Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Carlo Santini' _publ_contact_author_address ; Department of Chemical Sciences University of Camerino via S. Agostino, 1 Camerino Macerata 62032 ITALY ; _publ_contact_author_email CARLO.SANTINI@UNICAM.IT _publ_section_title ; Silver(I)-organophosphane complexes of electron withdrawing CF3- or NO2-substituted scorpionate ligands ; loop_ _publ_author_name 'Maura Pellei' 'Simone Alidori' 'Grazia Papini' 'Giancarlo Gioia Lobbia' 'John D. Gorden' H.V.R.Dias ; C.Santini ; data_dias186s _database_code_depnum_ccdc_archive 'CCDC 649307' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (H2B(3-(NO2)Pz)2)K _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H6 B K N6 O4' _chemical_formula_weight 276.08 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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 6.4667(2) _cell_length_b 22.3304(8) _cell_length_c 7.5362(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.073(1) _cell_angle_gamma 90.00 _cell_volume 1088.26(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8964 _cell_measurement_theta_min 2.70 _cell_measurement_theta_max 28.40 _exptl_crystal_description rods _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.685 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 560 _exptl_absorpt_coefficient_mu 0.506 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8622 _exptl_absorpt_correction_T_max 0.9279 _exptl_absorpt_process_details SADABS _exptl_special_details ; The beta-angle (90.073(1)deg) was uncomfortably closer to 90 deg indicating possible orthorhombic cell choice. However, data merging was relatively poor and the structure solution was difficult when the orthorhombic cell was used as compared to the monoclinic option. K[H2B(3-(NO2)pz)2] was solved in P21/c using direct methods. All the non hydrogen atoms were refined anisotropically. Hydrogen atoms on the pyrazolyl rings and on boron were located from the difference map and included, and refined isotropically. Final check using PLATON did not identify a higher symmetry alternative. ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8618 _diffrn_reflns_av_R_equivalents 0.0229 _diffrn_reflns_av_sigmaI/netI 0.0182 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 26.00 _reflns_number_total 2123 _reflns_number_gt 2075 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0357P)^2^+0.4737P] 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 2123 _refine_ls_number_parameters 187 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0256 _refine_ls_R_factor_gt 0.0251 _refine_ls_wR_factor_ref 0.0670 _refine_ls_wR_factor_gt 0.0666 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _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 K