# Electronic Supplementary Material (ESI) for CrystEngComm # 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_n121130b _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H44 Ag4 Cl4 N12 O20 S6' _chemical_formula_weight 1586.35 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 '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)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.2108(10) _cell_length_b 14.2447(10) _cell_length_c 14.5976(11) _cell_angle_alpha 90.00 _cell_angle_beta 113.3180(10) _cell_angle_gamma 90.00 _cell_volume 2522.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8844 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 28.36 _exptl_crystal_description BLOCK _exptl_crystal_colour COLOURLESS _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 2.088 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1568 _exptl_absorpt_coefficient_mu 2.072 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.6254 _exptl_absorpt_correction_T_max 0.6472 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12718 _diffrn_reflns_av_R_equivalents 0.0282 _diffrn_reflns_av_sigmaI/netI 0.0280 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 25.01 _reflns_number_total 4426 _reflns_number_gt 4152 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0320P)^2^+2.2111P] 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 4426 _refine_ls_number_parameters 322 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0288 _refine_ls_R_factor_gt 0.0263 _refine_ls_wR_factor_ref 0.0641 _refine_ls_wR_factor_gt 0.0628 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.003 _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 Ag1 Ag 0.169590(18) 0.942979(15) 0.491508(17) 0.01833(8) Uani 1 1 d . . . Ag2 Ag 0.124175(18) 1.082894(15) 0.644210(18) 0.01905(8) Uani 1 1 d U . . S1 S 0.51442(6) 1.05240(6) 0.72863(6) 0.02382(18) Uani 1 1 d . . . S2 S 0.06247(6) 0.62603(5) 0.45664(6) 0.02126(18) Uani 1 1 d . . . S3 S 0.00589(6) 1.22299(5) 0.31375(6) 0.01851(17) Uani 1 1 d . . . Cl1 Cl 0.18708(6) 0.93477(5) 0.25988(5) 0.01824(16) Uani 1 1 d . . . Cl2 Cl 0.50094(6) 0.82527(5) 0.87815(5) 0.02120(17) Uani 1 1 d . . . O1 O 0.1760(2) 0.86585(17) 0.32752(19) 0.0381(6) Uani 1 1 d . . . O2 O 0.26725(18) 1.00293(16) 0.31600(19) 0.0341(6) Uani 1 1 d . . . O3 O 0.08198(17) 0.98086(17) 0.20966(19) 0.0325(6) Uani 1 1 d . . . O4 O 0.2204(2) 0.8887(2) 0.19015(18) 0.0397(6) Uani 1 1 d . . . O5 O 0.44828(19) 0.80499(19) 0.77461(17) 0.0351(6) Uani 1 1 d . . . O6 O 0.4574(2) 0.91081(19) 0.9004(2) 0.0421(7) Uani 1 1 d . . . O7 O 0.61647(18) 0.84017(19) 0.9036(2) 0.0405(7) Uani 1 1 d . . . O8 O 0.4854(3) 0.7510(2) 0.9350(2) 0.0623(9) Uani 1 1 d . . . O9 O 0.13439(18) 1.09719(15) 0.81929(17) 0.0238(5) Uani 1 1 d . . . H9A H 0.1839 1.0646 0.8616 0.036 Uiso 1 1 d R . . H9B H 0.0737 1.0759 0.8159 0.036 Uiso 1 1 d R . . O10 O 0.30216(18) 0.49830(16) 0.46572(18) 0.0300(5) Uani 1 1 d . . . H10A H 0.3340 0.4621 0.5140 0.045 Uiso 1 1 d R . . H10B H 0.3507 0.5193 0.4477 0.045 Uiso 1 1 d R . . N1 N 0.32617(19) 0.99802(17) 0.61097(18) 0.0164(5) Uani 1 1 d . . . N2 N 0.30744(19) 1.06154(16) 0.67378(19) 0.0167(5) Uani 1 1 d . . . N3 N 0.09359(19) 0.80116(17) 0.47379(18) 0.0170(5) Uani 1 1 d . . . N4 N -0.01981(19) 0.78904(17) 0.42787(18) 0.0168(5) Uani 1 1 d . . . N5 N 0.07315(19) 1.07233(16) 0.41068(19) 0.0159(5) Uani 1 1 d . . . N6 N -0.04037(19) 1.06231(16) 0.36048(19) 0.0159(5) Uani 1 1 d . . . C1 C 0.3986(2) 1.0960(2) 0.7399(2) 0.0190(6) Uani 1 1 d . . . C2 C 0.4301(2) 0.9847(2) 0.6307(2) 0.0171(6) Uani 1 1 d . . . C3 C 0.4016(3) 1.1652(2) 0.8165(3) 0.0303(8) Uani 1 1 d . . . H3A H 0.4212 1.2271 0.7990 0.046 Uiso 1 1 calc R . . H3B H 0.4566 1.1460 0.8816 0.046 Uiso 1 1 calc R . . H3C H 0.3289 1.1685 0.8196 0.046 Uiso 1 1 calc R . . C4 C 0.4704(3) 0.9167(2) 0.5754(3) 0.0250(7) Uani 1 1 d . . . H4A H 0.4810 0.8552 0.6079 0.037 Uiso 1 1 calc R . . H4B H 0.5406 0.9388 0.5754 0.037 Uiso 1 1 calc R . . H4C H 0.4160 0.9113 0.5065 0.037 Uiso 1 1 calc R . . C5 C -0.0481(2) 0.7013(2) 0.4148(2) 0.0176(6) Uani 1 1 d . . . C6 C 0.1473(2) 0.7222(2) 0.4922(2) 0.0170(6) Uani 1 1 d . . . C7 C -0.1645(2) 0.6690(2) 0.3687(3) 0.0272(8) Uani 1 1 d . . . H7A H -0.2138 0.7217 0.3649 0.041 Uiso 1 1 calc R . . H7B H -0.1761 0.6189 0.4095 0.041 Uiso 1 1 calc R . . H7C H -0.1805 0.6452 0.3014 0.041 Uiso 1 1 calc R . . C8 C 0.2704(2) 0.7174(2) 0.5376(2) 0.0224(7) Uani 1 1 d . . . H8A H 0.2996 0.7437 0.4911 0.034 Uiso 1 1 calc R . . H8B H 0.2937 0.6518 0.5518 0.034 Uiso 1 1 calc R . . H8C H 0.2984 0.7535 0.5998 0.034 Uiso 1 1 calc R . . C9 C -0.0862(2) 1.1348(2) 0.3075(2) 0.0162(6) Uani 1 1 d . . . C10 C 0.1091(2) 1.1525(2) 0.3927(2) 0.0167(6) Uani 1 1 d . . . C11 C -0.2060(2) 1.1433(2) 0.2450(2) 0.0240(7) Uani 1 1 d . . . H11A H -0.2188 1.1349 0.1746 0.036 Uiso 1 1 calc R . . H11B H -0.2319 1.2055 0.2545 0.036 Uiso 1 1 calc R . . H11C H -0.2463 1.0950 0.2647 0.036 Uiso 1 1 calc R . . C12 C 0.2271(2) 1.1818(2) 0.4358(2) 0.0226(7) Uani 1 1 d . . . H12A H 0.2635 1.1560 0.5033 0.034 Uiso 1 1 calc R . . H12B H 0.2316 1.2505 0.4387 0.034 Uiso 1 1 calc R . . H12C H 0.2638 1.1582 0.3938 0.034 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.01450(13) 0.01329(13) 0.02070(14) -0.00330(9) 0.00004(10) -0.00220(8) Ag2 0.01361(13) 0.01466(13) 0.02616(14) -0.00084(9) 0.00498(10) -0.00042(8) S1 0.0105(4) 0.0287(4) 0.0258(4) -0.0030(3) 0.0002(3) -0.0039(3) S2 0.0168(4) 0.0123(4) 0.0277(4) 0.0004(3) 0.0013(3) -0.0010(3) S3 0.0142(4) 0.0144(4) 0.0221(4) 0.0032(3) 0.0022(3) -0.0020(3) Cl1 0.0152(3) 0.0191(4) 0.0173(4) -0.0018(3) 0.0029(3) -0.0013(3) Cl2 0.0163(4) 0.0250(4) 0.0196(4) -0.0004(3) 0.0043(3) -0.0005(3) O1 0.0502(16) 0.0270(14) 0.0383(15) 0.0072(11) 0.0190(13) -0.0013(12) O2 0.0224(12) 0.0258(13) 0.0394(15) -0.0084(11) -0.0036(11) -0.0038(10) O3 0.0148(11) 0.0311(13) 0.0430(15) 0.0076(11) 0.0021(11) 0.0019(10) O4 0.0321(14) 0.0621(18) 0.0233(13) -0.0098(12) 0.0093(11) 0.0004(13) O5 0.0271(13) 0.0500(16) 0.0200(12) -0.0064(11) 0.0006(10) 0.0051(11) O6 0.0231(13) 0.0482(17) 0.0517(17) -0.0194(13) 0.0113(13) 0.0070(11) O7 0.0147(11) 0.0460(16) 0.0511(17) -0.0090(13) 0.0027(12) 0.0044(11) O8 0.103(3) 0.0461(18) 0.0449(18) 0.0027(15) 0.0362(18) -0.0262(18) O9 0.0190(11) 0.0216(12) 0.0278(12) -0.0001(10) 0.0060(10) 0.0010(9) O10 0.0212(11) 0.0289(13) 0.0339(14) 0.0049(11) 0.0045(11) 0.0002(10) N1 0.0121(12) 0.0138(12) 0.0187(13) -0.0017(10) 0.0011(11) 0.0000(9) N2 0.0141(12) 0.0155(13) 0.0176(13) -0.0012(10) 0.0031(11) -0.0019(10) N3 0.0135(12) 0.0152(13) 0.0185(13) -0.0013(10) 0.0023(10) -0.0016(10) N4 0.0121(12) 0.0156(13) 0.0190(13) -0.0016(10) 0.0023(10) -0.0003(10) N5 0.0110(12) 0.0140(12) 0.0186(13) -0.0014(10) 0.0017(11) -0.0013(9) N6 0.0114(12) 0.0135(12) 0.0202(13) -0.0024(10) 0.0035(11) -0.0023(9) C1 0.0133(14) 0.0208(16) 0.0198(16) -0.0005(13) 0.0034(13) -0.0037(12) C2 0.0131(14) 0.0140(15) 0.0205(16) 0.0029(12) 0.0026(13) -0.0011(11) C3 0.0274(18) 0.034(2) 0.0281(18) -0.0145(16) 0.0094(15) -0.0146(15) C4 0.0206(16) 0.0195(16) 0.035(2) 0.0007(14) 0.0116(16) 0.0035(13) C5 0.0189(15) 0.0136(15) 0.0191(15) -0.0021(12) 0.0061(13) 0.0000(12) C6 0.0181(15) 0.0153(15) 0.0140(14) 0.0001(12) 0.0026(12) -0.0021(12) C7 0.0164(16) 0.0225(17) 0.039(2) -0.0044(15) 0.0066(15) -0.0024(13) C8 0.0162(15) 0.0185(16) 0.0255(17) 0.0004(13) 0.0008(13) 0.0003(12) C9 0.0157(14) 0.0145(15) 0.0165(15) -0.0028(12) 0.0044(12) -0.0026(12) C10 0.0158(14) 0.0144(15) 0.0172(15) -0.0023(12) 0.0037(12) -0.0009(12) C11 0.0165(15) 0.0196(16) 0.0307(18) 0.0034(14) 0.0038(14) -0.0021(12) C12 0.0161(15) 0.0183(16) 0.0266(17) -0.0009(13) 0.0014(14) -0.0043(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 Ag1 N3 2.225(2) . ? Ag1 N1 2.254(2) . ? Ag1 N5 2.285(2) . ? Ag1 Ag2 3.2187(4) . ? Ag2 N4 2.278(2) 3_576 ? Ag2 N2 2.305(2) . ? Ag2 N6 2.334(2) 3_576 ? Ag2 O9 2.514(2) . ? S1 C1 1.718(3) . ? S1 C2 1.719(3) . ? S2 C6 1.714(3) . ? S2 C5 1.718(3) . ? S3 C10 1.719(3) . ? S3 C9 1.726(3) . ? Cl1 O4 1.420(3) . ? Cl1 O2 1.431(2) . ? Cl1 O1 1.440(3) . ? Cl1 O3 1.446(2) . ? Cl2 O8 1.409(3) . ? Cl2 O5 1.421(2) . ? Cl2 O7 1.437(2) . ? Cl2 O6 1.439(3) . ? O9 H9A 0.8400 . ? O9 H9B 0.8400 . ? O10 H10A 0.8399 . ? O10 H10B 0.8398 . ? N1 C2 1.300(4) . ? N1 N2 1.379(3) . ? N2 C1 1.305(4) . ? N3 C6 1.300(4) . ? N3 N4 1.389(3) . ? N4 C5 1.296(4) . ? N4 Ag2 2.278(2) 3_576 ? N5 C10 1.302(4) . ? N5 N6 1.391(3) . ? N6 C9 1.288(4) . ? N6 Ag2 2.334(2) 3_576 ? C1 C3 1.480(4) . ? C2 C4 1.487(4) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C7 1.487(4) . ? C6 C8 1.495(4) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C11 1.487(4) . ? C10 C12 1.491(4) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 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 Ag1 N1 129.76(9) . . ? N3 Ag1 N5 122.58(9) . . ? N1 Ag1 N5 105.81(8) . . ? N3 Ag1 Ag2 116.33(7) . . ? N1 Ag1 Ag2 67.31(6) . . ? N5 Ag1 Ag2 68.87(6) . . ? N4 Ag2 N2 126.23(9) 3_576 . ? N4 Ag2 N6 120.18(8) 3_576 3_576 ? N2 Ag2 N6 109.84(8) . 3_576 ? N4 Ag2 O9 100.60(8) 3_576 . ? N2 Ag2 O9 100.99(8) . . ? N6 Ag2 O9 86.30(8) 3_576 . ? N4 Ag2 Ag1 114.88(6) 3_576 . ? N2 Ag2 Ag1 65.04(6) . . ? N6 Ag2 Ag1 69.35(6) 3_576 . ? O9 Ag2 Ag1 143.57(5) . . ? C1 S1 C2 88.52(15) . . ? C6 S2 C5 88.31(14) . . ? C10 S3 C9 88.02(14) . . ? O4 Cl1 O2 110.76(16) . . ? O4 Cl1 O1 108.73(17) . . ? O2 Cl1 O1 108.83(15) . . ? O4 Cl1 O3 110.75(15) . . ? O2 Cl1 O3 109.07(14) . . ? O1 Cl1 O3 108.64(15) . . ? O8 Cl2 O5 110.49(18) . . ? O8 Cl2 O7 110.3(2) . . ? O5 Cl2 O7 109.12(16) . . ? O8 Cl2 O6 109.7(2) . . ? O5 Cl2 O6 109.94(16) . . ? O7 Cl2 O6 107.20(15) . . ? Ag2 O9 H9A 114.5 . . ? Ag2 O9 H9B 104.2 . . ? H9A O9 H9B 106.9 . . ? H10A O10 H10B 106.9 . . ? C2 N1 N2 113.6(2) . . ? C2 N1 Ag1 133.3(2) . . ? N2 N1 Ag1 113.05(16) . . ? C1 N2 N1 112.5(2) . . ? C1 N2 Ag2 133.0(2) . . ? N1 N2 Ag2 114.45(16) . . ? C6 N3 N4 112.8(2) . . ? C6 N3 Ag1 125.29(19) . . ? N4 N3 Ag1 121.33(17) . . ? C5 N4 N3 112.6(2) . . ? C5 N4 Ag2 128.1(2) . 3_576 ? N3 N4 Ag2 117.62(17) . 3_576 ? C10 N5 N6 112.8(2) . . ? C10 N5 Ag1 129.59(19) . . ? N6 N5 Ag1 116.98(17) . . ? C9 N6 N5 112.7(2) . . ? C9 N6 Ag2 126.01(19) . 3_576 ? N5 N6 Ag2 120.40(17) . 3_576 ? N2 C1 C3 123.4(3) . . ? N2 C1 S1 112.9(2) . . ? C3 C1 S1 123.7(2) . . ? N1 C2 C4 123.2(3) . . ? N1 C2 S1 112.4(2) . . ? C4 C2 S1 124.3(2) . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N4 C5 C7 123.4(3) . . ? N4 C5 S2 113.2(2) . . ? C7 C5 S2 123.3(2) . . ? N3 C6 C8 122.6(3) . . ? N3 C6 S2 113.0(2) . . ? C8 C6 S2 124.3(2) . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N6 C9 C11 124.5(3) . . ? N6 C9 S3 113.5(2) . . ? C11 C9 S3 122.0(2) . . ? N5 C10 C12 124.4(3) . . ? N5 C10 S3 113.0(2) . . ? C12 C10 S3 122.6(2) . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? 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 N3 Ag1 Ag2 N4 -113.49(9) . . . 3_576 ? N1 Ag1 Ag2 N4 121.99(9) . . . 3_576 ? N5 Ag1 Ag2 N4 3.43(9) . . . 3_576 ? N3 Ag1 Ag2 N2 126.32(10) . . . . ? N1 Ag1 Ag2 N2 1.81(10) . . . . ? N5 Ag1 Ag2 N2 -116.75(9) . . . . ? N3 Ag1 Ag2 N6 1.18(9) . . . 3_576 ? N1 Ag1 Ag2 N6 -123.33(9) . . . 3_576 ? N5 Ag1 Ag2 N6 118.11(9) . . . 3_576 ? N3 Ag1 Ag2 O9 52.37(11) . . . . ? N1 Ag1 Ag2 O9 -72.14(11) . . . . ? N5 Ag1 Ag2 O9 169.30(11) . . . . ? N3 Ag1 N1 C2 73.7(3) . . . . ? N5 Ag1 N1 C2 -121.8(3) . . . . ? Ag2 Ag1 N1 C2 179.8(3) . . . . ? N3 Ag1 N1 N2 -109.09(19) . . . . ? N5 Ag1 N1 N2 55.4(2) . . . . ? Ag2 Ag1 N1 N2 -2.98(16) . . . . ? C2 N1 N2 C1 0.6(4) . . . . ? Ag1 N1 N2 C1 -177.2(2) . . . . ? C2 N1 N2 Ag2 -178.0(2) . . . . ? Ag1 N1 N2 Ag2 4.2(2) . . . . ? N4 Ag2 N2 C1 75.2(3) 3_576 . . . ? N6 Ag2 N2 C1 -126.8(3) 3_576 . . . ? O9 Ag2 N2 C1 -36.7(3) . . . . ? Ag1 Ag2 N2 C1 178.8(3) . . . . ? N4 Ag2 N2 N1 -106.54(19) 3_576 . . . ? N6 Ag2 N2 N1 51.4(2) 3_576 . . . ? O9 Ag2 N2 N1 141.46(18) . . . . ? Ag1 Ag2 N2 N1 -2.99(16) . . . . ? N1 Ag1 N3 C6 -39.2(3) . . . . ? N5 Ag1 N3 C6 158.6(2) . . . . ? Ag2 Ag1 N3 C6 -120.6(2) . . . . ? N1 Ag1 N3 N4 149.99(19) . . . . ? N5 Ag1 N3 N4 -12.2(2) . . . . ? Ag2 Ag1 N3 N4 68.5(2) . . . . ? C6 N3 N4 C5 1.2(4) . . . . ? Ag1 N3 N4 C5 173.1(2) . . . . ? C6 N3 N4 Ag2 -165.2(2) . . . 3_576 ? Ag1 N3 N4 Ag2 6.7(3) . . . 3_576 ? N3 Ag1 N5 C10 -160.8(2) . . . . ? N1 Ag1 N5 C10 33.4(3) . . . . ? Ag2 Ag1 N5 C10 90.7(3) . . . . ? N3 Ag1 N5 N6 9.2(2) . . . . ? N1 Ag1 N5 N6 -156.67(19) . . . . ? Ag2 Ag1 N5 N6 -99.3(2) . . . . ? C10 N5 N6 C9 -0.6(4) . . . . ? Ag1 N5 N6 C9 -172.2(2) . . . . ? C10 N5 N6 Ag2 169.3(2) . . . 3_576 ? Ag1 N5 N6 Ag2 -2.3(3) . . . 