# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Grapperhaus, Craig' 'Li, Ming' 'Mashuta, Mark S.' _publ_contact_author_name 'Prof Craig Grapperhaus' _publ_contact_author_address ; Department of Chemistry University of Louisville 2320 So. Brook St. Louisville Kentucky 40292 UNITED STATES OF AMERICA ; _publ_contact_author_email 'GRAPPERHAUS@LOUISVILLE.EDU' _publ_section_title ; Synthesis and Structure of an Asymmetric Dinuclear Ag(I) Complex with Three Distinct Intermolecular p-Stacking Interactions ; _publ_section_references ; Bruker Analytical X-ray Solutions: SHELXTL 6.12 (2001) Program Library for Structure Solution and Molecular Graphics, Madison, WI. Farrugia L. J. (1997). Ortep-3 for Windows: J. Appl. Cryst. 30, 565. Sheldrick, G. M. SHELXS-90. Acta Crystallogr. 1990, A46, 467. Sheldrick, G. M. SHELXL-97, Program for the Refinement of Crystal Structures; University of Gottingen, Germany, 1997. Sheldrick, G. M. (2001). SADABS-2.03. University of Gottingen, Germany. ; _publ_section_figure_captions ; Figure 1. ORTEP-3 (Farrugia, 1997) of 2. Figure 2. ORTEP-3 (Farrugia, 1997) of 3. ; _publ_section_acknowledgements ; We thank the Kentucky Research Challenge Trust Fund for the purchase of CCD X-ray equipment and upgrade of our X-ray facility. ; data_2 _database_code_CSD 186788 _audit_creation_method SHELXL-97 _audit_update_record ; Dec_19_2001 text and data added by Mark S. Mashuta May_16_2002 text and data added by Mark S. Mashuta ; _chemical_name_systematic ; 1,5-bis(benzothiazolyl)-3-thiapentane ; _chemical_name_common '1,5-bis(benzothiazolyl)-3-thiapentane' _chemical_melting_point ? _chemical_formula_moiety 'C18 H16 N2 S3' _chemical_formula_sum 'C18 H16 N2 S3' _chemical_formula_weight 356.51 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 31.066(4) _cell_length_b 4.9437(6) _cell_length_c 11.2118(14) _cell_angle_alpha 90.00 _cell_angle_beta 110.472(2) _cell_angle_gamma 90.00 _cell_volume 1613.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7223 _cell_measurement_theta_min 2.80 _cell_measurement_theta_max 28.16 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.468 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 744 _exptl_absorpt_coefficient_mu 0.459 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.962 _exptl_absorpt_correction_T_max 0.986 _exptl_absorpt_process_details ; Sheldrick, G. M.; SADABS (1996). ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART APEX CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 6626 _diffrn_reflns_av_R_equivalents 0.028 _diffrn_reflns_av_sigmaI/netI 0.031 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 40 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.80 _diffrn_reflns_theta_max 28.16 _reflns_number_total 1874 _reflns_number_gt 1633 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART 5.624 (Bruker, 1994)' _computing_cell_refinement 'SAINT 6.2 (Bruker, 1994)' _computing_data_reduction 'SAINT 6.2 (Bruker, 1994)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 6.12 (Bruker, 2001)' _computing_publication_material 'SHELXTL 6.12 (Bruker, 2001)' _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^)+(0.0290P)^2^+5.8200P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 1874 _refine_ls_number_parameters 137 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.050 _refine_ls_R_factor_gt 0.042 _refine_ls_wR_factor_ref 0.099 _refine_ls_wR_factor_gt 0.096 _refine_ls_goodness_of_fit_ref 1.09 _refine_ls_restrained_S_all 1.09 _refine_ls_shift/su_max 0.04 _refine_ls_shift/su_mean 0.01 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 S1 S 0.40702(2) 0.03682(12) 0.85417(5) 0.01813(17) Uani 1 1 d . . . S2 S 0.5000 0.73910(16) 1.2500 0.0190(2) Uani 1 2 d S . . N1 N 0.38500(7) 0.1131(4) 