K 0.17497(4) 0.556204(12) 0.25426(3) 0.01912(10) Uani 1 1 d . . . N1 N 0.65787(16) 0.60657(5) -0.00862(14) 0.0180(2) Uani 1 1 d . . . N2 N 0.47506(16) 0.57776(5) -0.01623(14) 0.0183(2) Uani 1 1 d . . . N3 N 0.26220(18) 0.53697(5) -0.24318(14) 0.0223(2) Uani 1 1 d . . . N4 N 0.59495(15) 0.67564(5) 0.25150(13) 0.0167(2) Uani 1 1 d . . . N5 N 0.42010(16) 0.65694(5) 0.33277(14) 0.0179(2) Uani 1 1 d . . . N6 N 0.12832(17) 0.70374(5) 0.46563(15) 0.0236(2) Uani 1 1 d . . . O1 O 0.12947(15) 0.52562(4) -0.13032(13) 0.0259(2) Uani 1 1 d . . . O2 O 0.24310(18) 0.52334(4) -0.40072(12) 0.0315(2) Uani 1 1 d . . . O3 O 0.06605(16) 0.65418(5) 0.51483(14) 0.0302(2) Uani 1 1 d . . . O4 O 0.03468(16) 0.75078(5) 0.49205(16) 0.0361(3) Uani 1 1 d . . . B B 0.7465(2) 0.62843(6) 0.17389(19) 0.0192(3) Uani 1 1 d . . . C1 C 0.4482(2) 0.56683(6) -0.18903(17) 0.0197(3) Uani 1 1 d . . . C2 C 0.6100(2) 0.58754(6) -0.29567(18) 0.0227(3) Uani 1 1 d . . . C3 C 0.7410(2) 0.61292(6) -0.17303(17) 0.0212(3) Uani 1 1 d . . . C4 C 0.32212(19) 0.70752(6) 0.37248(16) 0.0182(3) Uani 1 1 d . . . C5 C 0.4266(2) 0.75913(6) 0.32037(17) 0.0207(3) Uani 1 1 d . . . C6 C 0.6023(2) 0.73632(6) 0.24273(17) 0.0194(3) Uani 1 1 d . . . H2 H 0.623(2) 0.5861(7) -0.416(2) 0.028(4) Uiso 1 1 d . . . H3 H 0.865(3) 0.6342(8) -0.187(2) 0.027(4) Uiso 1 1 d . . . H5 H 0.387(2) 0.7980(8) 0.336(2) 0.025(4) Uiso 1 1 d . . . H6 H 0.712(2) 0.7556(7) 0.191(2) 0.022(4) Uiso 1 1 d . . . H1A H 0.898(2) 0.6485(6) 0.1443(19) 0.019(4) Uiso 1 1 d . . . H1B H 0.752(2) 0.5886(7) 0.2686(19) 0.019(4) 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 K 0.01934(16) 0.01966(16) 0.01837(16) -0.00034(9) 0.00121(11) -0.00234(9) N1 0.0184(5) 0.0158(5) 0.0198(5) 0.0011(4) 0.0041(4) 0.0015(4) N2 0.0203(5) 0.0160(5) 0.0187(5) -0.0005(4) 0.0020(4) 0.0000(4) N3 0.0316(6) 0.0146(5) 0.0206(5) -0.0001(4) -0.0027(4) 0.0021(4) N4 0.0157(5) 0.0176(5) 0.0169(5) 0.0001(4) 0.0013(4) -0.0017(4) N5 0.0164(5) 0.0200(5) 0.0172(5) -0.0008(4) 0.0032(4) -0.0017(4) N6 0.0199(6) 0.0279(6) 0.0229(6) -0.0085(5) 0.0035(4) -0.0022(4) O1 0.0239(5) 0.0258(5) 0.0279(5) -0.0045(4) 0.0006(4) -0.0024(4) O2 0.0534(7) 0.0227(5) 0.0183(5) -0.0008(4) -0.0075(4) -0.0040(4) O3 0.0279(5) 0.0316(6) 0.0311(5) -0.0032(4) 0.0108(4) -0.0083(4) O4 0.0268(5) 0.0329(6) 0.0486(7) -0.0137(5) 0.0121(5) 0.0034(4) B 0.0183(7) 0.0189(7) 0.0204(7) 0.0006(5) 0.0015(5) 0.0015(5) C1 0.0258(7) 0.0143(6) 0.0191(6) -0.0001(5) 0.0016(5) 0.0024(5) C2 0.0314(7) 0.0189(6) 0.0177(6) 0.0021(5) 0.0064(5) 0.0055(5) C3 0.0229(6) 0.0183(6) 0.0225(6) 0.0037(5) 0.0074(5) 0.0040(5) C4 0.0170(6) 0.0210(6) 0.0166(6) -0.0031(5) 0.0007(4) -0.0009(5) C5 0.0226(6) 0.0171(6) 0.0224(6) -0.0025(5) 0.0003(5) -0.0003(5) C6 0.0199(6) 0.0188(6) 0.0195(6) 0.0002(5) 