . . ? Zn1 N3 C15 C16 -16.5(2) . . . . ? C13 C14 C15 N3 2.3(3) . . . . ? C13 C14 C15 C16 -174.99(19) . . . . ? C20 N4 C16 C17 1.9(3) . . . . ? Zn1 N4 C16 C17 -168.10(16) . . . . ? C20 N4 C16 C15 -176.18(18) . . . . ? Zn1 N4 C16 C15 13.9(2) . . . . ? N3 C15 C16 N4 1.2(3) . . . . ? C14 C15 C16 N4 178.63(19) . . . . ? N3 C15 C16 C17 -176.80(19) . . . . ? C14 C15 C16 C17 0.6(3) . . . . ? N4 C16 C17 C18 0.0(3) . . . . ? C15 C16 C17 C18 177.9(2) . . . . ? C16 C17 C18 C19 -1.7(3) . . . . ? C17 C18 C19 C20 1.5(4) . . . . ? C16 N4 C20 C19 -2.1(3) . . . . ? Zn1 N4 C20 C19 166.41(17) . . . . ? C18 C19 C20 N4 0.4(4) . . . . ? C25 N5 C21 C22 -2.9(3) . . . . ? Zn1 N5 C21 C22 -174.04(13) . . . . ? C25 N5 C21 C26 175.22(16) . . . . ? Zn1 N5 C21 C26 4.1(2) . . . . ? N5 C21 C22 C23 2.3(3) . . . . ? C26 C21 C22 C23 -175.87(17) . . . . ? C21 C22 C23 C24 0.5(3) . . . . ? C22 C23 C24 C25 -2.4(3) . . . . ? C21 N5 C25 C24 0.9(3) . . . . ? Zn1 N5 C25 C24 171.99(14) . . . . ? C23 C24 C25 N5 1.8(3) . . . . ? N3 C11 C26 C27 171.40(16) . . . . ? C12 C11 C26 C27 -7.1(3) . . . . ? N3 C11 C26 C1 51.5(2) . . . . ? C12 C11 C26 C1 -126.99(19) . . . . ? N3 C11 C26 C21 -66.9(2) . . . . ? C12 C11 C26 C21 114.6(2) . . . . ? N1 C1 C26 C27 170.78(17) . . . . ? C2 C1 C26 C27 -7.7(3) . . . . ? N1 C1 C26 C11 -69.4(2) . . . . ? C2 C1 C26 C11 112.1(2) . . . . ? N1 C1 C26 C21 50.8(2) . . . . ? C2 C1 C26 C21 -127.7(2) . . . . ? N5 C21 C26 C27 176.92(16) . . . . ? C22 C21 C26 C27 -4.9(2) . . . . ? N5 C21 C26 C11 55.6(2) . . . . ? C22 C21 C26 C11 -126.27(19) . . . . ? N5 C21 C26 C1 -63.5(2) . . . . ? C22 C21 C26 C1 114.67(19) . . . . ? O3 S1 C28 F1 66.11(16) . . . . ? O2 S1 C28 F1 -56.17(16) . . . . ? O1 S1 C28 F1 -174.94(14) . . . . ? O3 S1 C28 F2 -53.51(17) . . . . ? O2 S1 C28 F2 -175.78(15) . . . . ? O1 S1 C28 F2 65.45(17) . . . . ? O3 S1 C28 F3 -174.19(14) . . . . ? O2 S1 C28 F3 63.54(16) . . . . ? O1 S1 C28 F3 -55.24(16) . . . . ? O5 S2 C29 F4 63.2(2) . . . . ? O4 S2 C29 F4 -58.0(2) . . . . ? O6 S2 C29 F4 -177.37(18) . . . . ? O5 S2 C29 F6 -58.2(2) . . . . ? O4 S2 C29 F6 -179.38(19) . . . . ? O6 S2 C29 F6 61.3(2) . . . . ? O5 S2 C29 F5 -177.75(17) . . . . ? O4 S2 C29 F5 61.03(19) . . . . ? O6 S2 C29 F5 -58.32(19) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.36 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.612 _refine_diff_density_min -0.539 _refine_diff_density_rms 0.062 _database_code_depnum_ccdc_archive 'CCDC 943491' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Co(bpy2pyCF3)OTf)OTf*5CH3CN' _chemical_melting_point ? _chemical_formula_moiety 'C30 H20 Co F9 N5 O6 S2' _chemical_formula_sum 'C32 H23 Co F9 N6 O6 S2' _chemical_formula_weight 881.61 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.1178(2) _cell_length_b 10.1848(2) _cell_length_c 18.5692(4) _cell_angle_alpha 93.0600(10) _cell_angle_beta 101.8380(10) _cell_angle_gamma 106.5480(10) _cell_volume 1782.45(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9945 _cell_measurement_theta_min 2.1929 _cell_measurement_theta_max 25.3853 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.643 