1.05503(17) 0.0168(4) Uani 1 1 d . . . C7 C 0.41407(8) 0.1857(5) 1.0019(2) 0.0159(4) Uani 1 1 d . . . C8 C 0.45256(8) 0.3811(5) 1.0572(2) 0.0185(5) Uani 1 1 d . . . C2 C 0.33325(9) -0.3362(5) 0.7814(2) 0.0219(5) Uani 1 1 d . . . C9 C 0.45285(8) 0.5043(5) 1.1820(2) 0.0179(5) Uani 1 1 d . . . C1 C 0.36071(8) -0.1447(5) 0.8651(2) 0.0170(5) Uani 1 1 d . . . C6 C 0.35412(8) -0.0773(5) 0.9794(2) 0.0170(5) Uani 1 1 d . . . C3 C 0.29966(8) -0.4617(5) 0.8151(2) 0.0233(5) Uani 1 1 d . . . C4 C 0.29278(8) -0.3986(5) 0.9287(2) 0.0224(5) Uani 1 1 d . . . C5 C 0.31967(8) -0.2046(5) 1.0111(2) 0.0201(5) Uani 1 1 d . . . H4 H 0.2697(10) -0.488(6) 0.952(3) 0.032(8) Uiso 1 1 d . . . H3 H 0.2805(10) -0.586(6) 0.763(3) 0.023(7) Uiso 1 1 d . . . H5 H 0.3155(9) -0.168(6) 1.089(3) 0.021(7) Uiso 1 1 d . . . H9A H 0.4255(9) 0.613(6) 1.169(2) 0.017(6) Uiso 1 1 d . . . H9B H 0.4559(9) 0.367(6) 1.249(3) 0.023(7) Uiso 1 1 d . . . H2 H 0.3383(10) -0.380(6) 0.707(3) 0.026(7) Uiso 1 1 d . . . H8A H 0.4810(10) 0.289(6) 1.072(3) 0.029(8) Uiso 1 1 d . . . H8B H 0.4495(10) 0.517(7) 0.994(3) 0.033(8) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0219(3) 0.0189(3) 0.0152(3) -0.0022(2) 0.0084(2) -0.0030(2) S2 0.0183(4) 0.0142(4) 0.0207(4) 0.000 0.0019(3) 0.000 N1 0.0197(9) 0.0159(10) 0.0141(9) 0.0007(7) 0.0051(7) 0.0000(8) C7 0.0194(11) 0.0151(11) 0.0116(9) 0.0003(8) 0.0035(8) 0.0023(9) C8 0.0205(12) 0.0189(12) 0.0162(10) 0.0002(9) 0.0067(9) -0.0022(9) C2 0.0250(12) 0.0193(12) 0.0194(11) -0.0038(9) 0.0052(10) 0.0004(10) C9 0.0166(11) 0.0169(11) 0.0192(11) -0.0026(9) 0.0049(9) -0.0017(9) C1 0.0173(11) 0.0152(11) 0.0179(11) 0.0024(9) 0.0051(9) 0.0008(9) C6 0.0171(11) 0.0175(11) 0.0149(10) 0.0020(8) 0.0034(8) 0.0017(9) C3 0.0187(12) 0.0200(12) 0.0258(12) -0.0025(10) 0.0009(10) -0.0013(10) C4 0.0143(11) 0.0242(13) 0.0270(12) 0.0043(10) 0.0052(9) -0.0014(9) C5 0.0173(11) 0.0245(13) 0.0179(11) 0.0032(9) 0.0055(9) 0.0022(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 S1 C1 1.736(2) . yes S1 C7 1.755(2) . yes S2 C9 1.815(2) . yes S2 C9 1.815(2) 2_657 yes N1 C7 1.295(3) . yes N1 C6 1.399(3) . yes C7 C8 1.493(3) . no C8 C9 1.523(3) . no C8 H8A 0.96(3) . no C8 H8B 0.95(3) . no C2 C3 1.375(4) . no C2 C1 1.394(3) . no C2 H2 0.92(3) . no C9 H9A 0.97(3) . no C9 H9B 0.99(3) . no C1 C6 1.406(3) . no C6 C5 1.391(3) . no C3 C4 1.398(4) . no C3 H3 0.91(3) . no C4 C5 1.390(3) . no C4 H4 0.95(3) . no C5 H5 0.94(3) . no 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 C1 S1 C7 89.04(11) . . yes C9 S2 C9 100.46(16) . 2_657 yes C7 N1 C6 110.38(19) . . yes N1 C7 C8 125.0(2) . . no N1 C7 S1 116.19(17) . . yes C8 C7 S1 118.76(16) . . yes C7 C8 C9 112.77(19) . . no C7 C8 H8A 108.7(18) . . no C9 C8 H8A 109.1(17) . . no C7 C8 H8B 106.9(19) . . no C9 C8 H8B 111.3(19) . . no H8A C8 H8B 108(3) . . no C3 C2 C1 117.8(2) . . no C3 C2 H2 121.7(18) . . no C1 C2 H2 120.5(18) . . no C8 C9 S2 112.71(16) . . no C8 C9 H9A 110.8(15) . . no S2 C9 H9A 104.1(16) . . no C8 C9 H9B 112.8(17) . . no S2 C9 H9B 105.8(16) . . no H9A C9 H9B 110(2) . . no C2 C1 C6 121.6(2) . . no C2 C1 S1 129.12(19) . . no C6 C1 S1 109.28(17) . . no C5 C6 N1 125.1(2) . . no C5 C6 C1 119.8(2) . . no N1 C6 C1 115.1(2) . . no C2 C3 C4 121.4(2) . . no C2 C3 H3 121.3(17) . . no C4 C3 H3 117.2(18) . . no C5 C4 C3 120.8(2) . . no C5 C4 H4 117.9(19) . . no C3 C4 H4 121.3(19) . . no C4 C5 C6 118.6(2) . . no C4 C5 H5 120.3(17) . . no C6 C5 H5 121.0(17) . . no _diffrn_measured_fraction_theta_max 0.945 _diffrn_reflns_theta_full 28.16 _diffrn_measured_fraction_theta_full 0.945 _refine_diff_density_max 0.443 _refine_diff_density_min -0.311 _refine_diff_density_rms 0.076 #===END data_3 _database_code_CSD 186789 _audit_creation_method SHELXL-97 _audit_update_record ; March_12_2002 text and