Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_global _database_code_CSD 171721 _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Frost, Christopher G.' 'Hague, Catherine' 'Mahon, M.' 'Patmore, Nathan J.' 'Weller, Andrew' _publ_contact_author_name 'Dr Andrew Weller' _publ_contact_author_address ; Dr Andrew Weller Chemistry University of Bath Claverton Down Bath BA2 7AY UNITED KINGDOM ; _publ_contact_author_email 'A.S.WELLER@BATH.AC.UK' _publ_section_title ; [(PPh3)Ag(CB11H6Y6)] (Y = H, Br): Highly Active, Selective and Recyclable Lewis Acids for a Hetero-Diels Alder Reaction. ; _database_code_CSD 168828 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Complex_(1) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H21 Ag B11 Br6 P' _chemical_formula_weight 986.57 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' 'P' 'P' 0.1023 0.0942 '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' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.89500(10) _cell_length_b 24.4140(4) _cell_length_c 14.4170(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.0720(10) _cell_angle_gamma 90.00 _cell_volume 3061.60(9) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12 _cell_measurement_theta_max 18 _exptl_crystal_description Tabloid _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.140 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1848 _exptl_absorpt_coefficient_mu 8.554 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.47 _exptl_absorpt_correction_T_max 0.66 _exptl_absorpt_process_details ? _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 KappaCCD _diffrn_measurement_method KappaCCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23164 _diffrn_reflns_av_R_equivalents 0.0519 _diffrn_reflns_av_sigmaI/netI 0.0534 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.71 _diffrn_reflns_theta_max 27.88 _reflns_number_total 7253 _reflns_number_gt 5880 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction 'Denzo and Scalepack (otwinowski & Minor, 1997' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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 [1.00000+0.00000exp(0.00(sin\q/\l)^2^)]/ [\s^2^(Fo^2^)+0.0000+3.9648*P+(0.0315P)^2^+0.0000sin\q/\l] where P = 0.00000Fo^2^ + 1.00000Fc^2^ ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7253 _refine_ls_number_parameters 349 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0521 _refine_ls_R_factor_gt 0.0358 _refine_ls_wR_factor_ref 0.0855 _refine_ls_wR_factor_gt 0.0783 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _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 Ag1 Ag 0.25058(4) 0.106027(14) 0.61893(2) 0.03305(10) Uani 1 1 d . . . P1 P 0.26550(11) 0.05366(4) 0.76172(7) 0.0203(2) Uani 1 1 d . . . Br7 Br 0.41773(5) 0.065959(15) 0.48275(3) 0.02495(10) Uani 1 1 d . . . Br8 Br 0.20269(4) 0.196586(16) 0.50967(3) 0.02638(10) Uani 1 1 d . . . Br9 Br 0.49275(5) 0.311739(16) 0.59636(3) 0.03111(11) Uani 1 1 d . . . Br10 Br 0.89784(5) 0.244693(16) 0.63940(3) 0.02646(10) Uani 1 1 d . . . Br11 Br 0.85072(5) 0.094405(16) 0.56362(3) 0.02943(11) Uani 1 1 d . . . Br12 Br 0.56611(5) 0.161458(15) 0.69193(3) 0.02412(10) Uani 1 1 d . . . B2 B 0.6220(5) 0.14813(19) 0.3794(3) 0.0258(10) Uani 1 1 d . . . H2 H 0.6484 0.1147 0.3320 0.031 Uiso 1 1 calc R . . B3 B 0.4342(5) 0.17800(19) 0.3632(3) 0.0237(9) Uani 1 1 d . . . H3 H 0.3376 0.1640 0.3052 0.028 Uiso 1 1 calc R . . B4 B 0.4553(5) 0.24814(19) 0.3970(3) 0.0237(9) Uani 1 1 d . . . H4 H 0.3725 0.2799 0.3609 0.028 Uiso 1 1 calc R . . B5 B 0.6570(5) 0.26196(18) 0.4353(3) 0.0226(9) Uani 1 1 d . . . H5 H 0.7066 0.3030 0.4242 0.027 Uiso 1 1 calc R . . B6 B 0.7589(5) 0.20025(18) 0.4239(3) 0.0232(9) Uani 1 1 d . . . H6 H 0.8751 0.2010 0.4054 0.028 Uiso 1 1 calc R . . B7 B 0.5068(5) 0.13770(18) 0.4646(3) 0.0209(9) Uani 1 1 d . . . B8 B 0.4071(5) 0.19907(18) 0.4761(3) 0.0201(9) Uani 1 1 