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 890 _exptl_absorpt_coefficient_mu 0.699 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8176 _exptl_absorpt_correction_T_max 0.9334 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'microfocus sealed tube' _diffrn_radiation_monochromator 'QUAZAR multilayer mirrors' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_reflns_number 20307 _diffrn_reflns_av_R_equivalents 0.0252 _diffrn_reflns_av_sigmaI/netI 0.0295 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 25.40 _reflns_number_total 6432 _reflns_number_gt 5647 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v. 2009.1' _computing_cell_refinement 'Bruker APEX2 v. 2009.1' _computing_data_reduction 'Bruker APEX2 v. 2009.1' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics DIAMOND _computing_publication_material CIFTAB _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^)+(0.0319P)^2^+2.0142P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6432 _refine_ls_number_parameters 507 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0397 _refine_ls_R_factor_gt 0.0332 _refine_ls_wR_factor_ref 0.0817 _refine_ls_wR_factor_gt 0.0783 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _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 Co1 Co 0.42787(3) 0.50577(3) 0.251318(16) 0.01104(8) Uani 1 1 d . . . S1 S 0.32096(5) 0.70327(6) 0.13278(3) 0.01362(12) Uani 1 1 d . . . S2 S -0.19649(6) 0.22444(6) 0.59623(3) 0.01911(14) Uani 1 1 d . . . F1 F -0.24943(16) 0.12712(18) 0.28159(11) 0.0475(5) Uani 1 1 d . . . F2 F -0.27696(17) 0.32947(18) 0.28521(12) 0.0526(5) Uani 1 1 d . . . F3 F -0.30483(16) 0.21405(19) 0.18172(11) 0.0497(5) Uani 1 1 d . . . F4 F 0.45597(14) 0.96535(14) 0.17181(8) 0.0250(3) Uani 1 1 d . . . F5 F 0.41259(15) 0.90060(15) 0.05444(8) 0.0286(3) Uani 1 1 d . . . F6 F 0.57797(13) 0.84943(14) 0.12976(8) 0.0245(3) Uani 1 1 d . . . F7 F 0.0013(3) 0.1261(3) 0.56958(15) 0.0920(9) Uani 1 1 d . . . F8 F 0.07075(18) 0.3447(3) 0.60127(11) 0.0693(7) Uani 1 1 d . . . F9 F -0.0556(2) 0.2607(3) 0.49196(11) 0.0846(8) Uani 1 1 d . . . O1 O 0.38293(15) 0.68131(15) 0.20781(8) 0.0155(3) Uani 1 1 d . . . O2 O 0.32547(17) 0.60414(16) 0.07559(9) 0.0205(4) Uani 1 1 d . . . O3 O 0.19014(16) 0.73559(17) 0.12573(9) 0.0192(4) Uani 1 1 d . . . O4 O -0.15533(18) 0.20047(17) 0.67230(9) 0.0248(4) Uani 1 1 d . . . O5 O -0.30131(18) 0.11128(18) 0.54814(9) 0.0275(4) Uani 1 1 d . . . O6 O -0.2192(2) 0.35673(18) 0.58788(10) 0.0314(4) Uani 1 1 d . . . N1 N 0.41091(18) 0.35409(18) 0.16686(10) 0.0118(4) Uani 1 1 d . . . N1S N 0.8968(3) 0.0871(3) 0.05745(13) 0.0388(6) Uani 1 1 d . . . N2 N 0.62145(18) 0.57969(19) 0.20998(10) 0.0144(4) Uani 1 1 d . . . N3 N 0.43363(18) 0.34764(18) 0.31702(10) 0.0118(4) Uani 1 1 d . . . N4 N 0.53628(18) 0.61214(19) 0.35684(10) 0.0148(4) Uani 1 1 d . . . N5 N 0.20611(18) 0.41811(18) 0.24270(10) 0.0122(4) Uani 1 1 d . . . C1 C 0.3085(2) 0.2331(2) 0.15546(12) 0.0123(4) Uani 1 1 d . . . C1S C 0.9334(3) 0.2026(3) 0.05434(14) 0.0280(6) Uani 1 1 d . . . C2 C 0.2702(2) 0.1513(2) 0.08775(12) 0.0151(5) Uani 1 1 d . . . H2 H 