# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'William Clegg' _publ_contact_author_email W.CLEGG@NCL.AC.UK _publ_section_title ; Complexes of copper(I) and silver(I) with bis(methimazolyl)borate and dihydrobis(2-mercaptothiazolyl)borate ligands ; loop_ _publ_author_name 'W Clegg' 'Azizolla Beheshti' 'Mohammad Panahi Mehr' 'Valiollah Nobakht' 'Luca Russo' # Attachment 'dalton.cif' data_ab77_compound1 _database_code_depnum_ccdc_archive 'CCDC 693769' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H36 B3 Cu3 N12 S6,0.77 C4 H8 O' _chemical_formula_sum 'C27.09 H42.18 B3 Cu3 N12 O0.77 S6' _chemical_formula_weight 963.76 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' B B 0.0013 0.0007 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'I 2/a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' _cell_length_a 20.842(7) _cell_length_b 10.536(3) _cell_length_c 38.478(15) _cell_angle_alpha 90.00 _cell_angle_beta 91.453(4) _cell_angle_gamma 90.00 _cell_volume 8447(5) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 999 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 27.5 _exptl_crystal_description plate _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.516 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3943 _exptl_absorpt_coefficient_mu 1.833 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.930 _exptl_absorpt_correction_T_max 0.982 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1K CCD diffractometer' _diffrn_measurement_method 'thin-slice \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 29617 _diffrn_reflns_av_R_equivalents 0.0938 _diffrn_reflns_av_sigmaI/netI 0.1100 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_theta_min 5.67 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7353 _reflns_number_gt 4129 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _refine_special_details ; Partial occupancy was freely refined for the THF solvent molecule. ; _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^)+(0.0342P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7353 _refine_ls_number_parameters 509 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1009 _refine_ls_R_factor_gt 0.0447 _refine_ls_wR_factor_ref 0.0909 _refine_ls_wR_factor_gt 0.0787 _refine_ls_goodness_of_fit_ref 0.889 _refine_ls_restrained_S_all 0.889 _refine_ls_shift/su_max 0.007 _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 0.36776(3) 0.49349(6) 0.092450(16) 0.03449(18) Uani 1 1 d . . . Cu2 Cu 0.39032(3) 0.40390(6) 0.180552(15) 0.02569(16) Uani 1 1 d . . . Cu3 Cu 0.45145(3) 0.27288(5) 0.125200(15) 0.02585(16) Uani 1 1 d . . . S1 S 0.43017(6) 0.33444(12) 0.06898(3) 0.0284(3) Uani 1 1 d . . . S2 S 0.33541(8) 0.66245(16) 0.05934(4) 0.0528(5) Uani 1 1 d . . . S3 S 0.31194(6) 0.41719(12) 0.13829(3) 0.0261(3) Uani 1 1 d . . . S4 S 0.38325(6) 0.31995(12) 0.23435(3) 0.0270(3) Uani 1 1 d . . . S5 S 0.49496(5) 0.42184(11) 0.16193(3) 0.0218(3) Uani 1 1 d . . . S6 S 0.38394(6) 0.11375(12) 0.13955(3) 0.0289(3) Uani 1 1 d . . . N1 N 0.50968(18) 0.5438(4) 0.06235(10) 0.0256(10) Uani 1 1 d . . . N2 N 0.53469(19) 0.3806(4) 0.03058(10) 0.0285(10) Uani 1 1 d . . . N3 N 0.4557(2) 0.7547(4) 0.07681(11) 0.0408(12) Uani 1 1 d . . . N4 N 0.3903(3) 0.8974(5) 0.05555(13) 0.0574(15) Uani 1 1 d . . . N5 N 0.25621(16) 0.5937(4) 0.18105(10) 0.0217(9) Uani 1 1 d . . . N6 N 0.20351(18) 0.5620(4) 0.13216(11) 0.0305(10) Uani 1 1 d . . . N7 N 0.28901(17) 0.5032(3) 0.24092(9) 0.0215(9) Uani 1 1 d . . . N8 N 0.28624(18) 0.3490(4) 0.27909(10) 0.0246(10) Uani 1 1 d . . . N9 N 0.54721(17) 0.2019(3) 0.19022(10) 0.0221(9) Uani 1 1 d . . . N10 N 0.54938(18) 0.3655(4) 0.22491(10) 0.0237(9) Uani 1 1 d . . . N11 N 0.4970(2) 0.0016(4) 0.16244(10) 0.0298(10) Uani 1 1 d . . . N12 N 0.4140(2) -0.1271(4) 0.15741(10) 0.0291(10) Uani 1 1 d . . . B1 B 0.4847(3) 0.6313(6) 0.09199(15) 0.0305(15) Uani 1 1 d . . . H1A H 0.447(2) 0.579(4) 0.1081(11) 0.029(12) Uiso 1 1 d . . . H1B H 0.528(2) 0.662(4) 0.1096(12) 0.037(14) Uiso 1 1 d . . . B2 B 0.3059(3) 0.5967(6) 0.21156(15) 0.0227(13) Uani 1 1 d . . . H2A H 0.3046(17) 0.691(4) 0.2226(10) 0.014(11) Uiso 1 1 d . . . H2B H 0.3586(18) 0.578(3) 0.2021(9) 0.012(10) Uiso 1 1 d . . . B3 B 0.5448(3) 0.1133(6) 0.15785(16) 0.0285(14) Uani 1 1 d . . . H3A H 0.5291(17) 0.168(4) 0.1325(10) 0.015(11) Uiso 1 1 d . . . H3B H 0.597(2) 0.081(4) 0.1541(11) 0.040(14) Uiso 1 1 d . . . C1 C 0.4931(2) 0.4241(5) 0.05430(12) 0.0253(12) Uani 1 1 d . . . C2 C 0.5625(2) 0.5761(6) 0.04268(13) 0.0353(14) Uani 1 1 d . . . H2 H 0.5840 0.6556 0.0430 0.042 Uiso 1 1 calc R . . C3 C 0.5776(2) 0.4754(6) 0.02314(14) 0.0390(14) Uani 1 1 d . . . H3 H 0.6115 0.4705 0.0072 0.047 Uiso 1 1 calc R . . C4 C 0.5350(3) 0.2524(5) 0.01635(13) 0.0444(16) Uani 1 1 d . . . H4A H 0.5416 0.1911 0.0353 0.067 Uiso 1 1 calc R . . H4B H 0.5697 0.2444 -0.0002 0.067 Uiso 1 1 calc R . . H4C H 0.4938 0.2354 0.0044 0.067 Uiso 1 1 calc R . . C5 C 0.3966(3) 0.7713(5) 0.06446(14) 0.0411(15) Uani 1 1 d . . . C6 C 0.4475(4) 0.9562(7) 0.06301(18) 0.067(2) Uani 1 1 d . . . H6 H 0.4567 1.0434 0.0593 0.081 Uiso 1 1 calc R . . C7 C 0.4883(4) 0.8712(6) 0.07636(16) 0.0531(17) Uani 1 1 d . . . H7 H 0.5312 0.8864 0.0841 0.064 Uiso 1 1 calc R . . C8 C 0.3316(4) 0.9571(8) 0.0417(2) 0.106(3) Uani 1 1 d . . . H8A H 0.3113 0.9011 0.0243 0.159 Uiso 1 1 calc R . . H8B H 0.3423 1.0383 0.0309 0.159 Uiso 1 1 calc R . . H8C H 0.3019 0.9716 0.0606 0.159 Uiso 1 1 calc R . . C9 C 0.2572(2) 0.5280(4) 0.15122(12) 0.0218(11) Uani 1 1 d . . . C10 C 0.2021(2) 0.6707(5) 0.18040(14) 0.0337(13) Uani 1 1 d . . . H10 H 0.1901 0.7278 0.1982 0.040 Uiso 1 1 calc R . . C11 C 0.1702(2) 0.6504(5) 0.15049(15) 0.0387(15) Uani 1 1 d . . . H11 H 0.1312 0.6903 0.1432 0.046 Uiso 1 1 calc R . . C12 C 0.1844(3) 0.5110(6) 0.09822(14) 0.0496(16) Uani 1 1 d . . . H12A H 0.1375 0.5095 0.0960 0.074 Uiso 1 1 calc R . . H12B H 0.2011 0.4245 0.0959 0.074 Uiso 1 1 calc R . . H12C H 0.2018 0.5647 0.0799 0.074 Uiso 1 1 calc R . . C13 C 0.3178(2) 0.3934(4) 0.25095(12) 0.0216(11) Uani 1 1 d . . . C14 C 0.2366(2) 0.4305(5) 0.28678(13) 0.0360(14) Uani 1 1 d . . . H14 H 0.2070 0.4217 0.3050 0.043 Uiso 1 1 calc R . . C15 C 0.2389(2) 0.5247(5) 0.26324(13) 0.0313(13) Uani 1 1 d . . . H15 H 0.2104 0.5951 0.2621 0.038 Uiso 1 1 calc R . . C16 C 0.3026(2) 0.2327(5) 0.29810(12) 0.0353(14) Uani 1 1 d . . . H16A H 0.3113 0.1645 0.2815 0.053 Uiso 1 1 calc R . . H16B H 0.2666 0.2082 0.3126 0.053 Uiso 1 1 calc R . . H16C H 0.3408 0.2474 0.3129 0.053 Uiso 1 1 calc R . . C17 C 0.5306(2) 0.3250(4) 0.19310(12) 0.0203(11) Uani 1 1 d . . . C18 C 0.5759(2) 0.1661(5) 0.22150(13) 0.0286(12) Uani 1 1 d . . . H18 H 0.5920 0.0839 0.2269 0.034 Uiso 1 1 calc R . . C19 C 0.5772(2) 0.2668(5) 0.24305(13) 0.0293(12) Uani 1 1 d . . . H19 H 0.5941 0.2690 0.2662 0.035 Uiso 1 1 calc R . . C20 C 0.5426(2) 0.4946(5) 0.23794(13) 0.0339(13) Uani 1 1 d . . . H20A H 0.5740 0.5498 0.2269 0.051 Uiso 1 1 calc R . . H20B H 0.5501 0.4952 0.2632 0.051 Uiso 1 1 calc R . . H20C H 0.4992 0.5255 0.2325 0.051 Uiso 1 1 calc R . . C21 C 0.4341(2) -0.0050(4) 0.15359(12) 0.0274(12) Uani 1 1 d . . . C22 C 0.4655(3) -0.1993(5) 0.16921(13) 0.0379(14) Uani 1 1 d . . . H22 H 0.4651 -0.2876 0.1742 0.046 Uiso 1 1 calc R . . C23 C 0.5159(3) -0.1213(5) 0.17221(13) 0.0369(14) Uani 1 1 d . . . H23 H 0.5579 -0.1453 0.1798 0.044 Uiso 1 1 calc R . . C24 C 0.3504(3) -0.1742(5) 0.14907(14) 0.0438(15) Uani 1 1 d . . . H24A H 0.3208 -0.1469 0.1670 0.066 Uiso 1 1 calc R . . H24B H 0.3513 -0.2672 0.1481 0.066 Uiso 1 1 calc R . . H24C H 0.3359 -0.1406 0.1265 0.066 Uiso 1 1 calc R . . C25 C 0.6522(5) -0.0304(12) 0.0564(3) 0.094(4) Uani 0.772(11) 1 d P . . H25A H 0.6101 -0.0145 0.0447 0.113 Uiso 0.772(11) 1 calc PR . . H25B H 0.6857 -0.0292 0.0387 0.113 Uiso 0.772(11) 1 calc PR . . C26 C 0.6652(5) 0.0663(11) 0.0822(3) 0.084(4) Uani 0.772(11) 1 d P . . H26A H 0.6251 0.1026 0.0913 0.100 Uiso 0.772(11) 1 calc PR . . H26B H 0.6920 0.1353 0.0729 0.100 Uiso 0.772(11) 1 calc PR . . C27 C 0.7022(5) -0.0128(16) 0.1104(3) 0.111(5) Uani 0.772(11) 1 d P . . H27A H 0.7487 -0.0141 0.1058 0.134 Uiso 0.772(11) 1 calc PR . . H27B H 0.6956 0.0226 0.1338 0.134 Uiso 0.772(11) 1 calc PR . . C28 C 0.6763(7) -0.1329(13) 