# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Hoefelmeyer, James D.' _publ_contact_author_email jhoefelm@usd.edu _publ_section_title ; Reactivity of the Bifunctional Ambiphilic Molecule 8-(dimesitylboryl)quinoline: Hydrolysis and Coordination to CuI, AgI and PdII ; loop_ _publ_author_name J.-H.Son M.Pudenz J.D.Hoefelmeyer # Attachment '- cif-file.cif' data_8-(dimesitylboryl)quinoline _database_code_depnum_ccdc_archive 'CCDC 758512' _audit_creation_method SHELXL-97 _chemical_name_systematic 8-(dimesitylboryl)quinoline _chemical_name_common 8-(dimesitylboryl)quinoline _chemical_melting_point 438 _chemical_formula_moiety 'C27 H28 B N' _chemical_formula_sum 'C27 H28 B N' _chemical_formula_weight 377.31 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 _symmetry_space_group_name_hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.205(3) _cell_length_b 11.278(4) _cell_length_c 13.017(5) _cell_angle_alpha 113.018(4) _cell_angle_beta 90.617(4) _cell_angle_gamma 105.553(4) _cell_volume 1059.0(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4225 _cell_measurement_theta_min 2.60 _cell_measurement_theta_max 25.38 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.79 _exptl_crystal_size_mid 0.59 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.183 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 404 _exptl_absorpt_coefficient_mu 0.067 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9491 _exptl_absorpt_correction_T_max 0.9841 _exptl_absorpt_process_details '(SADABS; Bruker, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type 'Bruker SMART APEXII' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX II' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10020 _diffrn_reflns_av_R_equivalents 0.0398 _diffrn_reflns_av_sigmaI/netI 0.0542 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 25.36 _reflns_number_total 3858 _reflns_number_gt 2540 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2006)' _computing_cell_refinement 'SAINT (Bruker, 2006)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 (Farrugia, 1997)' _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0569P)^2^+0.2085P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3858 _refine_ls_number_parameters 268 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0829 _refine_ls_R_factor_gt 0.0451 _refine_ls_wR_factor_ref 0.1173 _refine_ls_wR_factor_gt 0.1013 _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_restrained_S_all 0.994 _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 C2 C 0.5733(2) 0.4829(2) 0.86067(17) 0.0250(5) Uani 1 1 d . . . H2 H 0.5901 0.5437 0.9377 0.030 Uiso 1 1 calc R . . C3 C 0.6626(2) 0.5294(2) 0.78581(18) 0.0292(5) Uani 1 1 d . . . H3 H 0.7378 0.6186 0.8120 0.035 Uiso 1 1 calc R . . C4 C 0.6394(2) 0.4445(2) 0.67507(18) 0.0289(5) Uani 1 1 d . . . H4 H 0.6995 0.4736 0.6231 0.035 Uiso 1 1 calc R . . C5 C 0.4947(2) 0.2205(2) 0.52331(16) 0.0265(5) Uani 1 1 d . . . H5 H 0.5479 0.2477 0.4684 0.032 Uiso 1 1 calc R . . C6 C 0.3888(2) 0.0925(2) 0.49138(16) 0.0245(5) Uani 1 1 d . . . H6 H 0.3672 0.0310 0.4145 0.029 Uiso 1 1 calc R . . C7 C 0.3116(2) 0.0524(2) 0.57353(16) 0.0224(4) Uani 1 1 d . . . H7 H 0.2432 -0.0384 0.5507 0.027 Uiso 1 1 calc R . . C8 C 0.3309(2) 0.13921(19) 0.68593(15) 0.0190(4) Uani 1 1 d . . . C9 C 0.4409(2) 0.27343(19) 0.71918(16) 0.0197(4) Uani 1 1 d . . . C10 C 0.5259(2) 0.3129(2) 0.63758(16) 0.0227(4) Uani 1 1 d . . . C11 C 0.2199(2) -0.06310(19) 0.74712(15) 0.0197(4) Uani 1 1 d . . . C12 C 0.3712(2) -0.0889(2) 0.77399(15) 0.0212(4) Uani 1 1 d . . . C13 C 0.3752(2) -0.22075(19) 0.74200(15) 0.0228(5) Uani 1 1 d . . . H13 H 0.4768 -0.2361 0.7622 0.027 Uiso 1 1 calc R . . C14 C 0.2355(2) -0.3309(2) 0.68133(15) 0.0234(5) Uani 1 1 d . . . C15 C 0.0868(2) -0.3056(2) 0.65696(16) 0.0238(4) Uani 1 1 d . . . H15 H -0.0107 -0.3796 0.6166 0.029 Uiso 1 1 calc R . . C16 C 0.0757(2) -0.17467(19) 0.68983(15) 0.0210(4) Uani 1 1 d . . . C17 C 0.5282(2) 0.0255(2) 0.83921(17) 0.0269(5) Uani 1 1 d . . . H17A H 0.5339 0.0409 0.9188 0.040 Uiso 1 1 calc R . . H17B H 0.5228 0.1075 0.8317 0.040 Uiso 1 1 calc R . . H17C H 0.6301 0.0024 0.8095 0.040 Uiso 1 1 calc R . . C18 C 0.2460(3) -0.4734(2) 0.64066(18) 0.0336(5) Uani 1 1 d . . . H18A H 0.3193 -0.4893 0.5807 0.050 Uiso 1 1 calc R . . H18B H 0.1315 -0.5371 0.6114 0.050 Uiso 1 1 calc R . . H18C H 0.2941 -0.4863 0.7034 0.050 Uiso 1 1 calc R . . C19 C -0.0912(2) -0.1564(2) 0.65694(18) 0.0288(5) Uani 1 1 d . . . H19A H -0.0800 -0.1305 0.5931 0.043 Uiso 1 1 calc R . . H19B H -0.1184 -0.0856 0.7209 0.043 Uiso 1 1 calc R . . H19C H -0.1828 -0.2413 0.6355 0.043 Uiso 1 1 calc R . . C20 C 0.1021(2) 0.16262(18) 0.84089(15) 0.0191(4) Uani 1 1 d . . . C21 C 0.0020(2) 0.22295(19) 0.79869(15) 0.0198(4) Uani 1 1 d . . . C22 C -0.1036(2) 0.28978(19) 0.86651(16) 0.0222(4) Uani 1 1 d . . . H22 H -0.1695 0.3294 0.8369 0.027 Uiso 1 1 calc R . . C23 C -0.1156(2) 0.30037(19) 0.97606(16) 0.0233(5) Uani 1 1 d . . . C24 C -0.0194(2) 0.24008(19) 1.01665(16) 0.0227(4) Uani 1 1 d . . . H24 H -0.0272 0.2451 1.0909 0.027 Uiso 1 1 calc R . . C25 C 0.0884(2) 0.17230(18) 0.95206(15) 0.0198(4) Uani 1 1 d . . . C26 C -0.0013(2) 0.2138(2) 0.67940(16) 0.0260(5) Uani 1 1 d . . . H26A H -0.0932 0.2468 0.6632 0.039 Uiso 1 1 calc R . . H26B H -0.0210 0.1197 0.6266 0.039 Uiso 1 1 calc R . . H26C H 0.1083 0.2690 0.6712 0.039 Uiso 1 1 calc R . . C27 C -0.2304(3) 0.3737(2) 1.04716(17) 0.0310(5) Uani 1 1 d . . . H27A H -0.1767 0.4712 1.0747 0.046 Uiso 1 1 calc R . . H27B H -0.2492 0.3489 1.1113 0.046 Uiso 1 1 calc R . . H27C H -0.3401 0.3486 1.0018 0.046 Uiso 1 1 calc R . . C28 C 0.1953(2) 0.1167(2) 1.00639(16) 0.0250(5) Uani 1 1 d . . . H28A H 0.3154 0.1699 1.0190 0.038 Uiso 1 1 calc R . . H28B H 0.1829 0.0225 0.9567 0.038 Uiso 1 1 calc R . . H28C H 0.1570 0.1217 1.0786 0.038 Uiso 1 1 calc R . . B1 B 0.2201(3) 0.0846(2) 0.76532(17) 0.0196(5) Uani 1 1 d . . . N1 N 0.46738(19) 0.36042(16) 0.83129(13) 0.0220(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 C2 0.0208(10) 0.0218(12) 0.0299(12) 0.0074(10) 0.0006(9) 0.0072(9) C3 0.0198(11) 0.0265(12) 0.0414(14) 0.0175(11) 0.0004(9) 0.0018(9) C4 0.0201(11) 0.0350(13) 0.0373(13) 0.0226(11) 0.0084(9) 0.0052(10) C5 0.0235(11) 0.0382(14) 0.0274(12) 0.0198(11) 0.0098(9) 0.0140(10) C6 0.0244(11) 0.0307(13) 0.0228(11) 0.0110(10) 0.0049(8) 0.0146(10) C7 0.0192(10) 0.0252(11) 0.0252(11) 0.0106(9) 0.0028(8) 0.0098(9) C8 0.0146(9) 0.0226(11) 0.0230(11) 0.0105(9) 0.0023(8) 0.0086(8) C9 0.0140(9) 0.0240(11) 0.0259(11) 0.0125(9) 0.0029(8) 0.0093(8) C10 0.0158(10) 0.0277(12) 0.0302(11) 0.0157(10) 0.0058(8) 0.0090(9) C11 0.0182(10) 0.0231(11) 0.0190(10) 0.0094(9) 0.0048(8) 0.0064(9) C12 0.0184(10) 0.0267(11) 0.0207(10) 0.0112(9) 0.0051(8) 0.0075(9) C13 0.0238(10) 0.0273(12) 0.0230(11) 0.0135(9) 0.0040(8) 0.0115(9) C14 0.0292(11) 0.0235(11) 0.0209(11) 0.0115(9) 0.0064(9) 0.0093(9) C15 0.0235(11) 0.0217(11) 0.0229(11) 0.0094(9) 0.0011(8) 0.0013(9) C16 0.0192(10) 0.0252(11) 0.0199(10) 0.0110(9) 0.0046(8) 0.0056(9) C17 0.0192(10) 0.0291(12) 0.0334(12) 0.0133(10) 0.0004(9) 0.0080(9) C18 0.0427(13) 0.0279(13) 0.0311(12) 0.0114(10) 0.0014(10) 0.0128(11) C19 0.0184(10) 0.0269(12) 0.0377(12) 0.0118(10) -0.0004(9) 0.0037(9) C20 0.0141(9) 0.0178(10) 0.0233(10) 0.0083(9) 0.0006(8) 0.0017(8) C21 0.0138(9) 0.0190(11) 0.0247(11) 0.0094(9) 0.0015(8) 0.0012(8) C22 0.0156(10) 0.0217(11) 0.0314(12) 0.0128(9) 0.0021(8) 0.0056(9) C23 0.0173(10) 0.0233(12) 0.0277(11) 0.0089(9) 0.0051(8) 0.0058(9) C24 0.0203(10) 0.0267(11) 0.0186(10) 0.0087(9) 0.0031(8) 0.0042(9) C25 0.0146(9) 0.0184(11) 0.0228(10) 0.0068(9) 0.0012(8) 0.0016(8) C26 0.0224(10) 0.0319(12) 0.0312(12) 0.0185(10) 0.0058(9) 0.0112(9) C27 0.0305(12) 0.0372(13) 0.0315(12) 0.0151(11) 0.0117(9) 0.0178(10) C28 0.0244(11) 0.0300(12) 0.0231(11) 0.0123(9) 0.0032(8) 0.0097(9) B1 0.0125(10) 0.0226(13) 0.0180(11) 0.0051(10) -0.0059(8) 0.0014(9) N1 0.0185(8) 0.0213(10) 0.0249(9) 0.0081(8) 0.0023(7) 0.0060(7) _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 C2 N1 1.321(2) . ? C2 C3 1.404(3) . ? C2 H2 0.9500 . ? C3 C4 1.359(3) . ? C3 H3 0.9500 . ? C4 C10 1.411(3) . ? C4 H4 0.9500 . ? C5 C6 1.364(3) . ? C5 C10 1.414(3) . ? C5 H5 0.9500 . ? C6 C7 1.410(3) . ? C6 H6 0.9500 . ? C7 C8 1.384(3) . ? C7 H7 0.9500 . ? C8 C9 1.428(3) . ? C8 B1 1.578(3) . ? C9 N1 1.378(2) . ? C9 C10 1.426(3) . ? C11 C16 1.410(3) . ? C11 C12 1.419(3) . ? C11 B1 1.588(3) . ? C12 C13 1.388(3) . ? C12 C17 1.508(3) . ? C13 C14 1.390(3) . ? C13 H13 0.9500 . ? C14 C15 1.386(3) . ? C14 C18 1.510(3) . ? C15 C16 1.396(3) . ? C15 H15 0.9500 . ? C16 C19 1.519(3) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C25 1.416(3) . ? C20 C21 1.422(2) . ? C20 B1 1.575(3) . ? C21 C22 1.394(3) . ? C21 C26 1.515(3) . ? C22 C23 1.391(3) . ? C22 H22 0.9500 . ? C23 C24 1.387(3) . ? C23 C27 1.505(3) . ? C24 C25 1.396(3) . ? C24 H24 0.9500 . ? C25 C28 1.514(2) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? B1 N1 3.003(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 N1 C2 C3 124.44(19) . . ? N1 C2 H2 117.8 . . ? C3 C2 H2 117.8 . . ? C4 C3 C2 118.75(19) . . ? C4 C3 H3 120.6 . . ? C2 C3 H3 120.6 . . ? C3 C4 C10 119.77(19) . . ? C3 C4 H4 120.1 . . ? C10 C4 H4 120.1 . . ? C6 C5 C10 120.50(18) . . ? C6 C5 H5 119.7 . . ? C10 C5 H5 119.7 . . ? C5 C6 C7 119.44(19) . . ? C5 C6 H6 120.3 . . ? C7 C6 H6 120.3 . . ? C8 C7 C6 123.04(19) . . ? C8 C7 H7 118.5 . . ? C6 C7 H7 118.5 . . ? C7 C8 C9 117.42(17) . . ? C7 C8 B1 117.21(17) . . ? C9 C8 B1 125.24(17) . . ? N1 C9 C10 121.49(17) . . ? N1 C9 C8 118.61(16) . . ? C10 C9 C8 119.85(17) . . ? C4 C10 C5 122.45(18) . . ? C4 C10 C9 117.92(18) . . ? C5 C10 C9 119.62(18) . . ? C16 C11 C12 117.88(18) . . ? C16 C11 B1 120.62(16) . . ? C12 C11 B1 120.95(17) . . ? C13 C12 C11 120.07(18) . . ? C13 C12 C17 119.10(17) . . ? C11 C12 C17 120.82(18) . . ? C12 C13 C14 122.13(18) . . ? C12 C13 H13 118.9 . . ? C14 C13 H13 118.9 . . ? C15 C14 C13 117.69(18) . . ? C15 C14 C18 120.96(18) . . ? C13 C14 C18 121.33(18) . . ? C14 C15 C16 122.11(18) . . ? C14 C15 H15 118.9 . . ? C16 C15 H15 118.9 . . ? C15 C16 C11 120.04(17) . . ? C15 C16 C19 118.47(17) . . ? C11 C16 C19 121.41(17) . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C14 C18 H18A 109.5 . . ? C14 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C14 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C25 C20 C21 117.60(17) . . ? C25 C20 B1 121.35(16) . . ? C21 C20 B1 121.03(16) . . ? C22 C21 C20 120.07(17) . . ? C22 C21 C26 117.19(16) . . ? C20 C21 C26 122.70(16) . . ? C23 C22 C21 122.25(17) . . ? C23 C22 H22 118.9 . . ? C21 C22 H22 118.9 . . ? C24 C23 C22 117.61(17) . . ? C24 C23 C27 121.49(17) . . ? C22 C23 C27 120.89(17) . . ? C23 C24 C25 122.24(17) . . ? C23 C24 H24 118.9 . . ? C25 C24 H24 118.9 . . ? C24 C25 C20 120.22(17) . . ? C24 C25 C28 118.12(16) . . ? C20 C25 C28 121.59(16) . . ? C21 C26 H26A 109.5 . . ? C21 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C21 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C27 H27A 109.5 . . ? C23 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C23 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C20 B1 C8 121.85(17) . . ? C20 B1 C11 124.31(17) . . ? C8 B1 C11 113.27(16) . . ? C20 B1 N1 84.65(12) . . ? C8 B1 N1 53.13(10) . . ? C11 B1 N1 139.54(13) . . ? C2 N1 C9 117.61(17) . . ? C2 N1 B1 178.71(13) . . ? C9 N1 B1 62.78(11) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.36 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.256 _refine_diff_density_min -0.214 _refine_diff_density_rms 0.042 _exptl_crystal_recrystallization_method CH2Cl2/Hexane #===END data_Mesityl(quinolin-8-yl)borinic-acid _database_code_depnum_ccdc_archive 'CCDC 758513' _audit_creation_method SHELXL-97 _chemical_name_systematic 'Mesityl(quinolin-8-yl)borinic acid' _chemical_name_common 'Mesityl(quinolin-8-yl)borinic acid' _chemical_melting_point 423 _chemical_formula_moiety 'C18 H18 B N O' _chemical_formula_sum 'C18 H18 B N O' _chemical_formula_weight 275.14 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 _symmetry_space_group_name_hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.0600(16) _cell_length_b 8.5500(17) _cell_length_c 13.343(3) _cell_angle_alpha 92.64(3) _cell_angle_beta 105.65(3) _cell_angle_gamma 117.78(3) _cell_volume 767.