0.1953 0.0669 0.0788 0.018 Uiso 1 1 calc R . . C2S C 0.9818(3) 0.3501(3) 0.05125(16) 0.0358(7) Uani 1 1 d . . . H2SA H 0.9277 0.3726 0.0061 0.054 Uiso 1 1 calc R . . H2SB H 1.0827 0.3786 0.0509 0.054 Uiso 1 1 calc R . . H2SC H 0.9677 0.3987 0.0947 0.054 Uiso 1 1 calc R . . C3 C 0.3430(2) 0.1946(2) 0.03338(13) 0.0173(5) Uani 1 1 d . . . H3 H 0.3149 0.1421 -0.0140 0.021 Uiso 1 1 calc R . . C4 C 0.4563(2) 0.3144(2) 0.04800(12) 0.0166(5) Uani 1 1 d . . . H4 H 0.5105 0.3425 0.0123 0.020 Uiso 1 1 calc R . . C5 C 0.4884(2) 0.3920(2) 0.11645(12) 0.0132(4) Uani 1 1 d . . . C6 C 0.6128(2) 0.5162(2) 0.14269(12) 0.0136(5) Uani 1 1 d . . . C7 C 0.7181(2) 0.5592(2) 0.10369(13) 0.0183(5) Uani 1 1 d . . . H7 H 0.7085 0.5141 0.0559 0.022 Uiso 1 1 calc R . . C8 C 0.8370(2) 0.6690(2) 0.13565(14) 0.0212(5) Uani 1 1 d . . . H8 H 0.9105 0.7002 0.1102 0.025 Uiso 1 1 calc R . . C9 C 0.8473(2) 0.7323(2) 0.20493(13) 0.0200(5) Uani 1 1 d . . . H9 H 0.9287 0.8065 0.2284 0.024 Uiso 1 1 calc R . . C10 C 0.7370(2) 0.6860(2) 0.23971(13) 0.0177(5) Uani 1 1 d . . . H10 H 0.7435 0.7317 0.2868 0.021 Uiso 1 1 calc R . . C11 C 0.3625(2) 0.2153(2) 0.29246(12) 0.0122(4) Uani 1 1 d . . . C12 C 0.3926(2) 0.1109(2) 0.33133(12) 0.0162(5) Uani 1 1 d . . . H12 H 0.3424 0.0169 0.3137 0.019 Uiso 1 1 calc R . . C13 C 0.4975(2) 0.1463(2) 0.39646(13) 0.0194(5) Uani 1 1 d . . . H13 H 0.5223 0.0759 0.4227 0.023 Uiso 1 1 calc R . . C14 C 0.5660(2) 0.2831(2) 0.42323(13) 0.0175(5) Uani 1 1 d . . . H14 H 0.6359 0.3084 0.4685 0.021 Uiso 1 1 calc R . . C15 C 0.5297(2) 0.3829(2) 0.38201(12) 0.0140(5) Uani 1 1 d . . . C16 C 0.5833(2) 0.5331(2) 0.40644(12) 0.0143(5) Uani 1 1 d . . . C17 C 0.6681(2) 0.5900(2) 0.47608(13) 0.0191(5) Uani 1 1 d . . . H17 H 0.7017 0.5332 0.5097 0.023 Uiso 1 1 calc R . . C18 C 0.7028(2) 0.7302(3) 0.49567(13) 0.0217(5) Uani 1 1 d . . . H18 H 0.7616 0.7712 0.5429 0.026 Uiso 1 1 calc R . . C19 C 0.6515(2) 0.8110(3) 0.44609(13) 0.0212(5) Uani 1 1 d . . . H19 H 0.6724 0.9074 0.4592 0.025 Uiso 1 1 calc R . . C20 C 0.5692(2) 0.7481(2) 0.37719(13) 0.0183(5) Uani 1 1 d . . . H20 H 0.5345 0.8033 0.3429 0.022 Uiso 1 1 calc R . . C21 C 0.1477(2) 0.2795(2) 0.23472(11) 0.0121(4) Uani 1 1 d . . . C22 C 0.0083(2) 0.2216(2) 0.23851(12) 0.0158(5) Uani 1 1 d . . . H22 H -0.0324 0.1242 0.2322 0.019 Uiso 1 1 calc R . . C23 C -0.0718(2) 0.3070(2) 0.25163(13) 0.0190(5) Uani 1 1 d . . . C24 C -0.0114(2) 0.4483(2) 0.26095(13) 0.0180(5) Uani 1 1 d . . . H24 H -0.0640 0.5083 0.2707 0.022 Uiso 1 1 calc R . . C25 C 0.1279(2) 0.4998(2) 0.25562(12) 0.0151(5) Uani 1 1 d . . . H25 H 0.1701 0.5970 0.2613 0.018 Uiso 1 1 calc R . . C26 C 0.2424(2) 0.1898(2) 0.22161(12) 0.0126(4) Uani 1 1 d . . . C27 C 0.1564(2) 0.0368(2) 0.20709(12) 0.0150(5) Uani 1 1 d . . . H27A H 0.2164 -0.0180 0.1956 0.023 Uiso 1 1 calc R . . H27B H 0.0752 0.0224 0.1651 0.023 Uiso 1 1 calc R . . H27C H 0.1225 0.0080 0.2513 0.023 Uiso 1 1 calc R . . C28 C -0.2256(3) 0.2439(3) 0.25156(17) 0.0303(6) Uani 1 1 d . . . C29 C 0.4491(2) 0.8640(2) 0.12155(13) 0.0175(5) Uani 1 1 d . . . C30 C -0.0374(3) 0.2401(4) 0.56282(18) 