0.0010(5) -0.0031(5) _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 K O2 2.7369(10) 1_556 ? K N5 2.8144(11) . ? K O1 2.8429(10) 3_565 ? K N2 2.8572(11) . ? K O1 2.9918(10) . ? K O3 3.0235(10) . ? K B 3.2621(14) 1_455 ? K O2 3.4192(11) 3_565 ? K C2 3.5119(13) 3_665 ? K K 5.0162(5) 3_566 ? N1 N2 1.3470(15) . ? N1 C3 1.3586(17) . ? N1 B 1.5673(17) . ? N2 C1 1.3360(17) . ? N3 O2 1.2317(14) . ? N3 O1 1.2354(15) . ? N3 C1 1.4343(18) . ? N4 N5 1.3527(14) . ? N4 C6 1.3573(16) . ? N4 B 1.5542(17) . ? N5 C4 1.3295(16) . ? N6 O4 1.2287(15) . ? N6 O3 1.2350(15) . ? N6 C4 1.4397(16) . ? O1 K 2.8430(10) 3_565 ? O2 K 2.7368(10) 1_554 ? O2 K 3.4191(11) 3_565 ? B K 3.2622(14) 1_655 ? B H1A 1.102(15) . ? B H1B 1.140(15) . ? C1 C2 1.3985(18) . ? C2 C3 1.375(2) . ? C2 K 3.5119(13) 3_665 ? C2 H2 0.915(18) . ? C3 H3 0.939(17) . ? C4 C5 1.3927(18) . ? C5 C6 1.3761(18) . ? C5 H5 0.911(17) . ? C6 H6 0.919(17) . ? 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 O2 K N5 85.68(3) 1_556 . ? O2 K O1 104.50(3) 1_556 3_565 ? N5 K O1 166.51(3) . 3_565 ? O2 K N2 127.90(3) 1_556 . ? N5 K N2 68.43(3) . . ? O1 K N2 110.16(3) 3_565 . ? O2 K O1 151.01(3) 1_556 . ? N5 K O1 116.15(3) . . ? O1 K O1 57.85(3) 3_565 . ? N2 K O1 54.08(3) . . ? O2 K O3 67.32(3) 1_556 . ? N5 K O3 54.32(3) . . ? O1 K O3 121.11(3) 3_565 . ? N2 K O3 120.03(3) . . ? O1 K O3 140.50(3) . . ? O2 K B 116.40(4) 1_556 1_455 ? N5 K B 97.01(3) . 1_455 ? O1 K B 70.67(3) 3_565 1_455 ? N2 K B 111.21(3) . 1_455 ? O1 K B 81.40(3) . 1_455 ? O3 K B 64.17(3) . 1_455 ? O2 K O2 71.36(3) 1_556 3_565 ? N5 K O2 142.45(3) . 3_565 ? O1 K O2 39.16(3) 3_565 3_565 ? N2 K O2 148.86(3) . 3_565 ? O1 K O2 96.74(3) . 3_565 ? O3 K O2 88.93(3) . 3_565 ? B K O2 69.20(3) 1_455 3_565 ? O2 K C2 66.88(3) 1_556 3_665 ? N5 K C2 119.28(3) . 3_665 ? O1 K C2 73.48(3) 3_565 3_665 ? N2 K C2 87.03(3) . 3_665 ? O1 K C2 85.18(3) . 3_665 ? O3 K C2 134.12(3) . 3_665 ? B K C2 143.56(4) 1_455 3_665 ? O2 K C2 79.02(3) 3_565 3_665 ? O2 K K 40.23(2) 1_556 3_566 ? N5 K K 119.95(2) . 3_566 ? O1 K K 66.93(2) 3_565 3_566 ? N2 K K 156.72(2) . 3_566 ? O1 K K 123.86(2) . 3_566 ? O3 K K 77.11(2) . 3_566 ? B K K 90.03(3) 1_455 3_566 ? O2 K K 31.131(16) 3_565 3_566 ? C2 K K 69.88(2) 3_665 3_566 ? N2 N1 C3 111.05(11) . . ? N2 N1 B 120.39(10) . . ? C3 N1 B 128.55(11) . . ? C1 N2 N1 103.98(10) . . ? C1 N2 K 125.26(8) . . ? N1 N2 K 130.31(8) . . ? O2 N3 O1 122.96(12) . . ? O2 N3 C1 118.17(11) . . ? O1 N3 C1 118.87(10) . . ? N5 N4 C6 111.07(10) . . ? N5 N4 B 119.25(10) . . ? C6 N4 B 129.56(10) . . ? C4 N5 N4 103.80(10) . . ? C4 N5 K 117.25(8) . . ? N4 N5 K 128.50(7) . . ? O4 N6 O3 123.82(11) . . ? O4 N6 C4 117.28(11) . . ? O3 N6 C4 118.90(11) . . ? N3 O1 K 112.78(7) . 3_565 ? N3 O1 K 123.54(8) . . ? K O1 K 122.15(3) 3_565 . ? N3 O2 K 149.92(8) . 