3_576 ? N1 N2 C1 C3 -179.7(3) . . . . ? Ag2 N2 C1 C3 -1.4(5) . . . . ? N1 N2 C1 S1 0.3(3) . . . . ? Ag2 N2 C1 S1 178.49(15) . . . . ? C2 S1 C1 N2 -0.7(2) . . . . ? C2 S1 C1 C3 179.2(3) . . . . ? N2 N1 C2 C4 177.6(3) . . . . ? Ag1 N1 C2 C4 -5.2(5) . . . . ? N2 N1 C2 S1 -1.2(3) . . . . ? Ag1 N1 C2 S1 176.05(15) . . . . ? C1 S1 C2 N1 1.1(2) . . . . ? C1 S1 C2 C4 -177.7(3) . . . . ? N3 N4 C5 C7 179.0(3) . . . . ? Ag2 N4 C5 C7 -16.4(4) 3_576 . . . ? N3 N4 C5 S2 -0.6(3) . . . . ? Ag2 N4 C5 S2 164.03(14) 3_576 . . . ? C6 S2 C5 N4 0.0(2) . . . . ? C6 S2 C5 C7 -179.6(3) . . . . ? N4 N3 C6 C8 177.6(3) . . . . ? Ag1 N3 C6 C8 6.1(4) . . . . ? N4 N3 C6 S2 -1.2(3) . . . . ? Ag1 N3 C6 S2 -172.73(14) . . . . ? C5 S2 C6 N3 0.7(2) . . . . ? C5 S2 C6 C8 -178.0(3) . . . . ? N5 N6 C9 C11 179.2(3) . . . . ? Ag2 N6 C9 C11 9.9(4) 3_576 . . . ? N5 N6 C9 S3 0.1(3) . . . . ? Ag2 N6 C9 S3 -169.15(14) 3_576 . . . ? C10 S3 C9 N6 0.3(2) . . . . ? C10 S3 C9 C11 -178.8(3) . . . . ? N6 N5 C10 C12 -179.5(3) . . . . ? Ag1 N5 C10 C12 -9.2(4) . . . . ? N6 N5 C10 S3 0.8(3) . . . . ? Ag1 N5 C10 S3 171.12(14) . . . . ? C9 S3 C10 N5 -0.6(2) . . . . ? C9 S3 C10 C12 179.7(3) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.961 _refine_diff_density_min -0.756 _refine_diff_density_rms 0.089 _database_code_depnum_ccdc_archive 'CCDC 929125' ####################################################################### # # 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_creation_date 2013-05-16 _audit_creation_method ; Olex2 1.2 (compiled Apr 23 2013 17:54:37, GUI svn.r4466) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C12 H12 Ag2 F6 N4 O4 S2' _chemical_formula_sum 'C12 H12 Ag2 F6 N4 O4 S2' _chemical_formula_weight 670.12 _chemical_melting_point ? 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, -y, -z' _cell_length_a 8.9829(13) _cell_length_b 11.1316(16) _cell_length_c 11.1548(16) _cell_angle_alpha 70.620(2) _cell_angle_beta 79.114(2) _cell_angle_gamma 74.141(2) _cell_volume 1006.2(3) _cell_formula_units_Z 2 _cell_measurement_reflns_used 2914 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 28.23 _cell_measurement_theta_min 2.73 _exptl_absorpt_coefficient_mu 2.235 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_correction_T_min 0.6133 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_process_details ; SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0999 before and 0.0286 after correction. The Ratio of minimum to maximum transmission is 0.8224. The \l/2 correction factor is 0.0015. ; _exptl_crystal_colour ? _exptl_crystal_density_diffrn 2.212 _exptl_crystal_density_meas . _exptl_crystal_density_method 'not measured' _exptl_crystal_description ? _exptl_crystal_F_000 648 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.13 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0228 _diffrn_reflns_av_unetI/netI 0.0358 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 5185 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_theta_min 1.95 _diffrn_ambient_temperature 296.15 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number 0 _reflns_number_gt 3122 _reflns_number_total 3528 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ? _computing_data_collection ? _computing_data_reduction ? _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; SHELXL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _refine_diff_density_max 0.704 _refine_diff_density_min -1.262 _refine_diff_density_rms 0.099 _refine_ls_extinction_coef 0.0448(17) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 338 _refine_ls_number_reflns 3528 _refine_ls_number_restraints 117 _refine_ls_R_factor_all 0.0405 _refine_ls_R_factor_gt 0.0363 _refine_ls_restrained_S_all 1.121 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0412P)^2^+1.4891P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0892 _refine_ls_wR_factor_ref 0.0937 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.5 times of: All C(H,H,H) groups 2. Restrained distances F4-C12 = F5-C12 = F6-C12 = F4'-C12 = F5'-C12 = F6'-C12 1.35 with sigma of 0.01 O3-O4 = O2B-O1A 2.2 with sigma of 0.01 O1B-O2A 2.2 with sigma of 0.01 F4-F5 \\sim F4-F6 \\sim F5-F6 with sigma of 0.001 F4'-F5' \\sim F4'-F6' \\sim F5'-F6' with sigma of 0.001 3. Uiso/Uaniso restraints and constraints F2B \\sim F2A: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(O1B) \\sim Ueq, Uanis(O1A) \\sim Ueq, Uanis(O2A) \\sim Ueq, Uanis(O2B) \\sim Ueq, Uanis(F2B) \\sim Ueq, Uanis(F2A) \\sim Ueq, Uanis(F3A) \\sim Ueq, Uanis(F3B) \\sim Ueq, Uanis(F1B) \\sim Ueq, Uanis(F1A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(F4') \\sim Ueq, Uanis(F4) \\sim Ueq, Uanis(F5') \\sim Ueq, Uanis(F5) \\sim Ueq, Uanis(F6') \\sim Ueq, Uanis(F6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(O1A) = Uanis(O1B) Uanis(O2A) = Uanis(O2B) 4. Others Sof(F4')=Sof(F5')=Sof(F6')=1-FVAR(1) Sof(F4)=Sof(F5)=Sof(F6)=FVAR(1) Sof(F1B)=Sof(F2B)=Sof(F3B)=Sof(O1B)=Sof(O2B)=1-FVAR(2) Sof(O2A)=Sof(O1A)=Sof(F2A)=Sof(F1A)=Sof(F3A)=FVAR(2) 5.a Idealised Me refined as rotating group: C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 Ag1 Ag 0.44787(4) 0.14202(4) 0.04984(3) 0.05039(18) Uani 1 1 d . . . Ag2 Ag 0.64077(5) 0.22815(4) 0.21944(4) 0.06183(19) Uani 1 1 d . . . S1 S 0.20700(16) 0.05449(14) 0.47666(13) 0.0609(4) Uani 1 1 d . A . S2 S 0.68765(17) 0.47726(14) -0.22942(13) 0.0614(4) Uani 1 1 d . A . F1B F 1.0308(9) 0.3907(10) 0.3525(9) 0.145(3) Uani 0.818(7) 1 d PU A 2 F2B F 0.8179(12) 0.5026(7) 0.4239(11) 0.130(4) Uani 0.818(7) 1 d PU A 2 F3B F 0.9152(10) 0.3124(6) 0.5327(5) 0.114(2) Uani 0.818(7) 1 d PU A 2 F4 F 0.9543(12) -0.2310(10) 0.2403(7) 0.103(4) Uani 0.619(19) 1 d PDU A 1 F5 F 1.0191(10) -0.1408(8) 0.0473(12) 0.126(6) Uani 0.619(19) 1 d PDU A 1 F6 F 0.8680(11) -0.2680(8) 0.0973(13) 0.108(5) Uani 0.619(19) 1 d PDU A 1 F4' F 0.8841(19) -0.2818(11) 0.2145(16) 0.128(9) Uani 0.381(19) 1 d PDU A 2 F5' F 1.0401(11) -0.1605(16) 0.131(2) 0.099(6) Uani 0.381(19) 1 d PDU A 2 F6' F 0.9211(17) -0.2083(18) 0.0158(14) 0.105(6) Uani 0.381(19) 1 d PDU A 2 O1B O 0.8696(13) 0.2731(11) 0.2791(10) 0.161(4) Uani 0.818(7) 1 d PDU A 2 O2B O 0.6699(12) 0.3566(11) 0.3627(11) 0.163(4) Uani 0.818(7) 1 d PDU A 1 O3 O 0.7746(4) 0.0064(4) 0.1949(3) 0.0611(9) Uani 1 1 d D A . O4 O 0.6621(4) -0.0452(4) 0.0643(4) 0.0670(10) Uani 1 1 d D . . N1 N 0.4087(4) 0.1637(4) 0.3227(4) 0.0453(8) Uani 1 1 d . A . N2 N 0.3424(4) 0.1131(4) 0.2535(3) 0.0452(9) Uani 1 1 d . . . N3 N 0.5659(4) 0.3042(4) -0.0665(3) 0.0451(9) Uani 1 1 d . . . N4 N 0.6416(4) 0.3492(4) 0.0009(4) 0.0456(9) Uani 1 1 d . A . C1 C 0.2348(5) 0.0545(5) 0.3204(5) 0.0498(11) Uani 1 1 d . A . C2 C 0.3474(5) 0.1424(4) 0.4401(4) 0.0463(10) Uani 1 1 d . . . C3 C 0.1455(7) -0.0067(7) 0.2672(6) 0.0710(16) Uani 1 1 d . . . H3A H 0.0448 0.0499 0.2514 0.107 Uiso 1 1 calc R A . H3B H 0.1335 -0.0891 0.3272 0.107 Uiso 1 1 calc R . . H3C H 0.2006 -0.0203 0.1885 0.107 Uiso 1 1 calc R . . C4 C 0.3938(7) 0.1905(6) 0.5340(5) 0.0628(13) Uani 1 1 d . A . H4A H 0.4841 0.2258 0.4974 0.094 Uiso 1 1 calc R . . H4B H 0.4173 0.1194 0.6100 0.094 Uiso 1 1 calc R . . H4C H 0.3098 0.2574 0.5551 0.094 Uiso 1 1 calc R . . C5 C 0.7103(5) 0.4397(4) -0.0711(5) 0.0456(10) Uani 1 1 d . . . C6 C 0.5800(5) 0.3615(5) -0.1881(5) 0.0503(11) Uani 1 1 d . A . C7 C 0.8021(7) 0.5042(6) -0.0246(6) 0.0676(15) Uani 1 1 d . A . H7A H 0.7528 0.5954 -0.0405 0.101 Uiso 1 1 calc R . . H7B H 0.9053 0.4951 -0.0687 0.101 Uiso 1 1 calc R . . H7C H 0.8076 0.4641 0.0655 0.101 Uiso 1 1 calc R . . C8 C 0.5116(8) 0.3288(7) -0.2811(6) 0.0765(17) Uani 1 1 d . . . H8A H 0.4411 0.2733 -0.2359 0.115 Uiso 1 1 calc R A . H8B H 0.5932 0.2841 -0.3307 0.115 Uiso 1 1 calc R . . H8C H 0.4561 0.4077 -0.3368 0.115 Uiso 1 1 calc R . . C9 C 0.8050(8) 0.3252(6) 0.3557(6) 0.0688(15) Uani 1 1 d . . . C10 C 0.8912(7) 0.3862(5) 0.4142(6) 0.0671(15) Uani 1 1 d . A . C11 C 0.7658(5) -0.0586(4) 0.1288(4) 0.0406(9) Uani 1 1 d . A . C12 C 0.9018(5) -0.1750(5) 0.1256(4) 0.0578(13) Uani 1 1 d D . . O2A O 0.736(4) 0.251(5) 0.468(2) 0.163(4) Uani 0.182(7) 1 d PDU A 2 O1A O 0.873(4) 0.194(4) 0.380(5) 0.161(4) Uani 0.182(7) 1 d PDU A 1 F2A F 0.778(6) 0.456(4) 0.479(4) 0.120(9) Uani 0.182(7) 1 d PU A 1 F1A F 0.915(4) 0.498(3) 0.319(3) 0.107(9) Uani 0.182(7) 1 d PU A 1 F3A F 1.016(4) 0.350(3) 0.449(4) 0.109(9) Uani 0.182(7) 1 d PU A 1 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 Ag1 0.0530(3) 0.0568(3) 0.0491(2) -0.01955(17) -0.00396(16) -0.02113(17) Ag2 0.0629(3) 0.0810(3) 0.0556(3) -0.0234(2) -0.00966(19) -0.0328(2) S1 0.0579(7) 0.0768(9) 0.0511(7) -0.0192(6) 0.0100(6) -0.0306(7) S2 0.0644(8) 0.0647(8) 0.0543(7) -0.0057(6) -0.0044(6) -0.0299(6) F1B 0.099(5) 0.189(8) 0.157(7) -0.019(6) -0.001(5) -0.096(5) F2B 0.158(7) 0.075(4) 0.189(10) -0.056(5) -0.092(7) -0.005(4) F3B 0.157(6) 0.119(4) 0.070(3) -0.022(3) -0.055(4) -0.020(4) F4 0.118(7) 0.084(6) 0.096(5) -0.023(4) -0.061(5) 0.025(5) F5 0.067(6) 0.105(6) 0.149(9) -0.013(6) 0.046(6) 0.004(4) F6 0.105(6) 0.072(5) 0.179(12) -0.077(7) -0.062(7) 0.012(4) F4' 0.122(12) 0.060(7) 0.142(14) 0.011(8) 0.019(10) 0.000(7) F5' 0.048(5) 0.106(10) 0.168(15) -0.081(11) -0.026(8) 0.000(6) F6' 0.104(10) 0.104(11) 0.110(10) -0.070(9) -0.035(8) 0.033(8) O1B 0.194(7) 0.172(7) 0.149(7) -0.096(6) -0.053(6) -0.011(6) O2B 0.129(6) 0.190(7) 0.216(8) -0.072(6) -0.047(5) -0.075(5) O3 0.064(2) 0.067(2) 0.065(2) -0.0339(18) -0.0177(18) -0.0119(17) O4 0.054(2) 0.068(2) 0.095(3) -0.041(2) -0.034(2) 0.0012(17) N1 0.0423(19) 0.056(2) 0.044(2) -0.0199(17) -0.0004(16) -0.0183(17) N2 0.0384(18) 0.056(2) 0.047(2) -0.0189(17) -0.0027(16) -0.0168(17) N3 0.0428(19) 0.053(2) 0.044(2) -0.0125(17) -0.0071(16) -0.0187(16) N4 0.0421(19) 0.051(2) 0.049(2) -0.0180(17) -0.0060(17) -0.0137(17) C1 0.043(2) 0.059(3) 0.051(3) -0.018(2) 0.000(2) -0.017(2) C2 0.044(2) 0.050(2) 0.045(2) -0.016(2) -0.0028(19) -0.0080(19) C3 0.062(3) 0.093(4) 0.074(4) -0.028(3) 0.002(3) -0.045(3) C4 0.070(3) 0.075(3) 0.051(3) -0.029(3) -0.001(2) -0.019(3) C5 0.037(2) 0.044(2) 0.056(3) -0.017(2) -0.0033(19) -0.0092(18) C6 0.044(2) 0.056(3) 0.051(3) -0.013(2) -0.008(2) -0.013(2) C7 0.060(3) 0.067(3) 0.089(4) -0.030(3) -0.007(3) -0.028(3) C8 0.087(4) 0.099(4) 0.058(3) -0.019(3) -0.020(3) -0.042(4) C9 0.079(4) 0.062(3) 0.073(4) -0.022(3) -0.021(3) -0.016(3) C10 0.069(4) 0.055(3) 0.083(4) -0.016(3) -0.027(3) -0.017(3) C11 0.037(2) 0.044(2) 0.043(2) -0.0123(19) -0.0066(18) -0.0127(18) C12 0.053(3) 0.060(3) 0.064(3) -0.022(3) -0.015(3) -0.009(2) O2A 0.129(6) 0.190(7) 0.216(8) -0.072(6) -0.047(5) -0.075(5) O1A 0.194(7) 0.172(7) 0.149(7) -0.096(6) -0.053(6) -0.011(6) F2A 0.149(15) 0.103(15) 0.138(16) -0.079(12) -0.019(13) -0.023(13) F1A 0.137(18) 0.079(13) 0.120(16) -0.020(12) -0.012(14) -0.063(13) F3A 0.079(14) 0.114(16) 0.133(19) -0.034(15) -0.055(14) 0.004(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 Ag1 Ag2 3.2941(6) . ? Ag1 O4 2.403(3) . ? Ag1 O4 2.393(3) 2_655 ? Ag1 N2 2.243(4) . ? Ag1 N3 2.245(4) . ? Ag2 O1B 2.494(10) . ? Ag2 O2B 2.558(10) . ? Ag2 O3 2.513(4) . ? Ag2 N1 2.356(4) . ? Ag2 N4 2.361(4) . ? S1 C1 1.713(5) . ? S1 C2 1.712(5) . ? S2 C5 1.713(5) . ? S2 C6 1.711(5) . ? F1B C10 1.317(9) . ? F2B C10 1.313(10) . ? F3B C10 1.326(8) . ? F4 C12 1.337(6) . ? F5 C12 1.292(7) . ? F6 C12 1.299(7) . ? F4' C12 1.297(8) . ? F5' C12 1.310(8) . ? F6' C12 1.362(8) . ? O1B C9 1.166(10) . ? O2B C9 1.162(11) . ? O3 C11 1.217(5) . ? O4 Ag1 2.393(3) 2_655 ? O4 C11 1.230(5) . ? N1 N2 1.383(5) . ? N1 C2 1.292(6) . ? N2 C1 1.291(6) . ? N3 N4 1.381(5) . ? N3 C6 1.292(6) . ? N4 C5 1.287(6) . ? C1 C3 1.486(7) . ? C2 C4 1.488(7) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 C7 1.483(7) . ? C6 C8 1.483(7) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 C10 1.503(8) . ? C9 O2A 1.39(3) . ? C9 O1A 1.38(3) . ? C10 F2A 1.35(4) . ? C10 F1A 1.38(2) . ? C10 F3A 1.18(2) . ? C11 C12 1.524(6) . ? 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 O4 Ag1 Ag2 85.35(8) . . ? O4 Ag1 Ag2 170.48(8) 2_655 . ? O4 Ag1 O4 85.34(11) 2_655 . ? N2 Ag1 Ag2 67.12(9) . . ? N2 Ag1 O4 113.22(14) . 2_655 ? N2 Ag1 O4 102.93(14) . . ? N2 Ag1 N3 125.28(14) . . ? N3 Ag1 Ag2 66.73(9) . . ? N3 Ag1 O4 117.17(14) . 2_655 ? N3 Ag1 O4 101.01(14) . . ? O1B Ag2 Ag1 156.9(2) . . ? O1B Ag2 O2B 46.5(3) . . ? O1B Ag2 O3 96.6(2) . . ? O2B Ag2 Ag1 154.6(2) . . ? O3 Ag2 Ag1 69.10(8) . . ? O3 Ag2 O2B 133.8(3) . . ? N1 Ag2 Ag1 63.52(9) . . ? N1 Ag2 O1B 137.7(3) . . ? N1 Ag2 O2B 99.6(2) . . ? N1 Ag2 O3 93.75(13) . . ? N1 Ag2 N4 116.73(13) . . ? N4 Ag2 Ag1 64.15(9) . . ? N4 Ag2 O1B 102.0(3) . . ? N4 Ag2 O2B 113.7(3) . . ? N4 Ag2 O3 98.64(12) . . ? C2 S1 C1 88.2(2) . . ? C6 S2 C5 88.6(2) . . ? C9 O1B Ag2 98.7(7) . . ? C9 O2B Ag2 95.5(7) . . ? C11 O3 Ag2 136.4(3) . . ? Ag1 O4 Ag1 94.66(11) 2_655 . ? C11 O4 Ag1 118.2(3) . . ? C11 O4 Ag1 146.7(3) . 2_655 ? N2 N1 Ag2 114.2(3) . . ? C2 N1 Ag2 131.9(3) . . ? C2 N1 N2 112.3(4) . . ? N1 N2 Ag1 114.2(3) . . ? C1 N2 Ag1 132.5(3) . . ? C1 N2 N1 113.3(4) . . ? N4 N3 Ag1 115.8(3) . . ? C6 N3 Ag1 131.0(3) . . ? C6 N3 N4 113.2(4) . . ? N3 N4 Ag2 113.2(3) . . ? C5 N4 Ag2 133.5(3) . . ? C5 N4 N3 113.0(4) . . ? N2 C1 S1 112.8(4) . . ? N2 C1 C3 123.4(5) . . ? C3 C1 S1 123.9(4) . . ? N1 C2 S1 113.4(4) . . ? N1 C2 C4 123.2(4) . . ? C4 C2 S1 123.4(4) . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3B 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4B 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N4 C5 S2 112.7(3) . . ? N4 C5 C7 124.5(5) . . ? C7 C5 S2 122.7(4) . . ? N3 C6 S2 112.5(4) . . ? N3 C6 C8 123.4(5) . . ? C8 C6 S2 124.1(4) . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7B 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O1B C9 C10 120.4(8) . . ? O1B C9 O2A 117.5(19) . . ? O1B C9 O1A 54(2) . . ? O2B C9 O1B 118.0(9) . . ? O2B C9 C10 119.0(8) . . ? O2B C9 O2A 68.3(19) . . ? O2B C9 O1A 118(2) . . ? O2A C9 C10 98.2(15) . . ? O1A C9 C10 109.2(17) . . ? O1A C9 O2A 68(3) . . ? F1B C10 F3B 105.4(7) . . ? F1B C10 C9 111.0(7) . . ? F1B C10 F2A 139.0(18) . . ? F1B C10 F1A 60.1(15) . . ? F2B C10 F1B 109.7(7) . . ? F2B C10 F3B 105.3(7) . . ? F2B C10 C9 114.9(6) . . ? F2B C10 F2A 33.4(17) . . ? F2B C10 F1A 58.8(14) . . ? F3B C10 C9 110.0(6) . . ? F3B C10 F2A 80(2) . . ? F3B C10 F1A 145.4(13) . . ? F2A C10 C9 104.3(19) . . ? F2A C10 F1A 92(2) . . ? F1A C10 C9 104.7(13) . . ? F3A C10 F1B 48(2) . . ? F3A C10 F2B 113.5(16) . . ? F3A C10 F3B 58(2) . . ? F3A C10 C9 131.5(16) . . ? F3A C10 F2A 117(3) . . ? F3A C10 F1A 98(2) . . ? O3 C11 O4 129.5(4) . . ? O3 C11 C12 115.9(4) . . ? O4 C11 C12 114.6(4) . . ? F4 C12 F6' 135.8(7) . . ? F4 C12 C11 110.5(5) . . ? F5 C12 F4 105.8(4) . . ? F5 C12 F6 108.0(5) . . ? F5 C12 F4' 133.4(8) . . ? F5 C12 F5' 41.8(6) . . ? F5 C12 F6' 66.4(6) . . ? F5 C12 C11 112.1(5) . . ? F6 C12 F4 105.4(4) . . ? F6 C12 F5' 127.8(8) . . ? F6 C12 F6' 46.5(6) . . ? F6 C12 C11 114.4(5) . . ? F4' C12 F4 48.6(7) . . ? F4' C12 F6 59.9(7) . . ? F4' C12 F5' 106.5(6) . . ? F4' C12 F6' 103.5(6) . . ? F4' C12 C11 113.5(7) . . ? F5' C12 F4 65.3(6) . . ? F5' C12 F6' 102.8(6) . . ? F5' C12 C11 116.7(7) . . ? F6' C12 C11 112.5(6) . . ? 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 Ag1 Ag2 O1B C9 168.5(3) . . . . ? Ag1 Ag2 O2B C9 -170.0(3) . . . . ? Ag1 Ag2 O3 C11 13.4(4) . . . . ? Ag1 Ag2 N1 N2 7.7(2) . . . . ? Ag1 Ag2 N1 C2 171.9(4) . . . . ? Ag1 Ag2 N4 N3 -3.2(2) . . . . ? Ag1 Ag2 N4 C5 -175.2(4) . . . . ? Ag1 O4 C11 O3 -165.2(4) 2_655 . . . ? Ag1 O4 C11 O3 4.4(7) . . . . ? Ag1 O4 C11 C12 14.1(8) 2_655 . . . ? Ag1 O4 C11 C12 -176.3(3) . . . . ? Ag1 N2 C1 S1 176.6(2) . . . . ? Ag1 N2 C1 C3 -3.1(7) . . . . ? Ag1 N3 N4 Ag2 4.7(3) . . . . ? Ag1 N3 N4 C5 178.4(3) . . . . ? Ag1 N3 C6 S2 -178.0(2) . . . . ? Ag1 N3 C6 C8 1.3(8) . . . . ? Ag2 Ag1 O4 Ag1 178.01(12) . . . 2_655 ? Ag2 Ag1 O4 C11 3.7(4) . . . . ? Ag2 Ag1 N2 N1 7.9(2) . . . . ? Ag2 Ag1 N2 C1 -169.6(4) . . . . ? Ag2 Ag1 N3 N4 -3.4(2) . . . . ? Ag2 Ag1 N3 C6 174.2(4) . . . . ? Ag2 O1B C9 O2B -12.0(11) . . . . ? Ag2 O1B C9 C10 -173.7(5) . . . . ? Ag2 O1B C9 O2A 67(2) . . . . ? Ag2 O1B C9 O1A 94(2) . . . . ? Ag2 O2B C9 O1B 11.6(11) . . . . ? Ag2 O2B C9 C10 173.6(5) . . . . ? Ag2 O2B C9 O2A -99.0(17) . . . . ? Ag2 O2B C9 O1A -51(2) . . . . ? Ag2 O3 C11 O4 -15.9(8) . . . . ? Ag2 O3 C11 C12 164.7(3) . . . . ? Ag2 N1 N2 Ag1 -11.1(3) . . . . ? Ag2 N1 N2 C1 166.8(3) . . . . ? Ag2 N1 C2 S1 -162.8(2) . . . . ? Ag2 N1 C2 C4 17.7(7) . . . . ? Ag2 N4 C5 S2 171.9(2) . . . . ? Ag2 N4 C5 C7 -7.1(7) . . . . ? O1B Ag2 O2B C9 -6.6(6) . . . . ? O1B Ag2 O3 C11 -147.9(5) . . . . ? O1B Ag2 N1 N2 -160.7(4) . . . . ? O1B Ag2 N1 C2 3.5(6) . . . . ? O1B Ag2 N4 N3 157.1(3) . . . . ? O1B Ag2 N4 C5 -14.8(5) . . . . ? O1B C9 C10 F1B 10.7(11) . . . . ? O1B C9 C10 F2B 135.9(11) . . . . ? O1B C9 C10 F3B -105.5(10) . . . . ? O1B C9 C10 F2A 170(2) . . . . ? O1B C9 C10 F1A 73.9(19) . . . . ? O1B C9 C10 F3A -41(3) . . . . ? O2B Ag2 O1B C9 6.6(6) . . . . ? O2B Ag2 O3 C11 -179.7(5) . . . . ? O2B Ag2 N1 N2 167.7(4) . . . . ? O2B Ag2 N1 C2 -28.1(5) . . . . ? O2B Ag2 N4 N3 -155.3(3) . . . . ? O2B Ag2 N4 C5 32.7(5) . . . . ? O2B C9 C10 F1B -150.8(10) . . . . ? O2B C9 C10 F2B -25.6(13) . . . . ? O2B C9 C10 F3B 93.0(10) . . . . ? O2B C9 C10 F2A 8(2) . . . . ? O2B C9 C10 F1A -87.6(19) . . . . ? O2B C9 C10 F3A 157(3) . . . . ? O3 Ag2 O1B C9 -141.7(7) . . . . ? O3 Ag2 O2B C9 39.7(9) . . . . ? O3 Ag2 N1 N2 -56.7(3) . . . . ? O3 Ag2 N1 C2 107.5(4) . . . . ? O3 Ag2 N4 N3 58.5(3) . . . . ? O3 Ag2 N4 C5 -113.5(4) . . . . ? O3 C11 C12 F4 36.8(8) . . . . ? O3 C11 C12 F5 -80.9(9) . . . . ? O3 C11 C12 F6 155.5(8) . . . . ? O3 C11 C12 F4' 89.3(13) . . . . ? O3 C11 C12 F5' -35.0(12) . . . . ? O3 C11 C12 F6' -153.6(11) . . . . ? O4 Ag1 Ag2 O1B 61.1(9) 2_655 . . . ? O4 Ag1 Ag2 O1B 49.1(7) . . . . ? O4 Ag1 Ag2 O2B -162.8(6) . . . . ? O4 Ag1 Ag2 O2B -150.7(9) 2_655 . . . ? O4 Ag1 Ag2 O3 -5.26(14) . . . . ? O4 Ag1 Ag2 O3 6.8(7) 2_655 . . . ? O4 Ag1 Ag2 N1 -110.83(15) . . . . ? O4 Ag1 Ag2 N1 -98.8(7) 2_655 . . . ? O4 Ag1 Ag2 N4 118.1(7) 2_655 . . . ? O4 Ag1 Ag2 N4 106.06(15) . . . . ? O4 Ag1 O4 Ag1 0.0 2_655 . . 2_655 ? O4 Ag1 O4 C11 -174.3(5) 2_655 . . . ? O4 Ag1 N2 N1 177.5(3) 2_655 . . . ? O4 Ag1 N2 N1 87.1(3) . . . . ? O4 Ag1 N2 C1 -90.4(4) . . . . ? O4 Ag1 N2 C1 0.1(5) 2_655 . . . ? O4 Ag1 N3 N4 -83.4(3) . . . . ? O4 Ag1 N3 N4 -173.8(3) 2_655 . . . ? O4 Ag1 N3 C6 94.2(4) . . . . ? O4 Ag1 N3 C6 3.8(5) 2_655 . . . ? O4 C11 C12 F4 -142.6(7) . . . . ? O4 C11 C12 F5 99.6(9) . . . . ? O4 C11 C12 F6 -23.9(9) . . . . ? O4 C11 C12 F4' -90.1(13) . . . . ? O4 C11 C12 F5' 145.5(11) . . . . ? O4 C11 C12 F6' 27.0(11) . . . . ? N1 Ag2 O1B C9 -38.7(9) . . . . ? N1 Ag2 O2B C9 144.4(7) . . . . ? N1 Ag2 O3 C11 73.2(5) . . . . ? N1 Ag2 N4 N3 -40.2(3) . . . . ? N1 Ag2 N4 C5 147.8(4) . . . . ? N1 N2 C1 S1 -0.9(5) . . . . ? N1 N2 C1 C3 179.4(5) . . . . ? N2 Ag1 Ag2 O1B 155.2(7) . . . . ? N2 Ag1 Ag2 O2B -56.6(6) . . . . ? N2 Ag1 Ag2 O3 100.89(14) . . . . ? N2 Ag1 Ag2 N1 -4.69(15) . . . . ? N2 Ag1 Ag2 N4 -147.79(14) . . . . ? N2 Ag1 O4 Ag1 112.78(14) . . . 2_655 ? N2 Ag1 O4 C11 -61.5(4) . . . . ? N2 Ag1 N3 N4 31.3(3) . . . . ? N2 Ag1 N3 C6 -151.1(4) . . . . ? N2 N1 C2 S1 1.7(5) . . . . ? N2 N1 C2 C4 -177.9(4) . . . . ? N3 Ag1 Ag2 O1B -55.0(7) . . . . ? N3 Ag1 Ag2 O2B 93.1(6) . . . . ? N3 Ag1 Ag2 O3 -109.36(14) . . . . ? N3 Ag1 Ag2 N1 145.07(15) . . . . ? N3 Ag1 Ag2 N4 1.96(14) . . . . ? N3 Ag1 O4 Ag1 -116.80(14) . . . 2_655 ? N3 Ag1 O4 C11 68.9(4) . . . . ? N3 Ag1 N2 N1 -26.7(3) . . . . ? N3 Ag1 N2 C1 155.9(4) . . . . ? N3 N4 C5 S2 -0.1(5) . . . . ? N3 N4 C5 C7 -179.1(4) . . . . ? N4 Ag2 O1B C9 118.0(7) . . . . ? N4 Ag2 O2B C9 -90.7(7) . . . . ? N4 Ag2 O3 C11 -44.6(5) . . . . ? N4 Ag2 N1 N2 44.9(3) . . . . ? N4 Ag2 N1 C2 -150.9(4) . . . . ? N4 N3 C6 S2 -0.4(5) . . . . ? N4 N3 C6 C8 178.9(5) . . . . ? C1 S1 C2 N1 -1.8(4) . . . . ? C1 S1 C2 C4 177.7(4) . . . . ? C2 S1 C1 N2 1.5(4) . . . . ? C2 S1 C1 C3 -178.8(5) . . . . ? C2 N1 N2 Ag1 -178.5(3) . . . . ? C2 N1 N2 C1 -0.5(5) . . . . ? C5 S2 C6 N3 0.3(4) . . . . ? C5 S2 C6 C8 -179.0(5) . . . . ? C6 S2 C5 N4 -0.1(4) . . . . ? C6 S2 C5 C7 178.9(4) . . . . ? C6 N3 N4 Ag2 -173.3(3) . . . . ? C6 N3 N4 C5 0.3(5) . . . . ? O2A C9 C10 F1B 140(2) . . . . ? O2A C9 C10 F2B -95(2) . . . . ? O2A C9 C10 F3B 23(2) . . . . ? O2A C9 C10 F2A -62(3) . . . . ? O2A C9 C10 F1A -157(3) . . . . ? O2A C9 C10 F3A 88(4) . . . . ? O1A C9 C10 F1B 70(3) . . . . ? O1A C9 C10 F2B -165(3) . . . . ? O1A C9 C10 F3B -46(3) . . . . ? O1A C9 C10 F2A -131(3) . . . . ? O1A C9 C10 F1A 133(3) . . . . ? O1A C9 C10 F3A 18(4) . . . . ? _database_code_depnum_ccdc_archive 'CCDC 929124' ####################################################################### # # 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_date 2013-05-16 _audit_creation_method ; Olex2 1.2 (compiled Apr 23 2013 17:54:37, GUI svn.r4466) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C16 H24 Ag2 N8 S3, 4(As0.5 F3)' _chemical_formula_sum 'C16 H24 Ag2 As2 F12 N8 S3' _chemical_formula_weight 1018.19 _chemical_melting_point ? 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' S S 0.1246 0.1234 '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' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system orthorhombic _space_group_IT_number 56 _space_group_name_H-M_alt 'P c c n' _space_group_name_Hall '-P 2ab 2ac' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x+1/2, -y+1/2, z' 3 '-x, y+1/2, -z+1/2' 4 'x+1/2, -y, -z+1/2' 5 '-x, -y, -z' 6 'x-1/2, y-1/2, -z' 7 'x, -y-1/2, z-1/2' 8 '-x-1/2, y, z-1/2' _cell_length_a 12.862(2) _cell_length_b 19.608(4) _cell_length_c 26.579(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6703(2) _cell_formula_units_Z 8 _cell_measurement_reflns_used 4356 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 0.00 _cell_measurement_theta_min 0.00 _exptl_absorpt_coefficient_mu 3.405 _exptl_absorpt_correction_T_max ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_crystal_colour ? _exptl_crystal_density_diffrn 2.018 _exptl_crystal_density_meas . _exptl_crystal_density_method 'not measured' _exptl_crystal_description ? _exptl_crystal_F_000 3936 _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.16 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0650 _diffrn_reflns_av_unetI/netI 0.0467 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_number 32751 _diffrn_reflns_theta_full 25.01 _diffrn_reflns_theta_max 25.01 _diffrn_reflns_theta_min 1.53 _diffrn_ambient_temperature 296.15 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 3346 _reflns_number_total 5909 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ? _computing_data_collection ? _computing_data_reduction ? _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; SHELXL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _refine_diff_density_max 1.013 _refine_diff_density_min -1.015 _refine_diff_density_rms 0.104 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 398 _refine_ls_number_reflns 5909 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.1007 _refine_ls_R_factor_gt 0.0500 _refine_ls_restrained_S_all 1.269 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0789P)^2^+9.3985P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1345 _refine_ls_wR_factor_ref 0.1626 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.5 times of: All C(H,H,H) groups 2. Uiso/Uaniso restraints and constraints F1 \\sim F2 \\sim F3 \\sim As1: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02 F4 \\sim F5 \\sim F6: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02 F11 \\sim F7 \\sim F12 \\sim F8 \\sim F9 \\sim F10: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02 F5 \\sim F4 \\sim F6 \\sim As2: within 1.7A with sigma of 0.005 and sigma for terminal atoms of 0.01 Uanis(F6) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01 3.a Idealised Me refined as rotating group: C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C11(H11A, H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 Ag1 Ag 0.02198(7) 0.12841(5) 0.18173(3) 0.0736(3) Uani 1 1 d . . . Ag2 Ag 0.00233(6) 0.18122(5) 0.05796(3) 0.0729(3) Uani 1 1 d . . . As1 As 0.0000 0.5000 0.0000 0.0587(4) Uani 1 2 d SU . . As2 As 0.2500 0.2500 0.35774(5) 0.0697(5) Uani 1 2 d SU . . As3 As 0.21358(10) -0.06551(8) 0.16582(5) 0.0849(4) Uani 1 1 d . . . S1 S -0.1680(3) 0.3415(2) 0.17470(15) 0.0990(11) Uani 1 1 d . . . S2 S -0.1594(2) -0.04013(18) 0.08297(11) 0.0841(10) Uani 1 1 d . . . S3 S 0.3582(2) 0.14921(17) 0.10751(11) 0.0740(8) Uani 1 1 d . . . N1 N -0.0631(6) 0.2331(5) 0.1687(3) 0.070(2) Uani 1 1 d . . . N2 N -0.0861(6) 0.2504(5) 0.1200(3) 0.066(2) Uani 1 1 d . . . N3 N -0.0725(6) 0.0583(5) 0.1269(3) 0.059(2) Uani 1 1 d . . . N4 N -0.0766(6) 0.0755(5) 0.0764(3) 0.060(2) Uani 1 1 d . . . N5 N 0.1756(6) 0.1612(5) 0.1401(3) 0.061(2) Uani 1 1 d . . . N6 N 0.1684(6) 0.1640(4) 0.0879(3) 0.056(2) Uani 1 1 d . . . N7 N 0.0387(9) 0.0948(6) 0.2610(3) 0.091(3) Uani 1 1 d . . . N8 N -0.0322(8) 0.2218(6) -0.0183(4) 0.096(4) Uani 1 1 d . . . F1 F 0.1125(7) 0.4990(6) -0.0297(5) 0.168(4) Uani 1 1 d U . . F2 F -0.0138(7) 0.4200(5) -0.0206(4) 0.144(3) Uani 1 1 d U . . F3 F -0.0519(12) 0.5322(7) -0.0500(4) 0.202(5) Uani 1 1 d U . . F4 F 0.1660(8) 0.2569(9) 0.4017(4) 0.211(4) Uani 1 1 d U . . F5 F 0.1619(8) 0.2497(8) 0.3141(3) 0.191(4) Uani 1 1 d U . . F6 F 0.2869(12) 0.3285(7) 0.3592(6) 0.232(5) Uani 1 1 d U . . F7 F 0.2785(10) -0.0778(8) 0.1121(4) 0.209(6) Uani 1 1 d . . . F8 F 0.2741(9) -0.1332(6) 0.1907(5) 0.193(5) Uani 1 1 d . . . F9 F 0.1504(11) -0.0555(9) 0.2176(4) 0.237(7) Uani 1 1 d . . . F10 F 0.1560(9) 0.0002(6) 0.1386(5) 0.192(5) Uani 1 1 d . . . F11 F 0.3128(9) -0.0163(7) 0.1849(5) 0.187(5) Uani 1 1 d . . . F12 F 0.1157(10) -0.1125(7) 0.1471(6) 0.209(5) Uani 1 1 d . . . C1 C -0.1401(8) 0.3071(6) 0.1172(4) 0.072(3) Uani 1 1 d . . . C2 C -0.1004(9) 0.2754(7) 0.2028(5) 0.082(4) Uani 1 1 d . . . C3 C -0.1744(9) 0.3379(7) 0.0683(5) 0.098(4) Uani 1 1 d . . . H3A H -0.1477 0.3834 0.0656 0.147 Uiso 1 1 calc R . . H3B H -0.2490 0.3390 0.0671 0.147 Uiso 1 1 calc R . . H3C H -0.1486 0.3109 0.0409 0.147 Uiso 1 1 calc R . . C4 C -0.0846(11) 0.2664(8) 0.2569(4) 0.110(5) Uani 1 1 d . . . H4A H -0.1465 0.2476 0.2716 0.165 Uiso 1 1 calc R . . H4B H -0.0697 0.3097 0.2721 0.165 Uiso 1 1 calc R . . H4C H -0.0274 0.2359 0.2625 0.165 Uiso 1 1 calc R . . C5 C -0.1207(8) 0.0290(6) 0.0491(4) 0.066(3) Uani 1 1 d . . . C6 C -0.1121(8) -0.0004(7) 0.1364(4) 0.065(3) Uani 1 1 d . . . C7 C -0.1365(9) 0.0358(7) -0.0066(4) 0.085(4) Uani 1 1 d . . . H7A H -0.2090 0.0429 -0.0135 0.128 Uiso 1 1 calc R . . H7B H -0.1135 -0.0051 -0.0230 0.128 Uiso 1 1 calc R . . H7C H -0.0972 0.0739 -0.0188 0.128 Uiso 1 1 calc R . . C8 C -0.1213(10) -0.0323(8) 0.1878(4) 0.102(5) Uani 1 1 d . . . H8A H -0.0677 -0.0146 0.2093 0.153 Uiso 1 1 calc R . . H8B H -0.1139 -0.0809 0.1850 0.153 Uiso 1 1 calc R . . H8C H -0.1881 -0.0217 0.2019 0.153 Uiso 1 1 calc R . . C9 C 0.2566(8) 0.1575(5) 0.0660(4) 0.058(3) Uani 1 1 d . . . C10 C 0.2688(8) 0.1540(5) 0.1559(4) 0.060(3) Uani 1 1 d . . . C11 C 0.2703(8) 0.1582(7) 0.0095(4) 0.080(4) Uani 1 1 d . . . H11A H 0.2945 0.1144 -0.0015 0.119 Uiso 1 1 calc R . . H11B H 0.3202 0.1925 0.0005 0.119 Uiso 1 1 calc R . . H11C H 0.2049 0.1682 -0.0062 0.119 Uiso 1 1 calc R . . C12 C 0.2990(10) 0.1498(8) 0.2099(4) 0.098(4) Uani 1 1 d . . . H12A H 0.3539 0.1818 0.2166 0.148 Uiso 1 1 calc R . . H12B H 0.3227 0.1045 0.2174 0.148 Uiso 1 1 calc R . . H12C H 0.2400 0.1604 0.2306 0.148 Uiso 1 1 calc R . . C13 C 0.0446(9) 0.0727(7) 0.2991(4) 0.074(3) Uani 1 1 d . . . C14 C 0.0521(12) 0.0433(8) 0.3496(4) 0.111(5) Uani 1 1 d . . . H14A H -0.0164 0.0341 0.3622 0.167 Uiso 1 1 calc R . . H14B H 0.0867 0.0749 0.3715 0.167 Uiso 1 1 calc R . . H14C H 0.0910 0.0016 0.3481 0.167 Uiso 1 1 calc R . . C15 C -0.0505(10) 0.2438(8) -0.0555(5) 0.089(4) Uani 1 1 d . . . C16 C -0.0778(12) 0.2756(10) -0.1033(5) 0.137(7) Uani 1 1 d . . . H16A H -0.1517 0.2733 -0.1081 0.206 Uiso 1 1 calc R . . H16B H -0.0435 0.2520 -0.1302 0.206 Uiso 1 1 calc R . . H16C H -0.0561 0.3225 -0.1031 0.206 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0823(6) 0.0848(7) 0.0537(5) 0.0065(4) 0.0007(4) 0.0024(5) Ag2 0.0727(6) 0.0843(7) 0.0616(5) 0.0180(5) -0.0040(4) 0.0044(5) As1 0.0581(8) 0.0630(11) 0.0549(8) 0.0011(7) 0.0000(6) 0.0102(7) As2 0.0832(11) 0.0718(13) 0.0540(8) 0.000 0.000 -0.0035(9) As3 0.0781(8) 0.0768(10) 0.0999(9) 0.0109(8) 0.0081(7) 0.0107(7) S1 0.097(2) 0.070(2) 0.130(3) -0.010(2) 0.021(2) 0.017(2) S2 0.094(2) 0.081(3) 0.0772(18) 0.0015(17) -0.0073(16) -0.0236(19) S3 0.0579(16) 0.082(2) 0.0822(18) -0.0059(17) -0.0041(13) 0.0016(15) N1 0.061(5) 0.074(7) 0.077(6) -0.005(5) -0.001(4) 0.010(5) N2 0.055(5) 0.061(6) 0.081(6) 0.004(5) 0.008(4) 0.009(5) N3 0.060(5) 0.060(6) 0.057(5) 0.008(4) -0.001(4) -0.005(5) N4 0.055(5) 0.070(7) 0.056(5) 0.009(5) 0.002(4) 0.002(5) N5 0.058(5) 0.066(6) 0.058(5) 0.007(4) 0.001(4) 0.002(4) N6 0.055(5) 0.062(6) 0.051(4) 0.008(4) -0.003(4) 0.004(4) N7 0.122(8) 0.102(9) 0.049(5) 0.012(6) -0.008(5) -0.009(7) N8 0.105(8) 0.113(10) 0.071(6) 0.037(6) -0.005(6) 0.009(7) F1 0.122(7) 0.132(8) 0.249(10) -0.017(8) 0.085(7) -0.011(6) F2 0.167(8) 0.081(6) 0.183(9) -0.042(6) 0.028(6) -0.019(5) F3 0.288(12) 0.208(12) 0.111(6) 0.000(7) -0.067(8) 0.119(10) F4 0.136(6) 0.376(11) 0.122(6) -0.031(8) 0.036(6) -0.021(8) F5 0.137(6) 0.307(10) 0.129(6) 0.038(7) -0.040(5) -0.012(8) F6 0.253(8) 0.158(7) 0.287(8) -0.013(7) 0.016(7) -0.022(7) F7 0.202(11) 0.262(16) 0.161(9) 0.028(10) 0.069(8) 0.061(11) F8 0.169(9) 0.169(11) 0.240(12) 0.100(10) -0.006(9) 0.054(8) F9 0.229(13) 0.34(2) 0.146(9) -0.030(11) 0.057(9) 0.090(13) F10 0.172(10) 0.119(9) 0.286(14) 0.047(9) -0.051(9) 0.037(8) F11 0.151(9) 0.183(12) 0.228(11) 0.011(10) -0.038(8) -0.035(8) F12 0.185(11) 0.158(11) 0.283(15) 0.000(11) -0.061(11) -0.048(9) C1 0.058(6) 0.058(8) 0.100(8) 0.018(7) 0.007(6) -0.013(6) C2 0.068(7) 0.075(9) 0.102(9) -0.021(7) 0.020(6) -0.001(6) C3 0.075(8) 0.073(10) 0.148(12) 0.050(9) 0.018(7) 0.012(7) C4 0.130(12) 0.125(14) 0.076(8) -0.021(8) 0.006(8) 0.017(10) C5 0.052(6) 0.081(9) 0.065(6) 0.004(6) 0.004(5) 0.002(6) C6 0.059(6) 0.075(9) 0.061(6) 0.003(6) -0.006(5) -0.002(6) C7 0.081(8) 0.117(12) 0.057(6) -0.003(7) -0.005(5) 0.001(8) C8 0.113(10) 0.111(12) 0.082(8) 0.038(8) -0.006(7) -0.026(9) C9 0.062(6) 0.044(6) 0.069(6) 0.000(5) -0.003(5) 0.006(5) C10 0.063(6) 0.051(7) 0.065(6) -0.002(5) -0.004(5) 0.000(5) C11 0.070(7) 0.101(11) 0.068(7) 0.003(7) 0.009(5) 0.019(7) C12 0.104(9) 0.116(13) 0.075(7) -0.005(8) -0.027(7) -0.004(9) C13 0.077(7) 0.081(9) 0.062(7) 0.004(7) 0.003(6) -0.007(7) C14 0.118(11) 0.142(15) 0.074(8) 0.032(9) -0.025(7) -0.012(10) C15 0.087(8) 0.106(12) 0.073(8) 0.026(8) -0.002(6) 0.012(8) C16 0.132(13) 0.191(19) 0.089(9) 0.058(11) -0.018(9) 0.011(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.351(10) . ? Ag1 N3 2.343(8) . ? Ag1 N5 2.353(8) . ? Ag1 N7 2.218(9) . ? Ag2 N2 2.419(8) . ? Ag2 N4 2.359(9) . ? Ag2 N6 2.304(7) . ? Ag2 N8 2.222(10) . ? As1 F1 1.649(8) . ? As1 F1 1.649(8) 5_565 ? As1 F2 1.670(9) 5_565 ? As1 F2 1.670(9) . ? As1 F3 1.615(8) . ? As1 F3 1.615(8) 5_565 ? As2 F4 1.597(9) . ? As2 F4 1.597(9) 2 ? As2 F5 1.622(9) 2 ? As2 F5 1.622(9) . ? As2 F6 1.611(14) 2 ? As2 F6 1.611(14) . ? As3 F7 1.673(10) . ? As3 F8 1.674(10) . ? As3 F9 1.610(10) . ? As3 F10 1.652(10) . ? As3 F11 1.678(11) . ? As3 F12 1.637(11) . ? S1 C1 1.708(12) . ? S1 C2 1.729(14) . ? S2 C5 1.702(11) . ? S2 C6 1.729(11) . ? S3 C9 1.719(10) . ? S3 C10 1.728(10) . ? N1 N2 1.372(11) . ? N1 C2 1.318(13) . ? N2 C1 1.312(14) . ? N3 N4 1.387(10) . ? N3 C6 1.284(13) . ? N4 C5 1.296(13) . ? N5 N6 1.393(10) . ? N5 C10 1.278(12) . ? N6 C9 1.282(11) . ? N7 C13 1.103(13) . ? N8 C15 1.104(13) . ? C1 C3 1.500(15) . ? C2 C4 1.463(16) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 C7 1.499(14) . ? C6 C8 1.508(15) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 C11 1.510(13) . ? C10 C12 1.490(14) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.464(16) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C16 1.458(17) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N5 94.8(3) . . ? N3 Ag1 N1 100.3(3) . . ? N3 Ag1 N5 107.7(3) . . ? N7 Ag1 N1 116.4(4) . . ? N7 Ag1 N3 117.8(4) . . ? N7 Ag1 N5 116.5(3) . . ? N4 Ag2 N2 98.6(3) . . ? N6 Ag2 N2 106.4(3) . . ? N6 Ag2 N4 101.5(3) . . ? N8 Ag2 N2 109.1(4) . . ? N8 Ag2 N4 114.7(4) . . ? N8 Ag2 N6 123.5(3) . . ? F1 As1 F1 179.997(1) . 5_565 ? F1 As1 F2 94.3(5) 5_565 . ? F1 As1 F2 85.7(5) . . ? F1 As1 F2 85.7(5) 5_565 5_565 ? F1 As1 F2 94.3(5) . 5_565 ? F2 As1 F2 180.0(6) . 5_565 ? F3 As1 F1 88.5(7) 5_565 5_565 ? F3 As1 F1 91.5(7) . 5_565 ? F3 As1 F1 91.5(7) 5_565 . ? F3 As1 F1 88.5(7) . . ? F3 As1 F2 93.1(6) . . ? F3 As1 F2 93.1(6) 5_565 5_565 ? F3 As1 F2 86.9(6) 5_565 . ? F3 As1 F2 86.9(6) . 5_565 ? F3 As1 F3 179.998(2) 5_565 . ? F4 As2 F4 86.0(8) . 2 ? F4 As2 F5 174.7(8) . 2 ? F4 As2 F5 92.9(5) 2 2 ? F4 As2 F5 92.9(5) . . ? F4 As2 F5 174.7(8) 2 . ? F4 As2 F6 82.2(8) . 2 ? F4 As2 F6 95.8(8) 2 2 ? F4 As2 F6 95.8(8) . . ? F4 As2 F6 82.2(8) 2 . ? F5 As2 F5 88.6(7) . 2 ? F6 As2 F5 103.0(8) . . ? F6 As2 F5 78.9(7) 2 . ? F6 As2 F5 103.0(8) 2 2 ? F6 As2 F5 78.9(7) . 2 ? F6 As2 F6 177.3(11) . 2 ? F7 As3 F8 89.5(6) . . ? F7 As3 F11 87.8(7) . . ? F8 As3 F11 89.0(6) . . ? F9 As3 F7 178.7(8) . . ? F9 As3 F8 89.6(7) . . ? F9 As3 F10 93.1(8) . . ? F9 As3 F11 93.2(7) . . ? F9 As3 F12 86.6(8) . . ? F10 As3 F7 87.8(7) . . ? F10 As3 F8 177.2(7) . . ? F10 As3 F11 91.5(6) . . ? F12 As3 F7 92.5(7) . . ? F12 As3 F8 91.8(7) . . ? F12 As3 F10 87.7(6) . . ? F12 As3 F11 179.2(7) . . ? C1 S1 C2 89.1(6) . . ? C5 S2 C6 88.5(6) . . ? C9 S3 C10 88.1(5) . . ? N2 N1 Ag1 117.1(7) . . ? C2 N1 Ag1 128.2(8) . . ? C2 N1 N2 114.4(10) . . ? N1 N2 Ag2 113.8(6) . . ? C1 N2 Ag2 133.3(8) . . ? C1 N2 N1 112.2(9) . . ? N4 N3 Ag1 118.6(6) . . ? C6 N3 Ag1 127.6(7) . . ? C6 N3 N4 113.1(8) . . ? N3 N4 Ag2 113.5(6) . . ? C5 N4 Ag2 133.7(7) . . ? C5 N4 N3 112.8(9) . . ? N6 N5 Ag1 115.1(5) . . ? C10 N5 Ag1 127.2(7) . . ? C10 N5 N6 113.1(8) . . ? N5 N6 Ag2 114.3(5) . . ? C9 N6 Ag2 132.7(6) . . ? C9 N6 N5 113.0(7) . . ? C13 N7 Ag1 174.1(11) . . ? C15 N8 Ag2 177.7(13) . . ? N2 C1 S1 113.3(9) . . ? N2 C1 C3 123.1(11) . . ? C3 C1 S1 123.7(10) . . ? N1 C2 S1 111.0(10) . . ? N1 C2 C4 123.2(12) . . ? C4 C2 S1 125.8(10) . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3B 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4B 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N4 C5 S2 113.1(8) . . ? N4 C5 C7 123.3(11) . . ? C7 C5 S2 123.6(10) . . ? N3 C6 S2 112.5(8) . . ? N3 C6 C8 125.4(10) . . ? C8 C6 S2 122.0(10) . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7B 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N6 C9 S3 113.0(7) . . ? N6 C9 C11 123.6(9) . . ? C11 C9 S3 123.4(8) . . ? N5 C10 S3 112.8(7) . . ? N5 C10 C12 124.5(10) . . ? C12 C10 S3 122.7(8) . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N7 C13 C14 179.8(16) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N8 C15 C16 177.1(17) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16B 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Ag1 N1 N2 Ag2 -13.6(8) . . . . ? Ag1 N1 N2 C1 175.3(7) . . . . ? Ag1 N1 C2 S1 -173.8(5) . . . . ? Ag1 N1 C2 C4 6.4(17) . . . . ? Ag1 N3 N4 Ag2 -5.7(8) . . . . ? Ag1 N3 N4 C5 172.5(7) . . . . ? Ag1 N3 C6 S2 -171.2(4) . . . . ? Ag1 N3 C6 C8 10.6(16) . . . . ? Ag1 N5 N6 Ag2 24.6(8) . . . . ? Ag1 N5 N6 C9 -156.4(7) . . . . ? Ag1 N5 C10 S3 153.9(5) . . . . ? Ag1 N5 C10 C12 -25.8(16) . . . . ? Ag1 N7 C13 C14 -29(100) . . . . ? Ag2 N2 C1 S1 -170.1(5) . . . . ? Ag2 N2 C1 C3 10.5(16) . . . . ? Ag2 N4 C5 S2 177.0(5) . . . . ? Ag2 N4 C5 C7 -3.4(16) . . . . ? Ag2 N6 C9 S3 177.3(5) . . . . ? Ag2 N6 C9 C11 -1.8(17) . . . . ? Ag2 N8 C15 C16 -12(60) . . . . ? N1 Ag1 N3 N4 57.9(7) . . . . ? N1 Ag1 N3 C6 -131.6(9) . . . . ? N1 Ag1 N5 N6 -74.1(7) . . . . ? N1 Ag1 N5 C10 131.9(9) . . . . ? N1 Ag1 N7 C13 136(10) . . . . ? N1 N2 C1 S1 -1.3(11) . . . . ? N1 N2 C1 C3 179.3(10) . . . . ? N2 Ag2 N4 N3 -51.4(6) . . . . ? N2 Ag2 N4 C5 130.8(9) . . . . ? N2 Ag2 N6 N5 31.9(7) . . . . ? N2 Ag2 N6 C9 -146.8(10) . . . . ? N2 Ag2 N8 C15 14(31) . . . . ? N2 N1 C2 S1 -0.2(12) . . . . ? N2 N1 C2 C4 -179.9(11) . . . . ? N3 Ag1 N1 N2 -43.5(7) . . . . ? N3 Ag1 N1 C2 130.0(9) . . . . ? N3 Ag1 N5 N6 28.4(7) . . . . ? N3 Ag1 N5 C10 -125.7(9) . . . . ? N3 Ag1 N7 C13 17(11) . . . . ? N3 N4 C5 S2 -0.8(11) . . . . ? N3 N4 C5 C7 178.9(9) . . . . ? N4 Ag2 N2 N1 65.1(7) . . . . ? N4 Ag2 N2 C1 -126.2(10) . . . . ? N4 Ag2 N6 N5 -70.7(7) . . . . ? N4 Ag2 N6 C9 110.6(10) . . . . ? N4 Ag2 N8 C15 124(31) . . . . ? N4 N3 C6 S2 -0.3(11) . . . . ? N4 N3 C6 C8 -178.4(10) . . . . ? N5 Ag1 N1 N2 65.5(7) . . . . ? N5 Ag1 N1 C2 -121.0(9) . . . . ? N5 Ag1 N3 N4 -40.5(7) . . . . ? N5 Ag1 N3 C6 130.0(9) . . . . ? N5 Ag1 N7 C13 -113(10) . . . . ? N5 N6 C9 S3 -1.4(12) . . . . ? N5 N6 C9 C11 179.5(10) . . . . ? N6 Ag2 N2 N1 -39.6(7) . . . . ? N6 Ag2 N2 C1 129.1(10) . . . . ? N6 Ag2 N4 N3 57.4(6) . . . . ? N6 Ag2 N4 C5 -120.4(9) . . . . ? N6 Ag2 N8 C15 -112(31) . . . . ? N6 N5 C10 S3 -0.6(12) . . . . ? N6 N5 C10 C12 179.8(10) . . . . ? N7 Ag1 N1 N2 -171.8(7) . . . . ? N7 Ag1 N1 C2 1.7(11) . . . . ? N7 Ag1 N3 N4 -174.8(6) . . . . ? N7 Ag1 N3 C6 -4.3(10) . . . . ? N7 Ag1 N5 N6 163.2(7) . . . . ? N7 Ag1 N5 C10 9.2(11) . . . . ? N8 Ag2 N2 N1 -175.0(7) . . . . ? N8 Ag2 N2 C1 -6.3(11) . . . . ? N8 Ag2 N4 N3 -167.1(6) . . . . ? N8 Ag2 N4 C5 15.2(10) . . . . ? N8 Ag2 N6 N5 159.1(7) . . . . ? N8 Ag2 N6 C9 -19.6(12) . . . . ? C1 S1 C2 N1 -0.4(9) . . . . ? C1 S1 C2 C4 179.3(12) . . . . ? C2 S1 C1 N2 1.0(9) . . . . ? C2 S1 C1 C3 -179.6(10) . . . . ? C2 N1 N2 Ag2 172.0(7) . . . . ? C2 N1 N2 C1 0.9(13) . . . . ? C5 S2 C6 N3 -0.1(9) . . . . ? C5 S2 C6 C8 178.1(10) . . . . ? C6 S2 C5 N4 0.5(8) . . . . ? C6 S2 C5 C7 -179.1(9) . . . . ? C6 N3 N4 Ag2 -177.5(7) . . . . ? C6 N3 N4 C5 0.7(12) . . . . ? C9 S3 C10 N5 -0.1(9) . . . . ? C9 S3 C10 C12 179.5(11) . . . . ? C10 S3 C9 N6 0.9(9) . . . . ? C10 S3 C9 C11 -180.0(10) . . . . ? C10 N5 N6 Ag2 -177.6(7) . . . . ? C10 N5 N6 C9 1.3(13) . . . . ? _database_code_depnum_ccdc_archive 'CCDC 929120' ####################################################################### # # 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_110104b _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H6 Ag N3 O3 S' _chemical_formula_weight 284.0431 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 '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 6.9033(12) _cell_length_b 7.8520(13) _cell_length_c 8.6789(15) _cell_angle_alpha 99.337(2) _cell_angle_beta 97.714(2) _cell_angle_gamma 115.448(2) _cell_volume 408.04(12) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2077 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 28.22 _exptl_crystal_description BLOCK _exptl_crystal_colour COLOURLESS _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 2.312 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 276 _exptl_absorpt_coefficient_mu 2.695 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.6880 _exptl_absorpt_correction_T_max 0.7208 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1970 _diffrn_reflns_av_R_equivalents 0.0186 _diffrn_reflns_av_sigmaI/netI 0.0292 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.35 _diffrn_reflns_theta_max 25.01 _reflns_number_total 1349 _reflns_number_gt 1314 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0000P)^2^+4.5464P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.085(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1349 _refine_ls_number_parameters 112 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0312 _refine_ls_R_factor_gt 0.0306 _refine_ls_wR_factor_ref 0.0992 _refine_ls_wR_factor_gt 0.0989 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.52126(11) 0.51517(9) 0.80182(6) 0.0428(3) Uani 1 1 d . . . S1 S 0.8601(3) 0.1506(3) 0.9886(2) 0.0366(5) Uani 1 1 d . . . N3 N 0.2724(9) 0.2722(8) 0.4604(7) 0.0339(13) Uani 1 1 d . . . O3 O 0.2731(10) 0.4271(8) 0.5198(7) 0.0537(15) Uani 1 1 d . . . O2 O 0.2368(9) 0.2120(8) 0.3125(6) 0.0482(13) Uani 1 1 d . . . C2 C 0.7383(10) 0.2302(9) 1.1235(8) 0.0290(14) Uani 1 1 d . . . N2 N 0.6504(9) 0.3325(8) 1.0706(6) 0.0302(12) Uani 1 1 d . . . N1 N 0.6783(9) 0.3548(8) 0.9180(6) 0.0302(12) Uani 1 1 d . . . C3 C 0.8328(13) 0.2647(11) 0.6973(8) 0.0406(17) Uani 1 1 d . . . H3A H 0.7523 0.1345 0.6307 0.061 Uiso 1 1 calc R . . H3B H 0.9879 0.3087 0.7066 0.061 Uiso 1 1 calc R . . H3C H 0.7896 0.3491 0.6500 0.061 Uiso 1 1 calc R . . C1 C 0.7841(11) 0.2673(9) 0.8593(8) 0.0293(14) Uani 1 1 d . . . C4 C 0.7334(13) 0.1857(11) 1.2827(8) 0.0372(16) Uani 1 1 d . . . H4A H 0.8665 0.2802 1.3587 0.056 Uiso 1 1 calc R . . H4B H 0.7220 0.0583 1.2754 0.056 Uiso 1 1 calc R . . H4C H 0.6088 0.1899 1.3172 0.056 Uiso 1 1 calc R . . O1 O 0.3147(13) 0.1828(10) 0.5511(8) 0.074(2) 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 Ag1 0.0654(5) 0.0567(5) 0.0287(4) 0.0165(3) 0.0141(3) 0.0453(4) S1 0.0501(11) 0.0438(10) 0.0324(9) 0.0143(8) 0.0137(8) 0.0336(9) N3 0.037(3) 0.037(3) 0.028(3) 0.007(2) 0.009(2) 0.017(3) O3 0.059(4) 0.041(3) 0.062(4) 0.005(3) 0.018(3) 0.025(3) O2 0.056(3) 0.058(3) 0.025(3) 0.005(2) 0.009(2) 0.024(3) C2 0.032(3) 0.031(3) 0.025(3) 0.008(3) 0.007(3) 0.015(3) N2 0.041(3) 0.037(3) 0.021(3) 0.011(2) 0.008(2) 0.025(3) N1 0.041(3) 0.036(3) 0.022(3) 0.012(2) 0.010(2) 0.023(3) C3 0.050(4) 0.048(4) 0.029(4) 0.010(3) 0.016(3) 0.025(4) C1 0.033(3) 0.030(3) 0.025(3) 0.008(3) 0.005(3) 0.015(3) C4 0.048(4) 0.045(4) 0.028(3) 0.015(3) 0.009(3) 0.028(3) O1 0.113(6) 0.064(4) 0.047(4) 0.023(3) -0.001(4) 0.044(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.251(5) . ? Ag1 N2 2.280(5) 2_667 ? Ag1 O2 2.535(6) 2_666 ? Ag1 O3 2.590(6) . ? S1 C2 1.716(7) . ? S1 C1 1.721(6) . ? N3 O1 1.221(8) . ? N3 O3 1.240(8) . ? N3 O2 1.245(7) . ? O2 Ag1 2.535(6) 2_666 ? C2 N2 1.299(8) . ? C2 C4 1.480(9) . ? N2 N1 1.392(7) . ? N2 Ag1 2.280(5) 2_667 ? N1 C1 1.298(8) . ? C3 C1 1.488(9) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N2 123.63(18) . 