0.0526(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.01108(14) 0.01059(16) 0.01100(16) 0.00069(11) 0.00239(11) 0.00280(11) S1 0.0142(3) 0.0128(3) 0.0145(3) 0.0018(2) 0.0039(2) 0.0047(2) S2 0.0195(3) 0.0199(3) 0.0152(3) 0.0016(2) 0.0006(2) 0.0042(2) F1 0.0262(8) 0.0430(10) 0.0853(14) 0.0362(10) 0.0299(9) 0.0120(7) F2 0.0328(9) 0.0444(11) 0.0950(15) 0.0067(10) 0.0407(10) 0.0159(8) F3 0.0160(7) 0.0571(12) 0.0652(13) 0.0111(10) -0.0013(8) 0.0014(7) F4 0.0250(7) 0.0150(7) 0.0346(8) -0.0018(6) 0.0098(6) 0.0040(6) F5 0.0350(8) 0.0299(8) 0.0264(8) 0.0173(7) 0.0105(6) 0.0134(7) F6 0.0168(7) 0.0263(8) 0.0352(8) 0.0110(6) 0.0118(6) 0.0084(6) F7 0.0767(16) 0.121(2) 0.103(2) -0.0091(16) 0.0264(14) 0.0692(17) F8 0.0256(9) 0.1169(19) 0.0474(12) -0.0019(12) 0.0086(8) -0.0045(11) F9 0.0541(13) 0.156(2) 0.0320(11) -0.0014(13) 0.0228(10) 0.0069(14) O1 0.0167(7) 0.0147(8) 0.0155(8) 0.0034(6) 0.0037(6) 0.0050(6) O2 0.0259(9) 0.0193(9) 0.0176(9) 0.0003(7) 0.0052(7) 0.0090(7) O3 0.0145(8) 0.0225(9) 0.0212(9) 0.0028(7) 0.0031(7) 0.0071(7) O4 0.0336(9) 0.0193(9) 0.0172(9) 0.0028(7) -0.0025(7) 0.0072(7) O5 0.0338(10) 0.0204(9) 0.0207(9) -0.0011(7) -0.0033(8) 0.0039(8) O6 0.0425(11) 0.0187(10) 0.0244(10) 0.0034(7) -0.0069(8) 0.0062(8) N1 0.0111(8) 0.0125(9) 0.0128(9) 0.0021(7) 0.0034(7) 0.0047(7) N1S 0.0368(13) 0.0330(15) 0.0340(14) -0.0038(11) -0.0099(11) 0.0049(11) N2 0.0126(9) 0.0154(10) 0.0158(10) 0.0035(8) 0.0025(7) 0.0054(8) N3 0.0105(8) 0.0137(10) 0.0121(9) 0.0006(7) 0.0047(7) 0.0037(7) N4 0.0132(9) 0.0162(10) 0.0152(10) 0.0008(8) 0.0048(7) 0.0038(8) N5 0.0127(9) 0.0136(10) 0.0104(9) 0.0006(7) 0.0021(7) 0.0044(7) C1 0.0115(10) 0.0135(11) 0.0138(11) 0.0020(9) 0.0022(8) 0.0071(9) C1S 0.0253(13) 0.0325(17) 0.0195(13) -0.0040(11) -0.0062(10) 0.0078(12) C2 0.0155(10) 0.0125(11) 0.0170(12) 0.0000(9) 0.0039(9) 0.0039(9) C2S 0.0415(16) 0.0304(16) 0.0267(15) 0.0016(12) -0.0057(12) 0.0074(13) C3 0.0195(11) 0.0169(12) 0.0151(12) -0.0020(9) 0.0025(9) 0.0066(9) C4 0.0190(11) 0.0200(12) 0.0140(12) 0.0038(9) 0.0079(9) 0.0076(9) C5 0.0142(10) 0.0143(11) 0.0139(11) 0.0035(9) 0.0042(9) 0.0078(9) C6 0.0132(10) 0.0144(11) 0.0146(11) 0.0047(9) 0.0035(9) 0.0058(9) C7 0.0186(11) 0.0198(13) 0.0178(12) 0.0042(10) 0.0065(9) 0.0060(10) C8 0.0150(11) 0.0244(13) 0.0255(13) 0.0092(10) 0.0083(10) 0.0045(10) C9 0.0135(11) 0.0177(12) 0.0249(13) 0.0047(10) 0.0014(10) 0.0004(9) C10 0.0149(11) 0.0171(12) 0.0187(12) 0.0013(9) 0.0000(9) 0.0041(9) C11 0.0114(10) 0.0153(11) 0.0126(11) 0.0011(9) 0.0062(8) 0.0060(9) C12 0.0172(11) 0.0142(12) 0.0182(12) 0.0024(9) 0.0065(9) 0.0043(9) C13 0.0218(12) 0.0228(13) 0.0179(12) 0.0077(10) 0.0054(10) 0.0118(10) C14 0.0159(11) 0.0236(13) 0.0133(11) 0.0021(10) 0.0016(9) 0.0080(10) C15 0.0113(10) 0.0201(12) 0.0116(11) 0.0011(9) 0.0053(9) 0.0048(9) C16 0.0116(10) 0.0192(12) 0.0133(11) 0.0009(9) 0.0066(9) 0.0044(9) C17 0.0155(11) 0.0268(14) 0.0147(12) 0.0011(10) 0.0033(9) 0.0063(10) C18 0.0187(11) 0.0269(14) 0.0156(12) -0.0076(10) 0.0018(9) 0.0041(10) C19 0.0210(12) 0.0172(13) 0.0235(13) -0.0064(10) 0.0064(10) 0.0038(10) C20 0.0184(11) 0.0157(12) 0.0207(13) 0.0006(10) 