data added by Mark S. Mashuta May_17_2002 text and data added by Mark S. Mashuta ; _chemical_name_systematic ; Di[1,5-bis(benzothiazolyl)-3-thiapentane silver(I)] acetonitrile dihexafluorphosphate ; _chemical_name_common '[(bbttp)Ag]2 CH3CN (PF6)2' _chemical_melting_point ? _chemical_formula_moiety 'C38 H35 Ag2 N5 S6, C Cl2, 2(P F6)' _chemical_formula_sum 'C39 H35 Ag2 Cl2 F12 N5 P2 S6' _chemical_formula_weight 1342.66 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.408(1) _cell_length_b 16.540(2) _cell_length_c 13.188(1) _cell_angle_alpha 77.625(2) _cell_angle_beta 117.474(2) _cell_angle_gamma 112.922(2) _cell_volume 2387.8(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5160 _cell_measurement_theta_min 2.68 _cell_measurement_theta_max 28.00 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.867 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1332 _exptl_absorpt_coefficient_mu 1.346 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.748 _exptl_absorpt_correction_T_max 0.973 _exptl_absorpt_process_details ; Sheldrick, G. M.; SADABS (1996). ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART APEX CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 21070 _diffrn_reflns_av_R_equivalents 0.022 _diffrn_reflns_av_sigmaI/netI 0.040 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 28.28 _reflns_number_total 10667 _reflns_number_gt 8479 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART 5.624 (Bruker, 1994)' _computing_cell_refinement 'SAINT 6.2 (Bruker, 1994)' _computing_data_reduction 'SAINT 6.2 (Bruker, 1994)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 6.12 (Bruker, 2001)' _computing_publication_material 'SHELXTL 6.12 (Bruker, 2001)' _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^)+(0.0378P)^2^+0.9300P] 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_number_reflns 10667 _refine_ls_number_parameters 665 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.044 _refine_ls_R_factor_gt 0.033 _refine_ls_wR_factor_ref 0.079 _refine_ls_wR_factor_gt 0.077 _refine_ls_goodness_of_fit_ref 1.05 _refine_ls_restrained_S_all 1.05 _refine_ls_shift/su_max 0.032 _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 Ag1 Ag 0.768925(18) 0.428444(14) 0.617846(18) 0.02315(6) Uani 1 1 d . . . Ag2 Ag 0.522259(18) 0.103408(15) 0.564355(18) 0.02459(6) Uani 1 1 d . . . S1 S 1.06279(6) 0.41475(5) 0.99901(6) 0.02691(17) Uani 1 1 d . . . S2 S 0.95801(6) 0.53132(5) 0.58823(6) 0.02364(16) Uani 1 1 d . . . S3 S 0.56404(7) 0.59165(5) 0.30793(6) 0.02949(18) Uani 1 1 d . . . S4 S 0.85561(6) 0.06484(5) 0.88241(6) 0.02177(15) Uani 1 1 d . . . S5 S 0.69885(6) 0.26795(4) 0.56792(6) 0.01722(14) Uani 1 1 d . . . S6 S 0.38599(6) 0.21030(5) 0.18694(6) 0.02090(15) Uani 1 1 d . . . N1 N 0.8824(2) 0.42173(15) 0.80931(19) 0.0202(5) Uani 1 1 d . . . N2 N 0.6413(2) 0.48946(15) 0.47944(19) 0.0206(5) Uani 1 1 d . . . N3 N 0.65092(19) 0.06314(14) 0.72112(19) 0.0183(5) Uani 1 1 d . . . N4 N 0.42219(19) 0.12678(14) 0.38211(19) 0.0178(5) Uani 1 1 d . . . N5 N 0.4224(2) 0.16256(18) 0.6421(2) 0.0329(6) Uani 1 1 d . . . C1 C 0.9260(2) 0.33539(19) 0.9815(2) 0.0216(6) Uani 1 1 d . . . C2 C 0.8973(3) 0.2652(2) 1.0539(3) 0.0279(7) Uani 1 1 d . . . H2 H 0.9563 0.2563 1.1269 0.030(9) Uiso 1 1 calc R . . C3 C 0.7815(3) 0.2088(2) 1.0173(3) 0.0299(7) Uani 1 1 d . . . H3 H 0.7604 0.1601 1.0654 0.026(8) Uiso 1 1 calc R . . C4 C 0.6942(3) 0.2221(2) 0.9103(3) 0.0295(7) Uani 1 1 d . . . H4 H 0.6147 0.1821 0.8869 0.038(9) Uiso 1 1 calc R . . C5 C 0.7214(3) 0.29214(19) 0.8384(2) 0.0248(6) Uani 1 1 d . . . H5 H 0.6617 0.3012 0.7660 0.016(7) Uiso 1 1 calc R . . C6 C 0.8390(2) 0.34945(18) 0.8744(2) 0.0200(6) Uani 1 1 d . . . C7 C 0.9967(2) 0.46061(18) 0.8638(2) 0.0214(6) Uani 1 1 d . . . C8 C 1.0766(2) 