0.1075(3) 0.107(5) Uani 0.772(11) 1 d P . . H28A H 0.6416 -0.1432 0.1244 0.128 Uiso 0.772(11) 1 calc PR . . H28B H 0.7098 -0.1972 0.1128 0.128 Uiso 0.772(11) 1 calc PR . . O1 O 0.6516(4) -0.1500(8) 0.0733(2) 0.125(4) Uani 0.772(11) 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 Cu1 0.0332(4) 0.0437(4) 0.0269(4) 0.0019(3) 0.0081(3) 0.0055(3) Cu2 0.0209(3) 0.0298(4) 0.0266(3) 0.0044(3) 0.0046(3) 0.0025(3) Cu3 0.0295(4) 0.0226(3) 0.0256(4) 0.0021(3) 0.0040(3) -0.0016(3) S1 0.0351(8) 0.0286(8) 0.0217(7) -0.0002(6) 0.0039(6) 0.0004(6) S2 0.0493(10) 0.0636(11) 0.0459(10) 0.0157(8) 0.0096(8) 0.0225(9) S3 0.0249(7) 0.0295(7) 0.0240(7) -0.0026(6) 0.0032(6) 0.0040(6) S4 0.0243(7) 0.0290(7) 0.0278(7) 0.0067(6) 0.0050(6) 0.0055(6) S5 0.0203(6) 0.0194(7) 0.0260(7) 0.0030(6) 0.0037(5) 0.0006(5) S6 0.0285(7) 0.0238(7) 0.0347(8) 0.0025(6) 0.0062(6) -0.0031(6) N1 0.029(2) 0.028(2) 0.021(2) 0.0012(19) 0.0076(19) 0.0008(19) N2 0.029(2) 0.034(3) 0.023(2) 0.005(2) 0.0053(19) 0.016(2) N3 0.059(3) 0.031(3) 0.033(3) -0.001(2) 0.017(2) 0.006(3) N4 0.080(4) 0.042(3) 0.052(3) 0.012(3) 0.036(3) 0.030(3) N5 0.011(2) 0.022(2) 0.032(2) 0.003(2) 0.0033(18) 0.0054(18) N6 0.017(2) 0.044(3) 0.031(3) 0.002(2) 0.000(2) 0.006(2) N7 0.024(2) 0.018(2) 0.022(2) -0.0039(19) 0.0035(18) -0.0032(18) N8 0.031(2) 0.024(2) 0.019(2) -0.0056(19) 0.0088(19) -0.009(2) N9 0.019(2) 0.020(2) 0.028(2) 0.0059(19) -0.0006(18) -0.0003(18) N10 0.024(2) 0.025(2) 0.022(2) 0.0011(19) 0.0018(19) -0.0012(18) N11 0.038(3) 0.018(2) 0.034(3) 0.001(2) 0.002(2) 0.006(2) N12 0.050(3) 0.018(2) 0.020(2) 0.0016(19) 0.007(2) -0.007(2) B1 0.047(4) 0.028(4) 0.016(3) 0.004(3) 0.005(3) -0.002(3) B2 0.022(3) 0.019(3) 0.027(3) 0.000(3) -0.003(3) -0.001(3) B3 0.029(4) 0.025(3) 0.032(4) 0.002(3) 0.004(3) 0.005(3) C1 0.026(3) 0.031(3) 0.019(3) -0.001(2) 0.003(2) 0.009(2) C2 0.028(3) 0.046(4) 0.032(3) 0.014(3) 0.007(3) 0.002(3) C3 0.030(3) 0.057(4) 0.031(3) 0.014(3) 0.009(3) 0.009(3) C4 0.067(4) 0.033(4) 0.034(3) 0.004(3) 0.022(3) 0.020(3) C5 0.059(4) 0.034(3) 0.032(3) 0.008(3) 0.027(3) 0.015(3) C6 0.104(6) 0.045(4) 0.055(5) 0.003(4) 0.042(5) 0.008(5) C7 0.080(5) 0.032(4) 0.048(4) 0.001(3) 0.022(4) -0.005(4) C8 0.105(6) 0.096(6) 0.118(7) 0.052(5) 0.037(6) 0.063(5) C9 0.011(2) 0.029(3) 0.026(3) 0.004(2) 0.004(2) -0.004(2) C10 0.030(3) 0.033(3) 0.038(3) -0.001(3) 0.003(3) 0.009(3) C11 0.017(3) 0.048(4) 0.050(4) 0.002(3) 0.004(3) 0.018(3) C12 0.035(3) 0.082(5) 0.031(3) -0.003(3) -0.012(3) 0.005(3) C13 0.027(3) 0.017(3) 0.021(3) -0.007(2) 0.002(2) -0.008(2) C14 0.040(3) 0.041(3) 0.029(3) -0.016(3) 0.021(3) -0.017(3) C15 0.028(3) 0.031(3) 0.035(3) -0.011(3) 0.010(3) 0.000(2) C16 0.040(3) 0.042(3) 0.024(3) 0.009(3) 0.002(3) -0.014(3) C17 0.013(2) 0.025(3) 0.023(3) -0.001(2) 0.007(2) 0.003(2) C18 0.022(3) 0.025(3) 0.040(3) 0.014(3) 0.004(2) 0.004(2) C19 0.025(3) 0.038(3) 0.025(3) 0.009(3) -0.001(2) 0.002(3) C20 0.041(3) 0.028(3) 0.032(3) -0.009(3) 0.002(3) 0.000(3) C21 0.041(3) 0.022(3) 0.019(3) 0.001(2) 0.008(2) -0.006(3) C22 0.066(4) 0.019(3) 0.029(3) 0.001(2) 0.007(3) 0.004(3) C23 0.053(4) 0.025(3) 0.032(3) 0.005(3) -0.006(3) 0.011(3) C24 0.057(4) 0.035(3) 0.039(4) -0.003(3) 0.013(3) -0.021(3) C25 0.102(9) 0.117(10) 0.064(8) 0.047(8) 0.005(6) -0.003(7) C26 0.053(6) 0.124(10) 0.076(8) -0.013(8) 0.039(6) 0.014(6) C27 0.046(6) 0.198(15) 0.090(9) -0.068(10) 0.007(6) 0.025(9) C28 0.153(13) 0.104(10) 0.062(8) -0.018(7) -0.033(8) 0.038(9) O1 0.161(8) 0.117(7) 0.096(7) 0.012(6) -0.014(6) -0.009(6) _geom_special_details ; ; 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 S1 2.3185(15) . ? Cu1 S2 2.2811(17) . ? Cu1 S3 2.2835(15) . ? Cu1 H1A 1.97(4) . ? Cu2 Cu3 2.8641(11) . ? Cu2 S3 2.2800(15) . ? Cu2 S4 2.2594(15) . ? Cu2 S5 2.3205(14) . ? Cu3 S1 2.2910(16) . ? Cu3 S5 2.2843(14) . ? Cu3 S6 2.2661(14) . ? Cu3 H3A 1.97(4) . ? S1 C1 1.723(5) . ? S2 C5 1.722(6) . ? S3 C9 1.715(5) . ? S4 C13 1.706(5) . ? S5 C17 1.728(5) . ? S6 C21 1.710(5) . ? N1 B1 1.565(7) . ? N1 C1 1.342(6) . ? N1 C2 1.393(6) . ? N2 C1 1.355(5) . ? N2 C3 1.376(6) . ? N2 C4 1.457(6) . ? N3 B1 1.542(7) . ? N3 C5 1.322(7) . ? N3 C7 1.403(7) . ? N4 C5 1.378(7) . ? N4 C6 1.368(8) . ? N4 C8 1.464(8) . ? N5 B2 1.545(6) . ? N5 C9 1.341(6) . ? N5 C10 1.388(6) . ? N6 C9 1.370(5) . ? N6 C11 1.369(6) . ? N6 C12 1.458(6) . ? N7 B2 1.546(6) . ? N7 C13 1.355(5) . ? N7 C15 1.388(5) . ? N8 C13 1.363(5) . ? N8 C14 1.382(6) . ? N8 C16 1.463(6) . ? N9 B3 1.557(7) . ? N9 C17 1.347(5) . ? N9 C18 1.383(6) . ? N10 C17 1.345(5) . ? N10 C19 1.373(6) . ? N10 C20 1.457(6) . ? N11 B3 1.555(7) . ? N11 C21 1.348(6) . ? N11 C23 1.401(6) . ? N12 C21 1.362(6) . ? N12 C22 1.383(6) . ? N12 C24 1.444(6) . ? B1 H1A 1.15(4) . ? B1 H1B 1.16(4) . ? B2 H2A 1.08(4) . ? B2 H2B 1.18(4) . ? B3 H3A 1.17(4) . ? B3 H3B 1.15(4) . ? C2 H2 0.950 . ? C2 C3 1.343(7) . ? C3 H3 0.950 . ? C4 H4A 0.980 . ? C4 H4B 0.980 . ? C4 H4C 0.980 . ? C6 H6 0.950 . ? C6 C7 1.328(8) . ? C7 H7 0.950 . ? C8 H8A 0.980 . ? C8 H8B 0.980 . ? C8 H8C 0.980 . ? C10 H10 0.950 . ? C10 C11 1.332(7) . ? C11 H11 0.950 . ? C12 H12A 0.980 . ? C12 H12B 0.980 . ? C12 H12C 0.980 . ? C14 H14 0.950 . ? C14 C15 1.345(7) . ? C15 H15 0.950 . ? C16 H16A 0.980 . ? C16 H16B 0.980 . ? C16 H16C 0.980 . ? C18 H18 0.950 . ? C18 C19 1.346(7) . ? C19 H19 0.950 . ? C20 H20A 0.980 . ? C20 H20B 0.980 . ? C20 H20C 0.980 . ? C22 H22 0.950 . ? C22 C23 1.337(7) . ? C23 H23 0.950 . ? C24 H24A 0.980 . ? C24 H24B 0.980 . ? C24 H24C 0.980 . ? C25 H25A 0.990 . ? C25 H25B 0.990 . ? C25 C26 1.442(13) . ? C25 O1 1.417(11) . ? C26 H26A 0.990 . ? C26 H26B 0.990 . ? C26 C27 1.556(14) . ? C27 H27A 0.990 . ? C27 H27B 0.990 . ? C27 C28 1.378(14) . ? C28 H28A 0.990 . ? C28 H28B 0.990 . ? C28 O1 1.414(11) . ? 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 S1 Cu1 S2 120.49(6) . . ? S1 Cu1 S3 110.38(5) . . ? S1 Cu1 H1A 88.5(12) . . ? S2 Cu1 S3 123.84(6) . . ? S2 Cu1 H1A 92.7(12) . . ? S3 Cu1 H1A 111.6(12) . . ? Cu3 Cu2 S3 79.83(4) . . ? Cu3 Cu2 S4 122.22(5) . . ? Cu3 Cu2 S5 50.97(3) . . ? S3 Cu2 S4 127.98(5) . . ? S3 Cu2 S5 115.90(5) . . ? S4 Cu2 S5 113.48(5) . . ? Cu2 Cu3 S1 119.12(5) . . ? Cu2 Cu3 S5 52.11(4) . . ? Cu2 Cu3 S6 83.38(4) . . ? Cu2 Cu3 H3A 122.9(11) . . ? S1 Cu3 S5 117.00(5) . . ? S1 Cu3 S6 109.45(5) . . ? S1 Cu3 H3A 115.5(11) . . ? S5 Cu3 S6 126.64(5) . . ? S5 Cu3 H3A 89.2(11) . . ? S6 Cu3 H3A 93.6(11) . . ? Cu1 S1 Cu3 86.21(5) . . ? Cu1 S1 C1 99.81(17) . . ? Cu3 S1 C1 109.53(16) . . ? Cu1 S2 C5 104.4(2) . . ? Cu1 S3 Cu2 101.69(6) . . ? Cu1 S3 C9 109.89(16) . . ? Cu2 S3 C9 107.75(17) . . ? Cu2 S4 C13 103.70(17) . . ? Cu2 S5 Cu3 76.92(4) . . ? Cu2 S5 C17 97.39(15) . . ? Cu3 S5 C17 100.41(17) . . ? Cu3 S6 C21 103.87(17) . . ? B1 N1 C1 129.3(4) . . ? B1 N1 C2 122.3(4) . . ? C1 N1 C2 107.8(4) . . ? C1 N2 C3 109.0(4) . . ? C1 N2 C4 125.1(4) . . ? C3 N2 C4 125.9(4) . . ? B1 N3 C5 126.9(5) . . ? B1 N3 C7 123.9(5) . . ? C5 N3 C7 109.1(5) . . ? C5 N4 C6 107.9(6) . . ? C5 N4 C8 125.3(7) . . ? C6 N4 C8 126.8(6) . . ? B2 N5 C9 129.5(4) . . ? B2 N5 C10 122.0(4) . . ? C9 N5 C10 108.4(4) . . ? C9 N6 C11 108.7(4) . . ? C9 N6 C12 125.7(4) . . ? C11 N6 C12 125.6(4) . . ? B2 N7 C13 130.2(4) . . ? B2 N7 C15 122.5(4) . . ? C13 N7 C15 107.3(4) . . ? C13 N8 C14 109.6(4) . . ? C13 N8 C16 125.0(4) . . ? C14 N8 C16 125.4(4) . . ? B3 N9 C17 129.8(4) . . ? B3 N9 C18 122.5(4) . . ? C17 N9 C18 107.3(4) . . ? C17 N10 C19 109.3(4) . . ? C17 N10 C20 125.5(4) . . ? C19 N10 C20 125.1(4) . . ? B3 N11 C21 129.2(4) . . ? B3 N11 C23 123.6(4) . . ? C21 N11 C23 106.5(4) . . ? C21 N12 C22 108.4(4) . . ? C21 N12 C24 125.8(4) . . ? C22 N12 C24 125.7(4) . . ? N1 B1 N3 110.8(4) . . ? N1 B1 H1A 111(2) . . ? N1 B1 H1B 109(2) . . ? N3 B1 H1A 110(2) . . ? N3 B1 H1B 106(2) . . ? H1A B1 H1B 110(3) . . ? N5 B2 N7 112.5(4) . . ? N5 B2 H2A 107(2) . . ? N5 B2 H2B 111.9(18) . . ? N7 B2 H2A 107(2) . . ? N7 B2 H2B 110.3(18) . . ? H2A B2 H2B 108(3) . . ? N9 B3 N11 111.8(4) . . ? N9 B3 H3A 112.0(19) . . ? N9 B3 H3B 105(2) . . ? N11 B3 H3A 107.5(19) . . ? N11 B3 H3B 114(2) . . ? H3A B3 H3B 106(3) . . ? S1 C1 N1 129.3(4) . . ? S1 C1 N2 122.7(4) . . ? N1 C1 N2 107.9(4) . . ? N1 C2 H2 125.9 . . ? N1 C2 C3 108.1(5) . . ? H2 C2 C3 125.9 . . ? N2 C3 C2 107.1(5) . . ? N2 C3 H3 126.4 . . ? C2 