0.0053(10) 0.0048(9) C21 0.0133(10) 0.0139(11) 0.0084(10) 0.0012(8) 0.0017(8) 0.0037(9) C22 0.0155(11) 0.0155(12) 0.0161(12) 0.0021(9) 0.0037(9) 0.0041(9) C23 0.0144(11) 0.0241(13) 0.0201(12) 0.0052(10) 0.0058(9) 0.0065(10) C24 0.0191(11) 0.0208(13) 0.0198(12) 0.0044(10) 0.0083(10) 0.0118(10) C25 0.0192(11) 0.0125(11) 0.0139(11) -0.0003(9) 0.0033(9) 0.0061(9) C26 0.0131(10) 0.0106(11) 0.0144(11) 0.0016(9) 0.0040(9) 0.0033(8) C27 0.0145(10) 0.0125(11) 0.0174(12) 0.0018(9) 0.0044(9) 0.0026(9) C28 0.0207(13) 0.0278(15) 0.0500(18) 0.0116(13) 0.0184(13) 0.0107(11) C29 0.0181(11) 0.0176(12) 0.0207(13) 0.0064(10) 0.0075(9) 0.0087(9) C30 0.0349(17) 0.088(3) 0.0329(18) -0.0036(18) 0.0085(14) 0.0164(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N3 2.0783(18) . ? Co1 N1 2.0870(18) . ? Co1 N4 2.1050(18) . ? Co1 O1 2.1266(15) . ? Co1 N5 2.1339(17) . ? Co1 N2 2.1978(18) . ? S1 O3 1.4350(16) . ? S1 O2 1.4425(17) . ? S1 O1 1.4625(16) . ? S1 C29 1.828(2) . ? S2 O5 1.4338(18) . ? S2 O6 1.4408(18) . ? S2 O4 1.4430(17) . ? S2 C30 1.810(3) . ? F1 C28 1.321(3) . ? F2 C28 1.324(3) . ? F3 C28 1.345(3) . ? F4 C29 1.331(3) . ? F5 C29 1.330(3) . ? F6 C29 1.333(3) . ? F7 C30 1.331(5) . ? F8 C30 1.333(4) . ? F9 C30 1.327(4) . ? N1 C1 1.339(3) . ? N1 C5 1.344(3) . ? N1S C1S 1.137(3) . ? N2 C10 1.339(3) . ? N2 C6 1.350(3) . ? N3 C11 1.338(3) . ? N3 C15 1.343(3) . ? N4 C20 1.342(3) . ? N4 C16 1.357(3) . ? N5 C25 1.344(3) . ? N5 C21 1.353(3) . ? C1 C2 1.389(3) . ? C1 C26 1.542(3) . ? C1S C2S 1.449(4) . ? C2 C3 1.387(3) . ? C2 H2 0.9500 . ? C2S H2SA 0.9800 . ? C2S H2SB 0.9800 . ? C2S H2SC 0.9800 . ? C3 C4 1.384(3) . ? C3 H3 0.9500 . ? C4 C5 1.387(3) . ? C4 H4 0.9500 . ? C5 C6 1.483(3) . ? C6 C7 1.391(3) . ? C7 C8 1.386(3) . ? C7 H7 0.9500 . ? C8 C9 1.378(4) . ? C8 H8 0.9500 . ? C9 C10 1.383(3) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.386(3) . ? C11 C26 1.550(3) . ? C12 C13 1.389(3) . ? C12 H12 0.9500 . ? C13 C14 1.380(3) . ? C13 H13 0.9500 . ? C14 C15 1.390(3) . ? C14 H14 0.9500 . ? C15 C16 1.481(3) . ? C16 C17 1.388(3) . ? C17 C18 1.379(3) . ? C17 H17 0.9500 . ? C18 C19 1.387(3) . ? C18 H18 0.9500 . ? C19 C20 1.383(3) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C22 1.384(3) . ? C21 C26 1.543(3) . ? C22 C23 1.389(3) . ? C22 H22 0.9500 . ? C23 C24 1.380(3) . ? C23 C28 1.505(3) . ? C24 C25 1.384(3) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C27 1.532(3) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? 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 N3 Co1 N1 82.86(7) . . ? N3 Co1 N4 76.86(7) . . ? N1 Co1 N4 148.00(7) . . ? N3 Co1 O1 161.53(6) . . ? N1 Co1 O1 111.42(6) . . ? N4 Co1 O1 94.34(7) . . ? N3 Co1 N5 80.85(7) . . ? N1 Co1 N5 87.83(7) . . ? N4 Co1 N5 112.65(7) . . ? O1 Co1 N5 87.85(6) . . ? N3 Co1 N2 112.46(7) . . ? N1 Co1 N2 74.76(7) . . ? N4 Co1 N2 90.35(7) . . ? O1 Co1 N2 83.44(6) . . ? N5 Co1 N2 155.98(7) . . ? O3 S1 O2 116.21(10) . . ? O3 S1 O1 114.19(9) . . ? O2 S1 O1 113.93(9) . . ? O3 S1 C29 104.59(10) . . ? O2 S1 C29 104.37(10) . . ? O1 S1 C29 101.25(10) . . ? O5 S2 O6 114.62(10) . . ? O5 S2 O4 115.78(10) . . ? O6 