2_667 ? N1 Ag1 O2 117.3(2) . 2_666 ? N2 Ag1 O2 98.76(19) 2_667 2_666 ? N1 Ag1 O3 131.41(18) . . ? N2 Ag1 O3 94.98(18) 2_667 . ? O2 Ag1 O3 79.31(18) 2_666 . ? C2 S1 C1 88.7(3) . . ? O1 N3 O3 118.2(6) . . ? O1 N3 O2 120.6(6) . . ? O3 N3 O2 121.1(6) . . ? N3 O3 Ag1 99.9(4) . . ? N3 O2 Ag1 109.3(4) . 2_666 ? N2 C2 C4 123.8(6) . . ? N2 C2 S1 112.9(5) . . ? C4 C2 S1 123.4(5) . . ? C2 N2 N1 112.8(5) . . ? C2 N2 Ag1 128.8(4) . 2_667 ? N1 N2 Ag1 118.4(4) . 2_667 ? C1 N1 N2 113.0(5) . . ? C1 N1 Ag1 129.1(4) . . ? N2 N1 Ag1 117.7(4) . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N1 C1 C3 124.2(6) . . ? N1 C1 S1 112.6(5) . . ? C3 C1 S1 123.2(5) . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 N3 O3 Ag1 22.2(7) . . . . ? O2 N3 O3 Ag1 -155.5(5) . . . . ? N1 Ag1 O3 N3 -3.3(5) . . . . ? N2 Ag1 O3 N3 -148.2(4) 2_667 . . . ? O2 Ag1 O3 N3 113.8(4) 2_666 . . . ? O1 N3 O2 Ag1 -128.5(6) . . . 2_666 ? O3 N3 O2 Ag1 49.1(7) . . . 2_666 ? C1 S1 C2 N2 0.4(5) . . . . ? C1 S1 C2 C4 -179.9(6) . . . . ? C4 C2 N2 N1 179.6(6) . . . . ? S1 C2 N2 N1 -0.7(7) . . . . ? C4 C2 N2 Ag1 2.8(10) . . . 2_667 ? S1 C2 N2 Ag1 -177.5(3) . . . 2_667 ? C2 N2 N1 C1 0.7(8) . . . . ? Ag1 N2 N1 C1 177.8(4) 2_667 . . . ? C2 N2 N1 Ag1 176.9(4) . . . . ? Ag1 N2 N1 Ag1 -5.9(6) 2_667 . . . ? N2 Ag1 N1 C1 -178.2(5) 2_667 . . . ? O2 Ag1 N1 C1 -54.9(6) 2_666 . . . ? O3 Ag1 N1 C1 45.3(7) . . . . ? N2 Ag1 N1 N2 6.3(6) 2_667 . . . ? O2 Ag1 N1 N2 129.6(4) 2_666 . . . ? O3 Ag1 N1 N2 -130.3(4) . . . . ? N2 N1 C1 C3 178.8(6) . . . . ? Ag1 N1 C1 C3 3.1(10) . . . . ? N2 N1 C1 S1 -0.4(7) . . . . ? Ag1 N1 C1 S1 -176.1(3) . . . . ? C2 S1 C1 N1 0.0(5) . . . . ? C2 S1 C1 C3 -179.2(6) . . . . ? _diffrn_measured_fraction_theta_max 0.941 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.941 _refine_diff_density_max 0.568 _refine_diff_density_min -0.455 _refine_diff_density_rms 0.096 _database_code_depnum_ccdc_archive 'CCDC 929119' ####################################################################### # # 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_n110526b _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H12 Cu N6 O6 S2' _chemical_formula_weight 415.89 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' O O 0.0106 0.0060 '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' 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 6.6152(6) _cell_length_b 15.4671(14) _cell_length_c 8.1921(8) _cell_angle_alpha 90.00 _cell_angle_beta 113.2080(10) _cell_angle_gamma 90.00 _cell_volume 770.37(12) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3425 _cell_measurement_theta_min 3.01 _cell_measurement_theta_max 28.31 _exptl_crystal_description BLOCK _exptl_crystal_colour PURPLE _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 1.793 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 422 _exptl_absorpt_coefficient_mu 1.728 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.7238 _exptl_absorpt_correction_T_max 0.8195 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3820 _diffrn_reflns_av_R_equivalents 0.0153 _diffrn_reflns_av_sigmaI/netI 0.0161 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 24.99 _reflns_number_total 1344 _reflns_number_gt 1299 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0243P)^2^+0.9334P] 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 1344 _refine_ls_number_parameters 108 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0218 _refine_ls_R_factor_gt 0.0210 _refine_ls_wR_factor_ref 0.0553 _refine_ls_wR_factor_gt 0.0548 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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 0.0000 0.5000 0.5000 0.00994(11) Uani 1 2 d S . . S1 S 0.00749(8) 0.29964(3) 0.89559(6) 0.01540(13) Uani 1 1 d . . . O1 O -0.0689(3) 0.40613(9) 0.2321(2) 0.0255(3) Uani 1 1 d . . . O2 O -0.2949(2) 0.45539(9) 0.34372(17) 0.0159(3) Uani 1 1 d . . . O3 O -0.4215(3) 0.38417(12) 0.0959(2) 0.0402(5) Uani 1 1 d . . . N1 N 0.0341(2) 0.40401(10) 0.6694(2) 0.0115(3) Uani 1 1 d . . . N2 N 0.2042(3) 0.34601(10) 0.6977(2) 0.0126(3) Uani 1 1 d . . . N3 N -0.2626(3) 0.41372(11) 0.2187(2) 0.0197(4) Uani 1 1 d . . . C1 C -0.0835(3) 0.38918(12) 0.7630(2) 0.0130(4) Uani 1 1 d . . . C2 C 0.2102(3) 0.28730(12) 0.8133(2) 0.0123(4) Uani 1 1 d . . . C3 C -0.2718(3) 0.44357(13) 0.7575(3) 0.0180(4) Uani 1 1 d . . . H3A H -0.2233 0.4827 0.8565 0.027 Uiso 1 1 calc R . . H3B H -0.3861 0.4071 0.7637 0.027 Uiso 1 1 calc R . . H3C H -0.3275 0.4759 0.6487 0.027 Uiso 1 1 calc R . . C4 C 0.3769(3) 0.21644(12) 0.8695(3) 0.0163(4) Uani 1 1 d . . . H4A H 0.3079 0.1628 0.8184 0.024 Uiso 1 1 calc R . . H4B H 0.4381 0.2118 0.9966 0.024 Uiso 1 1 calc R . . H4C H 0.4920 0.2291 0.8295 0.024 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.01028(18) 0.00957(18) 0.00984(18) 0.00139(11) 0.00383(13) 0.00021(11) S1 0.0169(2) 0.0151(3) 0.0171(3) 0.00626(18) 0.0098(2) 0.00382(18) O1 0.0306(9) 0.0190(8) 0.0352(9) -0.0043(7) 0.0218(7) -0.0012(6) O2 0.0156(7) 0.0179(7) 0.0149(7) 0.0000(5) 0.0068(5) -0.0011(6) O3 0.0462(10) 0.0532(12) 0.0173(8) -0.0105(8) 0.0084(8) -0.0350(9) N1 0.0112(7) 0.0109(8) 0.0119(7) -0.0008(6) 0.0038(6) 0.0002(6) N2 0.0136(8) 0.0111(8) 0.0128(8) -0.0013(6) 0.0049(6) 0.0012(6) N3 0.0272(10) 0.0164(9) 0.0156(9) -0.0009(7) 0.0086(7) -0.0093(7) C1 0.0137(9) 0.0120(9) 0.0124(9) 0.0008(7) 0.0041(7) -0.0013(7) C2 0.0137(9) 0.0122(9) 0.0107(9) -0.0031(7) 0.0045(7) -0.0019(7) C3 0.0172(10) 0.0192(10) 0.0212(10) 0.0049(8) 0.0111(8) 0.0035(8) C4 0.0177(10) 0.0150(10) 0.0172(10) 0.0024(8) 0.0082(8) 0.0033(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 1.9834(15) 3_566 ? Cu1 N1 1.9834(15) . ? Cu1 O2 1.9880(13) . ? Cu1 O2 1.9880(13) 3_566 ? S1 C1 1.7159(19) . ? S1 C2 1.7326(19) . ? O1 N3 1.248(2) . ? O2 N3 1.297(2) . ? O3 N3 1.221(2) . ? N1 C1 1.310(2) . ? N1 N2 1.385(2) . ? N2 C2 1.301(2) . ? C1 C3 1.489(3) . ? C2 C4 1.493(3) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 N1 179.999(1) 3_566 . ? N1 Cu1 O2 89.83(6) 3_566 . ? N1 Cu1 O2 90.17(6) . . ? N1 Cu1 O2 90.17(6) 3_566 3_566 ? N1 Cu1 O2 89.83(6) . 3_566 ? O2 Cu1 O2 180.0 . 3_566 ? C1 S1 C2 88.55(9) . . ? N3 O2 Cu1 104.83(11) . . ? C1 N1 N2 114.77(15) . . ? C1 N1 Cu1 127.63(13) . . ? N2 N1 Cu1 117.58(11) . . ? C2 N2 N1 111.33(15) . . ? O3 N3 O1 123.89(19) . . ? O3 N3 O2 118.71(18) . . ? O1 N3 O2 117.40(16) . . ? N1 C1 C3 124.47(17) . . ? N1 C1 S1 111.77(14) . . ? C3 C1 S1 123.75(14) . . ? N2 C2 C4 122.92(17) . . ? N2 C2 S1 113.57(14) . . ? C4 C2 S1 123.51(14) . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Cu1 O2 N3 79.82(11) 3_566 . . . ? N1 Cu1 O2 N3 -100.18(11) . . . . ? O2 Cu1 O2 N3 172(2) 3_566 . . . ? N1 Cu1 N1 C1 -145(10) 3_566 . . . ? O2 Cu1 N1 C1 -64.28(16) . . . . ? O2 Cu1 N1 C1 115.72(16) 3_566 . . . ? N1 Cu1 N1 N2 36(10) 3_566 . . . ? O2 Cu1 N1 N2 117.41(12) . . . . ? O2 Cu1 N1 N2 -62.59(12) 3_566 . . . ? C1 N1 N2 C2 0.5(2) . . . . ? Cu1 N1 N2 C2 179.01(12) . . . . ? Cu1 O2 N3 O3 -175.05(15) . . . . ? Cu1 O2 N3 O1 5.13(19) . . . . ? N2 N1 C1 C3 178.86(17) . . . . ? Cu1 N1 C1 C3 0.5(3) . . . . ? N2 N1 C1 S1 -0.5(2) . . . . ? Cu1 N1 C1 S1 -178.88(9) . . . . ? C2 S1 C1 N1 0.33(14) . . . . ? C2 S1 C1 C3 -179.06(17) . . . . ? N1 N2 C2 C4 180.00(16) . . . . ? N1 N2 C2 S1 -0.21(19) . . . . ? C1 S1 C2 N2 -0.06(15) . . . . ? C1 S1 C2 C4 179.73(17) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.318 _refine_diff_density_min -0.322 _refine_diff_density_rms 0.056 _database_code_depnum_ccdc_archive 'CCDC 929122' ####################################################################### # # 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 ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H40 Cu8 N44 O8 S4' _chemical_formula_weight 1709.68 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' Cu Cu 0.3201 1.2651 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 14.629(2) _cell_length_b 12.3526(8) _cell_length_c 9.8215(10) _cell_angle_alpha 90.00 _cell_angle_beta 121.535(9) _cell_angle_gamma 90.00 _cell_volume 1512.7(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.877 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 852 _exptl_absorpt_coefficient_mu 2.974 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6639 _exptl_absorpt_correction_T_max 0.6985 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2669 _diffrn_reflns_av_R_equivalents 0.0450 _diffrn_reflns_av_sigmaI/netI 0.1148 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.43 _diffrn_reflns_theta_max 28.90 _reflns_number_total 1556 _reflns_number_gt 793 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _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^)+(0.0693P)^2^+6.0609P] 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 1556 _refine_ls_number_parameters 90 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1500 _refine_ls_R_factor_gt 0.0732 _refine_ls_wR_factor_ref 0.2044 _refine_ls_wR_factor_gt 0.1561 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.001 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 0.23227(11) 0.36754(8) -0.06395(13) 0.0501(5) Uani 1 1 d . . . S1 S 0.5872(4) 0.5000 0.2999(5) 0.0667(12) Uani 1 2 d S . . O4 O 0.1870(6) 0.4099(5) -0.2801(8) 0.061(2) Uani 1 1 d . . . N1 N 0.4028(7) 0.4442(5) 0.0787(9) 0.046(2) Uani 1 1 d . . . N3 N 0.2439(10) 0.2833(7) 0.1185(10) 0.0847(18) Uani 1 1 d . . . N4 N 0.2832(10) 0.3133(7) 0.2531(11) 0.0847(18) Uani 1 1 d . . . N5 N 0.3158(10) 0.3419(7) 0.3785(11) 0.0847(18) Uani 1 1 d . . . N9 N 0.1761(14) 0.5000 -0.0245(19) 0.091(3) Uani 1 2 d S . . N10 N 0.1383(13) 0.5000 0.0556(19) 0.091(3) Uani 1 2 d S . . N11 N 0.1031(13) 0.5000 0.1417(18) 0.091(3) Uani 1 2 d S . . C1 C 0.4935(9) 0.4035(7) 0.1857(12) 0.049(3) Uani 1 1 d . . . C2 C 0.5172(11) 0.2850(8) 0.2138(15) 0.084(4) Uani 1 1 d . . . H2A H 0.5923 0.2731 0.2568 0.125 Uiso 1 1 calc R . . H2B H 0.4763 0.2468 0.1146 0.125 Uiso 1 1 calc R . . H2C H 0.4983 0.2592 0.2881 0.125 Uiso 1 1 calc R . . C5 C 0.1654(11) 0.5000 -0.3478(15) 0.041(3) Uani 1 2 d S . . C6 C 0.1148(14) 0.5000 -0.5283(16) 0.069(5) Uani 1 2 d S . . H6A H 0.0732 0.4400 -0.5735 0.083 Uiso 1 1 d R . . H6B H 0.1679 0.4701 -0.5512 0.083 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0761(11) 0.0344(6) 0.0355(7) -0.0025(5) 0.0263(8) -0.0087(6) S1 0.046(3) 0.072(3) 0.051(2) 0.000 0.004(2) 0.000 O4 0.098(7) 0.042(3) 0.037(4) -0.004(3) 0.030(5) -0.008(4) N1 0.058(6) 0.033(3) 0.036(4) -0.001(3) 0.018(5) 0.008(4) N3 0.140(5) 0.058(3) 0.043(3) -0.010(3) 0.039(4) -0.009(4) N4 0.140(5) 0.058(3) 0.043(3) -0.010(3) 0.039(4) -0.009(4) N5 0.140(5) 0.058(3) 0.043(3) -0.010(3) 0.039(4) -0.009(4) N9 0.106(10) 0.112(6) 0.077(8) 0.000 0.063(8) 0.000 N10 0.106(10) 0.112(6) 0.077(8) 0.000 0.063(8) 0.000 N11 0.106(10) 0.112(6) 0.077(8) 0.000 0.063(8) 0.000 C1 0.059(8) 0.047(5) 0.036(5) -0.003(5) 0.020(6) -0.003(5) C2 0.088(11) 0.053(6) 0.089(9) -0.001(6) 0.032(10) 0.023(7) C5 0.024(9) 0.050(7) 0.030(6) 0.000 0.001(7) 0.000 C6 0.077(15) 0.067(10) 0.046(9) 0.000 0.020(11) 0.000 _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 O4 1.936(6) . ? Cu1 N9 1.958(8) . ? Cu1 N3 2.001(9) . ? Cu1 N3 2.019(9) 7 ? Cu1 N1 2.329(9) . ? Cu1 Cu1 3.098(2) 7 ? Cu1 Cu1 3.2724(19) 6_565 ? S1 C1 1.717(10) . ? S1 C1 1.717(10) 6_565 ? O4 C5 1.249(8) . ? N1 C1 1.288(12) . ? N1 N1 1.380(12) 6_565 ? N3 N4 1.192(11) . ? N3 Cu1 2.019(9) 7 ? N4 N5 1.120(11) . ? N9 N10 1.174(16) . ? N9 Cu1 1.958(8) 6_565 ? N10 N11 1.199(17) . ? C1 C2 1.496(12) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C5 O4 1.249(8) 6_565 ? C5 C6 1.522(17) . ? C6 H6A 0.9130 . ? C6 H6B 0.9867 . ? 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 O4 Cu1 N9 93.0(5) . . ? O4 Cu1 N3 160.5(3) . . ? N9 Cu1 N3 96.0(5) . . ? O4 Cu1 N3 88.1(3) . 7 ? N9 Cu1 N3 166.5(5) . 7 ? N3 Cu1 N3 79.2(4) . 7 ? O4 Cu1 N1 101.2(3) . . ? N9 Cu1 N1 88.3(5) . . ? N3 Cu1 N1 96.3(4) . . ? N3 Cu1 N1 104.8(4) 7 . ? O4 Cu1 Cu1 125.93(19) . 7 ? N9 Cu1 Cu1 134.5(4) . 7 ? N3 Cu1 Cu1 39.8(3) . 7 ? N3 Cu1 Cu1 39.4(2) 7 7 ? N1 Cu1 Cu1 103.74(18) . 