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3214 _cell_measurement_theta_min 2.78 _cell_measurement_theta_max 25.47 _exptl_crystal_description Prism _exptl_crystal_colour 'Pale Yellow' _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.46 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.191 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 292 _exptl_absorpt_coefficient_mu 0.072 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9621 _exptl_absorpt_correction_T_max 0.9829 _exptl_absorpt_process_details '(SADABS; Bruker, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type 'Bruker SMART APEXII' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEXII' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7609 _diffrn_reflns_av_R_equivalents 0.0325 _diffrn_reflns_av_sigmaI/netI 0.0424 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.75 _diffrn_reflns_theta_max 25.66 _reflns_number_total 2840 _reflns_number_gt 1900 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2006)' _computing_cell_refinement 'SAINT (Bruker, 2006)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 (Farrugia, 1997)' _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.4251P] 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 2840 _refine_ls_number_parameters 197 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0756 _refine_ls_R_factor_gt 0.0427 _refine_ls_wR_factor_ref 0.1199 _refine_ls_wR_factor_gt 0.1027 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C2 C 0.5970(3) 0.7452(2) 0.54922(14) 0.0255(4) Uani 1 1 d . . . H2 H 0.6058 0.6802 0.6044 0.031 Uiso 1 1 calc R . . C3 C 0.7674(3) 0.9097(2) 0.55594(15) 0.0274(4) Uani 1 1 d . . . H3 H 0.8873 0.9525 0.6136 0.033 Uiso 1 1 calc R . . C4 C 0.7566(3) 1.0055(2) 0.47849(14) 0.0261(4) Uani 1 1 d . . . H4 H 0.8688 1.1174 0.4819 0.031 Uiso 1 1 calc R . . C5 C 0.5552(3) 1.0295(2) 0.30881(14) 0.0273(4) Uani 1 1 d . . . H5 H 0.6639 1.1417 0.3091 0.033 Uiso 1 1 calc R . . C6 C 0.3782(3) 0.9578(2) 0.22731(15) 0.0289(5) Uani 1 1 d . . . H6 H 0.3648 1.0202 0.1713 0.035 Uiso 1 1 calc R . . C7 C 0.2152(3) 0.7908(2) 0.22648(14) 0.0241(4) Uani 1 1 d . . . H7 H 0.0942 0.7436 0.1691 0.029 Uiso 1 1 calc R . . C8 C 0.2248(2) 0.6933(2) 0.30572(13) 0.0200(4) Uani 1 1 d . . . C9 C 0.4114(2) 0.7697(2) 0.39088(13) 0.0195(4) Uani 1 1 d . . . C10 C 0.5767(3) 0.9376(2) 0.39230(14) 0.0227(4) Uani 1 1 d . . . C11 C -0.1708(2) 0.4340(2) 0.20858(13) 0.0197(4) Uani 1 1 d . . . C12 C -0.2160(3) 0.3280(2) 0.11087(14) 0.0222(4) Uani 1 1 d . . . C13 C -0.4012(2) 0.2603(2) 0.03168(14) 0.0232(4) Uani 1 1 d . . . H13 H -0.4292 0.1883 -0.0335 0.028 Uiso 1 1 calc R . . C14 C -0.5443(2) 0.2969(2) 0.04713(14) 0.0219(4) Uani 1 1 d . . . C15 C -0.4980(2) 0.4039(2) 0.14360(14) 0.0227(4) Uani 1 1 d . . . H15 H -0.5943 0.4304 0.1550 0.027 Uiso 1 1 calc R . . C16 C -0.3151(2) 0.4732(2) 0.22387(13) 0.0204(4) Uani 1 1 d . . . C17 C -0.0634(3) 0.2883(3) 0.08999(15) 0.0327(5) Uani 1 1 d . . . H17A H 0.0438 0.3983 0.0804 0.049 Uiso 1 1 calc R . . H17B H -0.1260 0.1947 0.0255 0.049 Uiso 1 1 calc R . . H17C H -0.0086 0.2459 0.1504 0.049 Uiso 1 1 calc R . . C18 C -0.7437(3) 0.2235(3) -0.03884(15) 0.0291(5) Uani 1 1 d . . . H18A H -0.7432 0.1640 -0.1032 0.044 Uiso 1 1 calc R . . H18B H -0.7687 0.3230 -0.0546 0.044 Uiso 1 1 calc R . . H18C H -0.8484 0.1361 -0.0144 0.044 Uiso 1 1 calc R . . C19 C -0.2671(3) 0.5936(3) 0.32637(14) 0.0298(5) Uani 1 1 d . . . H19A H -0.2341 0.5400 0.3867 0.045 Uiso 1 1 calc R . . H19B H -0.3826 0.6059 0.3253 0.045 Uiso 1 1 calc R . . H19C H -0.1537 0.7129 0.3335 0.045 Uiso 1 1 calc R . . B1 B 0.0360(3) 0.5086(3) 0.30073(15) 0.0217(5) Uani 1 1 d . . . N1 N 0.4254(2) 0.67574(19) 0.47070(11) 0.0217(3) Uani 1 1 d . . . O1 O 0.04704(19) 0.41041(17) 0.37649(10) 0.0290(3) Uani 1 1 d . . . H1 H 0.171(4) 0.479(4) 0.428(2) 0.086(10) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C2 0.0235(10) 0.0270(10) 0.0277(10) 0.0036(8) 0.0070(8) 0.0146(9) C3 0.0183(10) 0.0275(10) 0.0310(11) -0.0027(8) 0.0033(8) 0.0106(9) C4 0.0178(10) 0.0201(9) 0.0352(11) -0.0015(8) 0.0106(8) 0.0052(8) C5 0.0255(10) 0.0206(10) 0.0343(11) 0.0070(8) 0.0169(9) 0.0064(8) C6 0.0334(11) 0.0239(10) 0.0307(11) 0.0104(8) 0.0154(9) 0.0124(9) C7 0.0228(10) 0.0228(10) 0.0238(10) 0.0040(8) 0.0075(8) 0.0094(8) C8 0.0178(9) 0.0195(9) 0.0239(9) 0.0023(7) 0.0085(7) 0.0094(8) C9 0.0187(9) 0.0190(9) 0.0246(9) 0.0026(7) 0.0107(8) 0.0106(8) C10 0.0207(10) 0.0192(9) 0.0290(10) 0.0010(8) 0.0125(8) 0.0087(8) C11 0.0174(9) 0.0165(9) 0.0255(9) 0.0072(7) 0.0096(7) 0.0069(8) C12 0.0214(10) 0.0209(9) 0.0267(10) 0.0065(8) 0.0107(8) 0.0109(8) C13 0.0224(10) 0.0203(9) 0.0232(10) 0.0020(8) 0.0072(8) 0.0081(8) C14 0.0166(9) 0.0192(9) 0.0269(10) 0.0091(8) 0.0072(8) 0.0062(8) C15 0.0170(9) 0.0219(10) 0.0322(10) 0.0102(8) 0.0124(8) 0.0094(8) C16 0.0202(9) 0.0177(9) 0.0251(10) 0.0077(7) 0.0116(8) 0.0083(8) C17 0.0275(11) 0.0383(12) 0.0359(11) -0.0002(9) 0.0106(9) 0.0198(10) C18 0.0192(10) 0.0296(11) 0.0328(11) 0.0077(9) 0.0069(8) 0.0085(9) C19 0.0247(10) 0.0327(11) 0.0315(11) 0.0037(9) 0.0121(8) 0.0126(9) B1 0.0215(11) 0.0234(11) 0.0238(11) 0.0061(9) 0.0105(9) 0.0123(9) N1 0.0184(8) 0.0222(8) 0.0242(8) 0.0037(6) 0.0064(6) 0.0104(7) O1 0.0188(7) 0.0263(7) 0.0319(8) 0.0113(6) 0.0049(6) 0.0049(6) _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 C2 N1 1.326(2) . ? C2 C3 1.412(3) . ? C2 H2 0.9500 . ? C3 C4 1.357(3) . ? C3 H3 0.9500 . ? C4 C10 1.420(3) . ? C4 H4 0.9500 . ? C5 C6 1.371(3) . ? C5 C10 1.411(2) . ? C5 H5 0.9500 . ? C6 C7 1.416(3) . ? C6 H6 0.9500 . ? C7 C8 1.384(2) . ? C7 H7 0.9500 . ? C8 C9 1.440(2) . ? C8 B1 1.584(3) . ? C9 N1 1.375(2) . ? C9 C10 1.428(2) . ? C11 C12 1.408(2) . ? C11 C16 1.411(2) . ? C11 B1 1.590(3) . ? C12 C13 1.402(2) . ? C12 C17 1.507(2) . ? C13 C14 1.389(2) . ? C13 H13 0.9500 . ? C14 C15 1.395(2) . ? C14 C18 1.514(2) . ? C15 C16 1.395(2) . ? C15 H15 0.9500 . ? C16 C19 1.515(3) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? B1 O1 1.354(2) . ? O1 H1 0.93(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 N1 C2 C3 124.11(17) . . ? N1 C2 H2 117.9 . . ? C3 C2 H2 117.9 . . ? C4 C3 C2 118.71(17) . . ? C4 C3 H3 120.6 . . ? C2 C3 H3 120.6 . . ? C3 C4 C10 119.68(17) . . ? C3 C4 H4 120.2 . . ? C10 C4 H4 120.2 . . ? C6 C5 C10 120.37(17) . . ? C6 C5 H5 119.8 . . ? C10 C5 H5 119.8 . . ? C5 C6 C7 120.14(17) . . ? C5 C6 H6 119.9 . . ? C7 C6 H6 119.9 . . ? C8 C7 C6 122.81(17) . . ? C8 C7 H7 118.6 . . ? C6 C7 H7 118.6 . . ? C7 C8 C9 116.62(16) . . ? C7 C8 B1 120.25(16) . . ? C9 C8 B1 123.13(15) . . ? N1 C9 C10 121.08(16) . . ? N1 C9 C8 117.91(15) . . ? C10 C9 C8 121.01(16) . . ? C5 C10 C4 122.73(17) . . ? C5 C10 C9 119.05(17) . . ? C4 C10 C9 118.22(17) . . ? C12 C11 C16 118.30(16) . . ? C12 C11 B1 121.77(16) . . ? C16 C11 B1 119.94(15) . . ? C13 C12 C11 120.73(16) . . ? C13 C12 C17 119.32(15) . . ? C11 C12 C17 119.94(16) . . ? C14 C13 C12 121.03(16) . . ? C14 C13 H13 119.5 . . ? C12 C13 H13 119.5 . . ? C13 C14 C15 118.03(16) . . ? C13 C14 C18 120.70(16) . . ? C15 C14 C18 121.27(16) . . ? C16 C15 C14 122.28(16) . . ? C16 C15 H15 118.9 . . ? C14 C15 H15 118.9 . . ? C15 C16 C11 119.62(16) . . ? C15 C16 C19 120.97(16) . . ? C11 C16 C19 119.39(16) . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C14 C18 H18A 109.5 . . ? C14 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C14 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O1 B1 C8 120.25(16) . . ? O1 B1 C11 118.15(16) . . ? C8 B1 C11 121.59(15) . . ? C2 N1 C9 118.19(15) . . ? B1 O1 H1 107.4(17) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 N1 0.93(3) 1.85(3) 2.692(2) 149(2) . _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 25.66 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 0.229 _refine_diff_density_min -0.216 _refine_diff_density_rms 0.042 _exptl_crystal_recrystallization_method 'Acetone evaporation' #===END data_8-(dimesitylboryl)-1-methylquinolinium-triflate _database_code_depnum_ccdc_archive 'CCDC 758514' _audit_creation_method SHELXL-97 _chemical_name_systematic '8-(dimesitylboryl)-1-methylquinolinium triflate dichloromethane solvate' _chemical_name_common ;8-(dimesitylboryl)-1-methylquinolinium triflate dichloromethane solvate ; _chemical_melting_point 479 _chemical_formula_moiety 'C28 H31 B N, C F3 O3 S, C H2 Cl2' _chemical_formula_sum 'C30 H33 B Cl2 F3 N O3 S' _chemical_formula_weight 626.34 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 _symmetry_space_group_name_hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.3454(18) _cell_length_b 13.054(3) _cell_length_c 14.304(3) _cell_angle_alpha 89.985(2) _cell_angle_beta 76.034(2) _cell_angle_gamma 88.216(2) _cell_volume 1511.4(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8938 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 25.34 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.376 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 652 _exptl_absorpt_coefficient_mu 0.335 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8721 _exptl_absorpt_correction_T_max 0.9209 _exptl_absorpt_process_details '(SADABS; Bruker, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type 'Bruker SMART APEXII' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEXII' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14512 _diffrn_reflns_av_R_equivalents 0.0325 _diffrn_reflns_av_sigmaI/netI 0.0372 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 25.37 _reflns_number_total 5505 _reflns_number_gt 4274 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2006)' _computing_cell_refinement 'SAINT (Bruker, 2006)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 (Farrugia, 1997)' _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0522P)^2^+1.3806P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5505 _refine_ls_number_parameters 377 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0613 _refine_ls_R_factor_gt 0.0414 _refine_ls_wR_factor_ref 0.1158 _refine_ls_wR_factor_gt 0.1021 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _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 C2 C 0.3519(3) 0.92517(18) 0.43239(17) 0.0244(5) Uani 1 1 d . . . H2 H 0.3939 0.9920 0.4207 0.029 Uiso 1 1 calc R . . C3 C 0.2115(3) 0.9121(2) 0.50564(19) 0.0299(6) Uani 1 1 d . . . H3 H 0.1561 0.9692 0.5420 0.036 Uiso 1 1 calc R . . C4 C 0.1546(3) 0.8159(2) 0.52451(17) 0.0271(6) Uani 1 1 d . . . H4 H 0.0599 0.8052 0.5753 0.033 Uiso 1 1 calc R . . C5 C 0.1818(3) 0.63087(19) 0.49192(17) 0.0250(5) Uani 1 1 d . . . H5 H 0.0853 0.6204 0.5416 0.030 Uiso 1 1 calc R . . C6 C 0.2672(3) 0.54949(19) 0.44327(18) 0.0258(5) Uani 1 1 d . . . H6 H 0.2338 0.4818 0.4606 0.031 Uiso 1 1 calc R . . C7 C 0.4054(3) 0.56572(18) 0.36699(17) 0.0230(5) Uani 1 1 d . . . H7 H 0.4650 0.5073 0.3352 0.028 Uiso 1 1 calc R . . C8 C 0.4605(3) 0.66260(17) 0.33503(16) 0.0190(5) Uani 1 1 d . . . C9 C 0.3766(3) 0.74687(17) 0.39129(16) 0.0178(5) Uani 1 1 d . . . C10 C 0.2360(3) 0.73157(18) 0.46877(16) 0.0213(5) Uani 1 1 d . . . C11 C 0.5432(3) 0.71698(17) 0.14447(16) 0.0196(5) Uani 1 1 d . . . C12 C 0.3818(3) 0.72388(17) 0.12828(17) 0.0215(5) Uani 1 1 d . . . C13 C 0.3525(3) 0.78186(18) 0.05176(17) 0.0243(5) Uani 