C3 H3 126.4 . . ? N2 C4 H4A 109.5 . . ? N2 C4 H4B 109.5 . . ? N2 C4 H4C 109.5 . . ? H4A C4 H4B 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? S2 C5 N3 129.4(4) . . ? S2 C5 N4 123.3(5) . . ? N3 C5 N4 107.4(5) . . ? N4 C6 H6 125.6 . . ? N4 C6 C7 108.8(6) . . ? H6 C6 C7 125.6 . . ? N3 C7 C6 106.9(6) . . ? N3 C7 H7 126.6 . . ? C6 C7 H7 126.6 . . ? N4 C8 H8A 109.5 . . ? N4 C8 H8B 109.5 . . ? N4 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? S3 C9 N5 128.6(4) . . ? S3 C9 N6 124.3(4) . . ? N5 C9 N6 107.1(4) . . ? N5 C10 H10 126.0 . . ? N5 C10 C11 108.1(5) . . ? H10 C10 C11 126.0 . . ? N6 C11 C10 107.8(4) . . ? N6 C11 H11 126.1 . . ? C10 C11 H11 126.1 . . ? N6 C12 H12A 109.5 . . ? N6 C12 H12B 109.5 . . ? N6 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? S4 C13 N7 129.3(3) . . ? S4 C13 N8 123.3(4) . . ? N7 C13 N8 107.4(4) . . ? N8 C14 H14 127.0 . . ? N8 C14 C15 106.0(4) . . ? H14 C14 C15 127.0 . . ? N7 C15 C14 109.6(4) . . ? N7 C15 H15 125.2 . . ? C14 C15 H15 125.2 . . ? N8 C16 H16A 109.5 . . ? N8 C16 H16B 109.5 . . ? N8 C16 H16C 109.5 . . ? H16A C16 H16B 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? S5 C17 N9 128.2(4) . . ? S5 C17 N10 123.7(4) . . ? N9 C17 N10 108.1(4) . . ? N9 C18 H18 125.6 . . ? N9 C18 C19 108.8(4) . . ? H18 C18 C19 125.6 . . ? N10 C19 C18 106.4(4) . . ? N10 C19 H19 126.8 . . ? C18 C19 H19 126.8 . . ? N10 C20 H20A 109.5 . . ? N10 C20 H20B 109.5 . . ? N10 C20 H20C 109.5 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? S6 C21 N11 128.7(4) . . ? S6 C21 N12 122.5(4) . . ? N11 C21 N12 108.8(4) . . ? N12 C22 H22 126.5 . . ? N12 C22 C23 107.0(5) . . ? H22 C22 C23 126.5 . . ? N11 C23 C22 109.3(5) . . ? N11 C23 H23 125.4 . . ? C22 C23 H23 125.4 . . ? N12 C24 H24A 109.5 . . ? N12 C24 H24B 109.5 . . ? N12 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? H25A C25 H25B 108.4 . . ? H25A C25 C26 110.0 . . ? H25A C25 O1 110.0 . . ? H25B C25 C26 110.0 . . ? H25B C25 O1 110.0 . . ? C26 C25 O1 108.5(9) . . ? C25 C26 H26A 111.7 . . ? C25 C26 H26B 111.7 . . ? C25 C26 C27 100.4(9) . . ? H26A C26 H26B 109.5 . . ? H26A C26 C27 111.7 . . ? H26B C26 C27 111.7 . . ? C26 C27 H27A 110.8 . . ? C26 C27 H27B 110.8 . . ? C26 C27 C28 104.5(10) . . ? H27A C27 H27B 108.9 . . ? H27A C27 C28 110.8 . . ? H27B C27 C28 110.8 . . ? C27 C28 H28A 109.9 . . ? C27 C28 H28B 109.9 . . ? C27 C28 O1 108.9(11) . . ? H28A C28 H28B 108.3 . . ? H28A C28 O1 109.9 . . ? H28B C28 O1 109.9 . . ? C25 O1 C28 107.8(9) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.968 _refine_diff_density_min -0.596 _refine_diff_density_rms 0.094 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.250 0.099 0.500 129.6 38.2 2 0.750 -0.099 0.500 129.6 38.0 3 0.250 0.401 0.000 129.6 38.0 4 0.750 0.599 0.000 129.6 38.2 _platon_squeeze_details ; The void volume and electron counts are consistent with four additional THF molecules per unit cell, i.e. 0.5THF extra in the chemical formula. ; #===END data_ab76_compound2 _database_code_depnum_ccdc_archive 'CCDC 693770' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H27 Ag B N4 P S2' _chemical_formula_sum 'C26 H27 Ag B N4 P S2' _chemical_formula_weight 609.29 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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' _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 12.983(3) _cell_length_b 13.579(3) _cell_length_c 15.757(4) _cell_angle_alpha 89.743(4) _cell_angle_beta 83.854(4) _cell_angle_gamma 86.297(4) _cell_volume 2756.2(11) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 999 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.468 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1240 _exptl_absorpt_coefficient_mu 0.963 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.550 _exptl_absorpt_correction_T_max 0.700 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 SMART 1K CCD diffractometer' _diffrn_measurement_method 'thin-slice \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 19838 _diffrn_reflns_av_R_equivalents 0.0305 _diffrn_reflns_av_sigmaI/netI 0.0432 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 5.68 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9513 _reflns_number_gt 8396 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _refine_special_details ; ; _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^)+(0.0342P)^2^+6.1273P] 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 9513 _refine_ls_number_parameters 641 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0599 _refine_ls_R_factor_gt 0.0507 _refine_ls_wR_factor_ref 0.1124 _refine_ls_wR_factor_gt 0.1089 _refine_ls_goodness_of_fit_ref 1.206 _refine_ls_restrained_S_all 1.206 _refine_ls_shift/su_max 0.013 _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 0.77355(3) 0.52243(2) 0.26709(2) 0.02332(11) Uani 1 1 d . . . P1 P 0.66475(9) 0.52932(9) 0.15358(7) 0.0223(3) Uani 1 1 d . . . S1 S 0.96420(9) 0.49261(9) 0.26427(7) 0.0266(3) Uani 1 1 d . . . S2 S 0.69898(9) 0.60132(8) 0.40813(7) 0.0265(3) Uani 1 1 d . . . N1 N 0.9035(3) 0.3829(3) 0.4094(2) 0.0231(8) Uani 1 1 d . . . N2 N 1.0631(3) 0.4277(3) 0.3982(3) 0.0281(9) Uani 1 1 d . . . N3 N 0.7126(3) 0.4094(3) 0.4680(2) 0.0239(8) Uani 1 1 d . . . N4 N 0.6084(3) 0.5119(3) 0.5491(2) 0.0246(8) Uani 1 1 d . . . B1 B 0.7896(4) 0.3586(4) 0.3969(3) 0.0228(11) Uani 1 1 d . . . H1A H 0.769(4) 0.385(3) 0.331(3) 0.027 Uiso 1 1 d . . . H1B H 0.785(3) 0.274(3) 0.409(3) 0.027 Uiso 1 1 d . . . C1 C 0.5423(3) 0.6022(4) 0.1795(3) 0.0251(10) Uani 1 1 d . . . C2 C 0.5456(4) 0.6906(3) 0.2236(3) 0.0311(11) Uani 1 1 d . . . H2 H 0.6099 0.7100 0.2394 0.037 Uiso 1 1 calc R . . C3 C 0.4561(5) 0.7504(4) 0.2447(4) 0.0447(14) Uani 1 1 d . . . H3 H 0.4593 0.8108 0.2740 0.054 Uiso 1 1 calc R . . C4 C 0.3628(4) 0.7224(5) 0.2231(4) 0.0489(16) Uani 1 1 d . . . H4 H 0.3017 0.7639 0.2371 0.059 Uiso 1 1 calc R . . C5 C 0.3569(4) 0.6340(5) 0.1812(3) 0.0452(15) Uani 1 1 d . . . H5 H 0.2917 0.6145 0.1677 0.054 Uiso 1 1 calc R . . C6 C 0.4469(4) 0.5732(4) 0.1586(3) 0.0388(13) Uani 1 1 d . . . H6 H 0.4430 0.5128 0.1293 0.047 Uiso 1 1 calc R . . C7 C 0.6254(3) 0.4066(3) 0.1307(3) 0.0238(10) Uani 1 1 d . . . C8 C 0.5822(4) 0.3531(4) 0.1991(3) 0.0410(13) Uani 1 1 d . . . H8 H 0.5743 0.3813 0.2547 0.049 Uiso 1 1 calc R . . C9 C 0.5507(5) 0.2599(4) 0.1879(4) 0.0493(15) Uani 1 1 d . . . H9 H 0.5186 0.2254 0.2351 0.059 Uiso 1 1 calc R . . C10 C 0.5654(4) 0.2164(4) 0.1085(4) 0.0468(14) Uani 1 1 d . . . H10 H 0.5436 0.1519 0.1010 0.056 Uiso 1 1 calc R . . C11 C 0.6120(5) 0.2667(4) 0.0395(4) 0.0455(14) Uani 1 1 d . . . H11 H 0.6236 0.2364 -0.0152 0.055 Uiso 1 1 calc R . . C12 C 0.6418(4) 0.3623(4) 0.0512(3) 0.0315(11) Uani 1 1 d . . . H12 H 0.6736 0.3971 0.0040 0.038 Uiso 1 1 calc R . . C13 C 0.7176(3) 0.5748(3) 0.0505(3) 0.0225(9) Uani 1 1 d . . . C14 C 0.8245(4) 0.5572(4) 0.0276(3) 0.0327(11) Uani 1 1 d . . . H14 H 0.8665 0.5261 0.0670 0.039 Uiso 1 1 calc R . . C15 C 0.8691(4) 0.5848(4) -0.0517(4) 0.0455(14) Uani 1 1 d . . . H15 H 0.9417 0.5727 -0.0665 0.055 Uiso 1 1 calc R . . C16 C 0.8087(5) 0.6297(4) -0.1093(3) 0.0420(14) Uani 1 1 d . . . H16 H 0.8391 0.6462 -0.1646 0.050 Uiso 1 1 calc R . . C17 C 0.7042(5) 0.6508(5) -0.0867(3) 0.0462(14) Uani 1 1 d . . . H17 H 0.6633 0.6846 -0.1255 0.055 Uiso 1 1 calc R . . C18 C 0.6583(4) 0.6226(4) -0.0070(3) 0.0341(12) Uani 1 1 d . . . H18 H 0.5860 0.6363 0.0079 0.041 Uiso 1 1 calc R . . C19 C 0.9738(3) 0.4328(3) 0.3599(3) 0.0223(9) Uani 1 1 d . . . C20 C 0.9519(4) 0.3476(4) 0.4794(3) 0.0312(11) Uani 1 1 d . . . H20 H 0.9205 0.3097 0.5247 0.037 Uiso 1 1 calc R . . C21 C 1.0485(4) 0.3750(4) 0.4729(3) 0.0365(12) Uani 1 1 d . . . H21 H 1.0981 0.3610 0.5122 0.044 Uiso 1 1 calc R . . C22 C 1.1597(4) 0.4706(5) 0.3640(4) 0.0433(14) Uani 1 1 d . . . H22A H 1.1851 0.4398 0.3090 0.065 Uiso 1 1 calc R . . H22B H 1.2120 0.4589 0.4040 0.065 Uiso 1 1 calc R . . H22C H 1.1466 0.5418 0.3561 0.065 Uiso 1 1 calc R . . C23 C 0.6734(3) 0.5041(3) 0.4758(3) 0.0201(9) Uani 1 1 d . . . C24 C 0.6064(4) 0.4222(4) 0.5893(3) 0.0336(12) Uani 1 1 d . . . H24 H 0.5669 0.4072 0.6415 0.040 Uiso 1 1 calc R . . C25 C 0.6717(4) 0.3593(4) 0.5399(3) 0.0311(11) Uani 1 1 d . . . H25 H 0.6873 0.2918 0.5522 0.037 