7 ? O4 Cu1 Cu1 74.31(18) . 6_565 ? N9 Cu1 Cu1 33.3(4) . 6_565 ? N3 Cu1 Cu1 121.3(2) . 6_565 ? N3 Cu1 Cu1 157.4(3) 7 6_565 ? N1 Cu1 Cu1 66.03(17) . 6_565 ? Cu1 Cu1 Cu1 159.61(4) 7 6_565 ? C1 S1 C1 87.9(7) . 6_565 ? C5 O4 Cu1 132.1(7) . . ? C1 N1 N1 112.9(5) . 6_565 ? C1 N1 Cu1 130.9(6) . . ? N1 N1 Cu1 113.97(17) 6_565 . ? N4 N3 Cu1 126.7(8) . . ? N4 N3 Cu1 122.1(8) . 7 ? Cu1 N3 Cu1 100.8(4) . 7 ? N5 N4 N3 177.0(18) . . ? N10 N9 Cu1 121.7(4) . . ? N10 N9 Cu1 121.7(4) . 6_565 ? Cu1 N9 Cu1 113.3(7) . 6_565 ? N9 N10 N11 177.8(19) . . ? N1 C1 C2 124.9(9) . . ? N1 C1 S1 113.1(7) . . ? C2 C1 S1 122.0(8) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? O4 C5 O4 125.9(12) 6_565 . ? O4 C5 C6 117.0(6) 6_565 . ? O4 C5 C6 117.0(6) . . ? C5 C6 H6A 111.2 . . ? C5 C6 H6B 107.7 . . ? H6A C6 H6B 89.3 . . ? _diffrn_measured_fraction_theta_max 0.748 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.869 _refine_diff_density_max 1.441 _refine_diff_density_min -1.389 _refine_diff_density_rms 0.131 _database_code_depnum_ccdc_archive 'CCDC 929126' ####################################################################### # # 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_n110906c _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H44 Cl4 N9 Ni4.50 O28.50 S4' _chemical_formula_weight 1400.88 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' Cl Cl 0.1484 0.1585 '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' 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M P-3c1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' '-x, -x+y, -z+1/2' 'x-y, -y, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' 'x, x-y, z-1/2' '-x+y, y, z-1/2' _cell_length_a 25.7473(14) _cell_length_b 25.7473(14) _cell_length_c 23.3799(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 13422.6(13) _cell_formula_units_Z 12 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9945 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 28.04 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.080 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8556 _exptl_absorpt_coefficient_mu 2.393 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6461 _exptl_absorpt_correction_T_max 0.6461 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 66807 _diffrn_reflns_av_R_equivalents 0.0573 _diffrn_reflns_av_sigmaI/netI 0.0270 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 0.91 _diffrn_reflns_theta_max 25.01 _reflns_number_total 7890 _reflns_number_gt 6624 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SAINT (Bruker, 1997)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker, 2008)' _computing_publication_material SHELXTL _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^)+(0.0442P)^2^+64.1226P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7890 _refine_ls_number_parameters 778 _refine_ls_number_restraints 182 _refine_ls_R_factor_all 0.0484 _refine_ls_R_factor_gt 0.0377 _refine_ls_wR_factor_ref 0.1034 _refine_ls_wR_factor_gt 0.0950 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.065 _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 0.63060(2) 0.20011(2) 0.08423(2) 0.01250(13) Uani 1 1 d . C . Ni2 Ni 0.55333(2) 0.23760(2) 0.14963(2) 0.01184(13) Uani 1 1 d . C . Ni3 Ni 0.55028(2) 0.33702(2) 0.21300(2) 0.01294(13) Uani 1 1 d . . . Ni4 Ni 0.10665(3) 0.0000 0.2500 0.01406(17) Uani 1 2 d S . . Ni5 Ni 0.12366(2) 0.10925(2) 0.18559(2) 0.01538(13) Uani 1 1 d . . . Cl1 Cl 0.6667 0.3333 -0.10625(9) 0.0269(4) Uani 1 3 d S . . Cl2 Cl 0.46777(11) 0.51002(12) 0.21625(12) 0.0365(6) Uani 0.50 1 d PD A -1 Cl3 Cl 0.38174(6) 0.35492(6) -0.10239(5) 0.0281(3) Uani 1 1 d . . . Cl4 Cl 0.18991(6) 0.29795(5) 0.07132(5) 0.0296(3) Uani 1 1 d D . . Cl5 Cl 0.3228(4) 0.1974(6) 0.2208(5) 0.034(2) Uani 0.243(11) 1 d P B 1 Cl5' Cl 0.31961(10) 0.1738(2) 0.20532(15) 0.0307(8) Uani 0.757(11) 1 d P B 2 Cl6 Cl 0.0000 0.0000 0.0000 0.0348(7) Uani 1 6 d S . . S1 S 0.60579(6) 0.01193(5) 0.06262(6) 0.0324(3) Uani 1 1 d . C . S2 S 0.45236(5) 0.13987(5) -0.01257(5) 0.0171(2) Uani 1 1 d . C . S3 S 0.43104(5) 0.15980(5) 0.30682(5) 0.0215(2) Uani 1 1 d . C . S4 S 0.22476(6) 0.02775(6) 0.09196(5) 0.0282(3) Uani 1 1 d . . . O1 O 0.5160(3) 0.5003(3) 0.2054(3) 0.056(2) Uani 0.50 1 d PD A -1 O1A O 0.4738(4) 0.3402(4) 0.2097(4) 0.0218(13) Uani 0.470(8) 1 d PDU C 2 O1AA O 0.4865(3) 0.3611(3) 0.2326(3) 0.0218(13) Uani 0.530(8) 1 d PDU C 1 O2 O 0.58911(12) 0.18473(12) 0.16305(12) 0.0129(6) Uani 1 1 d D . . H2 H 0.5639(16) 0.1492(8) 0.1709(19) 0.018(13) Uiso 1 1 d D . . O3 O 0.68186(14) 0.23298(14) 0.01167(13) 0.0199(7) Uani 1 1 d . . . H3A H 0.6814 0.2035 -0.0073 0.030 Uiso 1 1 d R C . H3B H 0.6671 0.2503 -0.0100 0.030 Uiso 1 1 d R . . O4 O 0.60922(12) 0.30571(12) 0.20755(12) 0.0129(6) Uani 1 1 d . C . O5 O 0.52535(12) 0.29625(13) 0.13489(13) 0.0145(6) Uani 1 1 d D . . H5 H 0.4894(8) 0.282(2) 0.126(2) 0.023(14) Uiso 1 1 d D . . O6 O 0.62643(12) 0.27767(12) 0.09261(12) 0.0127(6) Uani 1 1 d . . . O7 O 0.58822(14) 0.38463(14) 0.28696(13) 0.0221(7) Uani 1 1 d . C . H7A H 0.6241 0.3888 0.2923 0.033 Uiso 1 1 d R . . H7B H 0.5921 0.4207 0.2849 0.033 Uiso 1 1 d R . . O8 O 0.05814(13) -0.08810(13) 0.23706(13) 0.0166(6) Uani 1 1 d D . . H8 H 0.0795(18) -0.104(2) 0.235(2) 0.021(13) Uiso 1 1 d D . . O9 O 0.05707(12) 0.02222(12) 0.19216(12) 0.0151(6) Uani 1 1 d . . . O10 O 0.19646(14) 0.19351(14) 0.17382(15) 0.0272(8) Uani 1 1 d . . . H10A H 0.2298 0.1927 0.1801 0.041 Uiso 1 1 d R . . H10B H 0.1971 0.2056 0.1384 0.041 Uiso 1 1 d R . . O11 O 0.08797(14) 0.12334(14) 0.11187(14) 0.0247(7) Uani 1 1 d . . . H11D H 0.1165 0.1539 0.0928 0.037 Uiso 1 1 d R . . H11E H 0.0731 0.0914 0.0897 0.037 Uiso 1 1 d R . . O12 O 0.6667 0.3333 -0.0460(4) 0.080(3) Uani 1 3 d S . . O13 O 0.6113(2) 0.3257(2) -0.1266(3) 0.0728(16) Uani 1 1 d . . . O14 O 0.47460(18) 0.56227(17) 0.18729(17) 0.0474(11) Uani 1 1 d DU A -1 O15 O 0.4596(3) 0.5145(3) 0.2767(2) 0.063(3) Uani 0.50 1 d PD A -1 O16 O 0.4115(3) 0.4576(2) 0.1946(3) 0.074(3) Uani 0.50 1 d PDU A -1 O17 O 0.43743(15) 0.37169(15) -0.07410(17) 0.0343(9) Uani 1 1 d . . . O18 O 0.34231(18) 0.29254(18) -0.0921(2) 0.0506(11) Uani 1 1 d . . . O19 O 0.35775(18) 0.39009(18) -0.08095(16) 0.0388(9) Uani 1 1 d . . . O20 O 0.3918(3) 0.3643(3) -0.16206(18) 0.0730(18) Uani 1 1 d . . . O21 O 0.2303(5) 0.3203(5) 0.1147(4) 0.063(4) Uani 0.474(19) 1 d PDU D 1 O21' O 0.2354(4) 0.3049(5) 0.1115(4) 0.052(3) Uani 0.526(19) 1 d PD D 2 O22 O 0.1326(4) 0.2491(4) 0.0914(6) 0.044(4) Uani 0.474(19) 1 d PD D 1 O22' O 0.1381(4) 0.2410(3) 0.0792(5) 0.072(5) Uani 0.526(19) 1 d PD D 2 O23 O 0.1795(4) 0.3407(4) 0.0444(8) 0.065(5) Uani 0.474(19) 1 d PD D 1 O23' O 0.1743(3) 0.3438(3) 0.0855(5) 0.043(3) Uani 0.526(19) 1 d PD D 2 O24 O 0.2097(5) 0.2711(8) 0.0275(5) 0.089(7) Uani 0.474(19) 1 d PD D 1 O24' O 0.2114(4) 0.3063(5) 0.0156(3) 0.048(3) Uani 0.526(19) 1 d PD D 2 O25 O 0.3302(12) 0.1403(13) 0.2075(11) 0.046(7) Uani 0.243(11) 1 d PU B 1 O25' O 0.3160(3) 0.1160(4) 0.1991(3) 0.0449(17) Uani 0.757(11) 1 d P B 2 O26 O 0.271(3) 0.176(3) 0.252(3) 0.08(2) Uani 0.243(11) 1 d P B 1 O26' O 0.2815(7) 0.1718(6) 0.2529(5) 0.032(2) Uani 0.757(11) 1 d P B 2 O27 O 0.3120(11) 0.2250(13) 0.1739(12) 0.075(7) Uani 0.243(11) 1 d PU B 1 O27' O 0.2991(2) 0.1866(3) 0.1529(2) 0.048(2) Uani 0.757(11) 1 d P B 2 O28 O 0.3749(8) 0.2395(8) 0.2486(9) 0.043(5) Uani 0.243(11) 1 d PU B 1 O28' O 0.3796(2) 0.2195(2) 0.2143(3) 0.0418(19) Uani 0.757(11) 1 d P B 2 O29 O 0.0072(6) -0.0409(6) -0.0323(5) 0.130(4) Uani 0.67 1 d PU . . O30 O 0.45473(16) 0.27320(16) -0.05660(16) 0.0314(8) Uani 1 1 d G . . H30A H 0.4482 0.3025 -0.0639 0.047 Uiso 1 1 d G . . H30B H 0.4210 0.2407 -0.0499 0.047 Uiso 1 1 d G . . N1 N 0.62559(16) 0.11732(16) 0.07409(15) 0.0165(8) Uani 1 1 d . . . N2 N 0.68113(17) 0.12275(17) 0.06552(17) 0.0218(8) Uani 1 1 d . C . N3 N 0.54740(15) 0.17456(15) 0.04417(15) 0.0140(7) Uani 1 1 d . . . N4 N 0.50870(15) 0.18240(15) 0.07929(15) 0.0141(7) Uani 1 1 d . C . N5 N 0.49265(15) 0.20659(15) 0.21827(15) 0.0135(7) Uani 1 1 d . . . N6 N 0.50047(15) 0.25376(15) 0.25273(15) 0.0133(7) Uani 1 1 d . C . N7 N 0.16641(16) 0.06655(17) 0.14643(16) 0.0196(8) Uani 1 1 d . . . N8 N 0.16624(16) 0.02245(16) 0.18055(16) 0.0189(8) Uani 1 1 d . . . N13 N 0.3857(12) 0.3349(17) 0.2414(13) 0.091(4) Uani 0.470(8) 1 d PDU C 2 N13' N 0.3940(11) 0.3485(15) 0.2365(11) 0.091(4) Uani 0.530(8) 1 d PDU C 1 C1 C 0.6780(2) 0.0714(2) 0.0580(2) 0.0250(10) Uani 1 1 d . . . C2 C 0.5817(2) 0.0620(2) 0.0740(2) 0.0243(10) Uani 1 1 d . C . C3 C 0.7301(3) 0.0636(2) 0.0456(2) 0.0353(13) Uani 1 1 d . C . H3C H 0.7294 0.0331 0.0713 0.053 Uiso 1 1 calc R . . H3D H 0.7673 0.1017 0.0516 0.053 Uiso 1 1 calc R . . H3E H 0.7281 0.0507 0.0059 0.053 Uiso 1 1 calc R . . C4 C 0.5171(2) 0.0421(2) 0.0813(3) 0.0366(13) Uani 1 1 d . . . H4A H 0.4978 0.0342 0.0436 0.055 Uiso 1 1 calc R C . H4B H 0.5130 0.0737 0.1006 0.055 Uiso 1 1 calc R . . H4C H 0.4978 0.0055 0.1043 0.055 Uiso 1 1 calc R . . C5 C 0.45697(19) 0.16556(18) 0.05584(18) 0.0145(9) Uani 1 1 d . . . C6 C 0.52438(19) 0.15326(18) -0.00613(18) 0.0160(9) Uani 1 1 d . C . C7 C 0.40647(19) 0.1674(2) 0.0844(2) 0.0192(9) Uani 1 1 d . C . H7C H 0.4015 0.1995 0.0676 0.029 Uiso 1 1 calc R . . H7D H 0.4150 0.1750 0.1253 0.029 Uiso 1 1 calc R . . H7E H 0.3695 0.1289 0.0790 0.029 Uiso 1 1 calc R . . C8 C 0.5556(2) 0.1411(2) -0.05248(19) 0.0226(10) Uani 1 1 d . . . H8A H 0.5265 0.1159 -0.0816 0.034 Uiso 1 1 calc R C . H8B H 0.5755 0.1202 -0.0369 0.034 Uiso 1 1 calc R . . H8C H 0.5856 0.1790 -0.0698 0.034 Uiso 1 1 calc R . . C9 C 0.47122(18) 0.23626(18) 0.30021(18) 0.0160(9) Uani 1 1 d . . . C10 C 0.45606(18) 0.15469(19) 0.24046(18) 0.0152(9) Uani 1 1 d . C . C11 C 0.4703(2) 0.2768(2) 0.3447(2) 0.0229(10) Uani 1 1 d . C . H11A H 0.4290 0.2616 0.3578 0.034 Uiso 1 1 calc R . . H11B H 0.4859 0.3171 0.3287 0.034 Uiso 1 1 calc R . . H11C H 0.4953 0.2786 0.3771 0.034 Uiso 1 1 calc R . . C12 C 0.4354(2) 0.09689(19) 0.21121(19) 0.0198(9) Uani 1 1 d . . . H12A H 0.4420 0.0701 0.2361 0.030 Uiso 1 1 calc R C . H12B H 0.4580 0.1036 0.1756 0.030 Uiso 1 1 calc R . . H12C H 0.3926 0.0786 0.2025 0.030 Uiso 1 1 calc R . . C13 C 0.19594(19) -0.0009(2) 0.1581(2) 0.0208(10) Uani 1 1 d . . . C14 C 0.1947(2) 0.0738(2) 0.0987(2) 0.0231(10) Uani 1 1 d . . . C15 C 0.2056(2) -0.0469(2) 0.1867(2) 0.0299(11) Uani 1 1 d . . . H15A H 0.1894 -0.0829 0.1627 0.045 Uiso 1 1 calc R . . H15B H 0.1852 -0.0572 0.2238 0.045 Uiso 1 1 calc R . . H15C H 0.2487 -0.0309 0.1925 0.045 Uiso 1 1 calc R . . C16 C 0.2006(2) 0.1171(2) 0.0534(2) 0.0306(11) Uani 1 1 d . . . H16A H 0.2403 0.1343 0.0357 0.046 Uiso 1 1 calc R . . H16B H 0.1959 0.1492 0.0705 0.046 Uiso 1 1 calc R . . H16C H 0.1696 0.0963 0.0243 0.046 Uiso 1 1 calc R . . C18 C 0.4405(9) 0.3398(11) 0.2073(11) 0.077(4) Uani 0.530(8) 1 d PDU C 1 H18 H 0.4340 0.3193 0.1719 0.092 Uiso 0.530(8) 1 calc PR C 1 C18' C 0.4358(10) 0.3496(14) 0.2177(13) 0.077(4) Uani 0.470(8) 1 d PDU C 2 H18' H 0.4461 0.3851 0.1968 0.092 Uiso 0.470(8) 1 calc PR C 2 C19 C 0.3339(14) 0.3230(19) 0.2053(17) 0.112(7) Uani 0.530(8) 1 d PDU C 1 H19A H 0.3393 0.3146 0.1664 0.168 Uiso 0.530(8) 1 d PR C 1 H19B H 0.3038 0.2868 0.2233 0.168 Uiso 0.530(8) 1 d PR C 1 H19C H 0.3213 0.3523 0.2058 0.168 Uiso 0.530(8) 1 d PR C 1 C19' C 0.3313(16) 0.312(2) 0.2182(18) 0.112(7) Uani 0.470(8) 1 d PDU C 2 H19D H 0.3360 0.3068 0.1782 0.168 Uiso 0.470(8) 1 d PR C 2 H19E H 0.3038 0.2733 0.2346 0.168 Uiso 0.470(8) 1 d PR C 2 H19F H 0.3160 0.3385 0.2232 0.168 Uiso 0.470(8) 1 d PR C 2 C20 C 0.3984(14) 0.3656(13) 0.2988(11) 0.102(6) Uani 0.530(8) 1 d PDU C 1 H20A H 0.4387 0.3798 0.3116 0.153 Uiso 0.530(8) 1 d PR C 1 H20B H 0.3887 0.3968 0.3035 0.153 Uiso 0.530(8) 1 d PR C 1 H20C H 0.3712 0.3313 0.3210 0.153 Uiso 0.530(8) 1 d PR C 1 C20' C 0.3859(17) 0.3436(14) 0.2966(13) 0.102(6) Uani 0.470(8) 1 d PDU C 2 H20D H 0.4258 0.3597 0.3113 0.153 Uiso 0.470(8) 1 d PR C 2 H20E H 0.3720 0.3713 0.3037 0.153 Uiso 0.470(8) 1 d PR C 2 H20F H 0.3598 0.3061 0.3151 0.153 Uiso 0.470(8) 1 d PR C 2 C21 C 0.6667 0.3333 0.0890(3) 0.0114(14) Uani 1 3 d SU . . C22 C 0.6667 0.3333 0.2090(3) 0.0101(14) Uani 1 3 d S . . C23 C 0.0000 0.0000 0.1899(3) 0.0124(14) Uani 1 3 d SU . . 