1_554 ? N3 O2 K 84.01(8) . 3_565 ? K O2 K 108.64(3) 1_554 3_565 ? N6 O3 K 112.16(7) . . ? N4 B N1 108.15(10) . . ? N4 B K 143.26(8) . 1_655 ? N1 B K 108.57(7) . 1_655 ? N4 B H1A 111.2(8) . . ? N1 B H1A 105.9(8) . . ? K B H1A 58.9(8) 1_655 . ? N4 B H1B 108.2(8) . . ? N1 B H1B 108.5(7) . . ? K B H1B 58.1(8) 1_655 . ? H1A B H1B 114.6(11) . . ? N2 C1 C2 113.80(12) . . ? N2 C1 N3 118.03(11) . . ? C2 C1 N3 128.16(12) . . ? C3 C2 C1 102.16(11) . . ? C3 C2 K 94.22(8) . 3_665 ? C1 C2 K 86.74(8) . 3_665 ? C3 C2 H2 128.7(10) . . ? C1 C2 H2 129.1(10) . . ? K C2 H2 91.1(10) 3_665 . ? N1 C3 C2 109.02(12) . . ? N1 C3 H3 119.7(10) . . ? C2 C3 H3 131.2(10) . . ? N5 C4 C5 114.07(11) . . ? N5 C4 N6 118.39(11) . . ? C5 C4 N6 127.52(11) . . ? C6 C5 C4 102.40(11) . . ? C6 C5 H5 129.5(10) . . ? C4 C5 H5 128.1(10) . . ? N4 C6 C5 108.66(11) . . ? N4 C6 H6 121.1(10) . . ? C5 C6 H6 130.3(10) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.261 _refine_diff_density_min -0.274 _refine_diff_density_rms 0.054 #===END data_rd40 _database_code_depnum_ccdc_archive 'CCDC 649308' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (H2B(3-(CF3)Pz)2)K _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H6 B F6 K N4' _chemical_formula_weight 322.08 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.280(3) _cell_length_b 5.983(2) _cell_length_c 19.165(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.41(2) _cell_angle_gamma 90.00 _cell_volume 1293.0(6) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description blocks _exptl_crystal_colour colorless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.654 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 640 _exptl_absorpt_coefficient_mu 0.476 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.7631 _exptl_absorpt_correction_T_max 0.8703 _exptl_absorpt_process_details none _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2449 _diffrn_reflns_av_R_equivalents 0.0541 _diffrn_reflns_av_sigmaI/netI 0.0401 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 22.49 _reflns_number_total 1695 _reflns_number_gt 1468 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0429P)^2^+0.7872P] 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 1695 _refine_ls_number_parameters 189 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0430 _refine_ls_R_factor_gt 0.0352 _refine_ls_wR_factor_ref 0.0906 _refine_ls_wR_factor_gt 0.0856 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _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 K K 0.09857(5) 1.18667(10) 0.30091(3) 0.0360(2) Uani 1 1 d . . . N1 N 0.31525(17) 0.7271(4) 0.29343(10) 0.0343(5) Uani 1 1 d . . . N2 N 0.28174(17) 0.9018(4) 0.33267(10) 0.0348(5) Uani 1 1 d . . . N3 N 0.20909(17) 0.7786(4) 0.17592(10) 