Uiso 1 1 calc R . . C26 C 0.5516(4) 0.6028(4) 0.5807(3) 0.0379(12) Uani 1 1 d . . . H26A H 0.5942 0.6380 0.6167 0.057 Uiso 1 1 calc R . . H26B H 0.4869 0.5869 0.6143 0.057 Uiso 1 1 calc R . . H26C H 0.5356 0.6446 0.5324 0.057 Uiso 1 1 calc R . . Ag2 Ag 0.26017(3) 0.00772(2) 0.27603(2) 0.02377(11) Uani 1 1 d . . . P2 P 0.15780(9) 0.00369(8) 0.15846(7) 0.0200(2) Uani 1 1 d . . . S3 S 0.45052(9) 0.02582(9) 0.26622(7) 0.0286(3) Uani 1 1 d . . . S4 S 0.20135(9) -0.08416(8) 0.41370(7) 0.0253(3) Uani 1 1 d . . . N5 N 0.3895(3) 0.1230(3) 0.4213(2) 0.0236(8) Uani 1 1 d . . . N6 N 0.5544(3) 0.0763(3) 0.3973(3) 0.0277(9) Uani 1 1 d . . . N7 N 0.2035(3) 0.1014(3) 0.4857(2) 0.0246(8) Uani 1 1 d . . . N8 N 0.1077(3) -0.0017(3) 0.5607(2) 0.0252(8) Uani 1 1 d . . . B2 B 0.2722(4) 0.1547(4) 0.4153(3) 0.0250(11) Uani 1 1 d . . . H2A H 0.2585 0.2395 0.4240 0.030 Uiso 1 1 calc R . . H2B H 0.2498 0.1343 0.3486 0.030 Uiso 1 1 calc R . . C27 C 0.0316(3) 0.0729(3) 0.1732(3) 0.0214(9) Uani 1 1 d . . . C28 C 0.0295(4) 0.1699(3) 0.2009(3) 0.0316(11) Uani 1 1 d . . . H28 H 0.0916 0.1975 0.2132 0.038 Uiso 1 1 calc R . . C29 C -0.0653(4) 0.2272(4) 0.2107(3) 0.0372(13) Uani 1 1 d . . . H29 H -0.0668 0.2942 0.2282 0.045 Uiso 1 1 calc R . . C30 C -0.1555(4) 0.1868(4) 0.1950(3) 0.0365(12) Uani 1 1 d . . . H30 H -0.2192 0.2259 0.2019 0.044 Uiso 1 1 calc R . . C31 C -0.1544(4) 0.0904(4) 0.1695(3) 0.0315(11) Uani 1 1 d . . . H31 H -0.2174 0.0626 0.1596 0.038 Uiso 1 1 calc R . . C32 C -0.0610(3) 0.0330(4) 0.1580(3) 0.0269(10) Uani 1 1 d . . . H32 H -0.0604 -0.0337 0.1397 0.032 Uiso 1 1 calc R . . C33 C 0.1241(3) -0.1211(3) 0.1359(3) 0.0209(9) Uani 1 1 d . . . C34 C 0.0957(3) -0.1808(3) 0.2058(3) 0.0255(10) Uani 1 1 d . . . H34 H 0.0979 -0.1565 0.2620 0.031 Uiso 1 1 calc R . . C35 C 0.0644(4) -0.2743(4) 0.1943(3) 0.0338(12) Uani 1 1 d . . . H35 H 0.0432 -0.3135 0.2423 0.041 Uiso 1 1 calc R . . C36 C 0.0641(4) -0.3110(4) 0.1123(4) 0.0398(13) Uani 1 1 d . . . H36 H 0.0436 -0.3759 0.1042 0.048 Uiso 1 1 calc R . . C37 C 0.0935(4) -0.2531(4) 0.0420(3) 0.0377(12) Uani 1 1 d . . . H37 H 0.0931 -0.2783 -0.0141 0.045 Uiso 1 1 calc R . . C38 C 0.1236(4) -0.1580(3) 0.0541(3) 0.0291(11) Uani 1 1 d . . . H38 H 0.1438 -0.1183 0.0061 0.035 Uiso 1 1 calc R . . C39 C 0.2176(3) 0.0503(3) 0.0574(3) 0.0223(9) Uani 1 1 d . . . C40 C 0.3218(4) 0.0217(4) 0.0332(4) 0.0421(13) Uani 1 1 d . . . H40 H 0.3590 -0.0202 0.0694 0.051 Uiso 1 1 calc R . . C41 C 0.3713(4) 0.0538(5) -0.0426(4) 0.0503(15) Uani 1 1 d . . . H41 H 0.4414 0.0317 -0.0594 0.060 Uiso 1 1 calc R . . C42 C 0.3198(5) 0.1178(4) -0.0942(3) 0.0432(14) Uani 1 1 d . . . H42 H 0.3547 0.1406 -0.1459 0.052 Uiso 1 1 calc R . . C43 C 0.2173(4) 0.1489(4) -0.0706(3) 0.0372(12) Uani 1 1 d . . . H43 H 0.1816 0.1934 -0.1057 0.045 Uiso 1 1 calc R . . C44 C 0.1668(4) 0.1143(4) 0.0050(3) 0.0302(11) Uani 1 1 d . . . H44 H 0.0961 0.1351 0.0208 0.036 Uiso 1 1 calc R . . C45 C 0.4627(3) 0.0766(3) 0.3643(3) 0.0220(9) Uani 1 1 d . . . C46 C 0.4398(4) 0.1491(3) 0.4908(3) 0.0291(11) Uani 1 1 d . . . H46 H 0.4073 0.1821 0.5406 0.035 Uiso 1 1 calc R . . C47 C 0.5403(4) 0.1208(4) 0.4768(3) 0.0340(12) Uani 1 1 d . . . H47 H 0.5919 0.1294 0.5141 0.041 Uiso 1 1 calc R . . C48 C 0.6541(4) 0.0348(5) 0.3559(4) 0.0447(14) Uani 1 1 d . . . H48A H 0.6637 -0.0349 0.3714 0.067 Uiso 1 1 calc R . . H48B H 0.7105 0.0710 0.3747 0.067 Uiso 1 1 calc R . . H48C H 0.6548 0.0405 0.2938 0.067 Uiso 1 1 calc R . . C49 C 0.1714(3) 0.0082(3) 0.4872(3) 0.0220(9) Uani 1 1 d . . . C50 C 0.1017(4) 0.0846(4) 0.6071(3) 0.0323(11) Uani 1 1 d . . . H50 H 0.0631 0.0970 0.6611 0.039 Uiso 1 1 calc R . . C51 C 0.1608(4) 0.1478(4) 0.5615(3) 0.0320(11) Uani 1 1 d . . . H51 H 0.1716 0.2132 0.5780 0.038 Uiso 1 1 calc R . . C52 C 0.0562(4) -0.0901(4) 0.5876(3) 0.0353(12) Uani 1 1 d . . . H52A H 0.0343 -0.1225 0.5377 0.053 Uiso 1 1 calc R . . H52B H -0.0048 -0.0722 0.6280 0.053 Uiso 1 1 calc R . . H52C H 0.1042 -0.1352 0.6152 0.053 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 0.02241(19) 0.0291(2) 0.01874(18) -0.00108(14) -0.00668(14) 0.00346(14) P1 0.0167(6) 0.0335(6) 0.0160(6) -0.0018(5) -0.0017(4) 0.0017(5) S1 0.0202(6) 0.0332(6) 0.0263(6) 0.0068(5) -0.0012(5) -0.0048(5) S2 0.0334(6) 0.0235(6) 0.0216(6) -0.0015(5) -0.0004(5) 0.0013(5) N1 0.0210(19) 0.0234(19) 0.025(2) 0.0014(16) -0.0039(16) 0.0024(15) N2 0.019(2) 0.034(2) 0.031(2) -0.0025(18) -0.0065(17) 0.0027(16) N3 0.0160(18) 0.0197(19) 0.036(2) 0.0013(16) -0.0009(16) -0.0043(15) N4 0.0155(18) 0.037(2) 0.0212(19) -0.0014(17) -0.0009(15) -0.0025(16) B1 0.020(3) 0.022(3) 0.026(3) 0.002(2) -0.001(2) -0.001(2) C1 0.021(2) 0.039(3) 0.014(2) 0.0099(19) -0.0014(18) 0.004(2) C2 0.031(3) 0.024(2) 0.037(3) 0.013(2) 0.003(2) 0.003(2) C3 0.048(4) 0.026(3) 0.055(4) 0.012(2) 0.008(3) 0.012(2) C4 0.038(3) 0.057(4) 0.044(3) 0.018(3) 0.010(3) 0.029(3) C5 0.021(3) 0.086(5) 0.027(3) 0.007(3) -0.003(2) 0.012(3) C6 0.027(3) 0.065(4) 0.023(3) -0.003(2) -0.001(2) 0.003(2) C7 0.018(2) 0.032(3) 0.020(2) 0.0016(19) -0.0017(18) 0.0041(19) C8 0.046(3) 0.044(3) 0.032(3) -0.001(2) 0.006(2) -0.009(3) C9 0.053(4) 0.049(4) 0.045(3) 0.012(3) 0.008(3) -0.014(3) C10 0.045(3) 0.031(3) 0.066(4) 0.006(3) -0.003(3) -0.011(2) C11 0.051(4) 0.043(3) 0.041(3) -0.008(3) -0.001(3) -0.002(3) C12 0.031(3) 0.034(3) 0.029(3) 0.003(2) 0.001(2) -0.005(2) C13 0.019(2) 0.029(2) 0.019(2) -0.0049(18) 0.0018(18) -0.0009(18) C14 0.020(2) 0.033(3) 0.042(3) -0.003(2) 0.009(2) 0.000(2) C15 0.034(3) 0.045(3) 0.052(4) -0.002(3) 0.020(3) -0.007(3) C16 0.054(4) 0.044(3) 0.026(3) -0.004(2) 0.017(3) -0.023(3) C17 0.051(4) 0.065(4) 0.025(3) 0.012(3) -0.009(3) -0.017(3) C18 0.025(3) 0.056(3) 0.023(2) 0.006(2) -0.005(2) -0.007(2) C19 0.017(2) 0.023(2) 0.027(2) -0.0048(18) -0.0041(19) 0.0020(18) C20 0.029(3) 0.034(3) 0.030(3) 0.006(2) -0.007(2) 0.008(2) C21 0.024(3) 0.046(3) 0.041(3) -0.003(2) -0.016(2) 0.010(2) C22 0.017(2) 0.070(4) 0.045(3) -0.005(3) -0.008(2) -0.007(2) C23 0.015(2) 0.027(2) 0.019(2) 0.0005(18) -0.0058(17) -0.0043(18) C24 0.030(3) 0.048(3) 0.022(2) 0.007(2) 0.000(2) -0.009(2) C25 0.028(3) 0.035(3) 0.032(3) 0.010(2) -0.006(2) -0.010(2) C26 0.034(3) 0.049(3) 0.027(3) -0.011(2) 0.010(2) 0.000(2) Ag2 0.02389(19) 0.02708(19) 0.02193(19) -0.00033(14) -0.00850(14) -0.00382(14) P2 0.0188(6) 0.0245(6) 0.0174(6) 0.0001(4) -0.0029(4) -0.0041(5) S3 0.0216(6) 0.0380(7) 0.0261(6) -0.0031(5) 0.0018(5) -0.0073(5) S4 0.0273(6) 0.0246(6) 0.0244(6) 0.0013(5) -0.0038(5) -0.0026(5) N5 0.0196(19) 0.0224(19) 0.029(2) -0.0005(16) -0.0036(16) -0.0028(15) N6 0.0155(19) 0.033(2) 0.035(2) 0.0038(18) -0.0060(17) -0.0044(16) N7 0.0194(19) 0.025(2) 0.029(2) -0.0037(16) -0.0016(16) 0.0019(16) N8 0.0164(19) 0.033(2) 0.025(2) 0.0049(17) 0.0003(16) 0.0031(16) B2 0.024(3) 0.021(3) 0.029(3) 0.001(2) -0.002(2) 0.001(2) C27 0.026(2) 0.020(2) 0.018(2) 0.0012(17) -0.0011(18) -0.0008(18) C28 0.040(3) 0.028(3) 0.026(3) 0.004(2) 0.003(2) -0.006(2) C29 0.056(4) 0.020(2) 0.032(3) -0.001(2) 0.005(3) 0.006(2) C30 0.034(3) 0.046(3) 0.028(3) 0.004(2) 0.001(2) 0.011(2) C31 0.025(2) 0.041(3) 0.027(3) 0.000(2) -0.001(2) 0.005(2) C32 0.025(2) 0.034(3) 0.021(2) -0.003(2) -0.0006(19) -0.001(2) C33 0.015(2) 0.022(2) 0.025(2) 0.0021(18) -0.0019(18) -0.0009(17) C34 0.022(2) 0.030(2) 0.025(2) -0.0024(19) -0.0017(19) 0.0002(19) C35 0.035(3) 0.026(3) 0.041(3) 0.009(2) -0.003(2) -0.007(2) C36 0.042(3) 0.023(3) 0.055(4) -0.004(2) -0.007(3) -0.007(2) C37 0.041(3) 0.037(3) 0.036(3) -0.009(2) -0.008(2) -0.006(2) C38 0.033(3) 0.031(3) 0.023(2) 0.000(2) -0.004(2) -0.006(2) C39 0.024(2) 0.024(2) 0.020(2) 0.0002(18) -0.0029(18) -0.0083(18) C40 0.026(3) 0.053(3) 0.045(3) 0.011(3) 0.003(2) 0.001(2) C41 0.030(3) 0.060(4) 0.057(4) 0.011(3) 0.019(3) -0.007(3) C42 0.054(4) 0.041(3) 0.033(3) 0.006(2) 0.014(3) -0.024(3) C43 0.051(3) 0.035(3) 0.027(3) 0.006(2) -0.003(2) -0.009(2) C44 0.033(3) 0.036(3) 0.021(2) 0.003(2) 0.000(2) -0.007(2) C45 0.022(2) 0.018(2) 0.026(2) 0.0054(18) 0.0010(19) -0.0051(18) C46 0.027(3) 0.030(3) 0.032(3) -0.008(2) -0.008(2) -0.004(2) C47 0.029(3) 0.041(3) 0.034(3) 0.004(2) -0.012(2) -0.008(2) C48 0.020(3) 0.069(4) 0.043(3) 0.005(3) 0.001(2) -0.002(3) C49 0.014(2) 0.025(2) 0.027(2) 0.0044(19) -0.0068(18) 0.0017(18) C50 