S2 O4 113.93(11) . . ? O5 S2 C30 104.08(14) . . ? O6 S2 C30 103.24(16) . . ? O4 S2 C30 102.96(13) . . ? S1 O1 Co1 131.67(9) . . ? C1 N1 C5 120.88(19) . . ? C1 N1 Co1 120.92(14) . . ? C5 N1 Co1 117.03(14) . . ? C10 N2 C6 117.97(19) . . ? C10 N2 Co1 127.96(16) . . ? C6 N2 Co1 113.71(14) . . ? C11 N3 C15 120.89(18) . . ? C11 N3 Co1 122.62(14) . . ? C15 N3 Co1 115.77(14) . . ? C20 N4 C16 118.61(19) . . ? C20 N4 Co1 126.61(15) . . ? C16 N4 Co1 114.65(15) . . ? C25 N5 C21 119.36(18) . . ? C25 N5 Co1 119.83(15) . . ? C21 N5 Co1 120.15(14) . . ? N1 C1 C2 120.2(2) . . ? N1 C1 C26 116.45(18) . . ? C2 C1 C26 123.29(19) . . ? N1S C1S C2S 179.2(3) . . ? C3 C2 C1 119.0(2) . . ? C3 C2 H2 120.5 . . ? C1 C2 H2 120.5 . . ? C1S C2S H2SA 109.5 . . ? C1S C2S H2SB 109.5 . . ? H2SA C2S H2SB 109.5 . . ? C1S C2S H2SC 109.5 . . ? H2SA C2S H2SC 109.5 . . ? H2SB C2S H2SC 109.5 . . ? C4 C3 C2 120.2(2) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C3 C4 C5 117.9(2) . . ? C3 C4 H4 121.0 . . ? C5 C4 H4 121.0 . . ? N1 C5 C4 121.4(2) . . ? N1 C5 C6 114.15(19) . . ? C4 C5 C6 124.3(2) . . ? N2 C6 C7 122.2(2) . . ? N2 C6 C5 114.80(19) . . ? C7 C6 C5 122.9(2) . . ? C8 C7 C6 118.9(2) . . ? C8 C7 H7 120.6 . . ? C6 C7 H7 120.6 . . ? C9 C8 C7 119.0(2) . . ? C9 C8 H8 120.5 . . ? C7 C8 H8 120.5 . . ? C8 C9 C10 118.9(2) . . ? C8 C9 H9 120.6 . . ? C10 C9 H9 120.6 . . ? N2 C10 C9 123.0(2) . . ? N2 C10 H10 118.5 . . ? C9 C10 H10 118.5 . . ? N3 C11 C12 120.63(19) . . ? N3 C11 C26 115.59(18) . . ? C12 C11 C26 123.71(19) . . ? C11 C12 C13 118.8(2) . . ? C11 C12 H12 120.6 . . ? C13 C12 H12 120.6 . . ? C14 C13 C12 120.3(2) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C13 C14 C15 118.1(2) . . ? C13 C14 H14 121.0 . . ? C15 C14 H14 121.0 . . ? N3 C15 C14 121.2(2) . . ? N3 C15 C16 114.14(19) . . ? C14 C15 C16 124.6(2) . . ? N4 C16 C17 121.7(2) . . ? N4 C16 C15 114.75(19) . . ? C17 C16 C15 123.4(2) . . ? C18 C17 C16 118.9(2) . . ? C18 C17 H17 120.5 . . ? C16 C17 H17 120.5 . . ? C17 C18 C19 119.7(2) . . ? C17 C18 H18 120.2 . . ? C19 C18 H18 120.2 . . ? C20 C19 C18 118.5(2) . . ? C20 C19 H19 120.8 . . ? C18 C19 H19 120.8 . . ? N4 C20 C19 122.6(2) . . ? N4 C20 H20 118.7 . . ? C19 C20 H20 118.7 . . ? N5 C21 C22 120.6(2) . . ? N5 C21 C26 117.55(18) . . ? C22 C21 C26 121.80(19) . . ? C21 C22 C23 119.5(2) . . ? C21 C22 H22 120.2 . . ? C23 C22 H22 120.2 . . ? C24 C23 C22 119.7(2) . . ? C24 C23 C28 120.8(2) . . ? C22 C23 C28 119.4(2) . . ? C23 C24 C25 118.0(2) . . ? C23 C24 H24 121.0 . . ? C25 C24 H24 121.0 . . ? N5 C25 C24 122.7(2) . . ? N5 C25 H25 118.6 . . ? C24 C25 H25 118.6 . . ? C27 C26 C1 110.05(18) . . ? C27 C26 C21 110.59(17) . . ? C1 C26 C21 109.94(17) . . ? C27 C26 C11 109.62(17) . . ? C1 C26 C11 109.04(16) . . ? C21 C26 C11 107.55(17) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? F1 C28 F2 109.2(2) . . ? F1 C28 F3 106.6(2) . . ? F2 C28 F3 105.3(2) . . ? F1 C28 C23 112.6(2) . . ? F2 C28 C23 112.4(2) . . ? F3 C28 C23 110.3(2) . . ? F5 C29 F4 108.58(18) . . ? F5 C29 F6 108.03(18) . . ? F4 C29 F6 108.17(18) . . ? F5 C29 S1 110.60(15) . . ? F4 C29 S1 110.62(15) . . ? F6 