d . . . B9 B 0.5422(5) 0.25136(17) 0.5207(3) 0.0196(9) Uani 1 1 d . . . B10 B 0.7290(5) 0.22133(17) 0.5371(3) 0.0212(9) Uani 1 1 d . . . B11 B 0.7081(5) 0.15076(18) 0.5019(3) 0.0212(9) Uani 1 1 d . . . B12 B 0.5750(5) 0.18231(16) 0.5632(3) 0.0168(8) Uani 1 1 d . . . C1 C 0.5891(4) 0.21541(16) 0.3480(3) 0.0226(8) Uani 1 1 d . . . H1 H 0.5946 0.2270 0.2736 0.027 Uiso 1 1 calc R . . C2 C 0.4690(4) 0.04187(16) 0.8106(3) 0.0226(8) Uani 1 1 d . . . C3 C 0.5452(5) 0.00407(19) 0.7634(3) 0.0343(10) Uani 1 1 d . . . H3A H 0.4882 -0.0179 0.7138 0.041 Uiso 1 1 calc R . . C4 C 0.7021(5) -0.0012(2) 0.7886(4) 0.0428(12) Uani 1 1 d . . . H4A H 0.7534 -0.0269 0.7565 0.051 Uiso 1 1 calc R . . C5 C 0.7866(5) 0.0309(2) 0.8612(3) 0.0388(11) Uani 1 1 d . . . H5A H 0.8952 0.0274 0.8785 0.047 Uiso 1 1 calc R . . C6 C 0.7115(5) 0.06766(19) 0.9074(3) 0.0332(10) Uani 1 1 d . . . H6A H 0.7692 0.0894 0.9569 0.040 Uiso 1 1 calc R . . C7 C 0.5540(5) 0.07368(17) 0.8834(3) 0.0277(9) Uani 1 1 d . . . H7 H 0.5038 0.0993 0.9161 0.033 Uiso 1 1 calc R . . C8 C 0.1790(4) -0.01436(15) 0.7536(3) 0.0221(8) Uani 1 1 d . . . C9 C 0.2180(5) -0.05242(17) 0.8269(3) 0.0297(9) Uani 1 1 d . . . H9 H 0.2945 -0.0437 0.8814 0.036 Uiso 1 1 calc R . . C10 C 0.1453(5) -0.10284(17) 0.8201(3) 0.0329(10) Uani 1 1 d . . . H10 H 0.1726 -0.1287 0.8700 0.039 Uiso 1 1 calc R . . C11 C 0.0333(5) -0.11582(18) 0.7413(3) 0.0319(10) Uani 1 1 d . . . H11 H -0.0182 -0.1501 0.7378 0.038 Uiso 1 1 calc R . . C12 C -0.0035(5) -0.07871(18) 0.6677(3) 0.0363(11) Uani 1 1 d . . . H12 H -0.0789 -0.0878 0.6129 0.044 Uiso 1 1 calc R . . C13 C 0.0694(5) -0.02804(17) 0.6736(3) 0.0305(9) Uani 1 1 d . . . H13 H 0.0440 -0.0027 0.6227 0.037 Uiso 1 1 calc R . . C14 C 0.1897(4) 0.09046(16) 0.8512(3) 0.0230(8) Uani 1 1 d . . . C15 C 0.1038(5) 0.13731(17) 0.8234(3) 0.0286(9) Uani 1 1 d . . . H15 H 0.0876 0.1492 0.7593 0.034 Uiso 1 1 calc R . . C16 C 0.0411(5) 0.16712(19) 0.8885(4) 0.0376(11) Uani 1 1 d . . . H16 H -0.0183 0.1990 0.8688 0.045 Uiso 1 1 calc R . . C17 C 0.0655(5) 0.15034(19) 0.9808(3) 0.0375(11) Uani 1 1 d . . . H17 H 0.0245 0.1711 1.0254 0.045 Uiso 1 1 calc R . . C18 C 0.1491(6) 0.10338(19) 1.0101(3) 0.0370(11) Uani 1 1 d . . . H18 H 0.1642 0.0918 1.0743 0.044 Uiso 1 1 calc R . . C19 C 0.2108(5) 0.07321(17) 0.9458(3) 0.0290(9) Uani 1 1 d . . . H19 H 0.2674 0.0408 0.9658 0.035 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 0.0398(2) 0.03388(18) 0.02656(18) 0.00838(13) 0.00950(15) -0.00383(15) P1 0.0215(5) 0.0195(5) 0.0198(5) -0.0001(4) 0.0046(4) -0.0004(4) Br7 0.0284(2) 0.01901(19) 0.0275(2) -0.00180(14) 0.00612(17) -0.00275(15) Br8 0.01807(19) 0.0271(2) 0.0350(2) 0.00690(16) 0.00802(17) 0.00264(15) Br9 0.0384(2) 0.0252(2) 0.0304(2) -0.00111(16) 0.00851(19) 0.00555(18) Br10 0.0240(2) 0.0256(2) 0.0270(2) 0.00075(15) -0.00119(16) -0.00360(16) Br11 0.0250(2) 0.0254(2) 0.0363(2) 0.00442(16) 0.00289(17) 0.00803(16) Br12 0.0311(2) 0.0250(2) 0.01627(19) 0.00159(14) 0.00487(15) -0.00429(16) B2 0.028(2) 0.027(2) 0.023(2) -0.0008(18) 0.0079(19) 0.0008(19) B3 0.021(2) 0.029(2) 0.020(2) 0.0057(18) 0.0014(18) -0.0016(19) B4 0.022(2) 0.027(2) 0.022(2) 0.0087(18) 0.0045(18) 0.0009(18) B5 0.022(2) 0.024(2) 0.023(2) 0.0041(17) 0.0064(18) -0.0003(18) B6 0.021(2) 0.027(2) 0.021(2) 0.0033(17) 0.0038(18) 0.0020(18) B7 0.019(2) 0.022(2) 0.022(2) 0.0003(17) 0.0042(17) -0.0015(17) B8 0.018(2) 0.022(2) 0.021(2) 0.0036(16) 0.0047(17) 0.0028(17) B9 0.019(2) 0.018(2) 0.021(2) 0.0014(16) 0.0032(17) 0.0019(17) B10 0.022(2) 0.019(2) 0.022(2) 0.0018(17) 0.0036(17) 0.0015(18) B11 0.022(2) 0.022(2) 0.019(2) 0.0033(16) 0.0036(17) 0.0027(18) B12 0.016(2) 0.0177(19) 0.016(2) 0.0002(15) 0.0018(16) 0.0005(16) C1 0.024(2) 0.026(2) 0.0175(19) 0.0054(15) 0.0047(15) -0.0030(16) C2 0.0222(19) 0.0224(19) 0.024(2) 0.0035(15) 0.0059(16) -0.0049(16) C3 0.028(2) 0.041(3) 0.034(2) -0.008(2) 0.0086(19) 0.003(2) C4 0.034(3) 0.050(3) 