0.028(3) 0.044(3) 0.023(2) -0.003(2) 0.000(2) 0.013(2) C51 0.028(3) 0.035(3) 0.032(3) -0.004(2) -0.004(2) 0.006(2) C52 0.028(3) 0.040(3) 0.035(3) 0.014(2) 0.001(2) 0.003(2) _geom_special_details ; ; 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 P1 2.3928(12) . ? Ag1 S1 2.4779(13) . ? Ag1 S2 2.5398(12) . ? Ag1 H1A 2.12(5) . ? P1 C1 1.826(4) . ? P1 C7 1.822(5) . ? P1 C13 1.816(4) . ? S1 C19 1.720(5) . ? S2 C23 1.720(4) . ? N1 B1 1.568(6) . ? N1 C19 1.351(6) . ? N1 C20 1.395(6) . ? N2 C19 1.362(6) . ? N2 C21 1.377(7) . ? N2 C22 1.467(6) . ? N3 B1 1.552(6) . ? N3 C23 1.354(5) . ? N3 C25 1.391(6) . ? N4 C23 1.355(5) . ? N4 C24 1.371(6) . ? N4 C26 1.458(6) . ? B1 H1A 1.15(5) . ? B1 H1B 1.16(5) . ? C1 C2 1.395(7) . ? C1 C6 1.396(7) . ? C2 H2 0.950 . ? C2 C3 1.385(7) . ? C3 H3 0.950 . ? C3 C4 1.369(9) . ? C4 H4 0.950 . ? C4 C5 1.382(9) . ? C5 H5 0.950 . ? C5 C6 1.400(7) . ? C6 H6 0.950 . ? C7 C8 1.386(7) . ? C7 C12 1.383(6) . ? C8 H8 0.950 . ? C8 C9 1.373(8) . ? C9 H9 0.950 . ? C9 C10 1.375(8) . ? C10 H10 0.950 . ? C10 C11 1.386(8) . ? C11 H11 0.950 . ? C11 C12 1.396(7) . ? C12 H12 0.950 . ? C13 C14 1.401(6) . ? C13 C18 1.384(6) . ? C14 H14 0.950 . ? C14 C15 1.381(7) . ? C15 H15 0.950 . ? C15 C16 1.379(8) . ? C16 H16 0.950 . ? C16 C17 1.377(8) . ? C17 H17 0.950 . ? C17 C18 1.394(7) . ? C18 H18 0.950 . ? C20 H20 0.950 . ? C20 C21 1.325(7) . ? C21 H21 0.950 . ? C22 H22A 0.980 . ? C22 H22B 0.980 . ? C22 H22C 0.980 . ? C24 H24 0.950 . ? C24 C25 1.351(7) . ? C25 H25 0.950 . ? C26 H26A 0.980 . ? C26 H26B 0.980 . ? C26 H26C 0.980 . ? Ag2 P2 2.3956(12) . ? Ag2 S3 2.4876(13) . ? Ag2 S4 2.5671(12) . ? P2 C27 1.828(4) . ? P2 C33 1.823(4) . ? P2 C39 1.825(4) . ? S3 C45 1.721(5) . ? S4 C49 1.709(5) . ? N5 B2 1.568(6) . ? N5 C45 1.361(6) . ? N5 C46 1.392(6) . ? N6 C45 1.350(6) . ? N6 C47 1.382(6) . ? N6 C48 1.466(6) . ? N7 B2 1.554(6) . ? N7 C49 1.357(6) . ? N7 C51 1.396(6) . ? N8 C49 1.360(6) . ? N8 C50 1.377(6) . ? N8 C52 1.451(6) . ? B2 H2A 1.160 . ? B2 H2B 1.160 . ? C27 C28 1.386(6) . ? C27 C32 1.395(6) . ? C28 H28 0.950 . ? C28 C29 1.408(7) . ? C29 H29 0.950 . ? C29 C30 1.370(8) . ? C30 H30 0.950 . ? C30 C31 1.370(7) . ? C31 H31 0.950 . ? C31 C32 1.394(6) . ? C32 H32 0.950 . ? C33 C34 1.397(6) . ? C33 C38 1.385(6) . ? C34 H34 0.950 . ? C34 C35 1.376(7) . ? C35 H35 0.950 . ? C35 C36 1.388(7) . ? C36 H36 0.950 . ? C36 C37 1.390(8) . ? C37 H37 0.950 . ? C37 C38 1.393(7) . ? C38 H38 0.950 . ? C39 C40 1.396(7) . ? C39 C44 1.382(6) . ? C40 H40 0.950 . ? C40 C41 1.377(8) . ? C41 H41 0.950 . ? C41 C42 1.378(8) . ? C42 H42 0.950 . ? C42 C43 1.382(8) . ? C43 H43 0.950 . ? C43 C44 1.392(7) . ? C44 H44 0.950 . ? C46 H46 0.950 . ? C46 C47 1.332(7) . ? C47 H47 0.950 . ? C48 H48A 0.980 . ? C48 H48B 0.980 . ? C48 H48C 0.980 . ? C50 H50 0.950 . ? C50 C51 1.342(7) . ? C51 H51 0.950 . ? C52 H52A 0.980 . ? C52 H52B 0.980 . ? C52 H52C 0.980 . ? 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 P1 Ag1 S1 130.71(4) . . ? P1 Ag1 S2 117.11(4) . . ? P1 Ag1 H1A 111.5(13) . . ? S1 Ag1 S2 109.91(4) . . ? S1 Ag1 H1A 84.1(12) . . ? S2 Ag1 H1A 87.0(12) . . ? Ag1 P1 C1 113.52(15) . . ? Ag1 P1 C7 110.47(14) . . ? Ag1 P1 C13 118.16(15) . . ? C1 P1 C7 104.1(2) . . ? C1 P1 C13 105.1(2) . . ? C7 P1 C13 104.2(2) . . ? Ag1 S1 C19 101.25(15) . . ? Ag1 S2 C23 105.13(15) . . ? B1 N1 C19 131.3(4) . . ? B1 N1 C20 121.6(4) . . ? C19 N1 C20 107.1(4) . . ? C19 N2 C21 109.3(4) . . ? C19 N2 C22 124.9(4) . . ? C21 N2 C22 125.8(4) . . ? B1 N3 C23 130.3(4) . . ? B1 N3 C25 122.7(4) . . ? C23 N3 C25 107.0(4) . . ? C23 N4 C24 109.7(4) . . ? C23 N4 C26 124.7(4) . . ? C24 N4 C26 125.6(4) . . ? N1 B1 N3 109.8(4) . . ? N1 B1 H1A 110(2) . . ? N1 B1 H1B 106(2) . . ? N3 B1 H1A 110(2) . . ? N3 B1 H1B 105(2) . . ? H1A B1 H1B 115(3) . . ? P1 C1 C2 117.4(4) . . ? P1 C1 C6 123.5(4) . . ? C2 C1 C6 119.1(4) . . ? C1 C2 H2 119.7 . . ? C1 C2 C3 120.7(5) . . ? H2 C2 C3 119.7 . . ? C2 C3 H3 120.0 . . ? C2 C3 C4 120.0(6) . . ? H3 C3 C4 120.0 . . ? C3 C4 H4 119.8 . . ? C3 C4 C5 120.4(5) . . ? H4 C4 C5 119.8 . . ? C4 C5 H5 119.9 . . ? C4 C5 C6 120.3(5) . . ? H5 C5 C6 119.9 . . ? C1 C6 C5 119.4(5) . . ? C1 C6 H6 120.3 . . ? C5 C6 H6 120.3 . . ? P1 C7 C8 117.1(4) . . ? P1 C7 C12 124.1(4) . . ? C8 C7 C12 118.7(5) . . ? C7 C8 H8 119.5 . . ? C7 C8 C9 121.1(5) . . ? H8 C8 C9 119.5 . . ? C8 C9 H9 119.9 . . ? C8 C9 C10 120.2(5) . . ? H9 C9 C10 119.9 . . ? C9 C10 H10 120.0 . . ? C9 C10 C11 120.1(5) . . ? H10 C10 C11 120.0 . . ? C10 C11 H11 120.3 . . ? C10 C11 C12 119.3(5) . . ? H11 C11 C12 120.3 . . ? C7 C12 C11 120.6(5) . . ? C7 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? P1 C13 C14 117.3(4) . . ? P1 C13 C18 123.9(3) . . ? C14 C13 C18 118.7(4) . . ? C13 C14 H14 119.7 . . ? C13 C14 C15 120.5(5) . . ? H14 C14 C15 119.7 . . ? C14 C15 H15 119.9 . . ? C14 C15 C16 120.1(5) . . ? H15 C15 C16 119.9 . . ? C15 C16 H16 120.0 . . ? C15 C16 C17 120.0(5) . . ? H16 C16 C17 120.0 . . ? C16 C17 H17 119.9 . . ? C16 C17 C18 120.2(5) . . ? H17 C17 C18 119.9 . . ? C13 C18 C17 120.3(5) . . ? C13 C18 H18 119.8 . . ? C17 C18 H18 119.8 . . ? S1 C19 N1 130.6(3) . . ? S1 C19 N2 122.0(3) . . ? N1 C19 N2 107.4(4) . . ? N1 C20 H20 125.2 . . ? N1 C20 C21 109.5(5) . . ? H20 C20 C21 125.2 . . ? N2 C21 C20 106.7(4) . . ? N2 C21 H21 126.7 . . ? C20 C21 H21 126.7 . . ? N2 C22 H22A 109.5 . . ? N2 C22 H22B 109.5 . . ? N2 C22 H22C 109.5 . . ? H22A C22 H22B 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? S2 C23 N3 128.2(3) . . ? S2 C23 N4 123.9(3) . . ? N3 C23 N4 107.9(4) . . ? N4 C24 H24 126.8 . . ? N4 C24 C25 106.3(4) . . ? H24 C24 C25 126.8 . . ? N3 C25 C24 109.1(4) . . ? N3 C25 H25 125.5 . . ? C24 C25 H25 125.5 . . ? N4 C26 H26A 109.5 . . ? N4 C26 H26B 109.5 . . ? N4 C26 H26C 109.5 . . ? H26A C26 H26B 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? P2 Ag2 S3 126.11(4) . . ? P2 Ag2 S4 118.91(4) . . ? S3 Ag2 S4 109.68(4) . . ? Ag2 P2 C27 115.75(14) . . ? Ag2 P2 C33 111.95(14) . . ? Ag2 P2 C39 115.70(14) . . ? C27 P2 C33 103.15(19) . . ? C27 P2 C39 103.4(2) . . ? C33 P2 C39 105.5(2) . . ? Ag2 S3 C45 101.32(15) . . ? Ag2 S4 C49 103.66(16) . . ? B2 N5 C45 131.4(4) . . ? B2 N5 C46 121.6(4) . . ? C45 N5 C46 106.8(4) . . ? C45 N6 C47 109.7(4) . . ? C45 N6 C48 125.4(4) . . ? C47 N6 C48 124.9(4) . . ? B2 N7 C49 129.8(4) . . ? B2 N7 C51 122.7(4) . . ? C49 N7 C51 107.5(4) . . ? C49 N8 C50 109.4(4) . . ? C49 N8 C52 125.6(4) . . ? C50 N8 C52 125.0(4) . . ? N5 B2 N7 109.6(4) . . ? N5 B2 H2A 109.7 . . ? N5 B2 H2B 109.7 . . ? N7 B2 H2A 109.7 . . ? N7 B2 H2B 109.7 . . ? H2A B2 H2B 108.2 . . ? P2 C27 C28 117.5(4) . . ? P2 C27 C32 123.2(3) . . ? C28 C27 C32 119.2(4) . . ? C27 C28 H28 120.2 . . ? C27 C28 C29 119.6(5) . . ? H28 C28 C29 120.2 . . ? C28 C29 H29 119.9 . . ? C28 C29 C30 120.3(5) . . ? H29 C29 C30 119.9 . . ? C29 C30 H30 119.8 . . ? C29 C30 C31 120.5(5) . . ? H30 C30 C31 119.8 . . ? C30 C31 H31 120.0 . . ? C30 C31 C32 120.1(5) . . ? H31 C31 C32 120.0 . . ? C27 C32 C31 120.2(4) . . ? C27 C32 H32 119.9 . . ? C31 C32 H32 119.9 . . ? P2 C33 C34 117.1(3) . . ? P2 C33 C38 123.6(3) . . ? C34 C33 C38 119.3(4) . . ? C33 C34 H34 119.6 . . ? C33 C34 C35 120.8(4) . . ? H34 C34 C35 119.6 . . ? C34 C35 H35 120.2 . . ? C34 C35 C36 119.7(5) . . ? H35 C35 C36 120.2 . . ? C35 C36 H36 119.9 . . ? C35 C36 C37 120.2(5) . . ? H36 C36 C37 119.9 . . ? C36 C37 H37 120.1 . . ? C36 C37 C38 119.7(5) . . ? H37 C37 C38 120.1 . . ? C33 C38 C37 120.2(5) . . ? C33 C38 H38 119.9 . . ? C37 C38 H38 119.9 . . ? P2 C39 C40 117.8(4) . . ? P2 C39 C44 123.8(3) . . ? C40 C39 C44 118.3(4) . . ? C39 C40 H40 119.7 . . ? C39 C40 C41 120.6(5) . . ? H40 C40 C41 119.7 . . ? C40 C41 H41 119.8 . . ? C40 C41 C42 120.4(5) . . ? H41 C41 C42 119.8 . . ? C41 C42 H42 120.0 . . ? C41 C42 C43 119.9(5) . . ? H42 C42 C43 120.0 . . ? C42 C43 H43 120.3 . . ? C42 C43 C44 119.5(5) . . ? H43 C43 C44 120.3 . . ? C39 C44 C43 121.2(5) . . ? C39 C44 H44 119.4 . . ? C43 C44 H44 119.4 . . ? S3 C45 N5 129.9(3) . . ? S3 C45 N6 122.6(3) . . ? N5 C45 N6 107.6(4) . . ? N5 C46 H46 125.2 . . ? N5 C46 C47 109.7(4) . . ? H46 C46 C47 125.2 . . ? N6 C47 C46 106.3(4) . . ? N6 C47 H47 126.9 . . ? C46 C47 H47 126.9 . . ? N6 C48 H48A 109.5 . . ? N6 C48 H48B 109.5 . . ? N6 C48 H48C 109.5 . . ? H48A C48 