1 1 d . . . H13 H 0.2439 0.7850 0.0418 0.029 Uiso 1 1 calc R . . C14 C 0.4749(3) 0.83497(18) -0.01020(17) 0.0248(5) Uani 1 1 d . . . C15 C 0.6332(3) 0.82700(18) 0.00508(17) 0.0246(5) Uani 1 1 d . . . H15 H 0.7192 0.8630 -0.0363 0.029 Uiso 1 1 calc R . . C16 C 0.6702(3) 0.76841(18) 0.07852(16) 0.0205(5) Uani 1 1 d . . . C17 C 0.2403(3) 0.6638(2) 0.18682(19) 0.0276(6) Uani 1 1 d . . . H17A H 0.1455 0.6703 0.1577 0.041 Uiso 1 1 calc R . . H17B H 0.2090 0.6908 0.2529 0.041 Uiso 1 1 calc R . . H17C H 0.2747 0.5915 0.1878 0.041 Uiso 1 1 calc R . . C18 C 0.4388(4) 0.8992(2) -0.09082(19) 0.0349(6) Uani 1 1 d . . . H18A H 0.3362 0.8772 -0.1055 0.052 Uiso 1 1 calc R . . H18B H 0.5300 0.8906 -0.1483 0.052 Uiso 1 1 calc R . . H18C H 0.4266 0.9715 -0.0711 0.052 Uiso 1 1 calc R . . C19 C 0.8486(3) 0.7615(2) 0.08624(17) 0.0263(5) Uani 1 1 d . . . H19A H 0.8952 0.6928 0.0667 0.040 Uiso 1 1 calc R . . H19B H 0.8530 0.7748 0.1530 0.040 Uiso 1 1 calc R . . H19C H 0.9127 0.8125 0.0440 0.040 Uiso 1 1 calc R . . C20 C 0.7254(3) 0.57020(17) 0.21605(16) 0.0188(5) Uani 1 1 d . . . C21 C 0.7444(3) 0.49427(18) 0.14280(16) 0.0217(5) Uani 1 1 d . . . C22 C 0.8626(3) 0.41614(19) 0.13472(17) 0.0259(5) Uani 1 1 d . . . H22 H 0.8707 0.3653 0.0861 0.031 Uiso 1 1 calc R . . C23 C 0.9706(3) 0.40939(19) 0.19548(17) 0.0242(5) Uani 1 1 d . . . C24 C 0.9543(3) 0.48423(18) 0.26631(16) 0.0209(5) Uani 1 1 d . . . H24 H 1.0273 0.4817 0.3080 0.025 Uiso 1 1 calc R . . C25 C 0.8348(3) 0.56282(17) 0.27829(15) 0.0188(5) Uani 1 1 d . . . C26 C 0.6329(4) 0.4926(2) 0.0731(2) 0.0350(7) Uani 1 1 d . . . H26A H 0.6629 0.5473 0.0258 0.052 Uiso 1 1 calc R . . H26B H 0.5176 0.5032 0.1089 0.052 Uiso 1 1 calc R . . H26C H 0.6462 0.4262 0.0398 0.052 Uiso 1 1 calc R . . C27 C 1.1000(3) 0.3241(2) 0.1847(2) 0.0371(7) Uani 1 1 d . . . H27A H 1.1953 0.3404 0.1324 0.056 Uiso 1 1 calc R . . H27B H 1.0536 0.2598 0.1696 0.056 Uiso 1 1 calc R . . H27C H 1.1352 0.3166 0.2450 0.056 Uiso 1 1 calc R . . C28 C 0.8326(3) 0.64219(19) 0.35581(17) 0.0249(5) Uani 1 1 d . . . H28A H 0.9096 0.6202 0.3945 0.037 Uiso 1 1 calc R . . H28B H 0.7208 0.6496 0.3974 0.037 Uiso 1 1 calc R . . H28C H 0.8660 0.7081 0.3257 0.037 Uiso 1 1 calc R . . C29 C 0.5836(3) 0.87249(19) 0.30647(18) 0.0270(5) Uani 1 1 d . . . H29A H 0.5610 0.8786 0.2425 0.041 Uiso 1 1 calc R . . H29B H 0.6673 0.8179 0.3052 0.041 Uiso 1 1 calc R . . H29C H 0.6242 0.9375 0.3243 0.041 Uiso 1 1 calc R . . C30 C 0.5158(3) 0.25798(19) 0.32568(19) 0.0278(6) Uani 1 1 d . . . C31 C 0.1186(3) 0.9918(2) 0.20372(19) 0.0341(6) Uani 1 1 d . . . H31A H 0.1578 1.0532 0.2310 0.041 Uiso 1 1 calc R . . H31B H 0.2135 0.9596 0.1566 0.041 Uiso 1 1 calc R . . B1 B 0.5828(3) 0.6542(2) 0.23083(19) 0.0196(5) Uani 1 1 d . . . N1 N 0.4305(2) 0.84763(14) 0.37761(13) 0.0198(4) Uani 1 1 d . . . O1 O 0.2805(2) 0.13296(13) 0.33155(12) 0.0301(4) Uani 1 1 d . . . O2 O 0.3644(2) 0.16595(13) 0.47979(12) 0.0300(4) Uani 1 1 d . . . O3 O 0.2127(2) 0.29803(13) 0.41278(12) 0.0303(4) Uani 1 1 d . . . F1 F 0.57112(19) 0.33020(12) 0.37522(12) 0.0403(4) Uani 1 1 d . . . F2 F 0.49783(19) 0.30002(12) 0.24367(11) 0.0366(4) Uani 1 1 d . . . F3 F 0.63284(19) 0.18375(13) 0.30350(12) 0.0412(4) Uani 1 1 d . . . S1 S 0.32105(7) 0.20853(4) 0.39573(4) 0.02232(15) Uani 1 1 d . . . Cl1 Cl 0.04309(9) 0.90436(5) 0.29702(5) 0.03736(18) Uani 1 1 d . . . Cl2 Cl -0.03595(12) 1.02882(7) 0.14462(8) 0.0658(3) 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 C2 0.0305(13) 0.0185(12) 0.0272(13) -0.0069(10) -0.0135(11) 0.0039(10) C3 0.0295(14) 0.0292(14) 0.0313(14) -0.0145(11) -0.0091(11) 0.0084(11) C4 0.0221(12) 0.0371(15) 0.0212(12) -0.0094(11) -0.0041(10) 0.0046(11) C5 0.0193(12) 0.0344(14) 0.0205(12) 0.0006(10) -0.0027(10) -0.0050(10) C6 0.0238(13) 0.0250(13) 0.0290(13) 0.0035(10) -0.0062(10) -0.0068(10) C7 0.0229(12) 0.0208(12) 0.0248(12) -0.0048(10) -0.0052(10) 0.0004(9) C8 0.0173(11) 0.0196(11) 0.0207(12) -0.0041(9) -0.0056(9) -0.0016(9) C9 0.0178(11) 0.0184(11) 0.0187(11) -0.0014(9) -0.0073(9) -0.0007(9) C10 0.0179(11) 0.0287(13) 0.0181(11) -0.0037(10) -0.0059(9) 0.0002(9) C11 0.0204(12) 0.0184(11) 0.0193(11) -0.0082(9) -0.0033(9) -0.0001(9) C12 0.0208(12) 0.0192(12) 0.0237(12) -0.0107(9) -0.0039(10) 0.0005(9) C13 0.0223(12) 0.0251(13) 0.0265(13) -0.0117(10) -0.0084(10) 0.0046(10) C14 0.0309(13) 0.0236(12) 0.0201(12) -0.0083(10) -0.0073(10) 0.0057(10) C15 0.0267(13) 0.0258(13) 0.0182(12) -0.0054(10) 0.0001(10) -0.0001(10) C16 0.0206(12) 0.0223(12) 0.0175(11) -0.0071(9) -0.0029(9) 0.0010(9) C17 0.0188(12) 0.0315(14) 0.0332(14) -0.0035(11) -0.0071(10) -0.0035(10) C18 0.0421(16) 0.0368(15) 0.0271(14) -0.0028(12) -0.0118(12) 0.0062(12) C19 0.0196(12) 0.0345(14) 0.0236(13) -0.0001(11) -0.0020(10) -0.0050(10) C20 0.0179(11) 0.0209(12) 0.0165(11) -0.0031(9) -0.0015(9) -0.0032(9) C21 0.0226(12) 0.0245(12) 0.0188(11) -0.0047(9) -0.0063(9) 0.0003(10) C22 0.0300(13) 0.0270(13) 0.0201(12) -0.0101(10) -0.0054(10) 0.0030(10) C23 0.0222(12) 0.0272(13) 0.0209(12) -0.0028(10) -0.0009(10) 0.0019(10) C24 0.0186(11) 0.0284(13) 0.0164(11) 0.0005(9) -0.0050(9) -0.0046(9) C25 0.0180(11) 0.0226(12) 0.0146(11) -0.0020(9) -0.0006(9) -0.0067(9) C26 0.0422(16) 0.0321(15) 0.0362(15) -0.0194(12) -0.0221(13) 0.0118(12) C27 0.0368(16) 0.0403(16) 0.0342(15) -0.0093(12) -0.0104(12) 0.0130(13) C28 0.0233(12) 0.0302(13) 0.0224(12) -0.0069(10) -0.0077(10) -0.0029(10) C29 0.0311(14) 0.0218(12) 0.0255(13) -0.0032(10) -0.0009(11) -0.0084(10) C30 0.0266(13) 0.0257(13) 0.0337(14) -0.0040(11) -0.0124(11) 0.0000(10) C31 0.0323(15) 0.0367(15) 0.0332(15) -0.0090(12) -0.0068(12) -0.0075(12) B1 0.0166(13) 0.0189(13) 0.0236(13) -0.0085(10) -0.0044(10) -0.0080(10) N1 0.0222(10) 0.0188(10) 0.0191(10) -0.0049(8) -0.0064(8) -0.0004(8) O1 0.0407(11) 0.0243(9) 0.0296(10) -0.0067(7) -0.0161(8) -0.0088(8) O2 0.0405(11) 0.0264(9) 0.0259(9) -0.0037(7) -0.0131(8) -0.0021(8) O3 0.0298(10) 0.0310(10) 0.0300(10) -0.0090(8) -0.0074(8) 0.0030(8) F1 0.0393(9) 0.0340(9) 0.0558(10) -0.0025(7) -0.0261(8) -0.0125(7) F2 0.0331(8) 0.0434(9) 0.0338(9) 0.0083(7) -0.0085(7) -0.0074(7) F3 0.0308(8) 0.0470(10) 0.0446(10) -0.0067(8) -0.0079(7) 0.0102(7) S1 0.0266(3) 0.0205(3) 0.0212(3) -0.0058(2) -0.0084(2) -0.0020(2) Cl1 0.0417(4) 0.0361(4) 0.0363(4) -0.0032(3) -0.0129(3) -0.0048(3) Cl2 0.0688(6) 0.0573(5) 0.0903(7) 0.0304(5) -0.0532(5) -0.0275(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C2 N1 1.334(3) . ? C2 C3 1.385(4) . ? C2 H2 0.9500 . ? C3 C4 1.361(4) . ? C3 H3 0.9500 . ? C4 C10 1.414(3) . ? C4 H4 0.9500 . ? C5 C6 1.355(3) . ? C5 C10 1.417(3) . ? C5 H5 0.9500 . ? C6 C7 1.405(3) . ? C6 H6 0.9500 . ? C7 C8 1.398(3) . ? C7 H7 0.9500 . ? C8 C9 1.424(3) . ? C8 B1 1.592(3) . ? C9 N1 1.402(3) . ? C9 C10 1.425(3) . ? C11 C12 1.421(3) . ? C11 C16 1.424(3) . ? C11 B1 1.577(4) . ? C12 C13 1.396(3) . ? C12 C17 1.513(3) . ? C13 C14 1.384(4) . ? C13 H13 0.9500 . ? C14 C15 1.392(4) . ? C14 C18 1.508(3) . ? C15 C16 1.388(3) . ? C15 H15 0.9500 . ? C16 C19 1.519(3) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.420(3) . ? C20 C25 1.422(3) . ? C20 B1 1.569(3) . ? C21 C22 1.382(3) . ? C21 C26 1.519(3) . ? C22 C23 1.396(3) . ? C22 H22 0.9500 . ? C23 C24 1.388(3) . ? C23 C27 1.508(3) . ? C24 C25 1.389(3) . ? C24 H24 0.9500 . ? C25 C28 1.514(3) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 N1 1.474(3) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 F2 1.334(3) . ? C30 F3 1.336(3) . ? C30 F1 1.338(3) . ? C30 S1 1.828(3) . ? C31 Cl2 1.760(3) . ? C31 Cl1 1.766(3) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? O1 S1 1.4497(17) . ? O2 S1 1.4433(18) . ? O3 S1 1.4390(18) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C2 C3 122.6(2) . . ? N1 C2 H2 118.7 . . ? C3 C2 H2 118.7 . . ? C4 C3 C2 118.7(2) . . ? C4 C3 H3 120.7 . . ? C2 C3 H3 120.7 . . ? C3 C4 C10 120.3(2) . . ? C3 C4 H4 119.9 . . ? C10 C4 H4 119.9 . . ? C6 C5 C10 120.1(2) . . ? C6 C5 H5 120.0 . . ? C10 C5 H5 120.0 . . ? C5 C6 C7 119.7(2) . . ? C5 C6 H6 120.2 . . ? C7 C6 H6 120.2 . . ? C8 C7 C6 124.0(2) . . ? C8 C7 H7 118.0 . . ? C6 C7 H7 118.0 . . ? C7 C8 C9 115.5(2) . . ? C7 C8 B1 110.30(19) . . ? C9 C8 B1 133.0(2) . . ? N1 C9 C8 122.8(2) . . ? N1 C9 C10 116.19(19) . . ? C8 C9 C10 120.9(2) . . ? C4 C10 C5 120.1(2) . . ? C4 C10 C9 120.3(2) . . ? C5 C10 C9 119.6(2) . . ? C12 C11 C16 117.3(2) . . ? C12 C11 B1 122.1(2) . . ? C16 C11 B1 120.6(2) . . ? C13 C12 C11 119.9(2) . . ? C13 C12 C17 117.7(2) . . ? C11 C12 C17 122.3(2) . . ? C14 C13 C12 122.8(2) . . ? C14 C13 H13 118.6 . . ? C12 C13 H13 118.6 . . ? C13 C14 C15 117.2(2) . . ? C13 C14 C18 121.6(2) . . ? C15 C14 C18 121.1(2) . . ? C16 C15 C14 122.5(2) . . ? C16 C15 H15 118.8 . . ? C14 C15 H15 118.8 . . ? C15 C16 C11 120.3(2) . . ? C15 C16 C19 118.1(2) . . ? C11 C16 C19 121.5(2) . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C14 C18 H18A 109.5 . . ? C14 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C14 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 C25 117.1(2) . . ? C21 C20 B1 120.9(2) . . ? C25 C20 B1 121.89(19) . . ? C22 C21 C20 120.6(2) . . ? C22 C21 C26 117.3(2) . . ? C20 C21 C26 122.1(2) . . ? C21 C22 C23 122.2(2) . . ? C21 C22 H22 118.9 . . ? C23 C22 H22 118.9 . . ? C24 C23 C22 117.4(2) . . ? C24 C23 C27 121.2(2) . . ? C22 C23 C27 121.4(2) . . ? C23 C24 C25 122.2(2) . . ? C23 C24 H24 118.9 . . ? C25 C24 H24 118.9 . . ? C24 C25 C20 120.4(2) . . ? C24 C25 C28 117.5(2) . . ? C20 C25 C28 122.0(2) . . ? C21 C26 H26A 109.5 . . ? C21 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C21 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C27 H27A 109.5 . . ? C23 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C23 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N1 C29 H29A 109.5 . . ? N1 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? N1 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? F2 C30 F3 108.0(2) . . ? F2 C30 F1 107.5(2) . . ? F3 C30 F1 107.6(2) . . ? F2 C30 S1 111.32(16) . . ? F3 C30 S1 111.37(17) . . ? F1 C30 S1 110.90(18) . . ? Cl2 C31 Cl1 111.09(15) . . ? Cl2 C31 H31A 109.4 . . ? Cl1 C31 H31A 109.4 . . ? Cl2 C31 H31B 109.4 . . ? Cl1 C31 H31B 109.4 . . ? H31A C31 H31B 108.0 . . ? C20 B1 C11 122.4(2) . . ? C20 B1 C8 116.9(2) . . ? C11 B1 C8 120.0(2) . . ? C2 N1 C9 121.9(2) . . ? C2 N1 C29 116.3(2) . . ? C9 N1 C29 121.72(18) . . ? O3 S1 O2 115.55(10) . . ? O3 S1 O1 114.79(11) . . ? O2 S1 O1 114.33(10) . . ? O3 S1 C30 103.31(11) . . ? O2 S1 C30 103.40(11) . . ? O1 S1 C30 103.13(11) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.37 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.605 _refine_diff_density_min -0.737 _refine_diff_density_rms 0.057 _exptl_crystal_recrystallization_method 'CH2Cl2 evaporation' #===END data_chloro[8-(dimesitylboryl)quinoline-kN]copper(I) _database_code_depnum_ccdc_archive 'CCDC 758515' _audit_creation_method SHELXL-97 _chemical_name_systematic chloro[8-(dimesitylboryl)quinoline-kN]copper(I) _chemical_name_common chloro(8-(dimesitylboryl)quinoline-kN)copper(i) _chemical_melting_point 495 _chemical_formula_moiety 'C54 H56 B2 Cl2 Cu2 N2' _chemical_formula_sum 'C54 H56 B2 Cl2 Cu2 N2' _chemical_formula_weight 952.61 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 _symmetry_space_group_name_hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.9701(7) _cell_length_b 10.7170(8) _cell_length_c 12.9059(9) _cell_angle_alpha 104.3880(10) _cell_angle_beta 100.9430(10) _cell_angle_gamma 101.1020(10) _cell_volume 1141.81(15) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7469 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 25.46 _exptl_crystal_description block _exptl_crystal_colour red-orange _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.385 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 