0.048(3) -0.002(2) 0.016(2) 0.010(2) C5 0.018(2) 0.053(3) 0.043(3) 0.012(2) 0.0018(19) -0.002(2) C6 0.029(2) 0.040(3) 0.028(2) 0.0047(19) -0.0006(18) -0.012(2) C7 0.029(2) 0.027(2) 0.027(2) 0.0022(17) 0.0056(18) -0.0047(18) C8 0.0193(19) 0.0230(19) 0.025(2) -0.0046(15) 0.0057(15) -0.0009(16) C9 0.039(2) 0.028(2) 0.022(2) 0.0003(17) 0.0046(18) -0.0052(19) C10 0.046(3) 0.023(2) 0.033(2) 0.0031(17) 0.015(2) -0.0011(19) C11 0.028(2) 0.025(2) 0.045(3) -0.0093(19) 0.014(2) -0.0065(18) C12 0.025(2) 0.031(2) 0.047(3) -0.012(2) -0.0064(19) 0.0018(19) C13 0.030(2) 0.025(2) 0.032(2) -0.0016(17) -0.0025(18) 0.0034(18) C14 0.020(2) 0.0226(19) 0.027(2) -0.0011(15) 0.0066(16) -0.0004(16) C15 0.029(2) 0.025(2) 0.032(2) -0.0008(17) 0.0072(18) -0.0025(18) C16 0.032(2) 0.031(2) 0.052(3) -0.006(2) 0.013(2) 0.002(2) C17 0.035(3) 0.038(2) 0.044(3) -0.017(2) 0.020(2) -0.008(2) C18 0.041(3) 0.043(3) 0.030(2) -0.005(2) 0.014(2) -0.003(2) C19 0.031(2) 0.028(2) 0.028(2) 0.0005(17) 0.0077(18) -0.0008(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 P1 2.4032(10) . ? Ag1 Br8 2.6963(5) . ? Ag1 Br7 2.8710(5) . ? P1 C14 1.813(4) . ? P1 C2 1.823(4) . ? P1 C8 1.824(4) . ? Br7 B7 1.962(4) . ? Br8 B8 1.978(4) . ? Br9 B9 1.938(4) . ? Br10 B10 1.957(4) . ? Br11 B11 1.955(4) . ? Br12 B12 1.942(4) . ? B2 C1 1.713(6) . ? B2 B11 1.773(6) . ? B2 B7 1.775(6) . ? B2 B6 1.785(6) . ? B2 B3 1.793(6) . ? B3 C1 1.706(6) . ? B3 B7 1.767(6) . ? B3 B8 1.771(6) . ? B3 B4 1.780(7) . ? B4 C1 1.705(6) . ? B4 B8 1.767(6) . ? B4 B9 1.791(6) . ? B4 B5 1.795(6) . ? B5 C1 1.710(6) . ? B5 B10 1.776(6) . ? B5 B9 1.775(6) . ? B5 B6 1.784(6) . ? B6 C1 1.711(6) . ? B6 B11 1.772(6) . ? B6 B10 1.783(6) . ? B7 B8 1.766(6) . ? B7 B11 1.787(6) . ? B7 B12 1.793(6) . ? B8 B9 1.779(6) . ? B8 B12 1.785(6) . ? B9 B10 1.786(6) . ? B9 B12 1.796(6) . ? B10 B12 1.773(6) . ? B10 B11 1.795(6) . ? B11 B12 1.792(6) . ? C2 C7 1.394(6) . ? C2 C3 1.403(6) . ? C3 C4 1.373(6) . ? C4 C5 1.395(7) . ? C5 C6 1.371(7) . ? C6 C7 1.379(6) . ? C8 C13 1.387(6) . ? C8 C9 1.395(6) . ? C9 C10 1.385(6) . ? C10 C11 1.382(6) . ? C11 C12 1.381(7) . ? C12 C13 1.391(6) . ? C14 C15 1.388(6) . ? C14 C19 1.402(6) . ? C15 C16 1.393(6) . ? C16 C17 1.365(7) . ? C17 C18 1.384(7) . ? C18 C19 1.384(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Ag1 Br8 155.55(3) . . ? P1 Ag1 Br7 117.44(3) . . ? Br8 Ag1 Br7 85.471(14) . . ? C14 P1 C2 106.85(18) . . ? C14 P1 C8 106.38(17) . . ? C2 P1 C8 104.62(17) . . ? C14 P1 Ag1 112.56(13) . . ? C2 P1 Ag1 106.72(12) . . ? C8 P1 Ag1 118.86(13) . . ? B7 Br7 Ag1 93.92(13) . . ? B8 Br8 Ag1 97.30(12) . . ? C1 B2 B11 104.1(3) . . ? C1 B2 B7 103.2(3) . . ? B11 B2 B7 60.5(2) . . ? C1 B2 B6 58.5(2) . . ? B11 B2 B6 59.8(2) . . ? B7 B2 B6 107.6(3) . . ? C1 B2 B3 58.2(2) . . ? B11 B2 B3 108.1(3) . . ? B7 B2 B3 59.4(2) . . ? B6 B2 B3 107.7(3) . . ? C1 B3 B7 103.8(3) . . ? C1 B3 B8 103.4(3) . . ? B7 B3 B8 59.9(2) . . ? C1 B3 B4 58.5(2) . . ? B7 B3 B4 108.1(3) . . ? B8 B3 B4 59.7(2) . . ? C1 B3 B2 58.6(2) . . ? B7 B3 B2 59.8(2) . . ? B8 B3 B2 107.5(3) . . ? B4 B3 B2 108.3(3) . . ? C1 B4 B8 103.6(3) . . ? C1 B4 B3 58.6(2) . . ? B8 B4 B3 59.9(2) . . ? C1 B4 B9 103.9(3) . . ? B8 B4 B9 60.0(2) . . ? B3 B4 B9 108.3(3) . . ? C1 B4 B5 58.4(2) . . ? B8 B4 B5 106.9(3) . . ? B3 B4 B5 107.8(3) . . ? B9 B4 B5 59.3(2) . . ? C1 B5 B10 104.4(3) . . ? C1 B5 B9 104.4(3) . . ? B10 B5 B9 60.4(2) . . ? C1 B5 B6 58.6(2) . . ? B10 B5 B6 60.1(2) . . ? B9 B5 B6 108.5(3) . . ? C1 B5 B4 58.2(2) . . ? B10 B5 B4 108.3(3) . . ? B9 B5 B4 60.2(2) . . ? B6 B5 B4 107.9(3) . . ? C1 B6 B11 104.2(3) . . ? C1 B6 B10 104.0(3) . . ? B11 B6 B10 60.6(2) . . ? C1 B6 B5 58.5(2) . . ? B11 B6 B5 108.4(3) . . ? B10 B6 B5 59.7(2) . . ? C1 B6 B2 58.6(2) . . ? B11 B6 B2 59.8(2) . . ? B10 B6 B2 108.3(3) . . ? B5 B6 B2 108.3(3) . . ? B3 B7 B8 60.1(2) . . ? B3 B7 B2 60.8(3) . . ? B8 B7 B2 108.5(3) . . ? B3 B7 B11 108.6(3) . . ? B8 B7 B11 108.1(3) . . ? B2 