H48B 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? S4 C49 N7 129.0(3) . . ? S4 C49 N8 123.6(3) . . ? N7 C49 N8 107.5(4) . . ? N8 C50 H50 126.5 . . ? N8 C50 C51 107.0(4) . . ? H50 C50 C51 126.5 . . ? N7 C51 C50 108.6(4) . . ? N7 C51 H51 125.7 . . ? C50 C51 H51 125.7 . . ? N8 C52 H52A 109.5 . . ? N8 C52 H52B 109.5 . . ? N8 C52 H52C 109.5 . . ? H52A C52 H52B 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.260 _refine_diff_density_min -0.880 _refine_diff_density_rms 0.089 #===END data_ab82_compound3 _database_code_depnum_ccdc_archive 'CCDC 693771' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H25 Ag B N2 P S4' _chemical_formula_sum 'C24 H25 Ag B N2 P S4' _chemical_formula_weight 619.35 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 8.8575(11) _cell_length_b 15.185(3) _cell_length_c 38.284(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5149.2(15) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 23583 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 27.5 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.598 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2512 _exptl_absorpt_coefficient_mu 1.186 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.535 _exptl_absorpt_correction_T_max 0.910 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD diffractometer' _diffrn_measurement_method 'thin-slice \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 19291 _diffrn_reflns_av_R_equivalents 0.0261 _diffrn_reflns_av_sigmaI/netI 0.0245 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_theta_min 5.74 _diffrn_reflns_theta_max 24.99 _reflns_number_total 4380 _reflns_number_gt 3864 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement EvalCCD _computing_data_reduction EvalCCD _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _refine_special_details ; ; _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^)+(0.0201P)^2^+3.9801P] 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 SHELXL _refine_ls_extinction_coef 0.0021(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4380 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0292 _refine_ls_R_factor_gt 0.0237 _refine_ls_wR_factor_ref 0.0588 _refine_ls_wR_factor_gt 0.0558 _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_restrained_S_all 1.107 _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 Ag Ag 0.067620(17) 0.249342(10) 0.145331(4) 0.02546(8) Uani 1 1 d . . . S1 S -0.09170(6) 0.18687(3) 0.192012(16) 0.02964(14) Uani 1 1 d . . . S2 S -0.32369(6) 0.24225(4) 0.240813(15) 0.03007(14) Uani 1 1 d . . . S3 S 0.25385(6) 0.36287(4) 0.166230(16) 0.03219(15) Uani 1 1 d . . . S4 S 0.25860(6) 0.54149(4) 0.194014(15) 0.03180(14) Uani 1 1 d . . . P P 0.14124(6) 0.18117(3) 0.091483(13) 0.01957(13) Uani 1 1 d . . . B B -0.1266(3) 0.40381(15) 0.16694(6) 0.0219(5) Uani 1 1 d . . . H1A H -0.083(2) 0.3557(16) 0.1461(6) 0.030(6) Uiso 1 1 d . . . H1B H -0.209(3) 0.4484(14) 0.1552(6) 0.026(6) Uiso 1 1 d . . . C1 C 0.1308(2) 0.25138(12) 0.05309(5) 0.0223(4) Uani 1 1 d . . . C2 C 0.0361(3) 0.32406(14) 0.05394(6) 0.0297(5) Uani 1 1 d . . . H2 H -0.0197 0.3369 0.0745 0.036 Uiso 1 1 calc R . . C3 C 0.0225(3) 0.37811(15) 0.02490(7) 0.0384(6) Uani 1 1 d . . . H3 H -0.0431 0.4276 0.0256 0.046 Uiso 1 1 calc R . . C4 C 0.1037(3) 0.36034(15) -0.00500(7) 0.0375(6) Uani 1 1 d . . . H4 H 0.0939 0.3973 -0.0249 0.045 Uiso 1 1 calc R . . C5 C 0.1989(3) 0.28877(16) -0.00590(6) 0.0367(6) Uani 1 1 d . . . H5 H 0.2552 0.2766 -0.0265 0.044 Uiso 1 1 calc R . . C6 C 0.2134(3) 0.23444(14) 0.02295(6) 0.0306(5) Uani 1 1 d . . . H6 H 0.2800 0.1854 0.0222 0.037 Uiso 1 1 calc R . . C7 C 0.0424(2) 0.08073(13) 0.07947(5) 0.0210(4) Uani 1 1 d . . . C8 C 0.0234(2) 0.01768(14) 0.10574(6) 0.0248(5) Uani 1 1 d . . . H8 H 0.0644 0.0277 0.1283 0.030 Uiso 1 1 calc R . . C9 C -0.0548(2) -0.05907(14) 0.09894(6) 0.0287(5) Uani 1 1 d . . . H9 H -0.0663 -0.1020 0.1168 0.034 Uiso 1 1 calc R . . C10 C -0.1163(3) -0.07384(14) 0.06634(7) 0.0338(5) Uani 1 1 d . . . H10 H -0.1694 -0.1269 0.0617 0.041 Uiso 1 1 calc R . . C11 C -0.1004(3) -0.01129(15) 0.04044(6) 0.0343(5) Uani 1 1 d . . . H11 H -0.1441 -0.0211 0.0181 0.041 Uiso 1 1 calc R . . C12 C -0.0209(2) 0.06596(14) 0.04690(6) 0.0273(5) Uani 1 1 d . . . H12 H -0.0100 0.1087 0.0289 0.033 Uiso 1 1 calc R . . C13 C 0.3397(2) 0.15004(13) 0.09396(5) 0.0209(4) Uani 1 1 d . . . C14 C 0.3914(2) 0.06380(14) 0.09202(5) 0.0245(4) Uani 1 1 d . . . H14 H 0.3235 0.0174 0.0865 0.029 Uiso 1 1 calc R . . C15 C 0.5422(3) 0.04567(15) 0.09807(6) 0.0298(5) Uani 1 1 d . . . H15 H 0.5772 -0.0134 0.0967 0.036 Uiso 1 1 calc R . . C16 C 0.6425(2) 0.11211(15) 0.10607(6) 0.0306(5) Uani 1 1 d . . . H16 H 0.7456 0.0989 0.1105 0.037 Uiso 1 1 calc R . . C17 C 0.5919(3) 0.19832(16) 0.10763(7) 0.0354(6) Uani 1 1 d . . . H17 H 0.6606 0.2445 0.1128 0.043 Uiso 1 1 calc R . . C18 C 0.4415(2) 0.21717(15) 0.10169(6) 0.0308(5) Uani 1 1 d . . . H18 H 0.4073 0.2764 0.1029 0.037 Uiso 1 1 calc R . . C19 C -0.2011(2) 0.27036(13) 0.20663(5) 0.0221(4) Uani 1 1 d . . . C20 C -0.3122(3) 0.40577(15) 0.21943(7) 0.0401(6) Uani 1 1 d . . . H20A H -0.3678 0.4490 0.2050 0.048 Uiso 1 1 calc R . . H20B H -0.2529 0.4385 0.2371 0.048 Uiso 1 1 calc R . . C21 C -0.4216(3) 0.34564(16) 0.23725(6) 0.0342(5) Uani 1 1 d . . . H21A H -0.5148 0.3390 0.2232 0.041 Uiso 1 1 calc R . . H21B H -0.4487 0.3685 0.2606 0.041 Uiso 1 1 calc R . . C22 C 0.1523(2) 0.45086(13) 0.17939(5) 0.0226(4) Uani 1 1 d . . . C23 C 0.0924(3) 0.61114(16) 0.19432(8) 0.0430(6) Uani 1 1 d . . . H23A H 0.0950 0.6526 0.2143 0.052 Uiso 1 1 calc R . . H23B H 0.0843 0.6452 0.1723 0.052 Uiso 1 1 calc R . . C24 C -0.0363(3) 0.54748(14) 0.19786(7) 0.0329(5) Uani 1 1 d . . . H24A H -0.0588 0.5373 0.2229 0.039 Uiso 1 1 calc R . . H24B H -0.1278 0.5721 0.1866 0.039 Uiso 1 1 calc R . . N1 N -0.20914(18) 0.35342(11) 0.19703(4) 0.0213(4) Uani 1 1 d . . . N2 N 0.00548(19) 0.46324(10) 0.18088(4) 0.0216(4) 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 Ag 0.02512(11) 0.02618(11) 0.02509(11) -0.00535(7) 0.00436(6) 0.00163(6) S1 0.0312(3) 0.0221(3) 0.0356(3) 0.0016(2) 0.0092(2) 0.0016(2) S2 0.0295(3) 0.0333(3) 0.0274(3) 0.0007(2) 0.0081(2) -0.0049(2) S3 0.0201(3) 0.0303(3) 0.0462(3) -0.0086(2) 0.0008(2) -0.0004(2) S4 0.0291(3) 0.0307(3) 0.0355(3) -0.0073(2) 0.0004(2) -0.0102(2) P 0.0189(3) 0.0181(2) 0.0217(3) -0.0009(2) 0.0019(2) 0.0024(2) B 0.0200(11) 0.0238(11) 0.0219(12) -0.0005(9) -0.0015(10) -0.0010(10) C1 0.0205(10) 0.0193(10) 0.0273(11) 0.0003(8) -0.0018(9) -0.0018(8) C2 0.0316(12) 0.0253(11) 0.0321(12) -0.0011(9) 0.0011(10) 0.0042(9) C3 0.0446(14) 0.0255(11) 0.0451(15) 0.0077(10) -0.0083(12) 0.0085(11) C4 0.0455(14) 0.0333(13) 0.0337(13) 0.0120(10) -0.0059(11) -0.0063(11) C5 0.0427(14) 0.0395(13) 0.0280(12) 0.0051(10) 0.0057(11) -0.0053(11) C6 0.0319(12) 0.0286(11) 0.0314(12) 0.0030(9) 0.0050(10) 0.0045(9) C7 0.0177(10) 0.0207(10) 0.0245(11) -0.0030(8) 0.0030(8) 0.0034(8) C8 0.0223(10) 0.0258(11) 0.0261(11) 0.0009(8) 0.0022(9) 0.0042(9) C9 0.0236(11) 0.0217(11) 0.0410(14) 0.0034(9) 0.0086(9) 0.0039(9) C10 0.0290(12) 0.0244(11) 0.0480(15) -0.0085(10) 0.0061(11) -0.0050(9) C11 0.0337(12) 0.0376(13) 0.0315(13) -0.0096(10) -0.0017(10) -0.0053(10) C12 0.0275(11) 0.0289(11) 0.0255(11) 0.0003(9) 0.0025(9) -0.0006(9) C13 0.0187(10) 0.0242(10) 0.0198(10) 0.0020(8) 0.0028(8) 0.0022(8) C14 0.0237(11) 0.0243(10) 0.0255(11) -0.0010(9) 0.0022(9) 0.0031(9) C15 0.0314(12) 0.0253(11) 0.0327(13) 0.0044(9) 0.0035(10) 0.0101(9) C16 0.0191(11) 0.0353(12) 0.0375(13) 0.0087(10) 0.0013(9) 0.0046(9) C17 0.0231(11) 0.0288(12) 0.0544(16) 0.0023(11) 0.0001(11) -0.0047(10) C18 0.0239(12) 0.0204(11) 0.0480(15) 0.0022(10) 0.0024(10) 0.0011(9) C19 0.0187(10) 0.0272(11) 0.0205(10) -0.0028(8) -0.0021(8) -0.0042(8) C20 0.0397(14) 0.0307(12) 0.0498(15) -0.0034(11) 0.0216(12) 0.0045(11) C21 0.0298(12) 0.0399(13) 0.0330(13) -0.0039(10) 0.0073(10) 0.0024(10) C22 0.0250(11) 0.0248(10) 0.0179(10) 0.0005(8) 0.0003(8) -0.0047(9) C23 0.0410(14) 0.0275(13) 0.0605(18) -0.0111(12) 0.0012(12) -0.0055(11) C24 0.0336(12) 0.0256(11) 0.0395(14) -0.0088(10) 0.0007(11) 0.0009(10) N1 0.0197(8) 0.0226(9) 0.0214(9) -0.0033(7) 0.0019(7) 0.0001(7) N2 0.0234(9) 0.0198(8) 