0.0330(5) Uani 1 1 d . . . N4 N 0.11798(17) 0.9264(4) 0.17161(10) 0.0314(5) Uani 1 1 d . . . C1 C 0.3743(2) 0.9449(5) 0.37514(12) 0.0348(6) Uani 1 1 d . . . C2 C 0.4679(2) 0.8003(5) 0.36357(15) 0.0452(7) Uani 1 1 d . . . H2 H 0.5432 0.7960 0.3868 0.054 Uiso 1 1 calc R . . C3 C 0.4264(2) 0.6663(5) 0.31117(15) 0.0433(7) Uani 1 1 d . . . H3 H 0.4694 0.5483 0.2904 0.052 Uiso 1 1 calc R . . C4 C 0.3625(2) 1.1210(5) 0.42810(14) 0.0435(7) Uani 1 1 d . . . C5 C 0.1298(2) 1.0285(5) 0.11026(12) 0.0336(6) Uani 1 1 d . . . C6 C 0.2268(3) 0.9501(6) 0.07514(14) 0.0487(8) Uani 1 1 d . . . H6 H 0.2541 0.9959 0.0309 0.058 Uiso 1 1 calc R . . C7 C 0.2741(2) 0.7925(6) 0.11849(14) 0.0491(8) Uani 1 1 d . . . H7 H 0.3425 0.7056 0.1095 0.059 Uiso 1 1 calc R . . C8 C 0.0410(3) 1.1949(5) 0.08804(14) 0.0443(7) Uani 1 1 d . . . F3 F 0.32828(18) 1.0426(4) 0.48959(8) 0.0742(6) Uani 1 1 d . . . F2 F 0.46203(16) 1.2314(4) 0.44153(11) 0.0734(6) Uani 1 1 d . . . F1 F 0.28102(16) 1.2741(3) 0.41011(9) 0.0608(5) Uani 1 1 d . . . F5 F -0.06901(14) 1.1115(4) 0.08395(10) 0.0652(5) Uani 1 1 d . . . F4 F 0.03241(16) 1.3644(3) 0.13354(10) 0.0651(5) Uani 1 1 d . . . F6 F 0.06209(19) 1.2802(4) 0.02655(10) 0.0857(7) Uani 1 1 d . . . B B 0.2274(3) 0.6229(6) 0.23935(16) 0.0367(7) Uani 1 1 d . . . H1A H 0.137(2) 0.595(4) 0.2647(11) 0.026(6) Uiso 1 1 d . . . H1B H 0.266(2) 0.463(5) 0.2214(12) 0.039(7) 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 K 0.0308(3) 0.0327(4) 0.0444(4) 0.0018(3) 0.0012(2) 0.0038(2) N1 0.0304(12) 0.0355(13) 0.0372(12) 0.0035(11) 0.0035(9) 0.0037(10) N2 0.0301(11) 0.0396(13) 0.0348(12) 0.0017(11) 0.0022(10) 0.0033(10) N3 0.0277(11) 0.0382(13) 0.0333(11) -0.0024(10) 0.0050(9) 0.0014(10) N4 0.0311(11) 0.0323(12) 0.0309(11) -0.0013(10) 0.0037(9) 0.0017(10) C1 0.0322(14) 0.0406(16) 0.0315(13) 0.0075(13) 0.0012(11) -0.0004(12) C2 0.0322(15) 0.0510(19) 0.0521(17) 0.0020(16) -0.0057(13) 0.0070(14) C3 0.0330(15) 0.0452(17) 0.0519(17) 0.0040(15) 0.0039(12) 0.0100(13) C4 0.0349(15) 0.0546(19) 0.0408(16) 0.0039(15) -0.0010(12) 0.0021(14) C5 0.0343(14) 0.0363(15) 0.0303(14) -0.0060(13) 0.0023(11) 0.0000(12) C6 0.0485(17) 0.061(2) 0.0374(15) 0.0078(16) 0.0148(13) 0.0082(15) C7 0.0405(16) 0.064(2) 0.0430(16) 0.0040(16) 0.0152(13) 0.0134(15) C8 0.0519(18) 0.0472(19) 0.0341(15) -0.0007(15) 0.0059(13) 0.0048(15) F3 0.1042(16) 0.0814(15) 0.0377(10) 0.0042(10) 0.0156(9) 0.0023(12) F2 0.0467(10) 0.0825(14) 0.0910(14) -0.0332(13) 0.0011(9) -0.0121(10) F1 0.0647(11) 0.0616(12) 0.0555(10) -0.0153(10) -0.0117(8) 0.0225(10) F5 0.0433(10) 0.0747(13) 0.0766(12) -0.0095(11) -0.0190(8) 0.0084(9) F4 0.0658(11) 0.0485(11) 0.0805(12) -0.0220(10) -0.0085(9) 0.0153(9) F6 0.1002(15) 0.0967(17) 0.0615(12) 0.0406(12) 0.0255(11) 0.0453(13) B 0.0339(16) 0.0366(18) 