B7 B11 59.7(2) . . ? B3 B7 B12 108.8(3) . . ? B8 B7 B12 60.2(2) . . ? B2 B7 B12 108.2(3) . . ? B11 B7 B12 60.1(2) . . ? B3 B7 Br7 121.3(3) . . ? B8 B7 Br7 121.3(3) . . ? B2 B7 Br7 121.9(3) . . ? B11 B7 Br7 121.7(3) . . ? B12 B7 Br7 121.0(3) . . ? B4 B8 B7 108.7(3) . . ? B4 B8 B3 60.4(2) . . ? B7 B8 B3 60.0(2) . . ? B4 B8 B9 60.7(2) . . ? B7 B8 B9 109.2(3) . . ? B3 B8 B9 109.2(3) . . ? B4 B8 B12 109.2(3) . . ? B7 B8 B12 60.6(2) . . ? B3 B8 B12 109.0(3) . . ? B9 B8 B12 60.5(2) . . ? B4 B8 Br8 122.5(3) . . ? B7 B8 Br8 120.2(3) . . ? B3 B8 Br8 121.6(3) . . ? B9 B8 Br8 121.3(3) . . ? B12 B8 Br8 119.8(3) . . ? B5 B9 B8 107.3(3) . . ? B5 B9 B10 59.8(2) . . ? B8 B9 B10 107.0(3) . . ? B5 B9 B4 60.4(2) . . ? B8 B9 B4 59.3(2) . . ? B10 B9 B4 108.0(3) . . ? B5 B9 B12 107.3(3) . . ? B8 B9 B12 59.9(2) . . ? B10 B9 B12 59.3(2) . . ? B4 B9 B12 107.6(3) . . ? B5 B9 Br9 120.7(3) . . ? B8 B9 Br9 122.2(3) . . ? B10 B9 Br9 123.5(3) . . ? B4 B9 Br9 119.5(3) . . ? B12 B9 Br9 124.2(3) . . ? B12 B10 B5 108.3(3) . . ? B12 B10 B6 108.0(3) . . ? B5 B10 B6 60.2(2) . . ? B12 B10 B9 60.6(2) . . ? B5 B10 B9 59.8(2) . . ? B6 B10 B9 108.1(3) . . ? B12 B10 B11 60.3(2) . . ? B5 B10 B11 107.7(3) . . ? B6 B10 B11 59.4(2) . . ? B9 B10 B11 108.6(3) . . ? B12 B10 Br10 120.2(3) . . ? B5 B10 Br10 123.2(3) . . ? B6 B10 Br10 122.4(3) . . ? B9 B10 Br10 121.7(3) . . ? B11 B10 Br10 120.7(3) . . ? B2 B11 B6 60.5(2) . . ? B2 B11 B7 59.8(2) . . ? B6 B11 B7 107.6(3) . . ? B2 B11 B12 108.3(3) . . ? B6 B11 B12 107.6(3) . . ? B7 B11 B12 60.1(2) . . ? B2 B11 B10 108.3(3) . . ? B6 B11 B10 60.0(2) . . ? B7 B11 B10 107.1(3) . . ? B12 B11 B10 59.2(2) . . ? B2 B11 Br11 122.1(3) . . ? B6 B11 Br11 122.7(3) . . ? B7 B11 Br11 121.7(3) . . ? B12 B11 Br11 120.7(3) . . ? B10 B11 Br11 121.9(3) . . ? B10 B12 B8 107.3(3) . . ? B10 B12 B7 107.9(3) . . ? B8 B12 B7 59.2(2) . . ? B10 B12 B11 60.5(2) . . ? B8 B12 B11 107.1(3) . . ? B7 B12 B11 59.8(2) . . ? B10 B12 B9 60.1(2) . . ? B8 B12 B9 59.6(2) . . ? B7 B12 B9 107.2(3) . . ? B11 B12 B9 108.2(3) . . ? B10 B12 Br12 122.1(3) . . ? B8 B12 Br12 122.5(3) . . ? B7 B12 Br12 121.6(3) . . ? B11 B12 Br12 121.4(3) . . ? B9 B12 Br12 122.4(3) . . ? B4 C1 B3 62.9(3) . . ? B4 C1 B6 115.8(3) . . ? B3 C1 B6 115.5(3) . . ? B4 C1 B5 63.4(3) . . ? B3 C1 B5 115.6(3) . . ? B6 C1 B5 62.9(3) . . ? B4 C1 B2 115.8(3) . . ? B3 C1 B2 63.3(3) . . ? B6 C1 B2 62.9(3) . . ? B5 C1 B2 115.4(3) . . ? C7 C2 C3 119.4(4) . . ? C7 C2 P1 122.8(3) . . ? C3 C2 P1 117.2(3) . . ? C4 C3 C2 120.0(4) . . ? C3 C4 C5 120.3(4) . . ? C6 C5 C4 119.5(4) . . ? C5 C6 C7 121.3(4) . . ? C6 C7 C2 119.5(4) . . ? C13 C8 C9 119.3(4) . . ? C13 C8 P1 119.1(3) . . ? C9 C8 P1 121.6(3) . . ? C10 C9 C8 120.0(4) . . ? C11 C10 C9 120.5(4) . . ? C12 C11 C10 119.7(4) . . ? C11 C12 C13 120.3(4) . . ? C8 C13 C12 120.2(4) . . ? C15 C14 C19 118.8(4) . . ? C15 C14 P1 117.8(3) . . ? C19 C14 P1 123.3(3) . . ? C14 C15 C16 120.6(4) . . ? C17 C16 C15 119.7(4) . . ? C16 C17 C18 120.8(4) . . ? C17 C18 C19 120.0(4) . . ? C18 C19 C14 120.0(4) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.081 _refine_diff_density_min -1.181 _refine_diff_density_rms 0.144 #===END data_k01asw3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Compound_(2) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H27 Ag B11 P' _chemical_formula_weight 513.16 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.282(2) _cell_length_b 10.988(2) _cell_length_c 11.308(2) _cell_angle_alpha 76.22(3) _cell_angle_beta 75.25(3) _cell_angle_gamma 75.61(3) _cell_volume 1175.7(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12 _cell_measurement_theta_max 18 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.450 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 516 _exptl_absorpt_coefficient_mu 0.932 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8355 _exptl_absorpt_correction_T_max 0.9126 _exptl_absorpt_process_details ? _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 KappaCCD _diffrn_measurement_method KappaCCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20702 _diffrn_reflns_av_R_equivalents 0.0387 _diffrn_reflns_av_sigmaI/netI 0.0389 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5374 _reflns_number_gt 4538 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction 'Denzo and Scalepack (otwinowski & Minor, 1997' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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^)+(0.0382P)^2^+0.6274P] 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 0.0094(9) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5374 _refine_ls_number_parameters 302 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0417 _refine_ls_R_factor_gt 0.0316 _refine_ls_wR_factor_ref 0.0813 _refine_ls_wR_factor_gt 0.0757 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.720007(17) 0.704344(19) 0.995120(16) 0.03930(9) Uani 1 1 d . . . P1 P 0.88805(5) 0.70947(5) 0.80838(5) 0.01947(12) Uani 1 1 d . . . B2 B 0.2780(2) 0.7632(3) 1.1521(2) 0.0302(5) Uani 1 1 d . . . H2 H 0.1945 0.7960 1.0978 0.036 Uiso 1 1 calc R . . B3 B 0.3852(3) 0.6073(3) 1.1559(2) 0.0294(5) Uani 1 1 d . . . H3 H 0.3730 0.5376 1.1036 0.035 Uiso 1 1 calc R . . B4 B 0.4297(3) 0.5567(3) 1.3054(2) 0.0314(6) Uani 1 1 d . . . H4 H 0.4461 0.4536 1.3520 0.038 Uiso 1 1 calc R . . B5 B 0.3517(3) 0.6807(3) 1.3887(2) 0.0319(6) Uani 1 1 d . . . H5 H 0.3158 0.6584 1.4922 0.038 Uiso 1 1 calc R . . B6 B 0.2582(3) 0.8067(3) 1.2968(3) 0.0325(6) Uani 1 1 d . . . H6 H 0.1609 0.8680 1.3386 0.039 Uiso 1 1 calc R . . B7 B 0.4540(2) 0.7456(2) 1.0794(2) 0.0275(5) Uani 1 1 d . . . H7 H 0.4884 0.7670 0.9757 0.033 Uiso 1 1 calc R . . B8 B 0.5481(2) 0.6175(2) 1.1754(2) 0.0270(5) Uani 1 1 d . . . H8 H 0.6448 0.5544 1.1351 0.032 Uiso 1 1 calc R . . B9 B 0.5265(3) 0.6634(3) 1.3210(2) 0.0314(6) Uani 1 1 d . . . H9 H 0.6083 0.6309 1.3773 0.038 Uiso 1 1 calc R . . B10 B 0.4198(3) 0.8188(3) 1.3158(3) 0.0352(6) Uani 1 1 d . . . H10 H 0.4307 0.8885 1.3688 0.042 Uiso 1 1 calc R . . B11 B 0.3754(2) 0.8699(2) 1.1665(3) 0.0319(6) Uani 1 1 d . . . H11 H 0.3579 0.9731 1.1206 0.038 Uiso 1 1 calc R . . B12 B 0.5420(2) 0.7800(2) 1.1816(2) 0.0276(5) Uani 1 1 d . . . H12 H 0.6350 0.8242 1.1451 0.033 Uiso 1 1 calc R . . C1 C 0.2716(2) 0.6502(2) 1.2863(2) 0.0345(5) Uani 1 1 d . . . H1 H 0.1786 0.6059 1.3222 0.041 Uiso 1 1 calc R . . C11 C 1.0284(2) 0.78360(18) 0.80733(18) 0.0196(4) Uani 1 1 d . . . C12 C 0.9956(2) 0.9025(2) 0.8435(2) 0.0274(5) Uani 1 1 d . . . H12A H 0.9026 0.9456 0.8613 0.033 Uiso 1 1 calc R . . C13 C 1.0995(3) 0.9575(2) 0.8534(2) 0.0318(5) Uani 1 1 d . . . H13 H 1.0771 1.0392 0.8763 0.038 Uiso 1 1 calc R . . C14 C 1.2347(2) 0.8948(2) 0.8304(2) 0.0320(5) Uani 1 1 d . . . H14A H 1.3048 0.9325 0.8389 0.038 Uiso 1 1 calc R . . C15 C 1.2680(2) 0.7773(2) 0.7950(2) 0.0314(5) Uani 1 1 d . . . H15 H 1.3612 0.7342 0.7789 0.038 Uiso 1 1 calc R . . C16 C 1.1657(2) 0.7214(2) 0.7827(2) 0.0252(4) Uani 1 1 d . . . H16 H 1.1894 0.6408 0.7575 0.030 Uiso 1 1 calc R . . C21 C 0.8133(2) 0.79399(18) 0.67516(19) 0.0210(4) Uani 1 1 d . . . C22 C 0.6896(2) 0.7665(2) 0.6698(2) 0.0280(5) Uani 1 1 d . . . H22 H 0.6474 0.7079 0.7356 0.034 Uiso 1 1 calc R . . C23 C 0.6282(2) 0.8238(2) 0.5695(2) 0.0294(5) Uani 1 1 d . . . H23 H 0.5450 0.8034 0.5658 0.035 Uiso 1 1 calc R . . C24 C 0.6879(2) 0.9109(2) 0.4746(2) 0.0271(5) Uani 1 1 d . . . H24 H 0.6452 0.9510 0.4060 0.033 Uiso 1 1 calc R . . C25 C 0.8095(2) 0.9394(2) 0.4796(2) 0.0309(5) Uani 1 1 d . . . H25 H 0.8499 0.9997 0.4144 0.037 Uiso 1 1 calc R . . C26 C 0.8734(2) 0.8809(2) 0.5788(2) 0.0267(5) Uani 1 1 d . . . H26 H 0.9578 0.9001 0.5810 0.032 Uiso 1 1 calc R . . C31 C 0.97078(19) 0.55268(18) 0.77183(19) 0.0203(4) Uani 1 1 d . . . C32 C 1.0397(2) 0.5379(2) 0.6506(2) 0.0246(4) Uani 1 1 d . . . H32 H 1.0398 0.6101 0.5847 0.030 Uiso 1 1 