496 _exptl_absorpt_coefficient_mu 1.088 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5963 _exptl_absorpt_correction_T_max 0.7802 _exptl_absorpt_process_details '(SADABS; Bruker, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type 'Bruker SMART APEXII' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEXII' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11413 _diffrn_reflns_av_R_equivalents 0.0246 _diffrn_reflns_av_sigmaI/netI 0.0289 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 25.36 _reflns_number_total 4159 _reflns_number_gt 3596 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2006)' _computing_cell_refinement 'SAINT (Bruker, 2006)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 (Farrugia, 1997)' _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0457P)^2^+0.9325P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4159 _refine_ls_number_parameters 286 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0396 _refine_ls_R_factor_gt 0.0318 _refine_ls_wR_factor_ref 0.0875 _refine_ls_wR_factor_gt 0.0829 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _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 C2 C 0.1738(3) 0.0981(3) -0.0300(2) 0.0247(5) Uani 1 1 d . . . H2 H 0.1902 0.0161 -0.0686 0.030 Uiso 1 1 calc R . . C3 C 0.0308(3) 0.1276(3) -0.0664(2) 0.0268(6) Uani 1 1 d . . . H3 H -0.0474 0.0665 -0.1277 0.032 Uiso 1 1 calc R . . C4 C 0.0059(3) 0.2449(3) -0.0126(2) 0.0233(5) Uani 1 1 d . . . H4 H -0.0903 0.2665 -0.0361 0.028 Uiso 1 1 calc R . . C5 C 0.1065(3) 0.4597(3) 0.1363(2) 0.0250(5) Uani 1 1 d . . . H5 H 0.0116 0.4847 0.1160 0.030 Uiso 1 1 calc R . . C6 C 0.2257(3) 0.5443(3) 0.2212(2) 0.0257(5) Uani 1 1 d . . . H6 H 0.2140 0.6283 0.2597 0.031 Uiso 1 1 calc R . . C7 C 0.3668(3) 0.5076(2) 0.2520(2) 0.0210(5) Uani 1 1 d . . . H7 H 0.4495 0.5694 0.3100 0.025 Uiso 1 1 calc R . . C8 C 0.3897(3) 0.3856(2) 0.20159(19) 0.0176(5) Uani 1 1 d . . . C9 C 0.2656(3) 0.2978(2) 0.11076(19) 0.0178(5) Uani 1 1 d . . . C10 C 0.1235(3) 0.3344(2) 0.07809(19) 0.0203(5) Uani 1 1 d . . . C11 C 0.6971(3) 0.4760(2) 0.29122(19) 0.0171(5) Uani 1 1 d . . . C12 C 0.7771(3) 0.5259(2) 0.40420(19) 0.0185(5) Uani 1 1 d . . . C13 C 0.8998(3) 0.6409(2) 0.4413(2) 0.0211(5) Uani 1 1 d . . . H13 H 0.9511 0.6745 0.5177 0.025 Uiso 1 1 calc R . . C14 C 0.9493(3) 0.7077(2) 0.3695(2) 0.0221(5) Uani 1 1 d . . . C15 C 0.8715(3) 0.6577(2) 0.2588(2) 0.0213(5) Uani 1 1 d . . . H15 H 0.9047 0.7018 0.2086 0.026 Uiso 1 1 calc R . . C16 C 0.7460(3) 0.5447(2) 0.21859(19) 0.0184(5) Uani 1 1 d . . . C17 C 0.7309(3) 0.4583(2) 0.4875(2) 0.0235(5) Uani 1 1 d . . . H17A H 0.7951 0.5102 0.5617 0.035 Uiso 1 1 calc R . . H17B H 0.7478 0.3686 0.4695 0.035 Uiso 1 1 calc R . . H17C H 0.6199 0.4525 0.4851 0.035 Uiso 1 1 calc R . . C18 C 1.0814(3) 0.8329(3) 0.4111(2) 0.0321(6) Uani 1 1 d . . . H18A H 1.0978 0.8667 0.3492 0.048 Uiso 1 1 calc R . . H18B H 1.1777 0.8130 0.4453 0.048 Uiso 1 1 calc R . . H18C H 1.0543 0.9004 0.4660 0.048 Uiso 1 1 calc R . . C19 C 0.6656(3) 0.4983(3) 0.0971(2) 0.0268(6) Uani 1 1 d . . . H19A H 0.5655 0.5232 0.0859 0.040 Uiso 1 1 calc R . . H19B H 0.6463 0.4013 0.0694 0.040 Uiso 1 1 calc R . . H19C H 0.7327 0.5402 0.0570 0.040 Uiso 1 1 calc R . . C20 C 0.5591(3) 0.2162(2) 0.27118(18) 0.0159(5) Uani 1 1 d . . . C21 C 0.6951(3) 0.1654(2) 0.26235(18) 0.0176(5) Uani 1 1 d . . . C22 C 0.7080(3) 0.0498(2) 0.29111(19) 0.0213(5) Uani 1 1 d . . . H22 H 0.7971 0.0165 0.2827 0.026 Uiso 1 1 calc R . . C23 C 0.5958(3) -0.0180(2) 0.33132(19) 0.0210(5) Uani 1 1 d . . . C24 C 0.4669(3) 0.0334(2) 0.34440(19) 0.0203(5) Uani 1 1 d . . . H24 H 0.3917 -0.0096 0.3754 0.024 Uiso 1 1 calc R . . C25 C 0.4440(3) 0.1447(2) 0.31393(19) 0.0179(5) Uani 1 1 d . . . C26 C 0.8360(3) 0.2401(2) 0.2335(2) 0.0210(5) Uani 1 1 d . . . H26A H 0.8954 0.3166 0.2971 0.032 Uiso 1 1 calc R . . H26B H 0.7998 0.2712 0.1702 0.032 Uiso 1 1 calc R . . H26C H 0.9035 0.1805 0.2147 0.032 Uiso 1 1 calc R . . C27 C 0.6104(3) -0.1440(3) 0.3590(2) 0.0325(6) Uani 1 1 d . . . H27A H 0.5405 -0.1623 0.4062 0.049 Uiso 1 1 calc R . . H27B H 0.7190 -0.1337 0.3981 0.049 Uiso 1 1 calc R . . H27C H 0.5813 -0.2182 0.2908 0.049 Uiso 1 1 calc R . . C28 C 0.3000(3) 0.1913(2) 0.3340(2) 0.0228(5) Uani 1 1 d . . . H28A H 0.2491 0.1406 0.3768 0.034 Uiso 1 1 calc R . . H28B H 0.2266 0.1772 0.2629 0.034 Uiso 1 1 calc R . . H28C H 0.3311 0.2862 0.3750 0.034 Uiso 1 1 calc R . . B1 B 0.5488(3) 0.3528(3) 0.2495(2) 0.0183(5) Uani 1 1 d . . . N1 N 0.2874(2) 0.17843(19) 0.05535(16) 0.0198(4) Uani 1 1 d . . . Cl1 Cl 0.60750(6) 0.12061(5) -0.04608(5) 0.01994(14) Uani 1 1 d . . . Cu1 Cu 0.48449(3) 0.11710(3) 0.09867(2) 0.01963(10) 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 C2 0.0224(13) 0.0239(13) 0.0256(13) 0.0067(11) 0.0036(10) 0.0039(10) C3 0.0187(12) 0.0330(14) 0.0257(13) 0.0134(11) -0.0006(10) -0.0003(11) C4 0.0123(11) 0.0341(14) 0.0279(13) 0.0181(11) 0.0052(10) 0.0041(10) C5 0.0192(12) 0.0322(14) 0.0331(14) 0.0168(12) 0.0115(11) 0.0142(11) C6 0.0278(13) 0.0243(13) 0.0313(14) 0.0105(11) 0.0120(11) 0.0135(11) C7 0.0193(12) 0.0201(12) 0.0253(13) 0.0093(10) 0.0070(10) 0.0046(10) C8 0.0155(11) 0.0206(12) 0.0204(12) 0.0100(10) 0.0089(9) 0.0035(9) C9 0.0144(11) 0.0220(12) 0.0218(12) 0.0120(10) 0.0073(9) 0.0054(9) C10 0.0154(11) 0.0267(13) 0.0228(12) 0.0135(10) 0.0079(10) 0.0039(10) C11 0.0136(11) 0.0178(11) 0.0223(12) 0.0077(9) 0.0047(9) 0.0072(9) C12 0.0161(11) 0.0204(12) 0.0214(12) 0.0068(10) 0.0057(9) 0.0086(9) C13 0.0177(12) 0.0224(12) 0.0209(12) 0.0028(10) 0.0015(10) 0.0080(10) C14 0.0148(11) 0.0182(12) 0.0311(13) 0.0041(10) 0.0046(10) 0.0044(9) C15 0.0178(12) 0.0207(12) 0.0299(13) 0.0121(10) 0.0087(10) 0.0061(10) C16 0.0141(11) 0.0198(12) 0.0221(12) 0.0073(10) 0.0035(9) 0.0056(9) C17 0.0213(12) 0.0275(13) 0.0221(12) 0.0080(10) 0.0052(10) 0.0065(10) C18 0.0254(14) 0.0240(14) 0.0385(16) 0.0036(12) 0.0045(12) -0.0018(11) C19 0.0208(13) 0.0334(15) 0.0242(13) 0.0142(11) 0.0010(10) -0.0009(11) C20 0.0136(11) 0.0175(11) 0.0142(11) 0.0021(9) 0.0023(9) 0.0032(9) C21 0.0146(11) 0.0198(12) 0.0150(11) 0.0011(9) 0.0030(9) 0.0023(9) C22 0.0203(12) 0.0227(13) 0.0216(12) 0.0038(10) 0.0053(10) 0.0101(10) C23 0.0253(13) 0.0170(12) 0.0194(12) 0.0036(9) 0.0037(10) 0.0062(10) C24 0.0198(12) 0.0189(12) 0.0220(12) 0.0065(10) 0.0065(10) 0.0023(10) C25 0.0154(11) 0.0188(12) 0.0185(11) 0.0033(9) 0.0049(9) 0.0043(9) C26 0.0128(11) 0.0250(13) 0.0244(12) 0.0053(10) 0.0057(10) 0.0044(10) C27 0.0372(15) 0.0232(14) 0.0442(17) 0.0145(12) 0.0158(13) 0.0126(12) C28 0.0188(12) 0.0241(13) 0.0319(14) 0.0141(11) 0.0119(10) 0.0072(10) B1 0.0175(13) 0.0214(14) 0.0163(13) 0.0042(10) 0.0067(10) 0.0046(11) N1 0.0177(10) 0.0219(10) 0.0188(10) 0.0056(8) 0.0041(8) 0.0035(8) Cl1 0.0157(3) 0.0208(3) 0.0213(3) 0.0031(2) 0.0065(2) 0.0022(2) Cu1 0.01537(16) 0.02146(17) 0.02129(17) 0.00391(12) 0.00539(12) 0.00527(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C2 N1 1.325(3) . ? C2 C3 1.402(4) . ? C2 H2 0.9500 . ? C3 C4 1.359(4) . ? C3 H3 0.9500 . ? C4 C10 1.410(3) . ? C4 H4 0.9500 . ? C5 C6 1.362(4) . ? C5 C10 1.418(3) . ? C5 H5 0.9500 . ? C6 C7 1.412(3) . ? C6 H6 0.9500 . ? C7 C8 1.381(3) . ? C7 H7 0.9500 . ? C8 C9 1.433(3) . ? C8 B1 1.584(3) . ? C9 N1 1.371(3) . ? C9 C10 1.424(3) . ? C11 C16 1.410(3) . ? C11 C12 1.412(3) . ? C11 B1 1.581(3) . ? C12 C13 1.394(3) . ? C12 C17 1.514(3) . ? C13 C14 1.389(3) . ? C13 H13 0.9500 . ? C14 C15 1.383(4) . ? C14 C18 1.511(3) . ? C15 C16 1.395(3) . ? C15 H15 0.9500 . ? C16 C19 1.507(3) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.441(3) . ? C20 C25 1.442(3) . ? C20 B1 1.573(3) . ? C20 Cu1 2.126(2) . ? C21 C22 1.397(3) . ? C21 C26 1.521(3) . ? C21 Cu1 2.422(2) . ? C22 C23 1.384(3) . ? C22 H22 0.9500 . ? C23 C24 1.394(3) . ? C23 C27 1.503(3) . ? C24 C25 1.384(3) . ? C24 H24 0.9500 . ? C25 C28 1.515(3) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? B1 Cu1 2.660(3) . ? N1 Cu1 2.031(2) . ? Cl1 Cu1 2.3474(6) . ? Cl1 Cu1 2.3979(6) 2_655 ? Cu1 Cl1 2.3979(6) 2_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C2 C3 123.6(2) . . ? N1 C2 H2 118.2 . . ? C3 C2 H2 118.2 . . ? C4 C3 C2 119.0(2) . . ? C4 C3 H3 120.5 . . ? C2 C3 H3 120.5 . . ? C3 C4 C10 119.7(2) . . ? C3 C4 H4 120.2 . . ? C10 C4 H4 120.2 . . ? C6 C5 C10 120.2(2) . . ? C6 C5 H5 119.9 . . ? C10 C5 H5 119.9 . . ? C5 C6 C7 120.2(2) . . ? C5 C6 H6 119.9 . . ? C7 C6 H6 119.9 . . ? C8 C7 C6 122.8(2) . . ? C8 C7 H7 118.6 . . ? C6 C7 H7 118.6 . . ? C7 C8 C9 117.0(2) . . ? C7 C8 B1 117.8(2) . . ? C9 C8 B1 125.3(2) . . ? N1 C9 C10 120.8(2) . . ? N1 C9 C8 118.5(2) . . ? C10 C9 C8 120.6(2) . . ? C4 C10 C5 122.6(2) . . ? C4 C10 C9 118.3(2) . . ? C5 C10 C9 119.1(2) . . ? C16 C11 C12 118.2(2) . . ? C16 C11 B1 121.1(2) . . ? C12 C11 B1 120.6(2) . . ? C13 C12 C11 120.0(2) . . ? C13 C12 C17 118.7(2) . . ? C11 C12 C17 121.3(2) . . ? C14 C13 C12 121.8(2) . . ? C14 C13 H13 119.1 . . ? C12 C13 H13 119.1 . . ? C15 C14 C13 118.0(2) . . ? C15 C14 C18 120.8(2) . . ? C13 C14 C18 121.2(2) . . ? C14 C15 C16 122.0(2) . . ? C14 C15 H15 119.0 . . ? C16 C15 H15 119.0 . . ? C15 C16 C11 120.0(2) . . ? C15 C16 C19 118.7(2) . . ? C11 C16 C19 121.3(2) . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C14 C18 H18A 109.5 . . ? C14 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C14 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 C25 116.6(2) . . ? C21 C20 B1 121.0(2) . . ? C25 C20 B1 122.00(19) . . ? C21 C20 Cu1 83.15(13) . . ? C25 C20 Cu1 102.77(15) . . ? B1 C20 Cu1 90.69(14) . . ? C22 C21 C20 120.0(2) . . ? C22 C21 C26 117.2(2) . . ? C20 C21 C26 122.5(2) . . ? C22 C21 Cu1 111.19(15) . . ? C20 C21 Cu1 60.63(12) . . ? C26 C21 Cu1 103.39(14) . . ? C23 C22 C21 122.5(2) . . ? C23 C22 H22 118.7 . . ? C21 C22 H22 118.7 . . ? C22 C23 C24 117.8(2) . . ? C22 C23 C27 121.5(2) . . ? C24 C23 C27 120.7(2) . . ? C25 C24 C23 122.6(2) . . ? C25 C24 H24 118.7 . . ? C23 C24 H24 118.7 . . ? C24 C25 C20 120.3(2) . . ? C24 C25 C28 117.2(2) . . ? C20 C25 C28 122.4(2) . . ? C21 C26 H26A 109.5 . . ? C21 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C21 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C27 H27A 109.5 . . ? C23 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C23 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C20 B1 C11 121.0(2) . . ? C20 B1 C8 123.9(2) . . ? C11 B1 C8 114.5(2) . . ? C20 B1 Cu1 53.05(11) . . ? C11 B1 Cu1 132.26(16) . . ? C8 B1 Cu1 94.46(14) . . ? C2 N1 C9 118.6(2) . . ? C2 N1 Cu1 118.13(16) . . ? C9 N1 Cu1 123.25(15) . . ? Cu1 Cl1 Cu1 84.72(2) . 2_655 ? N1 Cu1 C20 101.36(8) . . ? N1 Cu1 Cl1 104.68(6) . . ? C20 Cu1 Cl1 132.45(6) . . ? N1 Cu1 Cl1 103.75(6) . 2_655 ? C20 Cu1 Cl1 116.19(6) . 2_655 ? Cl1 Cu1 Cl1 95.28(2) . 2_655 ? N1 Cu1 C21 137.18(8) . . ? C20 Cu1 C21 36.22(8) . . ? Cl1 Cu1 C21 105.48(6) . . ? Cl1 Cu1 C21 102.96(6) 2_655 . ? N1 Cu1 B1 78.39(8) . . ? C20 Cu1 B1 36.26(8) . . ? Cl1 Cu1 B1 113.56(6) . . ? Cl1 Cu1 B1 149.79(6) 2_655 . ? C21 Cu1 B1 61.97(8) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.36 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.449 _refine_diff_density_min -0.303 _refine_diff_density_rms 0.065 _exptl_crystal_recrystallization_method CH2Cl2/Pentane #===END data_8-(dimesitylboryl)quinoline_2 _database_code_depnum_ccdc_archive 'CCDC 759392' _audit_creation_method SHELXL-97 _chemical_name_systematic 8-(dimesitylboryl)quinoline _chemical_name_common 8-(dimesitylboryl)quinoline _chemical_melting_point 438 _chemical_formula_moiety 'C27 H28 B N' _chemical_formula_sum 'C27 H28 B N' _chemical_formula_weight 377.31 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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c n' _symmetry_int_tables_number 60 _symmetry_space_group_name_hall '-P 2n 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y, z-1/2' _cell_length_a 12.9460(15) _cell_length_b 10.6126(13) _cell_length_c 15.6759(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2153.