0.53766(19) 0.8225(3) 0.0268(7) Uani 1 1 d . . . H8A H 1.1266 0.5163 0.8057 0.019(7) Uiso 1 1 calc R . . H8B H 1.1308 0.5785 0.8857 0.038(9) Uiso 1 1 calc R . . C9 C 1.0157(3) 0.58916(19) 0.7175(2) 0.0259(6) Uani 1 1 d . . . H9A H 1.0734 0.6480 0.7131 0.039(9) Uiso 1 1 calc R . . H9B H 0.9493 0.5972 0.7236 0.030(9) Uiso 1 1 calc R . . C10 C 0.4624(3) 0.49106(19) 0.3219(2) 0.0241(6) Uani 1 1 d . . . C11 C 0.3409(3) 0.4553(2) 0.2516(3) 0.0317(7) Uani 1 1 d . . . H11 H 0.3016 0.4874 0.1863 0.039(9) Uiso 1 1 calc R . . C12 C 0.2801(3) 0.3716(2) 0.2807(3) 0.0324(7) Uani 1 1 d . . . H12 H 0.1978 0.3453 0.2336 0.041(10) Uiso 1 1 calc R . . C13 C 0.3365(3) 0.3249(2) 0.3774(3) 0.0263(7) Uani 1 1 d . . . H13 H 0.2919 0.2678 0.3954 0.017(7) Uiso 1 1 calc R . . C14 C 0.4560(2) 0.36046(18) 0.4473(2) 0.0220(6) Uani 1 1 d . . . H14 H 0.4941 0.3285 0.5135 0.017(7) Uiso 1 1 calc R . . C15 C 0.5199(2) 0.44419(18) 0.4190(2) 0.0208(6) Uani 1 1 d . . . C16 C 0.6765(2) 0.56606(18) 0.4311(2) 0.0212(6) Uani 1 1 d . . . C17 C 0.7997(3) 0.63173(19) 0.4754(3) 0.0279(7) Uani 1 1 d . . . H17A H 0.8223 0.6436 0.5549 0.036(9) Uiso 1 1 calc R . . H17B H 0.7973 0.6873 0.4293 0.025(8) Uiso 1 1 calc R . . C18 C 0.8986(3) 0.6069(2) 0.4749(3) 0.0281(7) Uani 1 1 d . . . H18A H 0.9657 0.6617 0.4781 0.027(8) Uiso 1 1 calc R . . H18B H 0.8674 0.5808 0.4007 0.027(8) Uiso 1 1 calc R . . C19 C 0.7312(2) 0.01092(18) 0.9115(2) 0.0209(6) Uani 1 1 d . . . C20 C 0.7239(3) -0.0345(2) 1.0115(3) 0.0274(7) Uani 1 1 d . . . H20 H 0.7934 -0.0389 1.0770 0.023(8) Uiso 1 1 calc R . . C21 C 0.6129(3) -0.0728(2) 1.0117(3) 0.0300(7) Uani 1 1 d . . . H21 H 0.6056 -0.1047 1.0785 0.041(10) Uiso 1 1 calc R . . C22 C 0.5103(3) -0.0659(2) 0.9161(3) 0.0287(7) Uani 1 1 d . . . H22 H 0.4349 -0.0925 0.9193 0.037(9) Uiso 1 1 calc R . . C23 C 0.5171(2) -0.02118(18) 0.8176(2) 0.0226(6) Uani 1 1 d . . . H23 H 0.4474 -0.0166 0.7526 0.020(7) Uiso 1 1 calc R . . C24 C 0.6290(2) 0.01725(17) 0.8156(2) 0.0193(6) Uani 1 1 d . . . C25 C 0.7643(2) 0.09072(17) 0.7444(2) 0.0181(6) Uani 1 1 d . . . C26 C 0.8165(2) 0.14099(17) 0.6618(2) 0.0191(6) Uani 1 1 d . . . H26A H 0.7635 0.1155 0.5857 0.023(8) Uiso 1 1 calc R . . H26B H 0.8946 0.1339 0.6868 0.017(7) Uiso 1 1 calc R . . C27 C 0.8342(2) 0.23945(17) 0.6503(2) 0.0193(6) Uani 1 1 d . . . H27A H 0.8901 0.2703 0.6139 0.017(7) Uiso 1 1 calc R . . H27B H 0.8724 0.2619 0.7279 0.014(7) Uiso 1 1 calc R . . C28 C 0.2639(2) 0.15663(17) 0.2194(2) 0.0172(5) Uani 1 1 d . . . C29 C 0.1454(2) 0.15252(18) 0.1551(2) 0.0209(6) Uani 1 1 d . . . H29 H 0.1209 0.1813 0.0817 0.018(7) Uiso 1 1 calc R . . C30 C 0.0650(2) 0.10518(18) 0.2018(2) 0.0218(6) Uani 1 1 d . . . H30 H -0.0164 0.1009 0.1592 0.024(8) Uiso 1 1 calc R . . C31 C 0.1003(2) 0.06319(18) 0.3106(2) 0.0212(6) Uani 1 1 d . . . H31 H 0.0429 0.0314 0.3406 0.023(8) Uiso 1 1 calc R . . C32 C 0.2180(2) 0.06762(17) 0.3745(2) 0.0178(6) Uani 1 1 d . . . H32 H 0.2420 0.0390 0.4481 0.018(7) Uiso 1 1 calc R . . C33 C 0.3007(2) 0.11515(17) 0.3286(2) 0.0165(5) Uani 1 1 d . . . C34 C 0.4764(2) 0.17487(18) 0.3176(2) 0.0187(6) Uani 1 1 d . . . C35 C 0.6068(2) 0.1991(2) 0.3505(2) 0.0232(6) Uani 1 1 d . . . H35A H 0.6196 0.2090 0.2800 0.025(8) Uiso 1 1 calc R . . H35B H 0.6330 0.1491 0.3949 0.015(7) Uiso 1 1 calc R . . C36 C 0.6853(2) 0.28172(19) 0.4217(2) 0.0229(6) Uani 1 1 d . . . H36A H 0.6519 0.3295 0.3820 0.032(9) Uiso 1 1 calc R . . H36B H 0.7661 0.3007 0.4244 0.026(8) Uiso 1 1 calc R . . C37 C 0.3373(3) 0.15055(19) 0.6503(2) 0.0253(6) Uani 1 1 d . . . C38 C 0.2269(3) 0.1341(2) 0.6596(3) 0.0372(8) Uani 1 1 d . . . H38A H 0.1657 0.1426 0.5840 0.050(11) Uiso 1 1 calc R . . H38B H 0.2408 0.1751 0.7123 0.041(10) Uiso 1 1 calc R . . H38C H 0.1997 0.0737 0.6886 0.050(11) Uiso 1 1 calc R . . P1 P 0.12581(6) 0.86423(5) 0.63177(6) 0.01986(15) Uani 1 1 d . . . F1 F 0.00928(15) 0.79628(11) 0.64690(15) 0.0321(4) Uani 1 1 d . . . F2 F 0.24277(14) 0.93189(11) 0.61578(14) 0.0285(4) Uani 1 1 d . . . F3 F 0.20325(15) 0.80603(11) 0.72221(15) 0.0329(4) Uani 1 1 d . . . F4 F 0.05005(15) 0.92293(12) 0.54247(15) 0.0362(4) Uani 1 1 d . . . F5 F 0.15624(15) 0.91950(11) 0.73395(14) 0.0309(4) Uani 1 1 d . . . F6 F 0.09733(18) 0.80857(12) 0.53037(16) 0.0419(5) Uani 1 1 d . . . P2 P 0.17559(7) 0.28712(5) 0.85320(7) 0.02638(18) Uani 1 1 d . . . F7 F 0.09951(16) 0.24185(13) 0.73215(15) 0.0371(4) Uani 1 1 d . . . F8 F 0.25159(17) 0.33245(17) 0.97386(17) 0.0558(6) Uani 1 1 d . . . F9 F 0.06098(17) 0.25133(16) 0.87969(17) 0.0528(6) Uani 1 1 d . . . F10 F 0.2875(2) 0.3239(2) 0.8253(2) 0.1029(12) Uani 1 1 d . . . F11 F 0.1382(3) 0.37143(15) 0.7933(2) 0.0785(9) Uani 1 1 d . . . F12 F 0.2073(3) 0.20268(19) 0.9128(2) 0.0896(10) Uani 1 1 d . . . C50 C 0.5471(5) 0.4078(4) 0.0246(4) 0.0861(18) Uani 1 1 d . . . Cl1A Cl 0.6131(2) 0.43278(16) 0.1688(2) 0.0468(6) Uani 0.70 1 d P . . Cl1B Cl 0.5850(9) 0.4335(7) 0.1697(9) 0.029(2) Uiso 0.15 1 d P . . Cl1C Cl 0.605(4) 0.423(3) 0.144(3) 0.03(2) Uiso 0.15 1 d P . . Cl2A Cl 0.6033(2) 0.3363(2) 0.0033(3) 0.0726(9) Uani 0.70 1 d P . . Cl2B Cl 0.6183(8) 0.3135(6) 0.0690(8) 0.059(3) Uiso 0.15 1 d P . . Cl2C Cl 0.6189(12) 0.3675(7) -0.0132(13) 0.059(4) Uiso 0.15 1 d P . . 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 0.02057(11) 0.01719(11) 0.02039(12) 0.00175(8) 0.00272(9) 0.00373(8) Ag2 0.01529(11) 0.02836(13) 0.02110(12) 0.00614(9) 0.00397(9) 0.00665(9) S1 0.0222(4) 0.0321(4) 0.0202(4) -0.0034(3) 0.0020(3) 0.0103(3) S2 0.0230(4) 0.0260(4) 0.0228(4) 0.0000(3) 0.0112(3) 0.0078(3) S3 0.0295(4) 0.0267(4) 0.0229(4) 0.0059(3) 0.0058(3) 0.0102(3) S4 0.0169(3) 0.0233(4) 0.0203(4) 0.0012(3) 0.0046(3) 0.0070(3) S5 0.0146(3) 0.0157(3) 0.0181(3) -0.0008(3) 0.0045(3) 0.0045(3) S6 0.0157(3) 0.0268(4) 0.0176(3) 0.0004(3) 0.0068(3) 0.0054(3) N1 0.0198(12) 0.0218(12) 0.0180(12) -0.0028(9) 0.0070(10) 0.0060(10) N2 0.0209(12) 0.0198(12) 0.0203(12) -0.0004(9) 0.0068(10) 0.0085(10) N3 0.0174(11) 0.0167(12) 0.0196(12) -0.0006(9) 0.0060(10) 0.0067(9) N4 0.0160(11) 0.0178(12) 0.0178(12) -0.0034(9) 0.0042(9) 0.0060(9) N5 0.0317(15) 0.0397(16) 0.0317(15) -0.0037(12) 0.0145(12) 0.0138(13) C1 0.0230(14) 0.0268(15) 0.0176(14) -0.0041(12) 0.0060(12) 0.0125(12) C2 0.0386(18) 0.0304(17) 0.0209(16) 0.0048(12) 0.0124(14) 0.0211(15) C3 0.047(2) 0.0246(16) 0.0273(17) 0.0049(13) 0.0225(15) 0.0153(15) C4 0.0326(17) 0.0281(17) 0.0296(17) -0.0029(13) 0.0185(14) 0.0046(14) C5 0.0230(15) 0.0291(16) 0.0204(15) -0.0019(12) 0.0081(12) 0.0079(13) C6 0.0252(15) 0.0218(14) 0.0161(14) -0.0015(11) 0.0092(12) 0.0101(12) C7 0.0205(14) 0.0222(15) 0.0197(14) -0.0044(11) 0.0054(12) 0.0074(12) C8 0.0195(15) 0.0275(16) 0.0281(16) -0.0078(13) 0.0067(13) 0.0031(12) C9 0.0254(15) 0.0208(15) 0.0285(16) -0.0045(12) 0.0104(13) 0.0040(12) C10 0.0255(15) 0.0267(16) 0.0190(15) -0.0022(12) 0.0071(12) 0.0097(13) C11 0.0302(17) 0.0333(18) 0.0242(17) -0.0008(13) 0.0029(14) 0.0140(14) C12 0.0232(16) 0.0359(19) 0.0295(18) -0.0110(14) 0.0028(14) 0.0066(14) C13 0.0256(16) 0.0234(16) 0.0309(17) -0.0055(13) 0.0124(13) 0.0062(13) C14 0.0226(14) 0.0206(14) 0.0244(15) -0.0003(12) 0.0096(12) 0.0095(12) C15 0.0217(14) 0.0228(15) 0.0198(14) -0.0027(11) 0.0066(12) 0.0112(12) C16 0.0234(14) 0.0214(15) 0.0186(14) 0.0016(11) 0.0072(12) 0.0107(12) C17 0.0290(16) 0.0191(15) 0.0286(17) 0.0058(12) 0.0094(13) 0.0081(13) C18 0.0261(16) 0.0294(17) 0.0237(16) 0.0051(13) 0.0122(13) 0.0053(13) C19 0.0205(14) 0.0185(14) 0.0230(15) -0.0020(11) 0.0094(12) 0.0049(11) C20 0.0275(16) 0.0282(16) 0.0203(15) 0.0005(12) 0.0065(13) 0.0085(13) C21 0.0330(17) 