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 0.0118(3) 0.0116(3) 0.0141(3) -0.0016(2) 0.0000(2) 0.0058(2) Ni2 0.0096(3) 0.0111(3) 0.0140(3) -0.0015(2) 0.0001(2) 0.0046(2) Ni3 0.0113(3) 0.0131(3) 0.0151(3) 0.0010(2) 0.0014(2) 0.0066(2) Ni4 0.0124(3) 0.0145(4) 0.0160(4) 0.0023(3) 0.00113(15) 0.00724(19) Ni5 0.0129(3) 0.0149(3) 0.0165(3) 0.0030(2) 0.0006(2) 0.0056(2) Cl1 0.0236(6) 0.0236(6) 0.0336(12) 0.000 0.000 0.0118(3) Cl2 0.0218(12) 0.0409(15) 0.0458(17) 0.0098(12) 0.0039(11) 0.0148(11) Cl3 0.0361(7) 0.0342(6) 0.0255(6) -0.0030(5) -0.0045(5) 0.0263(6) Cl4 0.0356(7) 0.0286(6) 0.0282(7) 0.0054(5) -0.0003(5) 0.0187(5) Cl5 0.026(4) 0.034(5) 0.039(5) 0.000(4) -0.003(3) 0.014(4) Cl5' 0.0128(9) 0.042(2) 0.0315(14) 0.0081(12) 0.0016(8) 0.0090(11) Cl6 0.0297(10) 0.0297(10) 0.045(2) 0.000 0.000 0.0148(5) S1 0.0392(7) 0.0169(6) 0.0426(8) -0.0006(5) 0.0023(6) 0.0151(6) S2 0.0174(5) 0.0173(5) 0.0159(6) -0.0024(4) -0.0034(4) 0.0081(4) S3 0.0273(6) 0.0142(5) 0.0190(6) 0.0013(4) 0.0068(5) 0.0075(5) S4 0.0284(6) 0.0353(7) 0.0249(7) 0.0031(5) 0.0100(5) 0.0188(6) O1 0.045(5) 0.077(7) 0.066(6) 0.007(5) 0.005(4) 0.047(5) O1A 0.014(3) 0.026(3) 0.032(4) -0.003(2) 0.003(3) 0.015(3) O1AA 0.014(3) 0.026(3) 0.032(4) -0.003(2) 0.003(3) 0.015(3) O2 0.0102(14) 0.0092(14) 0.0163(15) 0.0005(12) 0.0006(12) 0.0025(12) O3 0.0253(17) 0.0194(16) 0.0187(17) 0.0027(13) 0.0040(13) 0.0139(14) O4 0.0093(14) 0.0117(14) 0.0176(15) -0.0017(12) -0.0001(11) 0.0052(12) O5 0.0101(14) 0.0136(14) 0.0178(16) -0.0001(12) -0.0008(12) 0.0045(12) O6 0.0117(14) 0.0112(14) 0.0150(15) -0.0025(11) -0.0014(11) 0.0056(12) O7 0.0284(17) 0.0213(16) 0.0209(17) -0.0029(13) -0.0028(14) 0.0158(14) O8 0.0158(15) 0.0175(15) 0.0217(17) 0.0014(12) 0.0022(12) 0.0122(13) O9 0.0120(14) 0.0134(14) 0.0189(16) 0.0016(12) 0.0006(12) 0.0057(12) O10 0.0149(16) 0.0260(18) 0.034(2) 0.0086(15) 0.0013(14) 0.0048(14) O11 0.0255(17) 0.0219(17) 0.0226(18) 0.0026(14) -0.0036(14) 0.0088(14) O12 0.093(5) 0.093(5) 0.053(6) 0.000 0.000 0.047(2) O13 0.041(3) 0.063(3) 0.109(5) 0.002(3) -0.013(3) 0.022(2) O14 0.060(3) 0.045(2) 0.050(3) 0.0154(19) 0.021(2) 0.037(2) O15 0.046(5) 0.109(9) 0.034(5) 0.024(5) 0.012(4) 0.039(6) O16 0.053(5) 0.071(6) 0.092(7) -0.015(5) -0.019(5) 0.025(5) O17 0.0255(18) 0.0268(19) 0.054(2) -0.0035(17) -0.0061(17) 0.0155(16) O18 0.038(2) 0.032(2) 0.073(3) -0.009(2) -0.018(2) 0.0121(19) O19 0.048(2) 0.051(2) 0.037(2) -0.0106(18) -0.0044(18) 0.039(2) O20 0.151(5) 0.122(4) 0.023(2) 0.012(2) 0.012(3) 0.126(4) O21 0.101(8) 0.049(6) 0.055(7) -0.029(5) -0.029(6) 0.050(6) O21' 0.069(7) 0.065(7) 0.050(6) -0.027(5) -0.036(5) 0.054(6) O22 0.040(6) 0.031(6) 0.056(8) 0.007(5) 0.016(5) 0.013(5) O22' 0.117(13) 0.017(5) 0.050(7) 0.004(5) 0.007(7) 0.010(6) O23 0.050(6) 0.042(6) 0.100(14) 0.037(7) -0.001(7) 0.021(5) O23' 0.039(5) 0.030(4) 0.063(8) 0.005(4) 0.003(5) 0.020(4) O24 0.073(9) 0.181(19) 0.047(8) -0.038(10) -0.013(6) 0.089(12) O24' 0.063(6) 0.054(6) 0.023(4) 0.007(4) 0.000(4) 0.026(5) O25 0.046(7) 0.046(7) 0.046(7) -0.0002(11) 0.0002(11) 0.023(4) O25' 0.031(3) 0.042(4) 0.051(4) -0.008(3) 0.007(3) 0.010(3) O26 0.020(17) 0.09(3) 0.12(3) 0.00(2) -0.003(15) 0.027(15) O26' 0.022(6) 0.038(4) 0.034(5) 0.004(3) 0.004(4) 0.013(4) O27 0.075(7) 0.075(7) 0.075(7) 0.0004(11) -0.0003(11) 0.037(4) O27' 0.037(3) 0.082(5) 0.030(3) 0.014(3) 0.002(2) 0.033(3) O28 0.042(5) 0.043(5) 0.043(5) 0.0001(11) -0.0004(11) 0.021(3) O28' 0.014(3) 0.033(3) 0.070(5) 0.005(3) -0.004(2) 0.005(2) O29 0.111(7) 0.141(8) 0.163(8) -0.062(6) -0.016(6) 0.082(6) O30 0.035(2) 0.033(2) 0.034(2) -0.0112(17) -0.0143(17) 0.0231(17) N1 0.0178(18) 0.0158(18) 0.018(2) -0.0012(14) 0.0009(15) 0.0096(16) N2 0.023(2) 0.021(2) 0.026(2) -0.0010(16) 0.0012(16) 0.0141(17) N3 0.0132(17) 0.0118(17) 0.0161(19) -0.0006(14) 0.0011(14) 0.0057(14) N4 0.0126(17) 0.0121(17) 0.0174(19) -0.0021(14) 0.0000(14) 0.0060(14) N5 0.0138(17) 0.0147(18) 0.0135(18) -0.0042(14) -0.0029(14) 0.0082(15) N6 0.0116(16) 0.0124(17) 0.0167(19) -0.0032(14) -0.0017(14) 0.0065(14) N7 0.0154(18) 0.023(2) 0.018(2) 0.0049(15) 0.0022(15) 0.0084(16) N8 0.0146(18) 0.022(2) 0.019(2) 0.0028(15) 0.0010(15) 0.0087(16) N13 0.078(6) 0.106(9) 0.087(6) -0.005(5) 0.009(4) 0.045(6) N13' 0.078(6) 0.106(9) 0.087(6) -0.005(5) 0.009(4) 0.045(6) C1 0.034(3) 0.021(2) 0.024(3) -0.0026(19) 0.001(2) 0.017(2) C2 0.030(3) 0.018(2) 0.026(3) -0.0010(19) 0.001(2) 0.013(2) C3 0.046(3) 0.036(3) 0.038(3) -0.003(2) 0.000(3) 0.031(3) C4 0.027(3) 0.019(3) 0.058(4) 0.007(2) 0.010(3) 0.007(2) C5 0.018(2) 0.0086(19) 0.016(2) 0.0015(16) 0.0009(17) 0.0060(17) C6 0.018(2) 0.011(2) 0.017(2) 0.0016(16) -0.0014(17) 0.0058(17) C7 0.014(2) 0.020(2) 0.024(3) -0.0013(18) -0.0015(18) 0.0083(18) C8 0.023(2) 0.026(2) 0.018(2) -0.0058(19) 0.0005(19) 0.012(2) C9 0.016(2) 0.013(2) 0.018(2) -0.0001(17) 0.0002(17) 0.0065(18) C10 0.015(2) 0.016(2) 0.016(2) 0.0000(17) -0.0012(17) 0.0084(18) C11 0.028(3) 0.018(2) 0.020(3) -0.0009(18) 0.0061(19) 0.010(2) C12 0.023(2) 0.014(2) 0.019(2) 0.0006(17) 0.0022(18) 0.0074(19) C13 0.016(2) 0.027(2) 0.020(3) -0.0008(19) 0.0022(18) 0.011(2) C14 0.017(2) 0.025(2) 0.025(3) -0.001(2) 0.0015(19) 0.0087(19) C15 0.031(3) 0.034(3) 0.033(3) 0.007(2) 0.010(2) 0.022(2) C16 0.028(3) 0.035(3) 0.026(3) 0.007(2) 0.007(2) 0.013(2) C18 0.087(6) 0.068(7) 0.080(7) -0.009(6) 0.023(5) 0.041(5) C18' 0.087(6) 0.068(7) 0.080(7) -0.009(6) 0.023(5) 0.041(5) C19 0.102(7) 0.118(9) 0.117(10) 0.001(7) -0.014(6) 0.055(6) C19' 0.102(7) 0.118(9) 0.117(10) 0.001(7) -0.014(6) 0.055(6) C20 0.098(8) 0.111(10) 0.096(7) -0.009(6) 0.010(5) 0.052(7) C20' 0.098(8) 0.111(10) 0.096(7) -0.009(6) 0.010(5) 0.052(7) C21 0.0054(17) 0.0054(17) 0.023(3) 0.000 0.000 0.0027(8) C22 0.008(2) 0.008(2) 0.015(4) 0.000 0.000 0.0039(10) C23 0.0087(18) 0.0087(18) 0.020(3) 0.000 0.000 0.0043(9) _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 O5 2.025(3) 2_655 ? Ni1 O3 2.054(3) . ? Ni1 O6 2.062(3) . ? Ni1 O2 2.067(3) . ? Ni1 N1 2.084(4) . ? Ni1 N3 2.119(3) . ? Ni2 O5 2.001(3) . ? Ni2 O2 2.014(3) . ? Ni2 N5 2.099(4) . ? Ni2 N4 2.100(3) . ? Ni2 O6 2.107(3) . ? Ni2 O4 2.111(3) . ? Ni2 Ni3 2.9926(7) . ? Ni3 O1A 2.012(8) . ? Ni3 O2 2.031(3) 3_665 ? Ni3 O5 2.044(3) . ? Ni3 O4 2.048(3) . ? Ni3 O7 2.061(3) . ? Ni3 O1AA 2.077(7) . ? Ni3 N6 2.087(3) . ? Ni4 O8 1.991(3) . ? Ni4 O8 1.991(3) 6 ? Ni4 N8 2.107(4) 6 ? Ni4 N8 2.107(4) . ? Ni4 O9 2.125(3) . ? Ni4 O9 2.125(3) 6 ? Ni5 O8 2.016(3) 2 ? Ni5 O9 2.035(3) . ? Ni5 O8 2.055(3) 6 ? Ni5 O10 2.057(3) . ? Ni5 O11 2.069(3) . ? Ni5 N7 2.114(4) . ? Cl1 O12 1.408(9) . ? Cl1 O13 1.419(5) 2_655 ? Cl1 O13 1.419(5) 3_665 ? Cl1 O13 1.419(5) . ? Cl2 O1 1.406(5) . ? Cl2 O14 1.436(4) . ? Cl2 O15 1.443(6) . ? Cl2 O16 1.491(6) . ? Cl3 O20 1.417(4) . ? Cl3 O19 1.418(4) . ? Cl3 O18 1.428(4) . ? Cl3 O17 1.436(4) . ? Cl4 O21 1.357(7) . ? Cl4 O24' 1.389(6) . ? Cl4 O23 1.406(6) . ? Cl4 O22' 1.417(6) . ? Cl4 O21' 1.441(6) . ? Cl4 O22 1.457(7) . ? Cl4 O23' 1.462(6) . ? Cl4 O24 1.463(7) . ? Cl5 O26 1.38(6) . ? Cl5 O28 1.39(2) . ? Cl5 O27 1.41(3) . ? Cl5 O25 1.61(3) . ? Cl5' O28' 1.413(5) . ? Cl5' O27' 1.436(6) . ? Cl5' O25' 1.453(8) . ? Cl5' O26' 1.467(14) . ? Cl6 O29 1.381(10) 9 ? Cl6 O29 1.381(10) 8 ? Cl6 O29 1.381(10) 3 ? Cl6 O29 1.381(10) . ? Cl6 O29 1.381(10) 7 ? Cl6 O29 1.381(10) 2 ? S1 C2 1.706(5) . ? S1 C1 1.722(5) . ? S2 C5 1.712(4) . ? S2 C6 1.715(4) . ? S3 C10 1.710(4) . ? S3 C9 1.713(4) . ? S4 C13 1.715(5) . ? S4 C14 1.717(5) . ? O1A C18' 1.136(17) . ? O1AA C18 1.185(17) . ? O2 Ni3 2.031(3) 2_655 ? O4 C22 1.282(3) . ? O5 Ni1 2.025(3) 3_665 ? O6 C21 1.284(3) . ? O8 Ni5 2.016(3) 3 ? O8 Ni5 2.055(3) 6 ? O9 C23 1.284(3) . ? N1 C2 1.303(6) . ? N1 N2 1.380(5) . ? N2 C1 1.296(6) . ? N3 C6 1.308(6) . ? N3 N4 1.382(5) . ? N4 C5 1.298(5) . ? N5 C10 1.298(5) . ? N5 N6 1.386(5) . ? N6 C9 1.290(5) . ? N7 C14 1.294(6) . ? N7 N8 1.386(5) . ? N8 C13 1.295(6) . ? N13 C18' 1.275(18) . ? N13 C20' 1.308(18) . ? N13 C19' 1.333(18) . ? N13' C18 1.491(17) . ? N13' C20 1.509(17) . ? N13' C19 1.531(17) . ? N13' C20 1.95(5) 4 ? C1 C3 1.483(7) . ? C2 C4 1.487(7) . ? C5 C7 1.483(6) . ? C6 C8 1.473(6) . ? C9 C11 1.483(6) . ? C10 C12 1.474(6) . ? C13 C15 1.487(7) . ? C14 C16 1.488(7) . ? C19 C20 1.69(5) 4 ? C19' C19' 1.73(10) 4 ? C19' C20' 1.81(6) 4 ? C20 C19 1.69(5) 4 ? C20 N13' 1.95(5) 4 ? C20' C19' 1.81(6) 4 ? C21 O6 1.284(3) 2_655 ? C21 O6 1.284(3) 3_665 ? C22 O4 1.282(3) 2_655 ? C22 O4 1.282(3) 3_665 ? C23 O9 1.284(3) 3 ? C23 O9 1.284(3) 2 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Ni1 O3 92.50(12) 2_655 . ? O5 Ni1 O6 94.40(11) 2_655 . ? O3 Ni1 O6 90.76(12) . . ? O5 Ni1 O2 81.12(11) 2_655 . ? O3 Ni1 O2 168.38(12) . . ? O6 Ni1 O2 80.13(11) . . ? O5 Ni1 N1 90.81(13) 2_655 . ? O3 Ni1 N1 91.48(13) . . ? O6 Ni1 N1 174.23(13) . . ? O2 Ni1 N1 98.27(13) . . ? O5 Ni1 N3 169.27(13) 2_655 . ? O3 Ni1 N3 95.99(13) . . ? O6 Ni1 N3 78.96(12) . . ? O2 Ni1 N3 89.38(12) . . ? N1 Ni1 N3 95.52(13) . . ? O5 Ni2 O2 174.79(12) . . ? O5 Ni2 N5 86.46(12) . . ? O2 Ni2 N5 97.40(12) . . ? O5 Ni2 N4 95.41(13) . . ? O2 Ni2 N4 86.84(12) . . ? N5 Ni2 N4 106.85(13) . . ? O5 Ni2 O6 95.28(11) . . ? O2 Ni2 O6 80.27(11) . . ? N5 Ni2 O6 169.23(12) . . ? N4 Ni2 O6 83.60(12) . . ? O5 Ni2 O4 80.60(11) . . ? O2 Ni2 O4 96.29(11) . . ? N5 Ni2 O4 83.92(12) . . ? N4 Ni2 O4 168.36(12) . . ? O6 Ni2 O4 85.88(11) . . ? O5 Ni2 Ni3 42.83(9) . . ? O2 Ni2 Ni3 135.87(8) . . ? N5 Ni2 Ni3 67.29(9) . . ? N4 Ni2 Ni3 136.64(9) . . ? O6 Ni2 Ni3 107.06(8) . . ? O4 Ni2 Ni3 43.14(7) . . ? O1A Ni3 O2 93.2(3) . 3_665 ? O1A Ni3 O5 85.6(3) . . ? O2 Ni3 O5 81.54(11) 3_665 . ? O1A Ni3 O4 161.1(3) . . ? O2 Ni3 O4 98.09(11) 3_665 . ? O5 Ni3 O4 81.16(11) . . ? O1A Ni3 O7 101.0(3) . . ? O2 Ni3 O7 92.64(12) 3_665 . ? O5 Ni3 O7 171.46(12) . . ? O4 Ni3 O7 93.57(12) . . ? O1A Ni3 O1AA 20.0(2) . . ? O2 Ni3 O1AA 91.0(2) 3_665 . ? O5 Ni3 O1AA 105.0(2) . . ? O4 Ni3 O1AA 169.8(2) . . ? O7 Ni3 O1AA 81.2(2) . . ? O1A Ni3 N6 87.0(3) . . ? O2 Ni3 N6 171.28(13) 3_665 . ? O5 Ni3 N6 89.78(12) . . ? O4 Ni3 N6 79.57(12) . . ? O7 Ni3 N6 95.89(13) . . ? O1AA Ni3 N6 92.1(2) . . ? O1A Ni3 Ni2 117.4(3) . . ? O2 Ni3 Ni2 105.52(8) 3_665 . ? O5 Ni3 Ni2 41.74(8) . . ? O4 Ni3 Ni2 44.82(8) . . ? O7 Ni3 Ni2 135.77(9) . . ? O1AA Ni3 Ni2 136.7(2) . . ? N6 Ni3 Ni2 66.87(9) . . ? O8 Ni4 O8 173.39(17) . 6 ? O8 Ni4 N8 85.23(13) . 6 ? O8 Ni4 N8 98.71(13) 6 6 ? O8 Ni4 N8 98.71(13) . . ? O8 Ni4 N8 85.23(13) 6 . ? N8 Ni4 N8 107.5(2) 6 . ? O8 Ni4 O9 95.22(11) . . ? O8 Ni4 O9 79.87(11) 6 . ? N8 Ni4 O9 168.69(13) 6 . ? N8 Ni4 O9 83.62(12) . . ? O8 Ni4 O9 79.87(11) . 6 ? O8 Ni4 O9 95.22(11) 6 6 ? N8 Ni4 O9 83.62(12) 6 6 ? N8 Ni4 O9 168.69(13) . 6 ? O9 Ni4 O9 85.33(15) . 6 ? O8 Ni5 O9 98.25(12) 2 . ? O8 Ni5 O8 81.68(12) 2 6 ? O9 Ni5 O8 80.56(11) . 6 ? O8 Ni5 O10 88.35(13) 2 . ? O9 Ni5 O10 173.35(13) . . ? O8 Ni5 O10 99.67(13) 6 . ? O8 Ni5 O11 93.90(13) 2 . ? O9 Ni5 O11 93.00(12) . . ? O8 Ni5 O11 171.54(12) 6 . ? O10 Ni5 O11 87.36(13) . . ? O8 Ni5 N7 169.00(13) 2 . ? O9 Ni5 N7 80.28(13) . . ? O8 Ni5 N7 87.33(13) 6 . ? O10 Ni5 N7 93.08(14) . . ? O11 Ni5 N7 97.05(14) . . ? O12 Cl1 O13 109.6(3) . 2_655 ? O12 Cl1 O13 109.6(3) . 3_665 ? O13 Cl1 O13 109.4(3) 2_655 3_665 ? O12 Cl1 O13 109.6(3) . . ? O13 Cl1 O13 109.4(3) 2_655 . ? O13 Cl1 O13 109.4(3) 3_665 . ? O1 Cl2 O14 112.1(3) . . ? O1 Cl2 O15 111.6(3) . . ? O14 Cl2 O15 109.9(3) . . ? O1 Cl2 O16 108.9(3) . . ? O14 Cl2 O16 107.2(3) . . ? O15 Cl2 O16 106.9(3) . . ? O20 Cl3 O19 109.9(2) . . ? O20 Cl3 O18 108.9(3) . . ? O19 Cl3 O18 111.5(3) . . ? O20 Cl3 O17 109.4(3) . . ? O19 Cl3 O17 109.5(2) . . ? O18 Cl3 O17 107.6(2) . . ? O21 Cl4 O24' 118.3(7) . . ? O21 Cl4 O23 114.1(4) . . ? O24' Cl4 O23 71.0(5) . . ? O21 Cl4 O22' 117.8(8) . . ? O24' Cl4 O22' 112.3(3) . . ? O23 Cl4 O22' 114.8(6) . . ? O21 Cl4 O21' 19.6(5) . . ? O24' Cl4 O21' 110.8(3) . . ? O23 Cl4 O21' 131.1(6) . . ? O22' Cl4 O21' 109.2(3) . . ? O21 Cl4 O22 110.9(4) . . ? O24' Cl4 O22 126.1(7) . . ? O23 Cl4 O22 108.1(4) . . ? O22' Cl4 O22 16.7(7) . . ? O21' Cl4 O22 108.0(8) . . ? O21 Cl4 O23' 87.1(5) . . ? O24' Cl4 O23' 109.6(3) . . ? O23 Cl4 O23' 39.8(5) . . ? O22' Cl4 O23' 108.0(3) . . ? O21' Cl4 O23' 106.7(3) . . ? O22 Cl4 O23' 93.1(6) . . ? O21 Cl4 O24 110.5(4) . . ? O24' Cl4 O24 38.0(6) . . ? O23 Cl4 O24 107.8(4) . . ? O22' Cl4 O24 88.4(8) . . ? O21' Cl4 O24 93.4(5) . . ? O22 Cl4 O24 105.1(4) . . ? O23' Cl4 O24 147.3(5) . . ? O26 Cl5 O28 116(3) . . ? O26 Cl5 O27 102(3) . . ? O28 Cl5 O27 109.1(14) . . ? O26 Cl5 O25 106(3) . . ? O28 Cl5 O25 107.1(13) . . ? O27 Cl5 O25 117.0(16) . . ? O28' Cl5' O27' 108.1(4) . . ? O28' Cl5' O25' 110.6(4) . . ? O27' Cl5' O25' 107.9(4) . . ? O28' Cl5' O26' 110.5(7) . . ? O27' Cl5' O26' 109.8(7) . . ? O25' Cl5' O26' 110.0(6) . . ? O29 Cl6 O29 93.0(8) 9 8 ? O29 Cl6 O29 180.0(12) 9 3 ? O29 Cl6 O29 87.0(8) 8 3 ? O29 Cl6 O29 87.0(8) 9 . ? O29 Cl6 O29 87.0(8) 8 . ? O29 Cl6 O29 93.0(8) 3 . ? O29 Cl6 O29 93.0(8) 9 7 ? O29 Cl6 O29 93.0(8) 8 7 ? O29 Cl6 O29 87.0(8) 3 7 ? O29 Cl6 O29 180.0(11) . 7 ? O29 Cl6 O29 87.0(8) 9 2 ? O29 Cl6 O29 180.0(17) 8 2 ? O29 Cl6 O29 93.0(8) 3 2 ? O29 Cl6 O29 93.0(8) . 2 ? O29 Cl6 O29 87.0(8) 7 2 ? C2 S1 C1 88.6(2) . . ? C5 S2 C6 88.9(2) . . ? C10 S3 C9 88.4(2) . . ? C13 S4 C14 88.0(2) . . ? C18' O1A Ni3 165.5(17) . . ? C18 O1AA Ni3 120.5(12) . . ? Ni2 O2 Ni3 120.49(13) . 2_655 ? Ni2 O2 Ni1 95.68(12) . . ? Ni3 O2 Ni1 98.20(12) 2_655 . ? C22 O4 Ni3 131.05(18) . . ? C22 O4 Ni2 126.6(3) . . ? Ni3 O4 Ni2 92.04(11) . . ? Ni2 O5 Ni1 123.76(14) . 3_665 ? Ni2 O5 Ni3 95.43(12) . . ? Ni1 O5 Ni3 99.13(12) 3_665 . ? C21 O6 Ni1 132.12(19) . . ? C21 O6 Ni2 127.8(3) . . ? Ni1 O6 Ni2 93.00(11) . . ? Ni4 O8 Ni5 121.27(14) . 3 ? Ni4 O8 Ni5 96.70(13) . 6 ? Ni5 O8 Ni5 98.31(12) 3 6 ? C23 O9 Ni5 129.35(19) . . ? C23 O9 Ni4 127.8(3) . . ? Ni5 O9 Ni4 93.19(11) . . ? C2 N1 N2 113.4(4) . . ? C2 N1 Ni1 134.1(3) . . ? N2 N1 Ni1 112.4(3) . . ? C1 N2 N1 112.5(4) . . ? C6 N3 N4 112.8(3) . . ? C6 N3 Ni1 134.7(3) . . ? N4 N3 Ni1 112.5(2) . . ? C5 N4 N3 113.2(3) . . ? C5 N4 Ni2 132.8(3) . . ? N3 N4 Ni2 111.9(2) . . ? C10 N5 N6 112.5(3) . . ? C10 N5 Ni2 135.8(3) . . ? N6 N5 Ni2 110.9(2) . . ? C9 N6 N5 113.0(3) . . ? C9 N6 Ni3 133.9(3) . . ? N5 N6 Ni3 112.8(2) . . ? C14 N7 N8 112.7(4) . . ? C14 N7 Ni5 134.4(3) . . ? N8 N7 Ni5 112.8(3) . . ? C13 N8 N7 112.7(4) . . ? C13 N8 Ni4 134.6(3) . . ? N7 N8 Ni4 111.8(3) . . ? C18' N13 C20' 118(3) . . ? C18' N13 C19' 129(4) . . ? C20' N13 C19' 113(3) . . ? C18 N13' C20 122(2) . . ? C18 N13' C19 116(3) . . ? C20 N13' C19 120(3) . . ? C18 N13' C20 120(2) . 