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9921 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 25.78 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 1.00 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.164 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 808 _exptl_absorpt_coefficient_mu 0.066 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9371 _exptl_absorpt_correction_T_max 0.9857 _exptl_absorpt_process_details '(SADABS; Bruker, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type 'Bruker SMART APEXII' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEXII' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18703 _diffrn_reflns_av_R_equivalents 0.0407 _diffrn_reflns_av_sigmaI/netI 0.0222 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.48 _diffrn_reflns_theta_max 25.80 _reflns_number_total 2068 _reflns_number_gt 1617 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2006)' _computing_cell_refinement 'SAINT (Bruker, 2006)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 (Farrugia, 1997)' _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0297P)^2^+3.1984P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2068 _refine_ls_number_parameters 161 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0943 _refine_ls_R_factor_gt 0.0736 _refine_ls_wR_factor_ref 0.1802 _refine_ls_wR_factor_gt 0.1684 _refine_ls_goodness_of_fit_ref 1.274 _refine_ls_restrained_S_all 1.274 _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 B1 B 0.0000 -0.1441(5) 0.7500 0.0429(13) Uani 1 2 d S . . C8 C 0.0091(4) -0.0015(5) 0.7918(4) 0.0269(9) Uani 0.50 1 d P A -1 C7 C 0.0308(5) 0.0248(6) 0.8732(5) 0.0300(16) Uani 0.50 1 d P A -1 H7 H 0.0342 -0.0410 0.9141 0.036 Uiso 0.50 1 calc PR A -1 C6 C 0.0495(14) 0.1582(13) 0.8996(12) 0.0352(10) Uani 0.50 1 d P A -1 H6 H 0.0699 0.1756 0.9566 0.042 Uiso 0.50 1 calc PR A -1 C5 C 0.0390(6) 0.2473(8) 0.8482(6) 0.0354(18) Uani 0.50 1 d P A -1 H5 H 0.0514 0.3309 0.8674 0.042 Uiso 0.50 1 calc PR A -1 C4 C -0.0097(4) 0.3265(5) 0.7046(4) 0.0352(10) Uani 0.50 1 d P A -1 H4 H -0.0023 0.4122 0.7213 0.042 Uiso 0.50 1 calc PR A -1 C3 C -0.0387(6) 0.2963(8) 0.6249(6) 0.0369(18) Uani 0.50 1 d P A -1 H3 H -0.0529 0.3621 0.5855 0.044 Uiso 0.50 1 calc PR A -1 C2 C -0.0495(15) 0.1626(19) 0.5960(10) 0.048(2) Uani 0.50 1 d P A -1 H2 H -0.0683 0.1435 0.5389 0.057 Uiso 0.50 1 calc PR A -1 N1 N -0.0326(5) 0.0744(6) 0.6501(5) 0.0352(10) Uani 0.50 1 d P A -1 C9 C -0.0030(8) 0.1008(5) 0.7323(3) 0.0205(17) Uani 0.50 1 d P A -1 C10 C 0.0097(6) 0.2279(4) 0.7633(5) 0.0269(9) Uani 0.50 1 d P A -1 C11 C 0.0703(2) -0.2163(3) 0.6853(2) 0.0370(7) Uani 1 1 d . A . C12 C 0.1772(2) -0.1891(3) 0.6781(2) 0.0374(7) Uani 1 1 d . . . C13 C 0.2390(2) -0.2593(3) 0.62318(19) 0.0412(8) Uani 1 1 d . A . H13 H 0.3104 -0.2396 0.6194 0.049 Uiso 1 1 calc R . . C14 C 0.2004(2) -0.3563(3) 0.5740(2) 0.0432(8) Uani 1 1 d . . . C15 C 0.0949(2) -0.3829(3) 0.5805(2) 0.0445(8) Uani 1 1 d . A . H15 H 0.0666 -0.4492 0.5472 0.053 Uiso 1 1 calc R . . C16 C 0.0304(2) -0.3146(3) 0.6345(2) 0.0396(7) Uani 1 1 d . . . C17 C 0.2278(2) -0.0862(3) 0.7313(2) 0.0464(8) Uani 1 1 d . A . H17A H 0.1953 -0.0050 0.7184 0.070 Uiso 1 1 calc R . . H17B H 0.3016 -0.0821 0.7178 0.070 Uiso 1 1 calc R . . H17C H 0.2189 -0.1053 0.7921 0.070 Uiso 1 1 calc R . . C18 C 0.2691(3) -0.4315(4) 0.5152(2) 0.0555(10) Uani 1 1 d . A . H18A H 0.3415 -0.4098 0.5260 0.083 Uiso 0.50 1 calc PR . . H18B H 0.2517 -0.4118 0.4558 0.083 Uiso 0.50 1 calc PR . . H18C H 0.2585 -0.5217 0.5255 0.083 Uiso 0.50 1 calc PR . . H18D H 0.2264 -0.4857 0.4788 0.083 Uiso 0.50 1 calc PR . . H18E H 0.3161 -0.4837 0.5491 0.083 Uiso 0.50 1 calc PR . . H18F H 0.3093 -0.3739 0.4793 0.083 Uiso 0.50 1 calc PR . . C19 C -0.0845(2) -0.3473(4) 0.6346(2) 0.0509(9) Uani 1 1 d . A . H19A H -0.1009 -0.3974 0.5838 0.076 Uiso 1 1 calc R . . H19B H -0.1253 -0.2695 0.6340 0.076 Uiso 1 1 calc R . . H19C H -0.1010 -0.3959 0.6859 0.076 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 B1 0.022(2) 0.024(3) 0.082(4) 0.000 -0.010(2) 0.000 C8 0.020(2) 0.0239(19) 0.037(3) 0.0014(18) -0.0005(17) -0.0007(17) C7 0.029(3) 0.015(3) 0.046(4) -0.004(3) -0.003(3) -0.005(3) C6 0.0269(19) 0.018(2) 0.061(3) 0.002(2) -0.0008(19) 0.0008(16) C5 0.029(3) 0.024(5) 0.053(6) -0.011(4) 0.005(3) -0.006(3) C4 0.0269(19) 0.018(2) 0.061(3) 0.002(2) -0.0008(19) 0.0008(16) C3 0.029(3) 0.029(5) 0.053(5) 0.008(3) -0.001(3) 0.000(3) C2 0.036(4) 0.086(7) 0.021(4) 0.025(4) -0.006(3) 0.006(4) N1 0.0269(19) 0.018(2) 0.061(3) 0.002(2) -0.0008(19) 0.0008(16) C9 0.017(2) 0.034(3) 0.011(5) 0.0037(19) -0.005(5) -0.002(3) C10 0.020(2) 0.0239(19) 0.037(3) 0.0014(18) -0.0005(17) -0.0007(17) C11 0.0290(14) 0.0339(16) 0.0480(18) 0.0154(14) -0.0054(13) -0.0034(12) C12 0.0293(14) 0.0368(17) 0.0461(18) 0.0136(14) -0.0039(13) -0.0033(12) C13 0.0280(14) 0.0476(19) 0.0479(18) 0.0113(16) -0.0027(14) -0.0042(13) C14 0.0373(16) 0.048(2) 0.0446(18) 0.0111(16) 0.0018(14) -0.0003(14) C15 0.0390(17) 0.0466(19) 0.0479(19) 0.0022(16) 0.0011(14) -0.0081(15) C16 0.0324(15) 0.0388(18) 0.0475(18) 0.0087(15) -0.0005(14) -0.0047(13) C17 0.0301(16) 0.050(2) 0.059(2) 0.0056(17) -0.0037(14) -0.0024(14) C18 0.0428(19) 0.070(3) 0.053(2) 0.0002(19) 0.0061(16) 0.0001(18) C19 0.0328(16) 0.057(2) 0.063(2) -0.0117(19) 0.0031(16) -0.0115(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B1 C11 1.564(4) . ? B1 C11 1.564(4) 4_556 ? B1 C8 1.653(7) . ? B1 C8 1.653(7) 4_556 ? C8 C7 1.336(9) . ? C8 C9 1.439(7) . ? C7 C6 1.495(16) . ? C7 H7 0.9500 . ? C6 C5 1.25(2) . ? C6 H6 0.9500 . ? C5 C10 1.400(11) . ? C5 H5 0.9500 . ? C4 C3 1.345(11) . ? C4 C10 1.415(8) . ? C4 H4 0.9500 . ? C3 C2 1.50(2) . ? C3 H3 0.9500 . ? C2 N1 1.282(18) . ? C2 H2 0.9500 . ? N1 C9 1.373(8) . ? C9 C10 1.443(7) . ? C11 C16 1.411(4) . ? C11 C12 1.417(4) . ? C12 C13 1.392(4) . ? C12 C17 1.522(4) . ? C13 C14 1.380(5) . ? C13 H13 0.9500 . ? C14 C15 1.398(4) . ? C14 C18 1.509(5) . ? C15 C16 1.393(5) . ? C15 H15 0.9500 . ? C16 C19 1.527(4) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C18 H18D 0.9800 . ? C18 H18E 0.9800 . ? C18 H18F 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 B1 C11 121.3(4) . 4_556 ? C11 B1 C8 131.6(3) . . ? C11 B1 C8 103.5(2) 4_556 . ? C11 B1 C8 103.5(2) . 4_556 ? C11 B1 C8 131.6(3) 4_556 4_556 ? C8 B1 C8 47.4(4) . 4_556 ? C7 C8 C9 118.9(5) . . ? C7 C8 B1 125.8(5) . . ? C9 C8 B1 115.2(4) . . ? C8 C7 C6 119.8(9) . . ? C8 C7 H7 120.1 . . ? C6 C7 H7 120.1 . . ? C5 C6 C7 121.3(14) . . ? C5 C6 H6 119.3 . . ? C7 C6 H6 119.3 . . ? C6 C5 C10 122.1(10) . . ? C6 C5 H5 118.9 . . ? C10 C5 H5 118.9 . . ? C3 C4 C10 118.5(6) . . ? C3 C4 H4 120.7 . . ? C10 C4 H4 120.7 . . ? C4 C3 C2 122.2(9) . . ? C4 C3 H3 118.9 . . ? C2 C3 H3 118.9 . . ? N1 C2 C3 118.5(13) . . ? N1 C2 H2 120.7 . . ? C3 C2 H2 120.7 . . ? C2 N1 C9 121.2(10) . . ? N1 C9 C8 118.9(5) . . ? N1 C9 C10 122.6(5) . . ? C8 C9 C10 118.4(4) . . ? C5 C10 C4 123.8(6) . . ? C5 C10 C9 119.2(5) . . ? C4 C10 C9 116.9(5) . . ? C16 C11 C12 117.6(3) . . ? C16 C11 B1 121.0(2) . . ? C12 C11 B1 121.3(3) . . ? C13 C12 C11 120.1(3) . . ? C13 C12 C17 118.4(3) . . ? C11 C12 C17 121.5(3) . . ? C14 C13 C12 122.5(3) . . ? C14 C13 H13 118.8 . . ? C12 C13 H13 118.8 . . ? C13 C14 C15 117.6(3) . . ? C13 C14 C18 121.5(3) . . ? C15 C14 C18 120.9(3) . . ? C16 C15 C14 121.7(3) . . ? C16 C15 H15 119.2 . . ? C14 C15 H15 119.2 . . ? C15 C16 C11 120.5(3) . . ? C15 C16 C19 117.8(3) . . ? C11 C16 C19 121.6(3) . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C14 C18 H18A 109.5 . . ? C14 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C14 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C14 C18 H18D 109.5 . . ? H18A C18 H18D 141.1 . . ? H18B C18 H18D 56.3 . . ? H18C C18 H18D 56.3 . . ? C14 C18 H18E 109.5 . . ? H18A C18 H18E 56.3 . . ? H18B C18 H18E 141.1 . . ? H18C C18 H18E 56.3 . . ? H18D C18 H18E 109.5 . . ? C14 C18 H18F 109.5 . . ? H18A C18 H18F 56.3 . . ? H18B C18 H18F 56.3 . . ? H18C C18 H18F 141.1 . . ? H18D C18 H18F 109.5 . . ? H18E C18 H18F 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C11 B1 C8 C7 -110.4(6) . . . . ? C11 B1 C8 C7 47.7(6) 4_556 . . . ? C8 B1 C8 C7 -177.3(9) 4_556 . . . ? C11 B1 C8 C9 66.4(7) . . . . ? C11 B1 C8 C9 -135.5(6) 4_556 . . . ? C8 B1 C8 C9 -0.5(5) 4_556 . . . ? C9 C8 C7 C6 -4.4(12) . . . . ? B1 C8 C7 C6 172.3(9) . . . . ? C8 C7 C6 C5 4.6(19) . . . . ? C7 C6 C5 C10 0(2) . . . . ? C10 C4 C3 C2 -1.0(13) . . . . ? C4 C3 C2 N1 2(2) . . . . ? C3 C2 N1 C9 -2(2) . . . . ? C2 N1 C9 C8 176.4(12) . . . . ? C2 N1 C9 C10 0.8(17) . . . . ? C7 C8 C9 N1 -175.3(8) . . . . ? B1 C8 C9 N1 7.6(11) . . . . ? C7 C8 C9 C10 0.5(12) . . . . ? B1 C8 C9 C10 -176.6(7) . . . . ? C6 C5 C10 C4 175.6(11) . . . . ? C6 C5 C10 C9 -3.8(15) . . . . ? C3 C4 C10 C5 -179.2(9) . . . . ? C3 C4 C10 C9 0.3(11) . . . . ? N1 C9 C10 C5 179.3(9) . . . . ? C8 C9 C10 C5 3.7(13) . . . . ? N1 C9 C10 C4 -0.1(13) . . . . ? C8 C9 C10 C4 -175.8(8) . . . . ? C11 B1 C11 C16 49.3(2) 4_556 . . . ? C8 B1 C11 C16 -155.8(3) . . . . ? C8 B1 C11 C16 -111.6(3) 4_556 . . . ? C11 B1 C11 C12 -128.0(3) 4_556 . . . ? C8 B1 C11 C12 26.9(5) . . . . ? C8 B1 C11 C12 71.1(3) 4_556 . . . ? C16 C11 C12 C13 -0.7(4) . . . . ? B1 C11 C12 C13 176.7(3) . . . . ? C16 C11 C12 C17 -179.0(3) . . . . ? B1 C11 C12 C17 -1.7(4) . . . . ? C11 C12 C13 C14 0.0(5) . . . . ? C17 C12 C13 C14 178.4(3) . . . . ? C12 C13 C14 C15 0.3(5) . . . . ? C12 C13 C14 C18 -179.7(3) . . . . ? C13 C14 C15 C16 -0.1(5) . . . . ? C18 C14 C15 C16 180.0(3) . . . . ? C14 C15 C16 C11 -0.6(5) . . . . ? C14 C15 C16 C19 177.7(3) . . . . ? C12 C11 C16 C15 0.9(4) . . . . ? B1 C11 C16 C15 -176.4(3) . . . . ? C12 C11 C16 C19 -177.2(3) . . . . ? B1 C11 C16 C19 5.4(4) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.80 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.263 _refine_diff_density_min -0.220 _refine_diff_density_rms 0.047 _exptl_crystal_recrystallization_method 'hexane evaporation' #===END data_triflato[8-(dimesitylboryl)quinoline-kN]silver(I) _database_code_depnum_ccdc_archive 'CCDC 759393' _audit_creation_method SHELXL-97 _chemical_name_systematic 'triflato[8-(dimesitylboryl)quinoline-kN]silver(I) ' _chemical_name_common triflato(8-(dimesitylboryl)quinoline-kN)silver(i) _chemical_melting_point 483 _chemical_formula_moiety 'C56 H56 Ag2 B2 F6 N2 O6 S2, 2(C H2 Cl2)' _chemical_formula_sum 'C58 H60 Ag2 B2 Cl4 F6 N2 O6 S2' _chemical_formula_weight 1438.36 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_int_tables_number 14 _symmetry_space_group_name_hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.4365(9) _cell_length_b 11.5448(7) _cell_length_c 16.4696(9) _cell_angle_alpha 90.00 _cell_angle_beta 108.4000(10) _cell_angle_gamma 90.00 _cell_volume 2965.