0.0216(9) -0.0012(7) 0.0016(7) -0.0012(7) _geom_special_details ; ; 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 Ag S1 2.4669(6) . ? Ag S3 2.5165(6) . ? Ag P 2.3972(6) . ? Ag H1A 2.09(2) . ? S1 C19 1.691(2) . ? S2 C19 1.753(2) . ? S2 C21 1.799(2) . ? S3 C22 1.688(2) . ? S4 C22 1.759(2) . ? S4 C23 1.813(3) . ? P C1 1.818(2) . ? P C7 1.818(2) . ? P C13 1.823(2) . ? B H1A 1.15(2) . ? B H1B 1.09(2) . ? B N1 1.564(3) . ? B N2 1.571(3) . ? C1 C2 1.387(3) . ? C1 C6 1.390(3) . ? C2 H2 0.950 . ? C2 C3 1.387(3) . ? C3 H3 0.950 . ? C3 C4 1.379(4) . ? C4 H4 0.950 . ? C4 C5 1.376(3) . ? C5 H5 0.950 . ? C5 C6 1.385(3) . ? C6 H6 0.950 . ? C7 C8 1.399(3) . ? C7 C12 1.385(3) . ? C8 H8 0.950 . ? C8 C9 1.380(3) . ? C9 H9 0.950 . ? C9 C10 1.380(3) . ? C10 H10 0.950 . ? C10 C11 1.380(3) . ? C11 H11 0.950 . ? C11 C12 1.390(3) . ? C12 H12 0.950 . ? C13 C14 1.389(3) . ? C13 C18 1.393(3) . ? C14 H14 0.950 . ? C14 C15 1.383(3) . ? C15 H15 0.950 . ? C15 C16 1.379(3) . ? C16 H16 0.950 . ? C16 C17 1.385(3) . ? C17 H17 0.950 . ? C17 C18 1.381(3) . ? C18 H18 0.950 . ? C19 N1 1.316(3) . ? C20 H20A 0.990 . ? C20 H20B 0.990 . ? C20 C21 1.496(3) . ? C20 N1 1.483(3) . ? C21 H21A 0.990 . ? C21 H21B 0.990 . ? C22 N2 1.315(3) . ? C23 H23A 0.990 . ? C23 H23B 0.990 . ? C23 C24 1.501(3) . ? C24 H24A 0.990 . ? C24 H24B 0.990 . ? C24 N2 1.482(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S1 Ag S3 114.08(2) . . ? S1 Ag P 127.78(2) . . ? S1 Ag H1A 85.6(6) . . ? S3 Ag P 113.01(2) . . ? S3 Ag H1A 83.3(6) . . ? P Ag H1A 121.2(6) . . ? Ag S1 C19 106.22(7) . . ? C19 S2 C21 91.70(10) . . ? Ag S3 C22 106.74(7) . . ? C22 S4 C23 91.38(11) . . ? Ag P C1 115.35(7) . . ? Ag P C7 116.67(7) . . ? Ag P C13 109.24(7) . . ? C1 P C7 105.24(9) . . ? C1 P C13 104.08(9) . . ? C7 P C13 105.08(9) . . ? H1A B H1B 109.5(16) . . ? H1A B N1 111.0(12) . . ? H1A B N2 110.4(11) . . ? H1B B N1 107.0(12) . . ? H1B B N2 106.4(11) . . ? N1 B N2 112.28(17) . . ? P C1 C2 118.58(16) . . ? P C1 C6 122.38(15) . . ? C2 C1 C6 119.03(19) . . ? C1 C2 H2 119.8 . . ? C1 C2 C3 120.3(2) . . ? H2 C2 C3 119.8 . . ? C2 C3 H3 119.9 . . ? C2 C3 C4 120.3(2) . . ? H3 C3 C4 119.9 . . ? C3 C4 H4 120.2 . . ? C3 C4 C5 119.7(2) . . ? H4 C4 C5 120.2 . . ? C4 C5 H5 119.8 . . ? C4 C5 C6 120.5(2) . . ? H5 C5 C6 119.8 . . ? C1 C6 C5 120.2(2) . . ? C1 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? P C7 C8 116.76(16) . . ? P C7 C12 123.95(16) . . ? C8 C7 C12 119.19(19) . . ? C7 C8 H8 119.9 . . ? C7 C8 C9 120.2(2) . . ? H8 C8 C9 119.9 . . ? C8 C9 H9 119.8 . . ? C8 C9 C10 120.4(2) . . ? H9 C9 C10 119.8 . . ? C9 C10 H10 120.1 . . ? C9 C10 C11 119.9(2) . . ? H10 C10 C11 120.1 . . ? C10 C11 H11 119.9 . . ? C10 C11 C12 120.3(2) . . ? H11 C11 C12 119.9 . . ? C7 C12 C11 120.1(2) . . ? C7 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? P C13 C14 124.03(16) . . ? P C13 C18 116.47(15) . . ? C14 C13 C18 119.19(19) . . ? C13 C14 H14 120.1 . . ? C13 C14 C15 119.8(2) . . ? H14 C14 C15 120.1 . . ? C14 C15 H15 119.5 . . ? C14 C15 C16 120.9(2) . . ? H15 C15 C16 119.5 . . ? C15 C16 H16 120.2 . . ? C15 C16 C17 119.5(2) . . ? H16 C16 C17 120.2 . . ? C16 C17 H17 120.0 . . ? C16 C17 C18 120.1(2) . . ? H17 C17 C18 120.0 . . ? C13 C18 C17 120.5(2) . . ? C13 C18 H18 119.7 . . ? C17 C18 H18 119.7 . . ? S1 C19 S2 114.80(12) . . ? S1 C19 N1 131.09(16) . . ? S2 C19 N1 114.10(15) . . ? H20A C20 H20B 108.2 . . ? H20A C20 C21 109.8 . . ? H20A C20 N1 109.8 . . ? H20B C20 C21 109.8 . . ? H20B C20 N1 109.8 . . ? C21 C20 N1 109.58(18) . . ? S2 C21 C20 104.78(15) . . ? S2 C21 H21A 110.8 . . ? S2 C21 H21B 110.8 . . ? C20 C21 H21A 110.8 . . ? C20 C21 H21B 110.8 . . ? H21A C21 H21B 108.9 . . ? S3 C22 S4 115.42(12) . . ? S3 C22 N2 130.77(16) . . ? S4 C22 N2 113.80(15) . . ? S4 C23 H23A 111.0 . . ? S4 C23 H23B 111.0 . . ? S4 C23 C24 103.99(16) . . ? H23A C23 H23B 109.0 . . ? H23A C23 C24 111.0 . . ? H23B C23 C24 111.0 . . ? C23 C24 H24A 109.9 . . ? C23 C24 H24B 109.9 . . ? C23 C24 N2 109.06(19) . . ? H24A C24 H24B 108.3 . . ? H24A C24 N2 109.9 . . ? H24B C24 N2 109.9 . . ? B N1 C19 130.49(17) . . ? B N1 C20 116.82(17) . . ? C19 N1 C20 112.68(17) . . ? B N2 C22 129.75(17) . . ? B N2 C24 117.31(16) . . ? C22 N2 C24 112.93(17) . . ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 0.309 _refine_diff_density_min -0.357 _refine_diff_density_rms 0.050 #===END data_ab79_compound4 _database_code_depnum_ccdc_archive 'CCDC 693772' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H25 B Cu N2 P S4' _chemical_formula_sum 'C24 H25 B Cu N2 P S4' _chemical_formula_weight 575.02 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' B B 0.0013 0.0007 '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' 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 8.9121(15) _cell_length_b 15.3215(9) _cell_length_c 37.188(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5077.9(13) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6530 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.504 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2368 _exptl_absorpt_coefficient_mu 1.269 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.630 _exptl_absorpt_correction_T_max 0.702 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD diffractometer' _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 35586 _diffrn_reflns_av_R_equivalents 0.0444 _diffrn_reflns_av_sigmaI/netI 0.0286 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_theta_min 5.73 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4393 _reflns_number_gt 3637 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement EvalCCD _computing_data_reduction EvalCCD _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _refine_special_details ; ; _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^)+(0.0346P)^2^+4.2155P] 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 SHELXL _refine_ls_extinction_coef 0.0016(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4393 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0408 _refine_ls_R_factor_gt 0.0283 _refine_ls_wR_factor_ref 0.0747 _refine_ls_wR_factor_gt 0.0674 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _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 Cu Cu 0.07178(3) 0.259044(18) 0.146953(7) 0.02403(11) Uani 1 1 d . . . S1 S -0.06655(7) 0.33317(4) 0.188168(17) 0.02888(16) Uani 1 1 d . . . S2 S -0.30990(7) 0.28968(4) 0.238118(16) 0.03038(17) Uani 1 1 d . . . S3 S 0.25003(7) 0.16413(4) 0.167858(18) 0.03227(17) Uani 1 1 d . . . S4 S 0.25295(7) -0.01347(4) 0.197602(17) 0.03249(17) Uani 1 1 d . . . P P 0.13988(6) 0.31975(4) 0.094986(15) 0.01974(15) Uani 1 1 d . . . B B -0.1188(3) 0.12411(17) 0.16398(7) 0.0215(5) Uani 1 1 d . . . H1A H -0.068(2) 0.1696(15) 0.1418(6) 0.024(6) Uiso 1 1 d . . . H1B H -0.201(3) 0.0808(16) 0.1507(6) 0.035(7) Uiso 1 1 d . . . C1 C 0.1293(2) 0.24941(14) 0.05550(6) 0.0216(5) Uani 1 1 d . . . C2 C 0.0329(3) 0.17855(15) 0.05595(7) 0.0299(6) Uani 1 1 d . . . H2 H -0.0244 0.1666 0.0769 0.036 Uiso 1 1 calc R . . C3 C 0.0191(3) 0.12468(17) 0.02610(7) 0.0368(6) Uani 1 1 d . . . H3 H -0.0472 0.0761 0.0267 0.044 Uiso 1 1 calc R . . C4 C 0.1017(3) 0.14177(17) -0.00439(7) 0.0363(6) Uani 1 1 d . . . H4 H 0.0919 0.1052 -0.0249 0.044 Uiso 1 1 calc R . . C5 C 0.1984(3) 0.21187(18) -0.00520(7) 0.0367(6) Uani 1 1 d . . . H5 H 0.2553 0.2234 -0.0263 0.044 Uiso 1 1 calc R . . C6 C 0.2131(3) 0.26544(16) 0.02447(7) 0.0309(6) Uani 1 1 d . . . H6 H 0.2806 0.3134 0.0238 0.037 Uiso 1 1 calc R . . C7 C 0.3375(2) 0.35210(14) 0.09626(6) 0.0207(5) Uani 1 1 d . . . C8 C 0.4413(3) 0.28623(16) 0.10342(7) 0.0288(6) Uani 1 1 d . . . H8 H 0.4090 0.2272 0.1047 0.035 Uiso 1 1 calc R . . C9 C 0.5911(3) 0.30635(17) 0.10868(7) 0.0327(6) Uani 1 1 d . . . H9 H 0.6610 0.2611 0.1136 0.039 Uiso 1 1 calc R . . C10 C 0.6395(3) 0.39189(17) 0.10681(6) 0.0308(6) Uani 1 1 d . . . H10 H 0.7420 0.4057 0.1108 0.037 Uiso 1 1 calc R . . C11 C 0.5377(3) 0.45693(16) 0.09907(6) 0.0282(5) Uani 1 1 d . . . H11 H 0.5712 0.5157 0.0974 0.034 Uiso 1 1 calc R . . C12 C 0.3870(3) 0.43793(15) 0.09374(6) 0.0244(5) Uani 1 1 d . . . H12 H 0.3180 0.4834 0.0884 0.029 Uiso 1 1 calc R . . C13 C 0.0414(2) 0.41892(14) 0.08185(6) 0.0216(5) Uani 1 1 d . . . C14 