4 ? C20 N13' C20 102(2) . 4 ? C19 N13' C20 57(2) . 4 ? N2 C1 C3 124.5(5) . . ? N2 C1 S1 112.8(4) . . ? C3 C1 S1 122.7(4) . . ? N1 C2 C4 125.8(4) . . ? N1 C2 S1 112.5(4) . . ? C4 C2 S1 121.7(4) . . ? N4 C5 C7 124.7(4) . . ? N4 C5 S2 112.6(3) . . ? C7 C5 S2 122.7(3) . . ? N3 C6 C8 124.7(4) . . ? N3 C6 S2 112.4(3) . . ? C8 C6 S2 122.9(3) . . ? N6 C9 C11 124.8(4) . . ? N6 C9 S3 113.0(3) . . ? C11 C9 S3 122.2(3) . . ? N5 C10 C12 124.3(4) . . ? N5 C10 S3 113.0(3) . . ? C12 C10 S3 122.6(3) . . ? N8 C13 C15 124.1(4) . . ? N8 C13 S4 113.3(3) . . ? C15 C13 S4 122.6(3) . . ? N7 C14 C16 124.2(4) . . ? N7 C14 S4 113.3(4) . . ? C16 C14 S4 122.6(4) . . ? O1AA C18 N13' 113(2) . . ? O1A C18' N13 149(4) . . ? N13' C19 C20 74(2) . 4 ? N13 C19' C19' 85(3) . 4 ? N13 C19' C20' 91(3) . 4 ? C19' C19' C20' 77(3) 4 4 ? N13' C20 C19 84(2) . 4 ? N13' C20 N13' 74(2) . 4 ? C19 C20 N13' 49.1(13) 4 4 ? N13 C20' C19' 82(2) . 4 ? O6 C21 O6 119.56(8) 2_655 . ? O6 C21 O6 119.56(8) 2_655 3_665 ? O6 C21 O6 119.56(8) . 3_665 ? O4 C22 O4 119.93(3) 2_655 3_665 ? O4 C22 O4 119.93(3) 2_655 . ? O4 C22 O4 119.93(3) 3_665 . ? O9 C23 O9 119.84(5) 3 2 ? O9 C23 O9 119.84(5) 3 . ? O9 C23 O9 119.84(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 O5 Ni2 Ni3 O1A 44.8(3) . . . . ? O2 Ni2 Ni3 O1A -142.5(3) . . . . ? N5 Ni2 Ni3 O1A -65.9(3) . . . . ? N4 Ni2 Ni3 O1A 24.9(3) . . . . ? O6 Ni2 Ni3 O1A 123.9(3) . . . . ? O4 Ni2 Ni3 O1A -172.1(3) . . . . ? O5 Ni2 Ni3 O2 -57.28(15) . . . 3_665 ? O2 Ni2 Ni3 O2 115.39(13) . . . 3_665 ? N5 Ni2 Ni3 O2 -167.96(13) . . . 3_665 ? N4 Ni2 Ni3 O2 -77.13(16) . . . 3_665 ? O6 Ni2 Ni3 O2 21.80(12) . . . 3_665 ? O4 Ni2 Ni3 O2 85.85(14) . . . 3_665 ? O2 Ni2 Ni3 O5 172.67(17) . . . . ? N5 Ni2 Ni3 O5 -110.68(15) . . . . ? N4 Ni2 Ni3 O5 -19.85(18) . . . . ? O6 Ni2 Ni3 O5 79.08(14) . . . . ? O4 Ni2 Ni3 O5 143.13(16) . . . . ? O5 Ni2 Ni3 O4 -143.13(16) . . . . ? O2 Ni2 Ni3 O4 29.53(16) . . . . ? N5 Ni2 Ni3 O4 106.18(15) . . . . ? N4 Ni2 Ni3 O4 -162.99(18) . . . . ? O6 Ni2 Ni3 O4 -64.06(14) . . . . ? O5 Ni2 Ni3 O7 -168.01(18) . . . . ? O2 Ni2 Ni3 O7 4.66(18) . . . . ? N5 Ni2 Ni3 O7 81.31(16) . . . . ? N4 Ni2 Ni3 O7 172.14(19) . . . . ? O6 Ni2 Ni3 O7 -88.93(15) . . . . ? O4 Ni2 Ni3 O7 -24.87(17) . . . . ? O5 Ni2 Ni3 O1AA 51.4(3) . . . . ? O2 Ni2 Ni3 O1AA -135.9(3) . . . . ? N5 Ni2 Ni3 O1AA -59.2(3) . . . . ? N4 Ni2 Ni3 O1AA 31.6(3) . . . . ? O6 Ni2 Ni3 O1AA 130.5(3) . . . . ? O4 Ni2 Ni3 O1AA -165.4(3) . . . . ? O5 Ni2 Ni3 N6 118.20(16) . . . . ? O2 Ni2 Ni3 N6 -69.14(15) . . . . ? N5 Ni2 Ni3 N6 7.52(14) . . . . ? N4 Ni2 Ni3 N6 98.34(17) . . . . ? O6 Ni2 Ni3 N6 -162.73(13) . . . . ? O4 Ni2 Ni3 N6 -98.67(15) . . . . ? O2 Ni3 O1A C18' -89(7) 3_665 . . . ? O5 Ni3 O1A C18' -170(7) . . . . ? O4 Ni3 O1A C18' 144(7) . . . . ? O7 Ni3 O1A C18' 4(7) . . . . ? O1AA Ni3 O1A C18' -5(7) . . . . ? N6 Ni3 O1A C18' 100(7) . . . . ? Ni2 Ni3 O1A C18' 162(7) . . . . ? O1A Ni3 O1AA C18 0.8(18) . . . . ? O2 Ni3 O1AA C18 97.4(17) 3_665 . . . ? O5 Ni3 O1AA C18 15.9(17) . . . . ? O4 Ni3 O1AA C18 -110(2) . . . . ? O7 Ni3 O1AA C18 -170.1(17) . . . . ? N6 Ni3 O1AA C18 -74.5(17) . . . . ? Ni2 Ni3 O1AA C18 -16.7(18) . . . . ? O5 Ni2 O2 Ni3 46.6(14) . . . 2_655 ? N5 Ni2 O2 Ni3 -91.13(17) . . . 2_655 ? N4 Ni2 O2 Ni3 162.28(17) . . . 2_655 ? O6 Ni2 O2 Ni3 78.24(16) . . . 2_655 ? O4 Ni2 O2 Ni3 -6.47(17) . . . 2_655 ? Ni3 Ni2 O2 Ni3 -26.3(2) . . . 2_655 ? O5 Ni2 O2 Ni1 -56.4(14) . . . . ? N5 Ni2 O2 Ni1 165.88(12) . . . . ? N4 Ni2 O2 Ni1 59.29(13) . . . . ? O6 Ni2 O2 Ni1 -24.76(10) . . . . ? O4 Ni2 O2 Ni1 -109.47(11) . . . . ? Ni3 Ni2 O2 Ni1 -129.29(8) . . . . ? O5 Ni1 O2 Ni2 121.44(12) 2_655 . . . ? O3 Ni1 O2 Ni2 64.2(6) . . . . ? O6 Ni1 O2 Ni2 25.35(11) . . . . ? N1 Ni1 O2 Ni2 -149.04(13) . . . . ? N3 Ni1 O2 Ni2 -53.55(12) . . . . ? O5 Ni1 O2 Ni3 -0.53(11) 2_655 . . 2_655 ? O3 Ni1 O2 Ni3 -57.8(6) . . . 2_655 ? O6 Ni1 O2 Ni3 -96.62(12) . . . 2_655 ? N1 Ni1 O2 Ni3 88.99(13) . . . 2_655 ? N3 Ni1 O2 Ni3 -175.52(13) . . . 2_655 ? O1A Ni3 O4 C22 167.5(9) . . . . ? O2 Ni3 O4 C22 41.4(5) 3_665 . . . ? O5 Ni3 O4 C22 121.5(5) . . . . ? O7 Ni3 O4 C22 -51.8(5) . . . . ? O1AA Ni3 O4 C22 -110.9(14) . . . . ? N6 Ni3 O4 C22 -147.1(5) . . . . ? Ni2 Ni3 O4 C22 145.3(5) . . . . ? O1A Ni3 O4 Ni2 22.2(9) . . . . ? O2 Ni3 O4 Ni2 -103.92(11) 3_665 . . . ? O5 Ni3 O4 Ni2 -23.84(11) . . . . ? O7 Ni3 O4 Ni2 162.91(12) . . . . ? O1AA Ni3 O4 Ni2 103.9(13) . . . . ? N6 Ni3 O4 Ni2 67.57(12) . . . . ? O5 Ni2 O4 C22 -123.3(3) . . . . ? O2 Ni2 O4 C22 52.5(3) . . . . ? N5 Ni2 O4 C22 149.3(3) . . . . ? N4 Ni2 O4 C22 -52.5(7) . . . . ? O6 Ni2 O4 C22 -27.2(3) . . . . ? Ni3 Ni2 O4 C22 -147.7(4) . . . . ? O5 Ni2 O4 Ni3 24.42(11) . . . . ? O2 Ni2 O4 Ni3 -159.80(11) . . . . ? N5 Ni2 O4 Ni3 -62.99(12) . . . . ? N4 Ni2 O4 Ni3 95.1(6) . . . . ? O6 Ni2 O4 Ni3 120.47(11) . . . . ? O2 Ni2 O5 Ni1 26.6(14) . . . 3_665 ? N5 Ni2 O5 Ni1 164.64(18) . . . 3_665 ? N4 Ni2 O5 Ni1 -88.75(18) . . . 3_665 ? O6 Ni2 O5 Ni1 -4.70(18) . . . 3_665 ? O4 Ni2 O5 Ni1 80.22(17) . . . 3_665 ? Ni3 Ni2 O5 Ni1 104.79(19) . . . 3_665 ? O2 Ni2 O5 Ni3 -78.2(13) . . . . ? N5 Ni2 O5 Ni3 59.85(12) . . . . ? N4 Ni2 O5 Ni3 166.45(12) . . . . ? O6 Ni2 O5 Ni3 -109.50(11) . . . . ? O4 Ni2 O5 Ni3 -24.57(11) . . . . ? O1A Ni3 O5 Ni2 -141.2(3) . . . . ? O2 Ni3 O5 Ni2 124.96(12) 3_665 . . . ? O4 Ni3 O5 Ni2 25.34(11) . . . . ? O7 Ni3 O5 Ni2 77.6(8) . . . . ? O1AA Ni3 O5 Ni2 -146.3(2) . . . . ? N6 Ni3 O5 Ni2 -54.14(13) . . . . ? O1A Ni3 O5 Ni1 93.3(3) . . . 3_665 ? O2 Ni3 O5 Ni1 -0.54(11) 3_665 . . 3_665 ? O4 Ni3 O5 Ni1 -100.16(12) . . . 3_665 ? O7 Ni3 O5 Ni1 -47.9(9) . . . 3_665 ? O1AA Ni3 O5 Ni1 88.2(2) . . . 3_665 ? N6 Ni3 O5 Ni1 -179.64(13) . . . 3_665 ? Ni2 Ni3 O5 Ni1 -125.50(16) . . . 3_665 ? O5 Ni1 O6 C21 46.8(5) 2_655 . . . ? O3 Ni1 O6 C21 -45.8(5) . . . . ? O2 Ni1 O6 C21 126.9(5) . . . . ? N1 Ni1 O6 C21 -158.7(12) . . . . ? N3 Ni1 O6 C21 -141.8(5) . . . . ? O5 Ni1 O6 Ni2 -104.24(11) 2_655 . . . ? O3 Ni1 O6 Ni2 163.20(12) . . . . ? O2 Ni1 O6 Ni2 -24.06(10) . . . . ? N1 Ni1 O6 Ni2 50.3(13) . . . . ? N3 Ni1 O6 Ni2 67.25(12) . . . . ? O5 Ni2 O6 C21 49.0(4) . . . . ? O2 Ni2 O6 C21 -128.2(4) . . . . ? N5 Ni2 O6 C21 -49.8(8) . . . . ? N4 Ni2 O6 C21 143.9(4) . . . . ? O4 Ni2 O6 C21 -31.1(4) . . . . ? Ni3 Ni2 O6 C21 7.0(4) . . . . ? O5 Ni2 O6 Ni1 -158.02(11) . . . . ? O2 Ni2 O6 Ni1 24.72(11) . . . . ? N5 Ni2 O6 Ni1 103.1(6) . . . . ? N4 Ni2 O6 Ni1 -63.15(12) . . . . ? O4 Ni2 O6 Ni1 121.83(11) . . . . ? Ni3 Ni2 O6 Ni1 159.89(6) . . . . ? O8 Ni4 O8 Ni5 38.32(15) 6 . . 3 ? N8 Ni4 O8 Ni5 165.13(18) 6 . . 3 ? N8 Ni4 O8 Ni5 -87.85(18) . . . 3 ? O9 Ni4 O8 Ni5 -3.52(18) . . . 3 ? O9 Ni4 O8 Ni5 80.77(17) 6 . . 3 ? O8 Ni4 O8 Ni5 -65.66(9) 6 . . 6 ? N8 Ni4 O8 Ni5 61.15(13) 6 . . 6 ? N8 Ni4 O8 Ni5 168.17(13) . . . 6 ? O9 Ni4 O8 Ni5 -107.50(12) . . . 6 ? O9 Ni4 O8 Ni5 -23.21(11) 6 . . 6 ? O8 Ni5 O9 C23 44.6(5) 2 . . . ? O8 Ni5 O9 C23 124.7(5) 6 . . . ? O10 Ni5 O9 C23 -142.8(11) . . . . ? O11 Ni5 O9 C23 -49.8(5) . . . . ? N7 Ni5 O9 C23 -146.4(5) . . . . ? O8 Ni5 O9 Ni4 -102.58(12) 2 . . . ? O8 Ni5 O9 Ni4 -22.50(11) 6 . . . ? O10 Ni5 O9 Ni4 70.1(11) . . . . ? O11 Ni5 O9 Ni4 163.04(12) . . . . ? N7 Ni5 O9 Ni4 66.39(13) . . . . ? O8 Ni4 O9 C23 50.9(4) . . . . ? O8 Ni4 O9 C23 -124.6(4) 6 . . . ? N8 Ni4 O9 C23 -40.9(8) 6 . . . ? N8 Ni4 O9 C23 149.1(4) . . . . ? O9 Ni4 O9 C23 -28.5(3) 6 . . . ? O8 Ni4 O9 Ni5 -161.17(12) . . . . ? O8 Ni4 O9 Ni5 23.31(11) 6 . . . ? N8 Ni4 O9 Ni5 107.1(6) 6 . . . ? N8 Ni4 O9 Ni5 -62.96(13) . . . . ? O9 Ni4 O9 Ni5 119.47(15) 6 . . . ? O5 Ni1 N1 C2 137.8(4) 2_655 . . . ? O3 Ni1 N1 C2 -129.7(4) . . . . ? O6 Ni1 N1 C2 -16.8(16) . . . . ? O2 Ni1 N1 C2 56.6(5) . . . . ? N3 Ni1 N1 C2 -33.6(5) . . . . ? O5 Ni1 N1 N2 -42.3(3) 2_655 . . . ? O3 Ni1 N1 N2 50.2(3) . . . . ? O6 Ni1 N1 N2 163.1(12) . . . . ? O2 Ni1 N1 N2 -123.4(3) . . . . ? N3 Ni1 N1 N2 146.4(3) . . . . ? C2 N1 N2 C1 1.3(6) . . . . ? Ni1 N1 N2 C1 -178.7(3) . . . . ? O5 Ni1 N3 C6 176.9(5) 2_655 . . . ? O3 Ni1 N3 C6 34.8(4) . . . . ? O6 Ni1 N3 C6 124.4(4) . . . . ? O2 Ni1 N3 C6 -155.5(4) . . . . ? N1 Ni1 N3 C6 -57.3(4) . . . . ? O5 Ni1 N3 N4 -2.9(8) 2_655 . . . ? O3 Ni1 N3 N4 -145.0(3) . . . . ? O6 Ni1 N3 N4 -55.4(2) . . . . ? O2 Ni1 N3 N4 24.7(3) . . . . ? N1 Ni1 N3 N4 122.9(3) . . . . ? C6 N3 N4 C5 1.7(5) . . . . ? Ni1 N3 N4 C5 -178.4(3) . . . . ? C6 N3 N4 Ni2 -164.3(3) . . . . ? Ni1 N3 N4 Ni2 15.6(3) . . . . ? O5 Ni2 N4 C5 -37.3(4) . . . . ? O2 Ni2 N4 C5 147.4(4) . . . . ? N5 Ni2 N4 C5 50.6(4) . . . . ? O6 Ni2 N4 C5 -132.0(4) . . . . ? O4 Ni2 N4 C5 -106.6(6) . . . . ? Ni3 Ni2 N4 C5 -23.9(5) . . . . ? O5 Ni2 N4 N3 125.1(3) . . . . ? O2 Ni2 N4 N3 -50.2(3) . . . . ? N5 Ni2 N4 N3 -147.0(2) . . . . ? O6 Ni2 N4 N3 30.3(2) . . . . ? O4 Ni2 N4 N3 55.8(7) . . . . ? Ni3 Ni2 N4 N3 138.5(2) . . . . ? O5 Ni2 N5 C10 140.9(4) . . . . ? O2 Ni2 N5 C10 -42.6(4) . . . . ? N4 Ni2 N5 C10 46.3(4) . . . . ? O6 Ni2 N5 C10 -119.4(6) . . . . ? O4 Ni2 N5 C10 -138.2(4) . . . . ? Ni3 Ni2 N5 C10 -179.5(4) . . . . ? O5 Ni2 N5 N6 -50.8(2) . . . . ? O2 Ni2 N5 N6 125.7(2) . . . . ? N4 Ni2 N5 N6 -145.3(2) . . . . ? O6 Ni2 N5 N6 48.9(8) . . . . ? O4 Ni2 N5 N6 30.2(2) . . . . ? Ni3 Ni2 N5 N6 -11.2(2) . . . . ? C10 N5 N6 C9 1.9(5) . . . . ? Ni2 N5 N6 C9 -169.3(3) . . . . ? C10 N5 N6 Ni3 -172.6(3) . . . . ? Ni2 N5 N6 Ni3 16.2(3) . . . . ? O1A Ni3 N6 C9 -62.8(5) . . . . ? O2 Ni3 N6 C9 -154.3(7) 3_665 . . . ? O5 Ni3 N6 C9 -148.5(4) . . . . ? O4 Ni3 N6 C9 130.5(4) . . . . ? O7 Ni3 N6 C9 37.9(4) . . . . ? O1AA Ni3 N6 C9 -43.5(5) . . . . ? Ni2 Ni3 N6 C9 175.6(4) . . . . ? O1A Ni3 N6 N5 110.1(4) . . . . ? O2 Ni3 N6 N5 18.6(9) 3_665 . . . ? O5 Ni3 N6 N5 24.5(3) . . . . ? O4 Ni3 N6 N5 -56.6(2) . . . . ? O7 Ni3 N6 N5 -149.1(2) . . . . ? O1AA Ni3 N6 N5 129.5(3) . . . . ? Ni2 Ni3 N6 N5 -11.4(2) . . . . ? O8 Ni5 N7 C14 -147.5(6) 2 . . . ? O9 Ni5 N7 C14 129.3(4) . . . . ? O8 Ni5 N7 C14 -149.8(4) 6 . . . ? O10 Ni5 N7 C14 -50.3(4) . . . . ? O11 Ni5 N7 C14 37.4(4) . . . . ? O8 Ni5 N7 N8 29.4(8) 2 . . . ? O9 Ni5 N7 N8 -53.9(3) . . . . ? O8 Ni5 N7 N8 27.0(3) 6 . . . ? O10 Ni5 N7 N8 126.6(3) . . . . ? O11 Ni5 N7 N8 -145.7(3) . . . . ? C14 N7 N8 C13 1.9(5) . . . . ? Ni5 N7 N8 C13 -175.6(3) . . . . ? C14 N7 N8 Ni4 -169.1(3) . . . . ? Ni5 N7 N8 Ni4 13.4(3) . . . . ? O8 Ni4 N8 C13 -42.8(4) . . . . ? O8 Ni4 N8 C13 142.5(4) 6 . . . ? N8 Ni4 N8 C13 44.9(4) 6 . . . ? O9 Ni4 N8 C13 -137.1(4) . . . . ? O9 Ni4 N8 C13 -124.7(6) 6 . . . ? O8 Ni4 N8 N7 125.5(3) . . . . ? O8 Ni4 N8 N7 -49.1(3) 6 . . . ? N8 Ni4 N8 N7 -146.8(3) 6 . . . ? O9 Ni4 N8 N7 31.2(3) . . . . ? O9 Ni4 N8 N7 43.6(8) 6 . . . ? N1 N2 C1 C3 177.5(5) . . . . ? N1 N2 C1 S1 -1.3(5) . . . . ? C2 S1 C1 N2 0.9(4) . . . . ? C2 S1 C1 C3 -178.0(5) . . . . ? N2 N1 C2 C4 -179.0(5) . . . . ? Ni1 N1 C2 C4 1.0(8) . . . . ? N2 N1 C2 S1 -0.6(5) . . . . ? Ni1 N1 C2 S1 179.3(2) . . . . ? C1 S1 C2 N1 -0.1(4) . . . . ? C1 S1 C2 C4 178.3(5) . . . . ? N3 N4 C5 C7 178.2(4) . . . . ? Ni2 N4 C5 C7 -19.6(6) . . . . ? N3 N4 C5 S2 -1.2(4) . . . . ? Ni2 N4 C5 S2 160.9(2) . . . . ? C6 S2 C5 N4 0.4(3) . . . . ? C6 S2 C5 C7 -179.1(4) . . . . ? N4 N3 C6 C8 179.3(4) . . . . ? Ni1 N3 C6 C8 -0.5(7) . . . . ? N4 N3 C6 S2 -1.4(4) . . . . ? Ni1 N3 C6 S2 178.8(2) . . . . ? C5 S2 C6 N3 0.6(3) . . . . ? C5 S2 C6 C8 180.0(4) . . . . ? N5 N6 C9 C11 -178.7(4) . . . . ? Ni3 N6 C9 C11 -5.8(7) . . . . ? N5 N6 C9 S3 -0.2(4) . . . . ? Ni3 N6 C9 S3 172.8(2) . . . . ? C10 S3 C9 N6 -1.1(3) . . . . ? C10 S3 C9 C11 177.5(4) . . . . ? N6 N5 C10 C12 174.6(4) . . . . ? Ni2 N5 C10 C12 -17.2(7) . . . . ? N6 N5 C10 S3 -2.7(4) . . . . ? Ni2 N5 C10 S3 165.5(2) . . . . ? C9 S3 C10 N5 2.2(3) . . . . ? C9 S3 C10 C12 -175.2(4) . . . . ? N7 N8 C13 C15 176.8(4) . . . . ? Ni4 N8 C13 C15 -14.9(7) . . . . ? N7 N8 C13 S4 -2.0(5) . . . . ? Ni4 N8 C13 S4 166.3(2) . . . . ? C14 S4 C13 N8 1.2(4) . . . . ? C14 S4 C13 C15 -177.7(4) . . . . ? N8 N7 C14 C16 178.5(4) . . . . ? Ni5 N7 C14 C16 -4.6(7) . . . . ? N8 N7 C14 S4 -1.0(5) . . . . ? Ni5 N7 C14 S4 175.8(2) . . . . ? C13 S4 C14 N7 -0.1(4) . . . . ? C13 S4 C14 C16 -179.6(4) . . . . ? Ni3 O1AA C18 N13' 164.1(17) . . . . ? C20 N13' C18 O1AA -17(4) . . . . ? C19 N13' C18 O1AA 179(3) . . . . ? C20 N13' C18 O1AA 114(3) 4 . . . ? Ni3 O1A C18' N13 -91(9) . . . . ? C20' N13 C18' O1A 73(7) . . . . ? C19' N13 C18' O1A -107(7) . . . . ? C18 N13' C19 C20 -110(3) . . . 4 ? C20 N13' C19 C20 85(3) . . . 4 ? C18' N13 C19' C19' -165(5) . . . 4 ? C20' N13 C19' C19' 14(4) . . . 4 ? C18' N13 C19' C20' -89(5) . . . 4 ? C20' N13 C19' C20' 91(4) . . . 4 ? C18 N13' C20 C19 -156(3) . . . 4 ? C19 N13' C20 C19 7(4) . . . 4 ? C20 N13' C20 C19 66(2) 4 . . 4 ? C18 N13' C20 N13' 155(2) . . . 4 ? C19 N13' C20 N13' -42(3) . . . 4 ? C20 N13' C20 N13' 17(2) 4 . . 4 ? C18' N13 C20' C19' 166(4) . . . 4 ? C19' N13 C20' C19' -14(4) . . . 4 ? Ni1 O6 C21 O6 -17.4(10) . . . 2_655 ? Ni2 O6 C21 O6 124.8(4) . . . 2_655 ? Ni1 O6 C21 O6 175.7(3) . . . 3_665 ? Ni2 O6 C21 O6 -42.1(8) . . . 3_665 ? Ni3 O4 C22 O4 176.6(3) . . . 2_655 ? Ni2 O4 C22 O4 -48.6(8) . . . 2_655 ? Ni3 O4 C22 O4 -8.7(9) . . . 3_665 ? Ni2 O4 C22 O4 126.1(4) . . . 3_665 ? Ni5 O9 C23 O9 176.5(3) . . . 3 ? Ni4 O9 C23 O9 -46.8(8) . . . 3 ? Ni5 O9 C23 O9 -11.5(9) . . . 2 ? Ni4 O9 C23 O9 125.2(4) . . . 2 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.421 _refine_diff_density_min -1.029 _refine_diff_density_rms 0.111 _database_code_depnum_ccdc_archive 'CCDC 929123'