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9919 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 25.30 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.69 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.611 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1456 _exptl_absorpt_coefficient_mu 0.982 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5528 _exptl_absorpt_correction_T_max 0.8385 _exptl_absorpt_process_details '(SADABS; Bruker, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type 'Bruker SMART APEXII' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEXII' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29038 _diffrn_reflns_av_R_equivalents 0.0437 _diffrn_reflns_av_sigmaI/netI 0.0314 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 25.35 _reflns_number_total 5419 _reflns_number_gt 4539 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2006)' _computing_cell_refinement 'SAINT (Bruker, 2006)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 (Farrugia, 1997)' _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0357P)^2^+2.5641P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5419 _refine_ls_number_parameters 405 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0409 _refine_ls_R_factor_gt 0.0304 _refine_ls_wR_factor_ref 0.0743 _refine_ls_wR_factor_gt 0.0693 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.032 _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 Cl1 Cl 0.09951(11) 0.66213(15) 0.49445(11) 0.0598(6) Uani 0.744(4) 1 d PD A 1 C30 C 0.0504(3) 0.6987(4) 0.5727(4) 0.0457(14) Uani 0.744(4) 1 d PD A 1 H30A H -0.0127 0.7001 0.5462 0.055 Uiso 1 1 calc R A 1 H30B H 0.0647 0.6395 0.6186 0.055 Uiso 1 1 calc R A 1 Cl2 Cl 0.08669(16) 0.8362(2) 0.61684(16) 0.0462(5) Uani 0.744(4) 1 d PD A 1 Cl3 Cl 0.0510(3) 0.5868(5) 0.5511(5) 0.114(3) Uani 0.256(4) 1 d PD A 2 C31 C 0.0993(15) 0.7157(14) 0.5309(19) 0.16(2) Uani 0.256(4) 1 d PD A 2 Cl4 Cl 0.0811(10) 0.8036(9) 0.6099(8) 0.150(6) Uani 0.256(4) 1 d PD A 2 C2 C 0.33770(19) 0.2040(2) 0.29748(18) 0.0205(6) Uani 1 1 d . . . H2 H 0.3879 0.1578 0.3083 0.025 Uiso 1 1 calc R . . C3 C 0.28945(19) 0.2252(3) 0.21226(18) 0.0233(6) Uani 1 1 d . . . H3 H 0.3055 0.1920 0.1668 0.028 Uiso 1 1 calc R . . C4 C 0.21925(19) 0.2943(2) 0.19584(18) 0.0221(6) Uani 1 1 d . . . H4 H 0.1863 0.3113 0.1384 0.026 Uiso 1 1 calc R . . C5 C 0.12281(18) 0.4121(2) 0.24959(19) 0.0223(6) Uani 1 1 d . . . H5 H 0.0910 0.4340 0.1928 0.027 Uiso 1 1 calc R . . C6 C 0.09806(18) 0.4502(2) 0.31643(19) 0.0228(7) Uani 1 1 d . . . H6 H 0.0498 0.4998 0.3066 0.027 Uiso 1 1 calc R . . C7 C 0.14453(18) 0.4154(2) 0.40022(19) 0.0201(6) Uani 1 1 d . . . H7 H 0.1238 0.4379 0.4456 0.024 Uiso 1 1 calc R . . C8 C 0.21910(17) 0.3500(2) 0.41992(17) 0.0172(6) Uani 1 1 d . . . C9 C 0.24542(17) 0.3123(2) 0.34926(17) 0.0157(6) Uani 1 1 d . . . C10 C 0.19535(17) 0.3404(2) 0.26410(18) 0.0183(6) Uani 1 1 d . . . C11 C 0.20338(18) 0.2904(2) 0.56984(18) 0.0195(6) Uani 1 1 d . . . C12 C 0.19409(18) 0.3584(3) 0.63810(18) 0.0229(6) Uani 1 1 d . . . C13 C 0.1356(2) 0.3244(3) 0.67899(19) 0.0297(7) Uani 1 1 d . . . H13 H 0.1279 0.3721 0.7230 0.036 Uiso 1 1 calc R . . C14 C 0.0880(2) 0.2230(3) 0.6575(2) 0.0332(8) Uani 1 1 d . . . C15 C 0.0991(2) 0.1561(3) 0.59196(19) 0.0290(7) Uani 1 1 d . . . H15 H 0.0679 0.0858 0.5772 0.035 Uiso 1 1 calc R . . C16 C 0.15390(19) 0.1881(2) 0.54723(18) 0.0221(6) Uani 1 1 d . . . C17 C 0.2453(2) 0.4675(3) 0.6682(2) 0.0292(7) Uani 1 1 d . . . H17A H 0.2205 0.5109 0.7058 0.044 Uiso 1 1 calc R . . H17B H 0.2440 0.5154 0.6187 0.044 Uiso 1 1 calc R . . H17C H 0.3048 0.4471 0.6998 0.044 Uiso 1 1 calc R . . C18 C 0.0257(2) 0.1882(4) 0.7029(2) 0.0475(10) Uani 1 1 d . . . H18A H -0.0290 0.1665 0.6608 0.071 Uiso 1 1 calc R . . H18B H 0.0167 0.2533 0.7373 0.071 Uiso 1 1 calc R . . H18C H 0.0488 0.1221 0.7404 0.071 Uiso 1 1 calc R . . C19 C 0.1609(2) 0.1117(3) 0.47504(19) 0.0264(7) Uani 1 1 d . . . H19A H 0.1379 0.0347 0.4802 0.040 Uiso 1 1 calc R . . H19B H 0.2212 0.1048 0.4781 0.040 Uiso 1 1 calc R . . H19C H 0.1280 0.1461 0.4201 0.040 Uiso 1 1 calc R . . C20 C 0.36162(17) 0.3590(2) 0.56864(17) 0.0160(6) Uani 1 1 d . . . C25 C 0.39928(18) 0.4644(2) 0.55064(17) 0.0169(6) Uani 1 1 d . . . C24 C 0.47752(18) 0.5006(2) 0.60518(18) 0.0186(6) Uani 1 1 d . . . H24 H 0.5005 0.5719 0.5936 0.022 Uiso 1 1 calc R . . C23 C 0.52420(18) 0.4366(2) 0.67661(18) 0.0178(6) Uani 1 1 d . . . C22 C 0.48937(18) 0.3334(2) 0.69278(18) 0.0189(6) Uani 1 1 d . . . H22 H 0.5212 0.2878 0.7402 0.023 Uiso 1 1 calc R . . C21 C 0.40905(17) 0.2938(2) 0.64201(17) 0.0165(6) Uani 1 1 d . . . C28 C 0.35399(19) 0.5417(2) 0.47657(18) 0.0208(6) Uani 1 1 d . . . H28A H 0.3893 0.6102 0.4769 0.031 Uiso 1 1 calc R . . H28B H 0.2987 0.5659 0.4818 0.031 Uiso 1 1 calc R . . H28C H 0.3445 0.4993 0.4228 0.031 Uiso 1 1 calc R . . C27 C 0.60937(18) 0.4790(3) 0.73516(18) 0.0232(6) Uani 1 1 d . . . H27A H 0.6551 0.4272 0.7308 0.035 Uiso 1 1 calc R . . H27B H 0.6082 0.4798 0.7943 0.035 Uiso 1 1 calc R . . H27C H 0.6201 0.5575 0.7184 0.035 Uiso 1 1 calc R . . C26 C 0.37481(19) 0.1858(2) 0.67178(18) 0.0211(6) Uani 1 1 d . . . H26A H 0.3433 0.2073 0.7111 0.032 Uiso 1 1 calc R . . H26B H 0.4227 0.1348 0.7013 0.032 Uiso 1 1 calc R . . H26C H 0.3363 0.1452 0.6222 0.032 Uiso 1 1 calc R . . C29 C 0.67914(18) 0.1537(2) 0.43654(18) 0.0206(6) Uani 1 1 d . . . B1 B 0.2645(2) 0.3291(3) 0.5182(2) 0.0171(7) Uani 1 1 d . . . N1 N 0.31763(14) 0.24433(19) 0.36414(15) 0.0173(5) Uani 1 1 d . . . O1 O 0.55444(13) 0.18410(16) 0.49747(13) 0.0220(4) Uani 1 1 d . . . O2 O 0.52728(13) 0.07136(18) 0.36649(13) 0.0270(5) Uani 1 1 d . . . O3 O 0.61429(13) -0.00867(17) 0.50344(13) 0.0257(5) Uani 1 1 d . . . F1 F 0.71259(11) 0.08024(15) 0.39338(11) 0.0275(4) Uani 1 1 d . . . F2 F 0.66229(12) 0.25255(15) 0.39328(11) 0.0292(4) Uani 1 1 d . . . F3 F 0.73893(11) 0.17508(16) 0.51154(11) 0.0286(4) Uani 1 1 d . . . S2 S 0.58250(4) 0.09267(6) 0.45178(5) 0.01788(16) Uani 1 1 d . . . Ag1 Ag 0.413288(13) 0.215068(18) 0.495756(13) 0.01817(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.0492(10) 0.0519(11) 0.0710(11) -0.0218(8) 0.0083(7) 0.0184(8) C30 0.030(3) 0.030(3) 0.075(4) 0.026(3) 0.014(3) 0.004(2) Cl2 0.0654(11) 0.0356(12) 0.0365(9) -0.0039(8) 0.0146(8) 0.0038(8) Cl3 0.057(3) 0.090(5) 0.207(8) -0.072(5) 0.057(4) -0.016(3) C31 0.058(16) 0.044(16) 0.40(6) 0.03(2) 0.10(3) 0.027(13) Cl4 0.256(13) 0.060(7) 0.074(5) -0.017(4) -0.032(6) 0.047(6) C2 0.0216(15) 0.0174(14) 0.0230(15) 0.0003(12) 0.0076(12) 0.0014(12) C3 0.0288(16) 0.0235(16) 0.0178(15) -0.0052(12) 0.0078(13) -0.0037(13) C4 0.0252(16) 0.0221(15) 0.0157(14) 0.0024(12) 0.0021(12) -0.0029(13) C5 0.0198(15) 0.0186(15) 0.0230(16) 0.0057(12) -0.0011(12) -0.0022(12) C6 0.0155(14) 0.0159(15) 0.0330(17) 0.0043(13) 0.0021(13) 0.0020(11) C7 0.0188(15) 0.0169(14) 0.0258(16) -0.0012(12) 0.0086(12) -0.0006(12) C8 0.0177(14) 0.0118(13) 0.0206(15) 0.0010(11) 0.0039(12) -0.0037(11) C9 0.0151(14) 0.0111(13) 0.0199(14) 0.0011(11) 0.0041(12) -0.0029(10) C10 0.0172(14) 0.0142(14) 0.0207(15) 0.0014(11) 0.0022(12) -0.0047(11) C11 0.0185(14) 0.0205(15) 0.0181(14) 0.0016(12) 0.0037(12) 0.0010(12) C12 0.0215(16) 0.0255(16) 0.0213(15) 0.0003(13) 0.0060(13) 0.0004(13) C13 0.0272(17) 0.043(2) 0.0196(16) -0.0023(14) 0.0084(14) -0.0022(15) C14 0.0291(17) 0.049(2) 0.0220(16) 0.0063(15) 0.0094(14) -0.0077(16) C15 0.0254(17) 0.0331(18) 0.0245(17) 0.0045(14) 0.0022(13) -0.0098(14) C16 0.0214(15) 0.0222(15) 0.0193(15) 0.0024(12) 0.0014(12) -0.0011(12) C17 0.0316(18) 0.0296(17) 0.0295(17) -0.0077(14) 0.0138(15) -0.0023(14) C18 0.038(2) 0.075(3) 0.032(2) 0.0032(19) 0.0147(17) -0.020(2) C19 0.0282(17) 0.0211(16) 0.0275(17) -0.0005(13) 0.0053(14) -0.0050(13) C20 0.0193(14) 0.0151(14) 0.0151(14) -0.0024(11) 0.0074(11) -0.0015(11) C25 0.0207(15) 0.0126(13) 0.0190(14) -0.0016(11) 0.0084(12) 0.0025(11) C24 0.0237(15) 0.0120(14) 0.0214(15) -0.0016(11) 0.0092(13) -0.0008(11) C23 0.0172(14) 0.0168(14) 0.0196(14) -0.0048(11) 0.0063(12) 0.0012(11) C22 0.0215(15) 0.0180(14) 0.0163(14) 0.0012(11) 0.0048(12) 0.0035(12) C21 0.0194(14) 0.0137(14) 0.0172(14) -0.0010(11) 0.0068(12) 0.0031(11) C28 0.0248(16) 0.0140(14) 0.0213(15) 0.0024(12) 0.0040(13) -0.0025(12) C27 0.0240(16) 0.0222(15) 0.0204(15) -0.0019(12) 0.0029(13) -0.0017(12) C26 0.0240(16) 0.0164(14) 0.0201(15) 0.0034(11) 0.0031(12) -0.0016(12) C29 0.0213(15) 0.0190(15) 0.0208(15) -0.0015(12) 0.0055(12) -0.0007(12) B1 0.0216(17) 0.0075(14) 0.0223(17) -0.0019(12) 0.0073(14) 0.0030(12) N1 0.0162(12) 0.0147(11) 0.0190(12) 0.0002(9) 0.0027(10) 0.0005(9) O1 0.0199(10) 0.0155(10) 0.0317(12) -0.0047(8) 0.0096(9) -0.0021(8) O2 0.0204(11) 0.0257(11) 0.0289(12) -0.0053(9) -0.0008(9) -0.0021(9) O3 0.0276(11) 0.0154(10) 0.0333(12) 0.0042(9) 0.0086(10) 0.0000(9) F1 0.0276(9) 0.0274(9) 0.0313(10) -0.0060(8) 0.0145(8) -0.0009(8) F2 0.0373(11) 0.0205(9) 0.0307(10) 0.0042(7) 0.0121(8) -0.0039(8) F3 0.0205(9) 0.0385(10) 0.0238(9) -0.0070(8) 0.0028(7) -0.0082(8) S2 0.0158(3) 0.0129(3) 0.0235(4) -0.0017(3) 0.0042(3) -0.0017(3) Ag1 0.01898(12) 0.01552(12) 0.01789(12) -0.00008(9) 0.00280(8) 0.00347(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl1 C30 1.775(6) . ? C30 Cl2 1.770(5) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? Cl3 C31 1.766(17) . ? C31 Cl4 1.75(2) . ? C2 N1 1.327(4) . ? C2 C3 1.399(4) . ? C2 H2 0.9500 . ? C3 C4 1.357(4) . ? C3 H3 0.9500 . ? C4 C10 1.407(4) . ? C4 H4 0.9500 . ? C5 C6 1.361(4) . ? C5 C10 1.408(4) . ? C5 H5 0.9500 . ? C6 C7 1.408(4) . ? C6 H6 0.9500 . ? C7 C8 1.388(4) . ? C7 H7 0.9500 . ? C8 C9 1.431(4) . ? C8 B1 1.572(4) . ? C9 N1 1.379(3) . ? C9 C10 1.422(4) . ? C11 C16 1.416(4) . ? C11 C12 1.418(4) . ? C11 B1 1.572(4) . ? C12 C13 1.393(4) . ? C12 C17 1.510(4) . ? C13 C14 1.390(5) . ? C13 H13 0.9500 . ? C14 C15 1.386(5) . ? C14 C18 1.500(5) . ? C15 C16 1.382(4) . ? C15 H15 0.9500 . ? C16 C19 1.514(4) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.428(4) . ? C20 C25 1.438(4) . ? C20 B1 1.587(4) . ? C20 Ag1 2.359(3) . ? C25 C24 1.380(4) . ? C25 C28 1.505(4) . ? C24 C23 1.396(4) . ? C24 H24 0.9500 . ? C23 C22 1.384(4) . ? C23 C27 1.509(4) . ? C22 C21 1.398(4) . ? C22 H22 0.9500 . ? C21 C26 1.512(4) . ? C21 Ag1 2.596(3) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C29 F2 1.328(3) . ? C29 F1 1.332(3) . ? C29 F3 1.336(3) . ? C29 S2 1.826(3) . ? N1 Ag1 2.266(2) . ? O1 S2 1.453(2) . ? O1 Ag1 2.339(2) . ? O2 S2 1.433(2) . ? O3 S2 1.444(2) . ? O3 Ag1 2.4264(19) 3_656 ? Ag1 O3 2.426(2) 3_656 ? 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 Cl2 C30 Cl1 109.8(3) . . ? Cl2 C30 H30A 109.7 . . ? Cl1 C30 H30A 109.7 . . ? Cl2 C30 H30B 109.7 . . ? Cl1 C30 H30B 109.7 . . ? H30A C30 H30B 108.2 . . ? Cl4 C31 Cl3 99.1(11) . . ? N1 C2 C3 123.9(3) . . ? N1 C2 H2 118.0 . . ? C3 C2 H2 118.0 . . ? C4 C3 C2 118.7(3) . . ? C4 C3 H3 120.7 . . ? C2 C3 H3 120.7 . . ? C3 C4 C10 119.8(3) . . ? C3 C4 H4 120.1 . . ? C10 C4 H4 120.1 . . ? C6 C5 C10 120.4(3) . . ? C6 C5 H5 119.8 . . ? C10 C5 H5 119.8 . . ? C5 C6 C7 119.5(3) . . ? C5 C6 H6 120.2 . . ? C7 C6 H6 120.2 . . ? C8 C7 C6 123.4(3) . . ? C8 C7 H7 118.3 . . ? C6 C7 H7 118.3 . . ? C7 C8 C9 116.5(2) . . ? C7 C8 B1 114.9(2) . . ? C9 C8 B1 128.6(2) . . ? N1 C9 C10 120.2(2) . . ? N1 C9 C8 119.5(2) . . ? C10 C9 C8 120.2(2) . . ? C4 C10 C5 121.5(3) . . ? C4 C10 C9 118.7(3) . . ? C5 C10 C9 119.8(3) . . ? C16 C11 C12 118.3(3) . . ? C16 C11 B1 120.5(3) . . ? C12 C11 B1 121.3(3) . . ? C13 C12 C11 119.4(3) . . ? C13 C12 C17 118.4(3) . . ? C11 C12 C17 122.2(3) . . ? C14 C13 C12 122.2(3) . . ? C14 C13 H13 118.9 . . ? C12 C13 H13 118.9 . . ? C15 C14 C13 117.7(3) . . ? C15 C14 C18 121.2(3) . . ? C13 C14 C18 121.1(3) . . ? C16 C15 C14 122.4(3) . . ? C16 C15 H15 118.8 . . ? C14 C15 H15 118.8 . . ? C15 C16 C11 120.0(3) . . ? C15 C16 C19 119.1(3) . . ? C11 C16 C19 120.9(3) . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C14 C18 H18A 109.5 . . ? C14 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C14 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 C25 117.7(2) . . ? C21 C20 B1 121.3(2) . . ? C25 C20 B1 120.2(2) . . ? C21 C20 Ag1 82.62(16) . . ? C25 C20 Ag1 104.10(17) . . ? B1 C20 Ag1 92.57(16) . . ? C24 C25 C20 119.7(3) . . ? C24 C25 C28 118.0(2) . . ? C20 C25 C28 122.3(2) . . ? C25 C24 C23 122.7(3) . . ? C25 C24 H24 118.7 . . ? C23 C24 H24 118.7 . . ? C22 C23 C24 117.8(3) . . ? C22 C23 C27 120.8(3) . . ? C24 C23 C27 121.3(3) . . ? C23 C22 C21 122.4(3) . . ? C23 C22 H22 118.8 . . ? C21 C22 H22 118.8 . . ? C22 C21 C20 119.6(3) . . ? C22 C21 C26 117.0(2) . . ? C20 C21 C26 123.3(2) . . ? C22 C21 Ag1 111.89(18) . . ? C20 C21 Ag1 64.32(14) . . ? C26 C21 Ag1 97.68(17) . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C23 C27 H27A 109.5 . . ? C23 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C23 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C21 C26 H26A 109.5 . . ? C21 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C21 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? F2 C29 F1 108.2(2) . . ? F2 C29 F3 107.8(2) . . ? F1 C29 F3 107.7(2) . . ? F2 C29 S2 111.24(19) . . ? F1 C29 S2 110.58(19) . . ? F3 C29 S2 111.23(19) . . ? C8 B1 C11 115.1(2) . . ? C8 B1 C20 125.3(3) . . ? C11 B1 C20 119.2(2) . . ? C2 N1 C9 118.5(2) . . ? C2 N1 Ag1 117.42(18) . . ? C9 N1 Ag1 123.60(18) . . ? S2 O1 Ag1 125.49(11) . . ? S2 O3 Ag1 139.95(12) . 3_656 ? O2 S2 O3 115.98(12) . . ? O2 S2 O1 115.22(12) . . ? O3 S2 O1 113.47(12) . . ? O2 S2 C29 103.93(13) . . ? O3 S2 C29 102.99(13) . . ? O1 S2 C29 102.89(12) . . ? N1 Ag1 O1 114.87(8) . . ? N1 Ag1 C20 97.42(9) . . ? O1 Ag1 C20 128.07(8) . . ? N1 Ag1 O3 94.43(7) . 3_656 ? O1 Ag1 O3 92.07(7) . 3_656 ? C20 Ag1 O3 126.22(8) . 3_656 ? N1 Ag1 C21 128.44(8) . . ? O1 Ag1 C21 111.06(8) . . ? C20 Ag1 C21 33.06(9) . . ? O3 Ag1 C21 106.21(8) 3_656 . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.718 _refine_diff_density_min -0.486 _refine_diff_density_rms 0.075 _exptl_crystal_recrystallization_method dichloromethane/pentane #===END data_8-(dimesitylboryl)quinoline_3 _database_code_depnum_ccdc_archive 'CCDC 761001' _audit_creation_method SHELXL-97 _chemical_name_systematic 8-(dimesitylboryl)quinoline-PdCl _chemical_name_common 8-(dimesitylboryl)quinoline-PdCl _chemical_melting_point 577 _chemical_formula_moiety '4(C27 H27 B Cl N Pd), C3' _chemical_formula_sum 'C111 H108 B4 Cl4 N4 Pd4' _chemical_formula_weight 2108.65 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_int_tables_number 14 _symmetry_space_group_name_hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 19.6288(17) _cell_length_b 7.8832(7) _cell_length_c 31.428(3) _cell_angle_alpha 90.00 _cell_angle_beta 95.0590(10) _cell_angle_gamma 90.00 _cell_volume 4844.2(7) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9813 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 25.50 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.446 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2148 _exptl_absorpt_coefficient_mu 0.892 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6741 _exptl_absorpt_correction_T_max 0.8348 _exptl_absorpt_process_details '(SADABS; Bruker, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type 'Bruker SMART APEXII' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEXII' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46882 _diffrn_reflns_av_R_equivalents 0.0349 _diffrn_reflns_av_sigmaI/netI 0.0263 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 25.52 _reflns_number_total 9025 _reflns_number_gt 7445 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2006)' _computing_cell_refinement 'SAINT (Bruker, 2006)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 (Farrugia, 1997)' _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0242P)^2^+26.9045P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9025 _refine_ls_number_parameters 574 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0569 _refine_ls_R_factor_gt 0.0460 _refine_ls_wR_factor_ref 0.0985 _refine_ls_wR_factor_gt 0.0937 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.086 _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 C61 C 0.4609(5) -0.6283(13) -0.0175(3) 0.104(3) Uiso 1 1 d . . . C60 C 0.5000 -0.5000 0.0000 0.172(8) Uiso 1 2 d S . . C2 C 0.1789(2) 0.7196(6) 0.98480(13) 0.0263(10) Uani 1 1 d . . . H2 H 0.1921 0.6037 0.9845 0.032 Uiso 1 1 calc R . . C3 C 0.1805(2) 0.8025(6) 1.02447(14) 0.0316(11) Uani 1 1 d . . . H3 H 0.1933 0.7434 1.0503 0.038 Uiso 1 1 calc R . . C4 C 0.1632(2) 0.9705(6) 1.02489(14) 0.0298(11) Uani 1 1 d . . . H4 H 0.1657 1.0305 1.0512 0.036 Uiso 1 1 calc R . . C5 C 0.1230(3) 1.2292(6) 0.98481(15) 0.0324(11) Uani 1 1 d . . . H5 H 0.1230 1.2928 1.0105 0.039 Uiso 1 1 calc R . . C6 C 0.1049(3) 1.3051(6) 0.94650(15) 0.0366(12) Uani 1 1 d . . . H6 H 0.0926 1.4217 0.9456 0.044 Uiso 1 1 calc R . . C7 C 0.1043(3) 1.2113(6) 0.90816(14) 0.0299(11) Uani 1 1 d . . . H7 H 0.0930 1.2682 0.8818 0.036 Uiso 1 1 calc R . . C8 C 0.1194(2) 1.0406(6) 0.90738(14) 0.0241(10) Uani 1 1 d . . . C9 C 0.1397(2) 0.9627(6) 0.94750(14) 0.0219(9) Uani 1 1 d . . . C10 C 0.1417(2) 1.0554(6) 0.98643(14) 0.0276(10) Uani 1 1 d . . . C11 C 0.0662(2) 0.7700(5) 0.86120(14) 0.0208(9) Uani 1 1 d . . . C12 C 0.0851(2) 0.6322(5) 0.83328(14) 0.0219(9) Uani 1 1 d . . . C13 C 0.0416(2) 0.4881(6) 0.82566(15) 0.0281(11) Uani 1 1 d . . . H13 H 0.0556 0.3972 0.8086 0.034 Uiso 1 1 calc R . . C14 C -0.0196(3) 0.4801(6) 0.84255(18) 0.0364(13) Uani 1 1 d . . . C15 C -0.0376(3) 0.6095(7) 0.87037(17) 0.0373(13) Uani 1 1 d . . . H15 H -0.0803 0.6011 0.8822 0.045 Uiso 1 1 calc R . . C16 C 0.0029(2) 0.7465(6) 0.88124(15) 0.0291(11) Uani 1 1 d . . . C17 C 0.1543(2) 0.6316(6) 0.82194(13) 0.0208(9) Uani 1 1 d . . . H17A H 0.1666 0.7250 0.8030 0.025 Uiso 1 1 calc R . . H17B H 0.1720 0.5203 0.8133 0.025 Uiso 1 1 calc R . . C18 C -0.0687(3) 0.3341(7) 0.8329(2) 0.0575(18) Uani 1 1 d . . . H18A H -0.0517 0.2617 0.8108 0.086 Uiso 1 1 calc R . . H18B H -0.1138 0.3788 0.8228 0.086 Uiso 1 1 calc R . . H18C H -0.0724 0.2675 0.8590 0.086 Uiso 1 1 calc R . . C19 C -0.0232(3) 0.8788(7) 0.91046(18) 0.0419(13) Uani 1 1 d . . . H19A H 0.0046 0.8771 0.9379 0.063 Uiso 1 1 calc R . . H19B H -0.0710 0.8541 0.9151 0.063 Uiso 1 1 calc R . . H19C H -0.0203 0.9911 0.8974 0.063 Uiso 1 1 calc R . . C20 C 0.1283(2) 1.0310(5) 0.82142(13) 0.0183(9) Uani 1 1 d . . . C21 C 0.0805(2) 1.0396(5) 0.78457(13) 0.0204(9) Uani 1 1 d . . . C22 C 0.0976(2) 1.1262(5) 0.74849(13) 0.0221(9) Uani 1 1 d . . . H22 H 0.0650 1.1303 0.7243 0.027 Uiso 1 1 calc R . . C23 C 0.1599(2) 1.2071(5) 0.74622(13) 0.0220(9) Uani 1 1 d . . . C24 C 0.2066(2) 1.1968(6) 0.78185(13) 0.0214(9) Uani 1 1 d . . . H24 H 0.2501 1.2492 0.7809 0.026 Uiso 1 1 calc R . . C25 C 0.1923(2) 1.1125(5) 0.81886(13) 0.0198(9) Uani 1 1 d . . . C26 C 0.0104(2) 0.9591(7) 0.78209(16) 0.0344(12) Uani 1 1 d . . . H26A H 0.0142 0.8382 0.7754 0.052 Uiso 1 1 calc R . . H26B H -0.0195 1.0148 0.7596 0.052 Uiso 1 1 calc R . . H26C H -0.0090 0.9722 0.8096 0.052 Uiso 1 1 calc R . . C27 C 0.1754(2) 1.3005(7) 0.70631(14) 0.0325(11) Uani 1 1 d . . . H27A H 0.2155 1.3733 0.7127 0.049 Uiso 1 1 calc R . . H27B H 0.1360 1.3705 0.6962 0.049 Uiso 1 1 calc R . . H27C H 0.1848 1.2185 0.6841 0.049 Uiso 1 1 calc R . . C28 C 0.2472(2) 1.1091(6) 0.85580(14) 0.0277(10) Uani 1 1 d . . . H28A H 0.2403 1.2038 0.8751 0.042 Uiso 1 1 calc R . . H28B H 0.2923 1.1193 0.8449 0.042 Uiso 1 1 calc R . . H28C H 0.2447 1.0018 0.8713 0.042 Uiso 1 1 calc R . . C29 C 0.3060(2) 0.2767(6) 0.00556(14) 0.0277(10) Uani 1 1 d . . . H29 H 0.2933 0.3930 0.0056 0.033 Uiso 1 1 calc R . . C30 C 0.3026(2) 0.1916(6) -0.03372(14) 0.0293(10) Uani 1 1 d . . . H30 H 0.2889 0.2499 -0.0595 0.035 Uiso 1 1 calc R . . C31 C 0.3193(2) 0.0228(6) -0.03422(14) 0.0268(10) Uani 1 1 d . . . H31 H 0.3165 -0.0377 -0.0605 0.032 Uiso 1 1 calc R . . C32 C 0.3569(3) -0.2351(6) 0.00632(14) 0.0284(11) Uani 1 1 d . . . H32 H 0.3553 -0.3006 -0.0191 0.034 Uiso 1 1 calc R . . C33 C 0.3746(3) -0.3097(6) 0.04488(14) 0.0322(11) Uani 1 1 d . . . H33 H 0.3851 -0.4273 0.0462 0.039 Uiso 1 1 calc R . . C34 C 0.3775(2) -0.2141(6) 0.08271(14) 0.0275(10) Uani 1 1 d . . . H34 H 0.3884 -0.2703 0.1092 0.033 Uiso 1 1 calc R . . C35 C 0.3652(2) -0.0410(5) 0.08301(13) 0.0204(9) Uani 1 1 d . . . C36 C 0.3444(2) 0.0348(5) 0.04278(13) 0.0191(9) Uani 1 1 d . . . C37 C 0.3408(2) -0.0605(6) 0.00426(13) 0.0229(9) Uani 1 1 d . . . C38 C 0.4267(2) 0.2261(5) 0.12681(13) 0.0158(8) Uani 1 1 d . . . C39 C 0.4117(2) 0.3694(5) 0.15402(13) 0.0183(9) Uani 1 1 d . . . C40 C 0.4583(2) 0.5086(6) 0.15919(15) 0.0270(10) Uani 1 1 d . . . H40 H 0.4472 0.6036 0.1759 0.032 Uiso 1 1 calc R . . C41 C 0.5187(2) 0.5068(6) 0.14034(17) 0.0322(11) Uani 1 1 d . . . C42 C 0.5322(2) 0.3686(6) 0.11364(16) 0.0303(11) Uani 1 1 d . . . H42 H 0.5741 0.3682 0.1007 0.036 Uiso 1 1 calc R . . C43 C 0.4887(2) 0.2364(6) 0.10535(14) 0.0218(9) Uani 1 1 d . . . C44 C 0.3440(2) 0.3801(6) 0.16776(13) 0.0228(10) Uani 1 1 d . . . H44A H 0.3292 0.4947 0.1760 0.027 Uiso 1 1 calc R . . H44B H 0.3319 0.2911 0.1880 0.027 Uiso 1 1 calc R . . C45 C 0.5710(3) 0.6463(7) 0.1475(2) 0.0521(16) Uani 1 1 d . . . H45A H 0.5569 0.7246 0.1693 0.078 Uiso 1 1 calc R . . H45B H 0.5747 0.7080 0.1208 0.078 Uiso 1 1 calc R . . H45C H 0.6155 0.5968 0.1572 0.078 Uiso 1 1 calc R . . C46 C 0.5101(2) 0.0946(6) 0.07713(15) 0.0315(11) Uani 1 1 d . . . H46A H 0.5573 0.1135 0.0704 0.047 Uiso 1 1 calc R . . H46B H 0.4798 0.0922 0.0506 0.047 Uiso 1 1 calc R . . H46C H 0.5072 -0.0139 0.0921 0.047 Uiso 1 1 calc R . . C47 C 0.3608(2) -0.0251(5) 0.16882(13) 0.0186(9) Uani 1 1 d . . . C48 C 0.2953(2) -0.0976(6) 0.17264(13) 0.0219(9) Uani 1 1 d . . . C49 C 0.2814(2) -0.1800(6) 0.21026(14) 0.0264(10) Uani 1 1 d . . . H49 H 0.2371 -0.2268 0.2122 0.032 Uiso 1 1 calc R . . C50 C 0.3296(2) -0.1959(6) 0.24484(14) 0.0253(10) Uani 1 1 d . . . C51 C 0.3938(2) -0.1260(5) 0.24102(13) 0.0233(10) Uani 1 1 d . . . H51 H 0.4277 -0.1358 0.2644 0.028 Uiso 1 1 calc R . . C52 C 0.4102(2) -0.0426(5) 0.20438(13) 0.0195(9) Uani 1 1 d . . . C53 C 0.2379(2) -0.0833(6) 0.13735(14) 0.0300(11) Uani 1 1 d . . . H53A H 0.1938 -0.0875 0.1497 0.045 Uiso 1 1 calc R . . H53B H 0.2408 -0.1776 0.1173 0.045 Uiso 1 1 calc R . . H53C H 0.2419 0.0244 0.1222 0.045 Uiso 1 1 calc R . . C54 C 0.3143(3) -0.2836(7) 0.28548(17) 0.0424(14) Uani 1 1 d . . . H54A H 0.3102 -0.1989 0.3079 0.064 Uiso 1 1 calc R . . H54B H 0.3515 -0.3623 0.2944 0.064 Uiso 1 1 calc R . . H54C H 0.2713 -0.3466 0.2806 0.064 Uiso 1 1 calc R . . C55 C 0.4826(2) 0.0247(6) 0.20451(14) 0.0279(10) Uani 1 1 d . . . H55A H 0.5121 -0.0334 0.2267 0.042 Uiso 1 1 calc R . . H55B H 0.4829 0.1468 0.2103 0.042 Uiso 1 1 calc R . . H55C H 0.4997 0.0040 0.1766 0.042 Uiso 1 1 calc R . . B1 B 0.1098(3) 0.9389(6) 0.86357(16) 0.0214(10) Uani 1 1 d . . . B2 B 0.3791(2) 0.0628(6) 0.12616(15) 0.0194(10) Uani 1 1 d . . . N1 N 0.16007(18) 0.7935(5) 0.94793(11) 0.0216(8) Uani 1 1 d . . . N2 N 0.32590(18) 0.2045(5) 0.04238(11) 0.0206(8) Uani 1 1 d . . . Cl2 Cl 0.21320(5) 0.42033(14) 0.09191(4) 0.0258(2) Uani 1 1 d . . . Pd1 Pd 0.166041(16) 0.68365(4) 0.886855(10) 0.01830(9) Uani 1 1 d . . . Pd2 Pd 0.326114(16) 0.32001(4) 0.103241(10) 0.01893(9) Uani 1 1 d . . . Cl1 Cl 0.27877(5) 0.58590(13) 0.90125(3) 0.0217(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C2 0.034(3) 0.025(3) 0.019(2) 0.0032(18) 0.0000(19) 0.005(2) C3 0.037(3) 0.034(3) 0.024(2) 0.004(2) 0.003(2) 0.011(2) C4 0.036(3) 0.032(3) 0.022(2) -0.003(2) 0.010(2) 0.004(2) C5 0.049(3) 0.024(3) 0.025(2) -0.0062(19) 0.009(2) 0.004(2) C6 0.060(3) 0.017(2) 0.033(3) -0.001(2) 0.009(2) 0.005(2) C7 0.046(3) 0.020(2) 0.024(2) 0.0021(19) 0.006(2) 0.005(2) C8 0.029(2) 0.022(2) 0.022(2) 0.0005(18) 0.0062(18) -0.0012(19) C9 0.023(2) 0.020(2) 0.024(2) 0.0018(18) 0.0065(18) 0.0018(18) C10 0.032(3) 0.027(3) 0.025(2) -0.0033(19) 0.008(2) 0.003(2) C11 0.020(2) 0.012(2) 0.029(2) 0.0046(17) -0.0028(18) -0.0007(17) C12 0.023(2) 0.014(2) 0.028(2) 0.0049(17) -0.0026(18) 0.0010(17) C13 0.030(3) 0.014(2) 0.037(3) 0.0023(19) -0.015(2) 0.0008(19) C14 0.029(3) 0.019(3) 0.057(3) 0.013(2) -0.014(2) -0.006(2) C15 0.022(2) 0.037(3) 0.054(3) 0.022(3) 0.004(2) 0.000(2) C16 0.024(2) 0.029(3) 0.035(3) 0.012(2) 0.006(2) 0.002(2) C17 0.021(2) 0.019(2) 0.021(2) -0.0030(17) -0.0044(17) 0.0014(17) C18 