calc R . . C33 C 1.1076(2) 0.4177(2) 0.6269(2) 0.0290(5) Uani 1 1 d . . . H33 H 1.1540 0.4074 0.5447 0.035 Uiso 1 1 calc R . . C34 C 1.1079(2) 0.3121(2) 0.7231(2) 0.0296(5) Uani 1 1 d . . . H34 H 1.1555 0.2300 0.7068 0.036 Uiso 1 1 calc R . . C35 C 1.0392(2) 0.3263(2) 0.8427(2) 0.0271(5) Uani 1 1 d . . . H35 H 1.0393 0.2538 0.9082 0.033 Uiso 1 1 calc R . . C36 C 0.9701(2) 0.44632(19) 0.86741(19) 0.0226(4) Uani 1 1 d . . . H36 H 0.9224 0.4557 0.9496 0.027 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 0.02751(12) 0.05226(15) 0.02852(12) -0.00794(9) 0.01084(8) -0.00724(8) P1 0.0166(2) 0.0209(3) 0.0179(3) -0.00264(19) -0.00032(19) -0.00266(19) B2 0.0194(11) 0.0405(14) 0.0287(14) -0.0033(11) -0.0032(10) -0.0073(10) B3 0.0286(12) 0.0336(13) 0.0270(13) -0.0085(10) -0.0003(10) -0.0110(10) B4 0.0280(13) 0.0331(14) 0.0289(14) 0.0021(11) -0.0023(10) -0.0099(11) B5 0.0251(12) 0.0496(16) 0.0221(13) -0.0053(11) -0.0018(10) -0.0139(11) B6 0.0213(12) 0.0401(15) 0.0342(15) -0.0125(12) 0.0017(10) -0.0053(10) B7 0.0202(11) 0.0336(13) 0.0237(12) -0.0013(10) 0.0004(9) -0.0049(10) B8 0.0224(11) 0.0289(13) 0.0246(13) -0.0036(10) 0.0008(10) -0.0029(10) B9 0.0214(12) 0.0453(15) 0.0261(13) -0.0037(11) -0.0040(10) -0.0081(11) B10 0.0264(13) 0.0458(16) 0.0371(15) -0.0191(13) -0.0001(11) -0.0096(11) B11 0.0174(11) 0.0284(13) 0.0437(16) -0.0033(11) -0.0008(11) -0.0022(10) B12 0.0180(11) 0.0304(13) 0.0319(14) -0.0041(10) -0.0022(10) -0.0052(9) C1 0.0233(11) 0.0501(14) 0.0322(13) -0.0093(11) -0.0038(9) -0.0114(10) C11 0.0213(9) 0.0207(9) 0.0148(9) 0.0000(7) -0.0027(7) -0.0049(8) C12 0.0317(11) 0.0234(11) 0.0238(11) -0.0038(8) -0.0034(9) -0.0028(9) C13 0.0490(14) 0.0239(11) 0.0250(12) -0.0034(9) -0.0084(10) -0.0125(10) C14 0.0410(13) 0.0361(13) 0.0251(12) 0.0044(9) -0.0141(10) -0.0213(10) C15 0.0235(11) 0.0347(12) 0.0366(13) -0.0018(10) -0.0098(10) -0.0075(9) C16 0.0222(10) 0.0243(10) 0.0284(12) -0.0064(9) -0.0050(9) -0.0024(8) C21 0.0182(9) 0.0211(10) 0.0220(10) -0.0064(8) -0.0016(8) -0.0013(8) C22 0.0237(10) 0.0293(11) 0.0294(12) 0.0004(9) -0.0044(9) -0.0094(9) C23 0.0212(10) 0.0350(12) 0.0335(13) -0.0058(10) -0.0078(9) -0.0069(9) C24 0.0279(11) 0.0273(11) 0.0262(11) -0.0051(9) -0.0100(9) -0.0011(9) C25 0.0350(12) 0.0325(12) 0.0255(12) 0.0027(9) -0.0080(10) -0.0134(10) C26 0.0251(10) 0.0317(11) 0.0256(11) -0.0019(9) -0.0063(9) -0.0122(9) C31 0.0168(9) 0.0213(10) 0.0232(10) -0.0036(8) -0.0039(8) -0.0054(7) C32 0.0240(10) 0.0246(10) 0.0225(11) -0.0024(8) -0.0025(8) -0.0043(8) C33 0.0253(11) 0.0356(12) 0.0264(12) -0.0122(9) -0.0020(9) -0.0040(9) C34 0.0268(11) 0.0238(11) 0.0410(14) -0.0117(10) -0.0121(10) 0.0006(8) C35 0.0301(11) 0.0213(10) 0.0334(12) 0.0005(9) -0.0156(9) -0.0074(8) C36 0.0219(10) 0.0244(10) 0.0231(11) -0.0024(8) -0.0072(8) -0.0071(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 H8 2.1413 . ? Ag1 H12 2.2607 . ? Ag1 H7 2.3611 . ? Ag1 P1 2.3625(10) . ? Ag1 B8 2.504(3) . ? Ag1 B12 2.569(3) . ? Ag1 B7 2.619(2) . ? P1 C21 1.814(2) . ? P1 C31 1.815(2) . ? P1 C11 1.821(2) . ? B2 C1 1.714(4) . ? B2 B6 1.760(4) . ? B2 B7 1.769(3) . ? B2 B11 1.778(4) . ? B2 B3 1.789(4) . ? B2 H2 1.1200 . ? B3 C1 1.715(4) . ? B3 B7 1.776(4) . ? B3 B8 1.778(3) . ? B3 B4 1.788(4) . ? B3 H3 1.1200 . ? B4 C1 1.729(4) . ? B4 B5 1.753(4) . ? B4 B8 1.764(4) . ? B4 B9 1.779(4) . ? B4 H4 1.1200 . ? B5 C1 1.715(3) . ? B5 B9 1.747(4) . ? B5 B6 1.756(4) . ? B5 B10 1.763(4) . ? B5 H5 1.1200 . ? B6 C1 1.721(4) . ? B6 B10 1.769(4) . ? B6 B11 1.769(4) . ? B6 H6 1.1200 . ? B7 B11 1.782(4) . ? B7 B12 1.791(4) . ? B7 B8 1.796(4) . ? B7 H7 1.1200 . ? B8 B9 1.780(4) . ? B8 B12 1.789(4) . ? B8 H8 1.1200 . ? B9 B12 1.779(4) . ? B9 B10 1.782(4) . ? B9 H9 1.1200 . ? B10 B12 1.770(4) . ? B10 B11 1.785(4) . ? B10 H10 1.1200 . ? B11 B12 1.779(3) . ? B11 H11 1.1200 . ? B12 H12 1.1200 . ? C1 H1 1.1200 . ? C11 C16 1.396(3) . ? C11 C12 1.398(3) . ? C12 C13 1.390(3) . ? C12 