C29 S1 110.75(15) . . ? F9 C30 F7 107.7(3) . . ? F9 C30 F8 107.7(3) . . ? F7 C30 F8 107.2(3) . . ? F9 C30 S2 111.9(2) . . ? F7 C30 S2 110.7(3) . . ? F8 C30 S2 111.5(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 O3 S1 O1 Co1 118.01(12) . . . . ? O2 S1 O1 Co1 -18.79(16) . . . . ? C29 S1 O1 Co1 -130.21(12) . . . . ? N3 Co1 O1 S1 -126.90(19) . . . . ? N1 Co1 O1 S1 11.98(14) . . . . ? N4 Co1 O1 S1 172.60(12) . . . . ? N5 Co1 O1 S1 -74.84(13) . . . . ? N2 Co1 O1 S1 82.74(13) . . . . ? N3 Co1 N1 C1 55.03(15) . . . . ? N4 Co1 N1 C1 105.78(18) . . . . ? O1 Co1 N1 C1 -112.84(15) . . . . ? N5 Co1 N1 C1 -26.01(15) . . . . ? N2 Co1 N1 C1 170.70(16) . . . . ? N3 Co1 N1 C5 -137.26(15) . . . . ? N4 Co1 N1 C5 -86.51(19) . . . . ? O1 Co1 N1 C5 54.86(16) . . . . ? N5 Co1 N1 C5 141.69(15) . . . . ? N2 Co1 N1 C5 -21.60(14) . . . . ? N3 Co1 N2 C10 -94.31(18) . . . . ? N1 Co1 N2 C10 -169.72(19) . . . . ? N4 Co1 N2 C10 -18.41(18) . . . . ? O1 Co1 N2 C10 75.92(18) . . . . ? N5 Co1 N2 C10 145.37(19) . . . . ? N3 Co1 N2 C6 92.79(15) . . . . ? N1 Co1 N2 C6 17.38(14) . . . . ? N4 Co1 N2 C6 168.70(15) . . . . ? O1 Co1 N2 C6 -96.97(15) . . . . ? N5 Co1 N2 C6 -27.5(3) . . . . ? N1 Co1 N3 C11 -33.18(16) . . . . ? N4 Co1 N3 C11 171.74(17) . . . . ? O1 Co1 N3 C11 108.7(2) . . . . ? N5 Co1 N3 C11 55.75(16) . . . . ? N2 Co1 N3 C11 -103.40(16) . . . . ? N1 Co1 N3 C15 137.14(15) . . . . ? N4 Co1 N3 C15 -17.94(14) . . . . ? O1 Co1 N3 C15 -81.0(2) . . . . ? N5 Co1 N3 C15 -133.93(15) . . . . ? N2 Co1 N3 C15 66.92(16) . . . . ? N3 Co1 N4 C20 -169.52(19) . . . . ? N1 Co1 N4 C20 138.39(18) . . . . ? O1 Co1 N4 C20 -5.97(18) . . . . ? N5 Co1 N4 C20 -95.44(18) . . . . ? N2 Co1 N4 C20 77.48(18) . . . . ? N3 Co1 N4 C16 14.71(14) . . . . ? N1 Co1 N4 C16 -37.4(2) . . . . ? O1 Co1 N4 C16 178.26(14) . . . . ? N5 Co1 N4 C16 88.78(15) . . . . ? N2 Co1 N4 C16 -98.30(15) . . . . ? N3 Co1 N5 C25 129.74(17) . . . . ? N1 Co1 N5 C25 -147.14(16) . . . . ? N4 Co1 N5 C25 58.21(17) . . . . ? O1 Co1 N5 C25 -35.60(16) . . . . ? N2 Co1 N5 C25 -104.2(2) . . . . ? N3 Co1 N5 C21 -40.87(16) . . . . ? N1 Co1 N5 C21 42.24(16) . . . . ? N4 Co1 N5 C21 -112.41(16) . . . . ? O1 Co1 N5 C21 153.79(16) . . . . ? N2 Co1 N5 C21 85.2(2) . . . . ? C5 N1 C1 C2 -7.0(3) . . . . ? Co1 N1 C1 C2 160.25(15) . . . . ? C5 N1 C1 C26 170.71(18) . . . . ? Co1 N1 C1 C26 -22.1(2) . . . . ? N1 C1 C2 C3 2.2(3) . . . . ? C26 C1 C2 C3 -175.33(19) . . . . ? C1 C2 C3 C4 3.1(3) . . . . ? C2 C3 C4 C5 -3.6(3) . . . . ? C1 N1 C5 C4 6.5(3) . . . . ? Co1 N1 C5 C4 -161.25(16) . . . . ? C1 N1 C5 C6 -169.89(18) . . . . ? Co1 N1 C5 C6 22.4(2) . . . . ? C3 C4 C5 N1 -1.1(3) . . . . ? C3 C4 C5 C6 174.91(19) . . . . ? C10 N2 C6 C7 -1.0(3) . . . . ? Co1 N2 C6 C7 172.62(16) . . . . ? C10 N2 C6 C5 174.78(18) . . . . ? Co1 N2 C6 C5 -11.6(2) . . . . ? N1 C5 C6 N2 -6.2(3) . . . . ? C4 C5 C6 N2 177.6(2) . . . . ? N1 C5 C6 C7 169.61(19) . . . . ? C4 C5 C6 C7 -6.6(3) . . . . ? N2 C6 C7 C8 1.4(3) . . . . ? C5 C6 C7 C8 -174.1(2) . . . . ? C6 C7 C8 C9 -0.1(3) . . . . ? C7 C8 C9 C10 -1.3(3) . . . . ? C6 N2 C10 C9 -0.6(3) . . . . ? Co1 N2 C10 C9 -173.19(16) . . . . ? C8 