0.039(3) 0.032(3) 0.097(5) 0.016(3) -0.017(3) -0.018(3) C19 0.031(3) 0.043(3) 0.055(3) 0.004(3) 0.021(3) 0.005(2) C20 0.024(2) 0.013(2) 0.017(2) -0.0013(16) 0.0011(17) 0.0027(17) C21 0.020(2) 0.015(2) 0.026(2) -0.0023(17) 0.0026(18) 0.0028(17) C22 0.027(2) 0.019(2) 0.020(2) -0.0013(17) -0.0016(18) 0.0046(18) C23 0.028(2) 0.018(2) 0.021(2) -0.0008(17) 0.0073(18) 0.0030(19) C24 0.022(2) 0.022(2) 0.020(2) -0.0047(18) 0.0028(17) -0.0009(19) C25 0.022(2) 0.018(2) 0.019(2) -0.0056(17) 0.0034(17) -0.0009(18) C26 0.025(3) 0.038(3) 0.039(3) 0.010(2) -0.006(2) -0.004(2) C27 0.031(3) 0.040(3) 0.027(2) 0.010(2) 0.006(2) 0.001(2) C28 0.031(3) 0.032(3) 0.020(2) -0.0035(19) -0.0005(19) -0.005(2) C29 0.029(2) 0.020(2) 0.033(3) 0.0018(19) 0.002(2) 0.0047(19) C30 0.036(3) 0.034(3) 0.017(2) 0.002(2) -0.0019(18) 0.003(2) C31 0.028(2) 0.033(3) 0.019(2) -0.0049(19) 0.0018(18) 0.001(2) C32 0.042(3) 0.022(2) 0.022(2) -0.0072(18) 0.004(2) -0.001(2) C33 0.055(3) 0.016(2) 0.025(2) -0.0014(19) 0.004(2) -0.001(2) C34 0.044(3) 0.019(2) 0.020(2) 0.0019(18) 0.003(2) 0.000(2) C35 0.025(2) 0.018(2) 0.019(2) 0.0002(17) 0.0045(17) -0.0016(18) C36 0.022(2) 0.018(2) 0.017(2) -0.0037(17) 0.0040(17) -0.0032(18) C37 0.026(2) 0.022(2) 0.021(2) -0.0002(18) 0.0062(18) -0.0020(19) C38 0.018(2) 0.0074(19) 0.021(2) 0.0019(15) -0.0038(16) 0.0017(16) C39 0.020(2) 0.016(2) 0.018(2) -0.0005(16) -0.0075(17) -0.0012(17) C40 0.034(3) 0.012(2) 0.034(3) -0.0007(18) -0.007(2) 0.0020(19) C41 0.024(3) 0.021(2) 0.050(3) 0.010(2) -0.005(2) -0.005(2) C42 0.022(2) 0.026(3) 0.043(3) 0.011(2) 0.007(2) 0.001(2) C43 0.019(2) 0.020(2) 0.027(2) 0.0072(18) 0.0041(18) 0.0000(18) C44 0.033(3) 0.021(2) 0.014(2) -0.0065(17) 0.0009(18) 0.0025(19) C45 0.035(3) 0.029(3) 0.091(5) 0.001(3) -0.007(3) -0.013(2) C46 0.028(3) 0.033(3) 0.035(3) 0.000(2) 0.011(2) 0.005(2) C47 0.023(2) 0.012(2) 0.021(2) -0.0039(16) 0.0053(17) 0.0012(17) C48 0.026(2) 0.019(2) 0.022(2) -0.0035(17) 0.0042(18) -0.0009(18) C49 0.028(2) 0.021(2) 0.032(2) -0.002(2) 0.0121(19) -0.004(2) C50 0.030(2) 0.020(2) 0.027(2) 0.0036(19) 0.0107(19) 0.004(2) C51 0.031(3) 0.020(2) 0.019(2) 0.0022(17) 0.0016(18) 0.0053(19) C52 0.021(2) 0.016(2) 0.021(2) -0.0017(17) 0.0019(17) 0.0023(18) C53 0.030(3) 0.033(3) 0.027(2) -0.002(2) 0.004(2) -0.012(2) C54 0.042(3) 0.047(3) 0.041(3) 0.016(3) 0.017(2) 0.003(3) C55 0.024(2) 0.031(3) 0.027(2) 0.008(2) -0.0036(19) -0.004(2) B1 0.021(3) 0.016(2) 0.027(3) 0.003(2) 0.004(2) 0.006(2) B2 0.021(2) 0.014(2) 0.023(2) -0.0001(19) 0.0028(19) 0.004(2) N1 0.0232(19) 0.020(2) 0.0225(18) -0.0013(15) 0.0049(15) 0.0023(16) N2 0.0229(19) 0.0197(19) 0.0190(17) 0.0024(15) 0.0007(14) -0.0004(15) Cl2 0.0190(5) 0.0259(6) 0.0324(6) 0.0008(5) 0.0022(4) 0.0045(4) Pd1 0.01905(17) 0.01537(17) 0.02035(17) -0.00144(13) 0.00102(12) 0.00122(13) Pd2 0.02021(17) 0.01607(17) 0.02061(17) -0.00112(13) 0.00234(12) 0.00117(14) Cl1 0.0165(5) 0.0234(5) 0.0244(5) -0.0011(4) -0.0030(4) 0.0044(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C61 C60 1.357(10) . ? C60 C61 1.357(10) 3_645 ? C2 N1 1.320(5) . ? C2 C3 1.406(6) . ? C2 H2 0.9500 . ? C3 C4 1.368(7) . ? C3 H3 0.9500 . ? C4 C10 1.413(6) . ? C4 H4 0.9500 . ? C5 C6 1.363(7) . ? C5 C10 1.418(7) . ? C5 H5 0.9500 . ? C6 C7 1.413(6) . ? C6 H6 0.9500 . ? C7 C8 1.378(6) . ? C7 H7 0.9500 . ? C8 C9 1.428(6) . ? C8 B1 1.590(6) . ? C9 N1 1.392(6) . ? C9 C10 1.423(6) . ? C11 C16 1.453(6) . ? C11 C12 1.465(6) . ? C11 B1 1.582(6) . ? C11 Pd1 2.163(4) . ? C12 C13 1.428(6) . ? C12 C17 1.434(6) . ? C12 Pd1 2.248(4) . ? C13 C14 1.356(7) . ? C13 H13 0.9500 . ? C14 C15 1.409(8) . ? C14 C18 1.515(7) . ? C15 C16 1.366(7) . ? C15 H15 0.9500 . ? C16 C19 1.509(7) . ? C17 Pd1 2.074(4) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C25 1.419(6) . ? C20 C21 1.426(6) . ? C20 B1 1.581(6) . ? C21 C22 1.390(6) . ? C21 C26 1.512(6) . ? C22 C23 1.387(6) . ? C22 H22 0.9500 . ? C23 C24 1.386(6) . ? C23 C27 1.508(6) . ? C24 C25 1.390(6) . ? C24 H24 0.9500 . ? C25 C28 1.514(6) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 N2 1.318(5) . ? C29 C30 1.401(6) . ? C29 H29 0.9500 . ? C30 C31 1.371(7) . ? C30 H30 0.9500 . ? C31 C37 1.408(6) . ? C31 H31 0.9500 . ? C32 C33 1.364(6) . ? C32 C37 1.412(6) . ? C32 H32 0.9500 . ? C33 C34 1.405(6) . ? C33 H33 0.9500 . ? C34 C35 1.386(6) . ? C34 H34 0.9500 . ? C35 C36 1.426(6) . ? C35 B2 1.586(6) . ? C36 N2 1.385(6) . ? C36 C37 1.422(6) . ? C38 C43 1.444(6) . ? C38 C39 1.462(6) . ? C38 B2 1.589(6) . ? C38 Pd2 2.176(4) . ? C39 C40 1.428(6) . ? C39 C44 1.435(6) . ? C39 Pd2 2.247(4) . ? C40 C41 1.372(7) . ? C40 H40 0.9500 . ? C41 C42 1.415(7) . ? C41 C45 1.508(7) . ? C42 C43 1.358(6) . ? C42 H42 0.9500 . ? C43 C46 1.510(6) . ? C44 Pd2 2.082(4) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 C52 1.420(6) . ? C47 C48 1.423(6) . ? C47 B2 1.578(6) . ? C48 C49 1.397(6) . ? C48 C53 1.514(6) . ? C49 C50 1.382(6) . ? C49 H49 0.9500 . ? C50 C51 1.390(6) . ? C50 C54 1.505(6) . ? C51 C52 1.388(6) . ? C51 H51 0.9500 . ? C52 C55 1.518(6) . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? B1 Pd1 2.379(5) . ? B2 Pd2 2.363(5) . ? N1 Pd1 2.118(3) . ? N2 Pd2 2.118(3) . ? Cl2 Pd2 2.3507(11) . ? Pd1 Cl1 2.3490(10) . ? 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 C61 C60 C61 180.0(11) . 3_645 ? N1 C2 C3 123.8(4) . . ? N1 C2 H2 118.1 . . ? C3 C2 H2 118.1 . . ? C4 C3 C2 118.2(4) . . ? C4 C3 H3 120.9 . . ? C2 C3 H3 120.9 . . ? C3 C4 C10 120.4(4) . . ? C3 C4 H4 119.8 . . ? C10 C4 H4 119.8 . . ? C6 C5 C10 120.2(4) . . ? C6 C5 H5 119.9 . . ? C10 C5 H5 119.9 . . ? C5 C6 C7 120.3(5) . . ? C5 C6 H6 119.8 . . ? C7 C6 H6 119.8 . . ? C8 C7 C6 122.7(4) . . ? C8 C7 H7 118.6 . . ? C6 C7 H7 118.6 . . ? C7 C8 C9 116.6(4) . . ? C7 C8 B1 119.9(4) . . ? C9 C8 B1 123.4(4) . . ? N1 C9 C10 119.8(4) . . ? N1 C9 C8 118.6(4) . . ? C10 C9 C8 121.5(4) . . ? C4 C10 C5 123.0(4) . . ? C4 C10 C9 118.4(4) . . ? C5 C10 C9 118.5(4) . . ? C16 C11 C12 115.9(4) . . ? C16 C11 B1 124.5(4) . . ? C12 C11 B1 119.2(4) . . ? C16 C11 Pd1 125.4(3) . . ? C12 C11 Pd1 73.8(2) . . ? B1 C11 Pd1 77.2(2) . . ? C13 C12 C17 121.4(4) . . ? C13 C12 C11 120.7(4) . . ? C17 C12 C11 116.6(4) . . ? C13 C12 Pd1 129.9(3) . . ? C17 C12 Pd1 64.2(2) . . ? C11 C12 Pd1 67.5(2) . . ? C14 C13 C12 120.6(5) . . ? C14 C13 H13 119.7 . . ? C12 C13 H13 119.7 . . ? C13 C14 C15 119.2(5) . . ? C13 C14 C18 121.8(5) . . ? C15 C14 C18 118.9(5) . . ? C16 C15 C14 123.7(5) . . ? C16 C15 H15 118.1 . . ? C14 C15 H15 118.1 . . ? C15 C16 C11 119.5(5) . . ? C15 C16 C19 118.4(5) . . ? C11 C16 C19 121.7(4) . . ? C12 C17 Pd1 77.3(3) . . ? C12 C17 H17A 115.7 . . ? Pd1 C17 H17A 115.7 . . ? C12 C17 H17B 115.7 . . ? Pd1 C17 H17B 115.7 . . ? H17A C17 H17B 112.7 . . ? C14 C18 H18A 109.5 . . ? C14 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C14 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C25 C20 C21 117.0(4) . . ? C25 C20 B1 121.7(4) . . ? C21 C20 B1 121.3(4) . . ? C22 C21 C20 119.8(4) . . ? C22 C21 C26 116.6(4) . . ? C20 C21 C26 123.6(4) . . ? C23 C22 C21 123.0(4) . . ? C23 C22 H22 118.5 . . ? C21 C22 H22 118.5 . . ? C24 C23 C22 117.1(4) . . ? C24 C23 C27 122.2(4) . . ? C22 C23 C27 120.7(4) . . ? C23 C24 C25 122.4(4) . . ? C23 C24 H24 118.8 . . ? C25 C24 H24 118.8 . . ? C24 C25 C20 120.6(4) . . ? C24 C25 C28 117.8(4) . . ? C20 C25 C28 121.5(4) . . ? C21 C26 H26A 109.5 . . ? C21 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C21 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C27 H27A 109.5 . . ? C23 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C23 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N2 C29 C30 123.7(4) . . ? N2 C29 H29 118.2 . . ? C30 C29 H29 118.2 . . ? C31 C30 C29 118.8(4) . . ? C31 C30 H30 120.6 . . ? C29 C30 H30 120.6 . . ? C30 C31 C37 119.8(4) . . ? C30 C31 H31 120.1 . . ? C37 C31 H31 120.1 . . ? C33 C32 C37 120.0(4) . . ? C33 C32 H32 120.0 . . ? C37 C32 H32 120.0 . . ? C32 C33 C34 120.6(4) . . ? C32 C33 H33 119.7 . . ? C34 C33 H33 119.7 . . ? C35 C34 C33 122.7(4) . . ? C35 C34 H34 118.7 . . ? C33 C34 H34 118.7 . . ? C34 C35 C36 116.3(4) . . ? C34 C35 B2 119.8(4) . . ? C36 C35 B2 123.8(4) . . ? N2 C36 C37 120.6(4) . . ? N2 C36 C35 117.9(4) . . ? C37 C36 C35 121.5(4) . . ? C31 C37 C32 122.9(4) . . ? C31 C37 C36 118.2(4) . . ? C32 C37 C36 118.8(4) . . ? C43 C38 C39 116.8(4) . . ? C43 C38 B2 123.9(4) . . ? C39 C38 B2 119.0(4) . . ? C43 C38 Pd2 126.7(3) . . ? C39 C38 Pd2 73.3(2) . . ? B2 C38 Pd2 75.9(2) . . ? C40 C39 C44 121.3(4) . . ? C40 C39 C38 120.0(4) . . ? C44 C39 C38 117.4(4) . . ? C40 C39 Pd2 130.2(3) . . ? C44 C39 Pd2 64.5(2) . . ? C38 C39 Pd2 68.1(2) . . ? C41 C40 C39 120.8(4) . . ? C41 C40 H40 119.6 . . ? C39 C40 H40 119.6 . . ? C40 C41 C42 118.6(4) . . ? C40 C41 C45 122.1(5) . . ? C42 C41 C45 119.4(5) . . ? C43 C42 C41 123.9(4) . . ? C43 C42 H42 118.0 . . ? C41 C42 H42 118.0 . . ? C42 C43 C38 119.7(4) . . ? C42 C43 C46 118.5(4) . . ? C38 C43 C46 121.5(4) . . ? C39 C44 Pd2 77.0(2) . . ? C39 C44 H44A 115.7 . . ? Pd2 C44 H44A 115.7 . . ? C39 C44 H44B 115.7 . . ? Pd2 C44 H44B 115.7 . . ? H44A C44 H44B 112.7 . . ? C41 C45 H45A 109.5 . . ? C41 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C41 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C43 C46 H46A 109.5 . . ? C43 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C43 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C52 C47 C48 117.0(4) . . ? C52 C47 B2 121.4(4) . . ? C48 C47 B2 121.6(4) . . ? C49 C48 C47 120.3(4) . . ? C49 C48 C53 117.8(4) . . ? C47 C48 C53 121.9(4) . . ? C50 C49 C48 122.4(4) . . ? C50 C49 H49 118.8 . . ? C48 C49 H49 118.8 . . ? C49 C50 C51 117.3(4) . . ? C49 C50 C54 122.3(4) . . ? C51 C50 C54 120.3(4) . . ? C52 C51 C50 122.5(4) . . ? C52 C51 H51 118.7 . . ? C50 C51 H51 118.7 . . ? C51 C52 C47 120.5(4) . . ? C51 C52 C55 116.7(4) . . ? C47 C52 C55 122.8(4) . . ? C48 C53 H53A 109.5 . . ? C48 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C48 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C50 C54 H54A 109.5 . . ? C50 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C50 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C52 C55 H55A 109.5 . . ? C52 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C52 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C20 B1 C11 120.7(4) . . ? C20 B1 C8 118.4(4) . . ? C11 B1 C8 119.2(4) . . ? C20 B1 Pd1 120.8(3) . . ? C11 B1 Pd1 62.4(2) . . ? C8 B1 Pd1 98.3(3) . . ? C47 B2 C35 117.7(4) . . ? C47 B2 C38 121.5(4) . . ? C35 B2 C38 119.0(4) . . ? C47 B2 Pd2 120.6(3) . . ? C35 B2 Pd2 98.3(3) . . ? C38 B2 Pd2 63.3(2) . . ? C2 N1 C9 119.3(4) . . ? C2 N1 Pd1 125.5(3) . . ? C9 N1 Pd1 114.9(3) . . ? C29 N2 C36 118.8(4) . . ? C29 N2 Pd2 125.7(3) . . ? C36 N2 Pd2 115.3(3) . . ? C17 Pd1 N1 164.16(15) . . ? C17 Pd1 C11 71.16(17) . . ? N1 Pd1 C11 95.07(15) . . ? C17 Pd1 C12 38.50(16) . . ? N1 Pd1 C12 131.35(15) . . ? C11 Pd1 C12 38.74(16) . . ? C17 Pd1 Cl1 98.37(12) . . ? N1 Pd1 Cl1 94.94(10) . . ? C11 Pd1 Cl1 169.26(12) . . ? C12 Pd1 Cl1 132.57(12) . . ? C17 Pd1 B1 81.75(17) . . ? N1 Pd1 B1 82.62(16) . . ? C11 Pd1 B1 40.42(16) . . ? C12 Pd1 B1 69.17(16) . . ? Cl1 Pd1 B1 137.75(13) . . ? C44 Pd2 N2 164.61(15) . . ? C44 Pd2 C38 71.07(16) . . ? N2 Pd2 C38 95.20(14) . . ? C44 Pd2 C39 38.48(16) . . ? N2 Pd2 C39 131.13(14) . . ? C38 Pd2 C39 38.57(14) . . ? C44 Pd2 Cl2 98.46(13) . . ? N2 Pd2 Cl2 94.65(10) . . ? C38 Pd2 Cl2 168.79(11) . . ? C39 Pd2 Cl2 133.26(11) . . ? C44 Pd2 B2 82.32(17) . . ? N2 Pd2 B2 82.65(15) . . ? C38 Pd2 B2 40.74(15) . . ? C39 Pd2 B2 69.55(16) . . ? Cl2 Pd2 B2 135.97(12) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.52 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.408 _refine_diff_density_min -1.261 _refine_diff_density_rms 0.095 _exptl_crystal_recrystallization_method 'ACN evaporation' #===END