0.0314(17) 0.0240(16) 0.0028(13) 0.0150(14) 0.0075(14) C22 0.0278(16) 0.0285(17) 0.0318(17) -0.0001(13) 0.0176(14) 0.0056(13) C23 0.0196(14) 0.0230(15) 0.0235(15) -0.0016(12) 0.0069(12) 0.0078(12) C24 0.0209(14) 0.0165(14) 0.0192(14) -0.0017(11) 0.0068(11) 0.0065(11) C25 0.0206(14) 0.0151(13) 0.0187(14) -0.0004(10) 0.0061(11) 0.0088(11) C26 0.0182(14) 0.0216(14) 0.0188(14) 0.0009(11) 0.0062(11) 0.0107(11) C27 0.0133(13) 0.0194(14) 0.0209(14) -0.0007(11) 0.0045(11) 0.0047(11) C28 0.0153(13) 0.0155(13) 0.0193(14) -0.0012(10) 0.0074(11) 0.0034(10) C29 0.0205(14) 0.0236(15) 0.0169(14) 0.0011(11) 0.0059(11) 0.0093(12) C30 0.0149(13) 0.0242(15) 0.0244(15) -0.0007(12) 0.0065(12) 0.0071(11) C31 0.0211(14) 0.0181(14) 0.0255(15) -0.0004(11) 0.0127(12) 0.0043(11) C32 0.0217(14) 0.0144(13) 0.0165(14) 0.0002(10) 0.0078(11) 0.0059(11) C33 0.0142(13) 0.0145(13) 0.0195(14) -0.0054(10) 0.0034(11) 0.0056(10) C34 0.0151(13) 0.0220(14) 0.0173(14) -0.0061(11) 0.0036(11) 0.0057(11) C35 0.0175(14) 0.0340(17) 0.0189(15) -0.0037(12) 0.0063(12) 0.0098(12) C36 0.0170(14) 0.0267(16) 0.0189(15) 0.0002(12) 0.0066(12) 0.0032(12) C37 0.0303(17) 0.0225(15) 0.0215(15) -0.0007(12) 0.0077(13) 0.0115(13) C38 0.0285(17) 0.0283(18) 0.056(2) -0.0014(16) 0.0196(17) 0.0092(14) P1 0.0182(4) 0.0212(4) 0.0205(4) 0.0006(3) 0.0095(3) 0.0060(3) F1 0.0247(9) 0.0309(10) 0.0415(11) -0.0006(8) 0.0211(8) 0.0016(8) F2 0.0202(8) 0.0294(9) 0.0338(10) 0.0079(8) 0.0146(8) 0.0069(7) F3 0.0353(10) 0.0313(10) 0.0428(11) 0.0153(8) 0.0243(9) 0.0208(8) F4 0.0251(9) 0.0462(11) 0.0315(10) 0.0128(8) 0.0074(8) 0.0191(8) F5 0.0372(10) 0.0296(10) 0.0278(10) -0.0056(7) 0.0143(8) 0.0100(8) F6 0.0526(12) 0.0392(11) 0.0394(11) -0.0136(9) 0.0295(10) 0.0022(9) P2 0.0209(4) 0.0339(4) 0.0227(4) 0.0023(3) 0.0095(3) 0.0089(3) F7 0.0312(10) 0.0472(12) 0.0315(10) -0.0090(9) 0.0071(8) 0.0155(9) F8 0.0283(11) 0.0955(18) 0.0363(12) -0.0270(12) 0.0061(9) 0.0102(11) F9 0.0294(11) 0.0840(17) 0.0410(12) -0.0102(11) 0.0171(9) 0.0084(11) F10 0.0356(13) 0.183(3) 0.0788(19) -0.069(2) 0.0391(13) -0.0264(16) F11 0.157(3) 0.0430(14) 0.0535(15) 0.0171(11) 0.0537(17) 0.0492(16) F12 0.149(3) 0.097(2) 0.0517(16) 0.0195(14) 0.0266(17) 0.100(2) C50 0.093(4) 0.148(5) 0.046(3) -0.017(3) 0.008(3) 0.088(4) Cl1A 0.0389(11) 0.0517(10) 0.0512(10) -0.0073(6) 0.0269(9) 0.0040(9) Cl2A 0.0369(10) 0.075(2) 0.102(2) -0.0491(19) 0.0017(12) 0.0254(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 N2 2.225(2) . yes Ag1 N1 2.274(2) . yes Ag1 S5 2.5687(7) . yes Ag1 S2 2.5969(8) . yes Ag2 N3 2.170(2) . yes Ag2 N4 2.181(2) . yes Ag2 N5 2.553(3) . yes Ag2 S5 2.8191(7) . yes S1 C1 1.733(3) . no S1 C7 1.739(3) . no S2 C18 1.818(3) . no S2 C9 1.824(3) . no S3 C10 1.730(3) . no S3 C16 1.741(3) . no S4 C19 1.735(3) . no S4 C25 1.735(3) . no S5 C27 1.823(3) . no S5 C36 1.823(3) . no S6 C34 1.725(3) . no S6 C28 1.733(3) . no N1 C7 1.301(3) . no N1 C6 1.408(4) . no N2 C16 1.304(3) . no N2 C15 1.398(3) . no N3 C25 1.305(3) . no N3 C24 1.405(3) . no N4 C34 1.309(3) . no N4 C33 1.394(3) . no N5 C37 1.131(4) . no C1 C2 1.387(4) . no C1 C6 1.401(4) . no C2 C3 1.374(4) . no C2 H2 0.95 . no C3 C4 1.397(4) . no C3 H3 0.95 . no C4 C5 1.377(4) . no C4 H4 0.95 . no C5 C6 1.395(4) . no C5 H5 0.95 . no C7 C8 1.499(4) . no C8 C9 1.517(4) . no C8 H8A 0.99 . no C8 H8B 0.99 . no C9 H9A 0.99 . no C9 H9B 0.99 . no C10 C11 1.398(4) . no C10 C15 1.401(4) . no C11 C12 1.382(5) . no C11 H11 0.95 . no C12 C13 1.391(4) . no C12 H12 0.95 . no C13 C14 1.379(4) . no C13 H13 0.95 . no C14 C15 1.393(4) . no C14 H14 0.95 . no C16 C17 1.495(4) . no C17 C18 1.537(4) . no C17 H17A 0.99 . no C17 H17B 0.99 . no C18 H18A 0.99 . no C18 H18B 0.99 . no C19 C24 1.395(4) . no C19 C20 1.396(4) . no C20 C21 1.374(4) . no C20 H20 0.95 . no C21 