H12A 0.9500 . ? C13 C14 1.379(4) . ? C13 H13 0.9500 . ? C14 C15 1.380(3) . ? C14 H14A 0.9500 . ? C15 C16 1.392(3) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C21 C26 1.392(3) . ? C21 C22 1.396(3) . ? C22 C23 1.381(3) . ? C22 H22 0.9500 . ? C23 C24 1.382(3) . ? C23 H23 0.9500 . ? C24 C25 1.381(3) . ? C24 H24 0.9500 . ? C25 C26 1.387(3) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C31 C36 1.390(3) . ? C31 C32 1.401(3) . ? C32 C33 1.385(3) . ? C32 H32 0.9500 . ? C33 C34 1.388(3) . ? C33 H33 0.9500 . ? C34 C35 1.382(3) . ? C34 H34 0.9500 . ? C35 C36 1.390(3) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? 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 H8 Ag1 H12 84.8 . . ? H8 Ag1 H7 82.8 . . ? H12 Ag1 H7 80.1 . . ? H8 Ag1 P1 134.2 . . ? H12 Ag1 P1 136.7 . . ? H7 Ag1 P1 116.8 . . ? H8 Ag1 B8 26.5 . . ? H12 Ag1 B8 64.8 . . ? H7 Ag1 B8 63.7 . . ? P1 Ag1 B8 158.22(6) . . ? H8 Ag1 B12 65.2 . . ? H12 Ag1 B12 25.8 . . ? H7 Ag1 B12 62.6 . . ? P1 Ag1 B12 160.32(6) . . ? B8 Ag1 B12 41.26(8) . . ? H8 Ag1 B7 64.5 . . ? H12 Ag1 B7 62.9 . . ? H7 Ag1 B7 25.3 . . ? P1 Ag1 B7 142.11(6) . . ? B8 Ag1 B7 40.98(8) . . ? B12 Ag1 B7 40.37(8) . . ? C21 P1 C31 104.50(9) . . ? C21 P1 C11 107.69(9) . . ? C31 P1 C11 104.83(9) . . ? C21 P1 Ag1 111.28(7) . . ? C31 P1 Ag1 113.94(7) . . ? C11 P1 Ag1 113.90(7) . . ? C1 B2 B6 59.34(15) . . ? C1 B2 B7 105.23(18) . . ? B6 B2 B7 107.85(18) . . ? C1 B2 B11 106.08(18) . . ? B6 B2 B11 60.00(15) . . ? B7 B2 B11 60.30(14) . . ? C1 B2 B3 58.58(15) . . ? B6 B2 B3 107.79(19) . . ? B7 B2 B3 59.87(14) . . ? B11 B2 B3 108.35(17) . . ? C1 B2 H2 124.0 . . ? B6 B2 H2 121.6 . . ? B7 B2 H2 122.4 . . ? B11 B2 H2 121.7 . . ? B3 B2 H2 121.7 . . ? C1 B3 B7 104.93(18) . . ? C1 B3 B8 104.98(18) . . ? B7 B3 B8 60.72(14) . . ? C1 B3 B4 59.12(14) . . ? B7 B3 B4 107.94(18) . . ? B8 B3 B4 59.32(14) . . ? C1 B3 B2 58.55(15) . . ? B7 B3 B2 59.53(14) . . ? B8 B3 B2 107.81(18) . . ? B4 B3 B2 107.59(19) . . ? C1 B3 H3 124.4 . . ? B7 B3 H3 122.2 . . ? B8 B3 H3 122.3 . . ? B4 B3 H3 121.7 . . ? B2 B3 H3 121.9 . . ? C1 B4 B5 59.00(15) . . ? C1 B4 B8 104.97(18) . . ? B5 B4 B8 107.05(18) . . ? C1 B4 B9 105.39(18) . . ? B5 B4 B9 59.28(15) . . ? B8 B4 B9 60.32(14) . . ? C1 B4 B3 58.35(14) . . ? B5 B4 B3 107.10(19) . . ? B8 B4 B3 60.07(14) . . ? B9 B4 B3 108.26(18) . . ? C1 B4 H4 124.3 . . ? B5 B4 H4 122.3 . . ? B8 B4 H4 122.4 . . ? B9 B4 H4 122.0 . . ? B3 B4 H4 121.8 . . ? C1 B5 B9 107.45(19) . . ? C1 B5 B4 59.81(15) . . ? B9 B5 B4 61.11(15) . . ? C1 B5 B6 59.42(15) . . ? B9 B5 B6 109.54(19) . . ? B4 B5 B6 109.58(19) . . ? C1 B5 B10 107.02(19) . . ? B9 B5 B10 61.02(15) . . ? B4 B5 B10 110.30(19) . . ? B6 B5 B10 60.36(15) . . ? C1 B5 H5 123.2 . . ? B9 B5 H5 120.9 . . ? B4 B5 H5 120.2 . . ? B6 B5 H5 120.9 . . ? B10 B5 H5 121.1 . . ? C1 B6 B5 59.09(15) . . ? C1 B6 B2 59.00(15) . . ? B5 B6 B2 107.93(19) . . ? C1 B6 B10 106.50(19) . . ? B5 B6 B10 60.02(16) . . ? B2 B6 B10 109.18(18) . . ? C1 B6 B11 106.21(19) . . ? B5 B6 B11 108.11(18) . . ? B2 B6 B11 60.50(15) . . ? B10 B6 B11 60.58(15) . . ? C1 B6 H6 123.6 . . ? B5 B6 H6 121.8 . . ? B2 B6 H6 121.2 . . ? B10 B6 H6 121.4 . . ? B11 B6 H6 121.8 . . ? B2 B7 B3 60.60(15) . . ? B2 B7 B11 60.10(14) . . ? B3 B7 B11 108.76(18) . . ? B2 B7 B12 107.56(18) . . ? B3 B7 B12 107.81(18) . . ? B11 B7 B12 59.74(14) . . ? B2 B7 B8 107.85(17) . . ? B3 B7 B8 59.70(14) . . ? B11 B7 B8 107.88(18) . . ? B12 B7 B8 59.82(14) . . ? B2 B7 Ag1 173.70(16) . . ? B3 B7 Ag1 115.46(15) . . ? B11 B7 Ag1 119.27(14) . . ? B12 B7 Ag1 68.33(11) . . ? B8 B7 Ag1 66.07(11) . . ? B2 B7 H7 121.7 . . ? B3 B7 H7 121.3 . . ? B11 B7 H7 121.5 . . ? B12 B7 H7 122.1 . . ? B8 B7 H7 122.0 . . ? Ag1 B7 H7 64.4 . . ? B4 B8 B3 60.62(14) . . ? B4 B8 B9 60.25(15) . . ? B3 B8 B9 108.64(17) . . ? B4 B8 B12 107.99(18) . . ? B3 B8 B12 107.81(17) . . ? B9 B8 B12 59.79(15) . . ? B4 B8 B7 108.06(17) . . ? B3 B8 B7 59.58(14) . . ? B9 B8 