C9 C10 N2 1.8(3) . . . . ? C15 N3 C11 C12 -4.1(3) . . . . ? Co1 N3 C11 C12 165.77(16) . . . . ? C15 N3 C11 C26 172.95(18) . . . . ? Co1 N3 C11 C26 -17.2(2) . . . . ? N3 C11 C12 C13 0.3(3) . . . . ? C26 C11 C12 C13 -176.4(2) . . . . ? C11 C12 C13 C14 2.6(3) . . . . ? C12 C13 C14 C15 -1.9(3) . . . . ? C11 N3 C15 C14 4.8(3) . . . . ? Co1 N3 C15 C14 -165.67(16) . . . . ? C11 N3 C15 C16 -171.41(18) . . . . ? Co1 N3 C15 C16 18.1(2) . . . . ? C13 C14 C15 N3 -1.8(3) . . . . ? C13 C14 C15 C16 174.1(2) . . . . ? C20 N4 C16 C17 -2.3(3) . . . . ? Co1 N4 C16 C17 173.79(16) . . . . ? C20 N4 C16 C15 173.94(19) . . . . ? Co1 N4 C16 C15 -9.9(2) . . . . ? N3 C15 C16 N4 -5.1(3) . . . . ? C14 C15 C16 N4 178.8(2) . . . . ? N3 C15 C16 C17 171.1(2) . . . . ? C14 C15 C16 C17 -5.0(3) . . . . ? N4 C16 C17 C18 1.3(3) . . . . ? C15 C16 C17 C18 -174.6(2) . . . . ? C16 C17 C18 C19 0.7(3) . . . . ? C17 C18 C19 C20 -1.6(3) . . . . ? C16 N4 C20 C19 1.4(3) . . . . ? Co1 N4 C20 C19 -174.24(17) . . . . ? C18 C19 C20 N4 0.6(3) . . . . ? C25 N5 C21 C22 1.1(3) . . . . ? Co1 N5 C21 C22 171.74(15) . . . . ? C25 N5 C21 C26 -178.74(18) . . . . ? Co1 N5 C21 C26 -8.1(2) . . . . ? N5 C21 C22 C23 -0.9(3) . . . . ? C26 C21 C22 C23 179.0(2) . . . . ? C21 C22 C23 C24 -0.2(3) . . . . ? C21 C22 C23 C28 176.7(2) . . . . ? C22 C23 C24 C25 1.0(3) . . . . ? C28 C23 C24 C25 -175.8(2) . . . . ? C21 N5 C25 C24 -0.3(3) . . . . ? Co1 N5 C25 C24 -170.94(17) . . . . ? C23 C24 C25 N5 -0.8(3) . . . . ? N1 C1 C26 C27 -165.63(17) . . . . ? C2 C1 C26 C27 12.0(3) . . . . ? N1 C1 C26 C21 72.3(2) . . . . ? C2 C1 C26 C21 -110.1(2) . . . . ? N1 C1 C26 C11 -45.4(2) . . . . ? C2 C1 C26 C11 132.3(2) . . . . ? N5 C21 C26 C27 -175.05(18) . . . . ? C22 C21 C26 C27 5.1(3) . . . . ? N5 C21 C26 C1 -53.3(2) . . . . ? C22 C21 C26 C1 126.9(2) . . . . ? N5 C21 C26 C11 65.3(2) . . . . ? C22 C21 C26 C11 -114.5(2) . . . . ? N3 C11 C26 C27 -171.36(18) . . . . ? C12 C11 C26 C27 5.6(3) . . . . ? N3 C11 C26 C1 68.1(2) . . . . ? C12 C11 C26 C1 -115.0(2) . . . . ? N3 C11 C26 C21 -51.1(2) . . . . ? C12 C11 C26 C21 125.9(2) . . . . ? C24 C23 C28 F1 -145.5(2) . . . . ? C22 C23 C28 F1 37.7(3) . . . . ? C24 C23 C28 F2 -21.6(4) . . . . ? C22 C23 C28 F2 161.5(2) . . . . ? C24 C23 C28 F3 95.6(3) . . . . ? C22 C23 C28 F3 -81.2(3) . . . . ? O3 S1 C29 F5 -62.62(17) . . . . ? O2 S1 C29 F5 59.92(17) . . . . ? O1 S1 C29 F5 178.47(15) . . . . ? O3 S1 C29 F4 57.73(17) . . . . ? O2 S1 C29 F4 -179.74(14) . . . . ? O1 S1 C29 F4 -61.18(16) . . . . ? O3 S1 C29 F6 177.65(15) . . . . ? O2 S1 C29 F6 -59.82(18) . . . . ? O1 S1 C29 F6 58.74(17) . . . . ? O5 S2 C30 F9 57.8(3) . . . . ? O6 S2 C30 F9 -62.2(3) . . . . ? O4 S2 C30 F9 179.0(3) . . . . ? O5 S2 C30 F7 -62.3(2) . . . . ? O6 S2 C30 F7 177.6(2) . . . . ? O4 S2 C30 F7 58.8(3) . . . . ? O5 S2 C30 F8 178.5(2) . . . . ? O6 S2 C30 F8 58.4(3) . . . . ? O4 S2 C30 F8 -60.4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.40 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.624 _refine_diff_density_min -0.410 _refine_diff_density_rms 0.061 _database_code_depnum_ccdc_archive 'CCDC 943492'