C22 1.399(4) . no C21 H21 0.95 . no C22 C23 1.374(4) . no C22 H22 0.95 . no C23 C24 1.394(4) . no C23 H23 0.95 . no C25 C26 1.493(4) . no C26 C27 1.536(4) . no C26 H26A 0.99 . no C26 H26B 0.99 . no C27 H27A 0.99 . no C27 H27B 0.99 . no C28 C29 1.395(4) . no C28 C33 1.404(4) . no C29 C30 1.380(4) . no C29 H29 0.95 . no C30 C31 1.403(4) . no C30 H30 0.95 . no C31 C32 1.383(4) . no C31 H31 0.95 . no C32 C33 1.397(4) . no C32 H32 0.95 . no C34 C35 1.495(4) . no C35 C36 1.541(4) . no C35 H35A 0.99 . no C35 H35B 0.99 . no C36 H36A 0.99 . no C36 H36B 0.99 . no C37 C38 1.456(4) . no C38 H38A 0.98 . no C38 H38B 0.98 . no C38 H38C 0.98 . no P1 F1 1.6025(17) . no P1 F2 1.6103(17) . no P1 F3 1.6035(18) . no P1 F4 1.5924(18) . no P1 F5 1.5964(18) . no P1 F6 1.6014(19) . no P2 F7 1.6015(19) . no P2 F8 1.598(2) . no P2 F9 1.591(2) . no P2 F10 1.568(2) . no P2 F11 1.590(2) . no P2 F12 1.560(2) . no C50 Cl1C 1.43(4) . no C50 Cl2C 1.644(15) . no C50 Cl1A 1.753(5) . no C50 Cl2A 1.754(5) . no C50 Cl1B 1.841(12) . no C50 Cl2B 1.984(11) . no 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 N2 Ag1 N1 144.77(8) . . yes N2 Ag1 S5 107.14(6) . . yes N1 Ag1 S5 101.14(6) . . yes N2 Ag1 S2 96.90(6) . . yes N1 Ag1 S2 89.66(6) . . yes S5 Ag1 S2 114.96(2) . . yes N3 Ag2 N4 159.83(8) . . yes N3 Ag2 N5 101.44(9) . . yes N4 Ag2 N5 98.73(8) . . yes N3 Ag2 S5 89.46(6) . . yes N4 Ag2 S5 89.21(6) . . yes N5 Ag2 S5 93.39(6) . . yes C1 S1 C7 90.16(13) . . no C18 S2 C9 102.87(14) . . no C18 S2 Ag1 101.49(10) . . no C9 S2 Ag1 91.84(10) . . no C10 S3 C16 90.02(14) . . no C19 S4 C25 89.76(13) . . no C27 S5 C36 103.45(13) . . no C27 S5 Ag1 102.40(9) . . no C36 S5 Ag1 101.14(10) . . no C27 S5 Ag2 100.98(9) . . no C36 S5 Ag2 102.00(9) . . no Ag1 S5 Ag2 142.01(3) . . yes C34 S6 C28 90.00(13) . . no C7 N1 C6 111.3(2) . . no C7 N1 Ag1 127.54(19) . . no C6 N1 Ag1 118.03(17) . . no C16 N2 C15 112.1(2) . . no C16 N2 Ag1 122.42(19) . . no C15 N2 Ag1 124.14(18) . . no C25 N3 C24 111.4(2) . . no C25 N3 Ag2 122.12(18) . . no C24 N3 Ag2 125.80(17) . . no C34 N4 C33 111.4(2) . . no C34 N4 Ag2 121.28(18) . . no C33 N4 Ag2 125.15(18) . . no C37 N5 Ag2 144.8(2) . . no C2 C1 C6 121.0(3) . . no C2 C1 S1 129.8(2) . . no C6 C1 S1 109.2(2) . . no C3 C2 C1 118.3(3) . . no C3 C2 H2 120.8 . . no C1 C2 H2 120.8 . . no C2 C3 C4 121.0(3) . . no C2 C3 H3 119.5 . . no C4 C3 H3 119.5 . . no C5 C4 C3 121.1(3) . . no C5 C4 H4 119.5 . . no C3 C4 H4 119.5 . . no C4 C5 C6 118.4(3) . . no C4 C5 H5 120.8 . . no C6 C5 H5 120.8 . . no C5 C6 C1 120.1(3) . . no C5 C6 N1 125.4(3) . . no C1 C6 N1 114.4(2) . . no N1 C7 C8 127.7(3) . . no N1 C7 S1 115.0(2) . . no C8 C7 S1 117.3(2) . . no C7 C8 C9 116.6(2) . . no C7 C8 H8A 108.2 . . no C9 C8 H8A 108.2 . . no C7 C8 H8B 108.2 . . no C9 C8 H8B 108.2 . . no H8A C8 H8B 107.3 . . no C8 C9 S2 110.4(2) . . no C8 C9 H9A 109.6 . . no S2 C9 H9A 109.6 . . no C8 C9 H9B 109.6 . . no S2 C9 H9B 109.6 . . no H9A C9 H9B 108.1 . . no C11 C10 C15 121.2(3) . . no C11 C10 S3 129.1(2) . . no C15 C10 S3 109.7(2) . . no C12 C11 C10 117.4(3) . . no C12 C11 H11 121.3 . . no C10 C11 H11 121.3 . . no C11 C12 C13 121.7(3) . . no C11 C12 H12 119.2 . . no C13 C12 H12 119.2 . . no C14 C13 C12 120.9(3) . . no C14 C13 H13 119.5 . . no C12 C13 H13 119.5 . . no C13 C14 C15 118.6(3) . . no C13 C14 H14 120.7 . . no C15 C14 H14 120.7 . . no C14 C15 N2 126.1(3) . . no C14 C15 C10 120.1(3) . . no N2 C15 C10 113.8(2) . . no N2 C16 C17 125.7(3) . . no N2 C16 S3 114.4(2) . . no C17 C16 S3 119.8(2) . . no C16 C17 C18 116.9(3) . . no C16 C17 H17A 108.1 . . no C18 C17 H17A 108.1 . . no C16 C17 H17B 108.1 . . no C18 C17 H17B 108.1 . . no H17A C17 H17B 107.3 . . no C17 C18 S2 117.5(2) . . no C17 C18 H18A 107.9 . . no S2 C18 H18A 107.9 . . no C17 C18 H18B 107.9 . . no S2 C18 H18B 107.9 . . no H18A C18 H18B 107.2 . . no C24 C19 C20 120.9(3) . . no C24 C19 S4 109.8(2) . . no C20 C19 S4 129.3(2) . . no C21 C20 C19 117.7(3) . . no C21 C20 H20 121.1 . . no C19 C20 H20 121.1 . . no C20 C21 C22 121.5(3) . . no C20 C21 H21 119.2 . . no C22 C21 H21 119.2 . . no C23 C22 C21 120.9(3) . . no C23 C22 H22 119.5 . . no C21 C22 H22 119.5 . . no C22 C23 C24 118.2(3) . . no C22 C23 H23 120.9 . . no C24 C23 H23 120.9 . . no C19 C24 C23 120.7(3) . . no C19 C24 N3 114.0(2) . . no C23 C24 N3 125.3(2) . . no N3 C25 C26 124.5(2) . . no N3 C25 S4 115.1(2) . . no C26 C25 S4 120.4(2) . . no C25 C26 C27 113.8(2) . . no C25 C26 H26A 108.8 . . no C27 C26 H26A 108.8 . . no C25 C26 H26B 108.8 . . no C27 C26 H26B 108.8 . . no H26A C26 H26B 107.7 . . no C26 C27 S5 115.57(18) . . no C26 C27 H27A 108.4 . . no S5 C27 H27A 108.4 . . no C26 C27 H27B 108.4 . . no S5 C27 H27B 108.4 . . no H27A C27 H27B 107.4 . . no C29 C28 C33 121.3(2) . . no C29 C28 S6 129.4(2) . . no C33 C28 S6 109.27(19) . . no C30 C29 C28 117.7(3) . . no C30 C29 H29 121.2 . . no C28 C29 H29 121.2 . . no C29 C30 C31 121.7(3) . . no C29 C30 H30 119.2 . . no C31 C30 H30 119.2 . . no C32 C31 C30 120.7(3) . . no C32 C31 H31 119.7 . . no C30 C31 H31 119.7 . . no C31 C32 C33 118.5(2) . . no C31 C32 H32 120.7 . . no C33 C32 H32 120.7 . . no N4 C33 C32 125.7(2) . . no N4 C33 C28 114.1(2) . . no C32 C33 C28 120.2(2) . . no N4 C34 C35 124.4(2) . . no N4 C34 S6 115.2(2) . . no C35 C34 S6 120.3(2) . . no C34 C35 C36 114.1(2) . . no C34 C35 H35A 108.7 . . no C36 C35 H35A 108.7 . . no C34 C35 H35B 108.7 . . no C36 C35 H35B 108.7 . . no H35A C35 H35B 107.6 . . no C35 C36 S5 115.1(2) . . no C35 C36 H36A 108.5 . . no S5 C36 H36A 108.5 . . no C35 C36 H36B 108.5 . . no S5 C36 H36B 108.5 . . no H36A C36 H36B 107.5 . . no N5 C37 C38 179.1(4) . . no C37 C38 H38A 109.5 . . no C37 C38 H38B 109.5 . . no H38A C38 H38B 109.5 . . no C37 C38 H38C 109.5 . . no H38A C38 H38C 109.5 . . no H38B C38 H38C 109.5 . . no F4 P1 F5 90.08(10) . . no F4 P1 F6 90.69(11) . . no F5 P1 F6 179.08(11) . . no F4 P1 F1 90.52(10) . . no F5 P1 F1 90.28(10) . . no F6 P1 F1 90.20(10) . . no F4 P1 F3 179.40(12) . . no F5 P1 F3 89.56(10) . . no F6 P1 F3 89.66(11) . . no F1 P1 F3 89.96(10) . . no F4 P1 F2 89.59(9) . . no F5 P1 F2 90.24(10) . . no F6 P1 F2 89.27(10) . . no F1 P1 F2 179.46(11) . . no F3 P1 F2 89.94(9) . . no F12 P2 F10 91.0(2) . . no F12 P2 F11 177.55(18) . . no F10 P2 F11 91.41(19) . . no F12 P2 F9 90.13(16) . . no F10 P2 F9 178.80(18) . . no F11 P2 F9 87.42(15) . . no F12 P2 F8 89.19(14) . . no F10 P2 F8 91.36(12) . . no F11 P2 F8 90.93(14) . . no F9 P2 F8 88.92(11) . . no F12 P2 F7 90.88(13) . . no F10 P2 F7 88.57(12) . . no F11 P2 F7 89.00(12) . . no F9 P2 F7 91.15(11) . . no F8 P2 F7 179.90(17) . . no Cl1C C50 Cl2C 112(2) . . no Cl1C C50 Cl1A 4.6(19) . . no Cl2C C50 Cl1A 115.8(6) . . no Cl1C C50 Cl2A 107.0(19) . . no Cl2C C50 Cl2A 17.1(4) . . no Cl1A C50 Cl2A 111.5(3) . . no Cl1C C50 Cl1B 16(2) . . no Cl2C C50 Cl1B 127.2(7) . . no Cl1A C50 Cl1B 12.1(3) . . no Cl2A C50 Cl1B 120.9(4) . . no Cl1C C50 Cl2B 84.8(18) . . no Cl2C C50 Cl2B 38.9(6) . . no Cl1A C50 Cl2B 89.4(3) . . no Cl2A C50 Cl2B 24.8(3) . . no Cl1B C50 Cl2B 97.4(5) . . no Cl1C Cl1B C50 39(4) . . no Cl1B Cl1C C50 125(6) . . no Cl2C Cl2A Cl2B 134(2) . . no Cl2C Cl2A C50 69.3(17) . . no Cl2B Cl2A C50 93.3(7) . . no Cl2A Cl2B Cl2C 17.2(8) . . no Cl2A Cl2B C50 62.0(6) . . no Cl2C Cl2B C50 55.7(8) . . no Cl2A Cl2C Cl2B 28.5(15) . . no Cl2A Cl2C C50 93.5(19) . . no Cl2B Cl2C C50 85.4(9) . . no _diffrn_measured_fraction_theta_max 0.900 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.900 _refine_diff_density_max 1.048 _refine_diff_density_min -0.646 _refine_diff_density_rms 0.095 #===END