C -0.0232(3) 0.43229(16) 0.04826(6) 0.0271(5) Uani 1 1 d . . . H14 H -0.0144 0.3888 0.0302 0.033 Uiso 1 1 calc R . . C15 C -0.1004(3) 0.50888(17) 0.04104(7) 0.0346(6) Uani 1 1 d . . . H15 H -0.1457 0.5172 0.0182 0.042 Uiso 1 1 calc R . . C16 C -0.1118(3) 0.57292(17) 0.06684(7) 0.0353(6) Uani 1 1 d . . . H16 H -0.1632 0.6257 0.0616 0.042 Uiso 1 1 calc R . . C17 C -0.0486(3) 0.56060(15) 0.10035(7) 0.0299(6) Uani 1 1 d . . . H17 H -0.0566 0.6049 0.1181 0.036 Uiso 1 1 calc R . . C18 C 0.0263(3) 0.48377(15) 0.10804(6) 0.0253(5) Uani 1 1 d . . . H18 H 0.0677 0.4750 0.1313 0.030 Uiso 1 1 calc R . . C19 C -0.1885(2) 0.25728(15) 0.20363(6) 0.0216(5) Uani 1 1 d . . . C20 C -0.3172(3) 0.12725(18) 0.21517(9) 0.0475(8) Uani 1 1 d . . . H20A H -0.2659 0.0881 0.2324 0.057 Uiso 1 1 calc R . . H20B H -0.3797 0.0909 0.1990 0.057 Uiso 1 1 calc R . . C21 C -0.4146(3) 0.18963(17) 0.23512(7) 0.0336(6) Uani 1 1 d . . . H21A H -0.4377 0.1669 0.2594 0.040 Uiso 1 1 calc R . . H21B H -0.5100 0.1991 0.2221 0.040 Uiso 1 1 calc R . . C22 C 0.1513(3) 0.07570(15) 0.18050(6) 0.0233(5) Uani 1 1 d . . . C23 C 0.0884(3) -0.08295(17) 0.19553(8) 0.0403(7) Uani 1 1 d . . . H23A H 0.0871 -0.1172 0.1730 0.048 Uiso 1 1 calc R . . H23B H 0.0857 -0.1237 0.2162 0.048 Uiso 1 1 calc R . . C24 C -0.0419(3) -0.02019(16) 0.19689(7) 0.0312(6) Uani 1 1 d . . . H24A H -0.1289 -0.0450 0.1839 0.037 Uiso 1 1 calc R . . H24B H -0.0718 -0.0098 0.2222 0.037 Uiso 1 1 calc R . . N1 N -0.2042(2) 0.17525(12) 0.19370(5) 0.0216(4) Uani 1 1 d . . . N3 N 0.0052(2) 0.06306(12) 0.17988(5) 0.0222(4) 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 Cu 0.02246(17) 0.02550(18) 0.02412(17) 0.00399(12) 0.00229(11) -0.00121(12) S1 0.0310(3) 0.0227(3) 0.0330(3) -0.0017(3) 0.0070(3) -0.0035(3) S2 0.0297(3) 0.0310(4) 0.0305(3) -0.0029(3) 0.0077(3) 0.0028(3) S3 0.0206(3) 0.0336(4) 0.0426(4) 0.0101(3) -0.0022(3) -0.0001(3) S4 0.0304(3) 0.0335(4) 0.0336(3) 0.0074(3) -0.0003(3) 0.0107(3) P 0.0184(3) 0.0186(3) 0.0223(3) 0.0009(2) 0.0013(2) -0.0021(2) B 0.0194(12) 0.0230(14) 0.0221(13) -0.0012(11) -0.0021(11) 0.0006(11) C1 0.0207(11) 0.0205(12) 0.0238(12) 0.0000(9) 0.0003(10) 0.0012(9) C2 0.0327(14) 0.0273(13) 0.0297(13) -0.0002(11) 0.0002(11) -0.0057(11) C3 0.0445(16) 0.0271(14) 0.0390(15) -0.0053(12) -0.0043(13) -0.0092(12) C4 0.0444(16) 0.0311(15) 0.0333(14) -0.0106(12) -0.0046(12) 0.0044(12) C5 0.0402(15) 0.0411(16) 0.0288(14) -0.0056(12) 0.0086(12) 0.0038(13) C6 0.0276(13) 0.0311(14) 0.0340(14) -0.0028(11) 0.0053(11) -0.0036(11) C7 0.0182(11) 0.0238(12) 0.0200(11) -0.0016(9) 0.0024(9) -0.0019(9) C8 0.0228(12) 0.0223(13) 0.0413(15) 0.0013(11) 0.0024(11) -0.0012(10) C9 0.0224(12) 0.0333(15) 0.0423(15) 0.0035(12) 0.0021(11) 0.0053(11) C10 0.0199(12) 0.0392(15) 0.0333(14) -0.0031(11) 0.0015(10) -0.0080(11) C11 0.0289(13) 0.0256(13) 0.0301(13) -0.0030(11) 0.0034(10) -0.0082(11) C12 0.0236(12) 0.0230(12) 0.0266(12) 0.0009(10) 0.0015(10) -0.0013(10) C13 0.0176(11) 0.0220(12) 0.0250(12) 0.0026(10) 0.0027(9) -0.0026(9) C14 0.0260(12) 0.0295(13) 0.0260(13) -0.0011(10) 0.0030(10) 0.0011(10) C15 0.0334(14) 0.0402(16) 0.0301(14) 0.0102(12) 0.0001(11) 0.0074(12) C16 0.0293(13) 0.0269(14) 0.0496(17) 0.0099(12) 0.0072(12) 0.0063(11) C17 0.0255(12) 0.0210(13) 0.0433(15) -0.0019(11) 0.0091(11) -0.0027(10) C18 0.0217(12) 0.0270(13) 0.0272(13) -0.0009(10) 0.0031(10) -0.0053(10) C19 0.0204(11) 0.0253(13) 0.0190(11) 0.0038(9) -0.0025(9) 0.0040(10) C20 0.0455(16) 0.0325(16) 0.0646(19) -0.0031(14) 0.0309(15) -0.0071(13) C21 0.0309(14) 0.0373(15) 0.0325(14) 0.0014(11) 0.0080(11) -0.0036(12) C22 0.0248(12) 0.0278(13) 0.0173(11) -0.0011(10) 0.0008(9) 0.0040(10) C23 0.0436(16) 0.0272(15) 0.0502(17) 0.0086(12) 0.0007(13) 0.0052(12) C24 0.0345(14) 0.0250(13) 0.0342(14) 0.0061(11) -0.0009(11) -0.0013(11) N1 0.0198(9) 0.0228(11) 0.0221(10) 0.0031(8) 0.0009(8) -0.0003(8) N3 0.0231(10) 0.0203(10) 0.0232(10) 0.0006(8) 0.0008(8) 0.0001(8) _geom_special_details ; ; 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 Cu S1 2.2713(7) . ? Cu S3 2.2898(7) . ? Cu P 2.2289(7) . ? Cu H1A 1.86(2) . ? S1 C19 1.692(2) . ? S2 C19 1.750(2) . ? S2 C21 1.798(3) . ? S3 C22 1.683(2) . ? S4 C22 1.759(2) . ? S4 C23 1.813(3) . ? P C1 1.824(2) . ? P C7 1.830(2) . ? P C13 1.821(2) . ? B H1A 1.17(2) . ? B H1B 1.11(3) . ? B N1 1.554(3) . ? B N3 1.564(3) . ? C1 C2 1.384(3) . ? C1 C6 1.396(3) . ? C2 H2 0.950 . ? C2 C3 1.389(3) . ? C3 H3 0.950 . ? C3 C4 1.377(4) . ? C4 H4 0.950 . ? C4 C5 1.377(4) . ? C5 H5 0.950 . ? C5 C6 1.381(4) . ? C6 H6 0.950 . ? C7 C8 1.395(3) . ? C7 C12 1.390(3) . ? C8 H8 0.950 . ? C8 C9 1.384(3) . ? C9 H9 0.950 . ? C9 C10 1.381(4) . ? C10 H10 0.950 . ? C10 C11 1.378(4) . ? C11 H11 0.950 . ? C11 C12 1.389(3) . ? C12 H12 0.950 . ? C13 C14 1.391(3) . ? C13 C18 1.398(3) . ? C14 H14 0.950 . ? C14 C15 1.387(3) . ? C15 H15 0.950 . ? C15 C16 1.376(4) . ? C16 H16 0.950 . ? C16 C17 1.380(4) . ? C17 H17 0.950 . ? C17 C18 1.383(3) . ? C18 H18 0.950 . ? C19 N1 1.318(3) . ? C20 H20A 0.990 . ? C20 H20B 0.990 . ? C20 C21 1.489(4) . ? C20 N1 1.481(3) . ? C21 H21A 0.990 . ? C21 H21B 0.990 . ? C22 N3 1.317(3) . ? C23 H23A 0.990 . ? C23 H23B 0.990 . ? C23 C24 1.509(4) . ? C24 H24A 0.990 . ? C24 H24B 0.990 . ? C24 N3 1.484(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S1 Cu S3 117.71(3) . . ? S1 Cu P 121.62(3) . . ? S1 Cu H1A 94.3(7) . . ? S3 Cu P 111.75(3) . . ? S3 Cu H1A 91.8(7) . . ? P Cu H1A 113.6(7) . . ? Cu S1 C19 103.55(8) . . ? C19 S2 C21 91.92(11) . . ? Cu S3 C22 104.08(8) . . ? C22 S4 C23 91.38(11) . . ? Cu P C1 115.94(7) . . ? Cu P C7 110.64(7) . . ? Cu P C13 116.71(7) . . ? C1 P C7 103.34(10) . . ? C1 P C13 104.60(10) . . ? C7 P C13 104.16(10) . . ? H1A B H1B 107.5(17) . . ? H1A B N1 112.9(11) . . ? H1A B N3 110.4(11) . . ? H1B B N1 107.1(13) . . ? H1B B N3 106.2(13) . . ? N1 B N3 112.24(18) . . ? P C1 C2 119.06(17) . . ? P C1 C6 122.26(17) . . ? C2 C1 C6 118.7(2) . . ? C1 C2 H2 119.6 . . ? C1 C2 C3 120.8(2) . . ? H2 C2 C3 119.6 . . ? C2 C3 H3 120.1 . . ? C2 C3 C4 119.9(2) . . ? H3 C3 C4 120.1 . . ? C3 C4 H4 120.0 . . ? C3 C4 C5 120.1(2) . . ? H4 C4 C5 120.0 . . ? C4 C5 H5 119.8 . . ? C4 C5 C6 120.3(2) . . ? H5 C5 C6 119.8 . . ? C1 C6 C5 120.3(2) . . ? C1 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? P C7 C8 116.58(17) . . ? P C7 C12 124.05(17) . . ? C8 C7 C12 119.1(2) . . ? C7 C8 H8 119.8 . . ? C7 C8 C9 120.4(2) . . ? H8 C8 C9 119.8 . . ? C8 C9 H9 119.8 . . ? C8 C9 C10 120.3(2) . . ? H9 C9 C10 119.8 . . ? C9 C10 H10 120.3 . . ? C9 C10 C11 119.4(2) . . ? H10 C10 C11 120.3 . . ? C10 C11 H11 119.5 . . ? C10 C11 C12 121.0(2) . . ? H11 C11 C12 119.5 . . ? C7 C12 C11 119.7(2) . . ? C7 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? P C13 C14 124.28(18) . . ? P C13 C18 116.91(17) . . ? C14 C13 C18 118.8(2) . . ? C13 C14 H14 119.9 . . ? C13 C14 C15 120.3(2) . . ? H14 C14 C15 119.9 . . ? C14 C15 H15 119.8 . . ? C14 C15 C16 120.3(2) . . ? H15 C15 C16 119.8 . . ? C15 C16 H16 119.9 . . ? C15 C16 C17 120.1(2) . . ? H16 C16 C17 119.9 . . ? C16 C17 H17 120.0 . . ? C16 C17 C18 120.0(2) . . ? H17 C17 C18 120.0 . . ? C13 C18 C17 120.5(2) . . ? C13 C18 H18 119.8 . . ? C17 C18 H18 119.8 . . ? S1 C19 S2 116.83(13) . . ? S1 C19 N1 128.93(17) . . ? S2 C19 N1 114.23(16) . . ? H20A C20 H20B 108.1 . . ? H20A C20 C21 109.6 . . ? H20A C20 N1 109.6 . . ? H20B C20 C21 109.6 . . ? H20B C20 N1 109.6 . . ? C21 C20 N1 110.3(2) . . ? S2 C21 C20 106.02(17) . . ? S2 C21 H21A 110.5 . . ? S2 C21 H21B 110.5 . . ? C20 C21 H21A 110.5 . . ? C20 C21 H21B 110.5 . . ? H21A C21 H21B 108.7 . . ? S3 C22 S4 117.20(13) . . ? S3 C22 N3 129.12(18) . . ? S4 C22 N3 113.67(17) . . ? S4 C23 H23A 110.9 . . ? S4 C23 H23B 110.9 . . ? S4 C23 C24 104.28(17) . . ? H23A C23 H23B 108.9 . . ? H23A C23 C24 110.9 . . ? H23B C23 C24 110.9 . . ? C23 C24 H24A 110.0 . . ? C23 C24 H24B 110.0 . . ? C23 C24 N3 108.4(2) . . ? H24A C24 H24B 108.4 . . ? H24A C24 N3 110.0 . . ? H24B C24 N3 110.0 . . ? B N1 C19 128.93(19) . . ? B N1 C20 117.79(19) . . ? C19 N1 C20 113.26(19) . . ? B N3 C22 128.12(19) . . ? B N3 C24 118.41(18) . . ? C22 N3 C24 113.48(19) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.304 _refine_diff_density_min -0.316 _refine_diff_density_rms 0.057 #===END