B7 107.92(18) . . ? B12 B8 B7 59.94(14) . . ? B4 B8 Ag1 178.37(17) . . ? B3 B8 Ag1 120.96(15) . . ? B9 B8 Ag1 118.30(15) . . ? B12 B8 Ag1 71.33(12) . . ? B7 B8 Ag1 72.95(11) . . ? B4 B8 H8 121.4 . . ? B3 B8 H8 121.5 . . ? B9 B8 H8 121.5 . . ? B12 B8 H8 122.0 . . ? B7 B8 H8 122.0 . . ? Ag1 B8 H8 58.4 . . ? B5 B9 B4 59.61(15) . . ? B5 B9 B12 106.82(18) . . ? B4 B9 B12 107.77(18) . . ? B5 B9 B8 106.61(18) . . ? B4 B9 B8 59.43(15) . . ? B12 B9 B8 60.33(14) . . ? B5 B9 B10 59.95(16) . . ? B4 B9 B10 108.25(18) . . ? B12 B9 B10 59.61(15) . . ? B8 B9 B10 108.01(18) . . ? B5 B9 H9 122.7 . . ? B4 B9 H9 121.8 . . ? B12 B9 H9 122.0 . . ? B8 B9 H9 122.1 . . ? B10 B9 H9 121.5 . . ? B5 B10 B6 59.62(15) . . ? B5 B10 B12 106.47(19) . . ? B6 B10 B12 107.23(19) . . ? B5 B10 B9 59.03(15) . . ? B6 B10 B9 107.35(19) . . ? B12 B10 B9 60.10(15) . . ? B5 B10 B11 107.11(18) . . ? B6 B10 B11 59.71(15) . . ? B12 B10 B11 60.06(15) . . ? B9 B10 B11 108.28(19) . . ? B5 B10 H10 122.9 . . ? B6 B10 H10 122.2 . . ? B12 B10 H10 122.2 . . ? B9 B10 H10 121.8 . . ? B11 B10 H10 121.7 . . ? B6 B11 B2 59.50(15) . . ? B6 B11 B12 106.83(19) . . ? B2 B11 B12 107.68(18) . . ? B6 B11 B7 106.90(18) . . ? B2 B11 B7 59.60(14) . . ? B12 B11 B7 60.38(14) . . ? B6 B11 B10 59.71(15) . . ? B2 B11 B10 107.68(19) . . ? B12 B11 B10 59.56(15) . . ? B7 B11 B10 107.91(18) . . ? B6 B11 H11 122.6 . . ? B2 B11 H11 122.0 . . ? B12 B11 H11 122.0 . . ? B7 B11 H11 121.9 . . ? B10 B11 H11 121.8 . . ? B10 B12 B9 60.29(16) . . ? B10 B12 B11 60.38(16) . . ? B9 B12 B11 108.68(18) . . ? B10 B12 B8 108.18(18) . . ? B9 B12 B8 59.87(15) . . ? B11 B12 B8 108.33(17) . . ? B10 B12 B7 108.17(17) . . ? B9 B12 B7 108.23(17) . . ? B11 B12 B7 59.88(15) . . ? B8 B12 B7 60.24(14) . . ? B10 B12 Ag1 175.32(17) . . ? B9 B12 Ag1 115.25(15) . . ? B11 B12 Ag1 121.90(16) . . ? B8 B12 Ag1 67.40(12) . . ? B7 B12 Ag1 71.31(12) . . ? B10 B12 H12 121.5 . . ? B9 B12 H12 121.5 . . ? B11 B12 H12 121.4 . . ? B8 B12 H12 121.6 . . ? B7 B12 H12 121.7 . . ? Ag1 B12 H12 61.5 . . ? B5 C1 B2 112.05(18) . . ? B5 C1 B3 112.27(17) . . ? B2 C1 B3 62.87(15) . . ? B5 C1 B6 61.49(16) . . ? B2 C1 B6 61.66(16) . . ? B3 C1 B6 113.16(19) . . ? B5 C1 B4 61.19(15) . . ? B2 C1 B4 113.86(18) . . ? B3 C1 B4 62.53(15) . . ? B6 C1 B4 112.42(17) . . ? B5 C1 H1 119.9 . . ? B2 C1 H1 118.4 . . ? B3 C1 H1 118.3 . . ? B6 C1 H1 119.2 . . ? B4 C1 H1 118.6 . . ? C16 C11 C12 119.11(19) . . ? C16 C11 P1 122.50(15) . . ? C12 C11 P1 118.14(16) . . ? C13 C12 C11 119.9(2) . . ? C13 C12 H12A 120.1 . . ? C11 C12 H12A 120.1 . . ? C14 C13 C12 120.7(2) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C15 C14 C13 119.8(2) . . ? C15 C14 H14A 120.1 . . ? C13 C14 H14A 120.1 . . ? C14 C15 C16 120.4(2) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C15 C16 C11 120.1(2) . . ? C15 C16 H16 119.9 . . ? C11 C16 H16 119.9 . . ? C26 C21 C22 119.25(19) . . ? C26 C21 P1 123.80(15) . . ? C22 C21 P1 116.94(16) . . ? C23 C22 C21 120.5(2) . . ? C23 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? C22 C23 C24 120.0(2) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C25 C24 C23 119.9(2) . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C24 C25 C26 120.7(2) . . ? C24 C25 H25 119.7 . . ? C26 C25 H25 119.7 . . ? C25 C26 C21 119.66(19) . . ? C25 C26 H26 120.2 . . ? C21 C26 H26 120.2 . . ? C36 C31 C32 119.70(19) . . ? C36 C31 P1 118.99(16) . . ? C32 C31 P1 121.26(15) . . ? C33 C32 C31 119.8(2) . . ? C33 C32 H32 120.1 . . ? C31 C32 H32 120.1 . . ? C32 C33 C34 120.2(2) . . ? C32 C33 H33 119.9 . . ? C34 C33 H33 119.9 . . ? C35 C34 C33 120.1(2) . . ? C35 C34 H34 119.9 . . ? C33 C34 H34 119.9 . . ? C34 C35 C36 120.2(2) . . ? C34 C35 H35 119.9 . . ? C36 C35 H35 119.9 . . ? C35 C36 C31 119.9(2) . . ? C35 C36 H36 120.0 . . ? C31 C36 H36 120.0 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.544 _refine_diff_density_min -0.923 _refine_diff_density_rms 0.071 #===END