0.0399(17) 0.0008(15) 0.0038(13) 0.0006(14) _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 K N2 2.735(2) . ? K F4 2.7513(19) 2_545 ? K N4 2.892(2) 2 ? K N4 2.939(2) . ? K F1 2.9457(19) . ? K B 3.225(3) 1_565 ? K F5 3.388(2) 2 ? K K 4.1819(12) 2_545 ? K K 4.1819(12) 2 ? N1 C3 1.342(3) . ? N1 N2 1.347(3) . ? N1 B 1.548(4) . ? N2 C1 1.333(3) . ? N3 C7 1.340(3) . ? N3 N4 1.357(3) . ? N3 B 1.541(4) . ? N4 C5 1.335(3) . ? N4 K 2.892(2) 2_545 ? C1 C2 1.387(4) . ? C1 C4 1.471(4) . ? C2 C3 1.359(4) . ? C2 H2 0.9500 . ? C3 H3 0.9500 . ? C4 F2 1.322(3) . ? C4 F3 1.334(3) . ? C4 F1 1.337(3) . ? C5 C6 1.381(4) . ? C5 C8 1.467(4) . ? C6 C7 1.357(4) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 F6 1.311(3) . ? C8 F5 1.338(3) . ? C8 F4 1.342(3) . ? F5 K 3.388(2) 2_545 ? F4 K 2.7514(19) 2 ? B K 3.225(3) 1_545 ? B H1A 1.15(2) . ? B H1B 1.11(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 N2 K F4 82.69(6) . 2_545 ? N2 K N4 154.85(6) . 2 ? F4 K N4 78.41(6) 2_545 2 ? N2 K N4 77.64(6) . . ? F4 K N4 93.76(6) 2_545 . ? N4 K N4 119.80(4) 2 . ? N2 K F1 56.08(6) . . ? F4 K F1 100.00(6) 2_545 . ? N4 K F1 111.16(6) 2 . ? N4 K F1 128.89(5) . . ? N2 K B 103.95(8) . 1_565 ? F4 K B 170.43(7) 2_545 1_565 ? N4 K B 93.17(7) 2 1_565 ? N4 K B 94.40(7) . 1_565 ? F1 K B 78.64(7) . 1_565 ? N2 K F5 114.11(6) . 2 ? F4 K F5 99.55(6) 2_545 2 ? N4 K F5 54.00(5) 2 2 ? N4 K F5 163.16(6) . 2 ? F1 K F5 58.82(5) . 2 ? B K F5 71.55(7) 1_565 2 ? N2 K K 92.76(5) . 2_545 ? F4 K K 55.00(4) 2_545 2_545 ? N4 K K 89.89(5) 2 2_545 ? N4 K K 43.73(4) . 2_545 ? F1 K K 144.37(4) . 2_545 ? B K K 130.35(6) 1_565 2_545 ? F5 K K 141.34(4) 2 2_545 ? N2 K K 159.99(5) . 2 ? F4 K K 115.41(5) 2_545 2 ? N4 K K 44.64(4) 2 2 ? N4 K K 92.02(5) . 2 ? F1 K K 123.96(4) . 2 ? B K K 59.30(6) 1_565 2 ? F5 K K 72.99(4) 2 2 ? K K K 91.34(3) 2_545 2 ? C3 N1 N2 110.0(2) . . ? C3 N1 B 129.8(2) . . ? N2 N1 B 120.2(2) . . ? C1 N2 N1 105.4(2) . . ? C1 N2 K 126.23(18) . . ? N1 N2 K 125.45(14) . . ? C7 N3 N4 109.8(2) . . ? C7 N3 B 128.3(2) . . ? N4 N3 B 121.9(2) . . ? C5 N4 N3 105.08(19) . . ? C5 N4 K 119.37(15) . 2_545 ? N3 N4 K 107.91(14) . 2_545 ? C5 N4 K 120.76(16) . . ? N3 N4 K 111.47(14) . . ? K N4 K 91.63(6) 2_545 . ? N2 C1 C2 111.7(2) . . ? N2 C1 C4 118.5(2) . . ? C2 C1 C4 129.7(2) . . ? C3 C2 C1 103.7(2) . . ? C3 C2 H2 128.1 . . ? C1 C2 H2 128.1 . . ? N1 C3 C2 109.3(2) . . ? N1 C3 H3 125.4 . . ? C2 C3 H3 125.4 . . ? F2 C4 F3 105.5(2) . . ? F2 C4 F1 106.4(3) . . ? F3 C4 F1 104.9(2) . . ? F2 C4 C1 113.7(2) . . ? F3 C4 C1 113.0(3) . . ? F1 C4 C1 112.7(2) . . ? N4 C5 C6 111.8(2) . . ? N4 C5 C8 118.9(2) . . ? C6 C5 C8 129.2(2) . . ? C7 C6 C5 104.0(2) . . ? C7 C6 H6 128.0 . . ? C5 C6 H6 128.0 . . ? N3 C7 C6 109.4(2) . . ? N3 C7 H7 125.3 . . ? C6 C7 H7 125.3 . . ? F6 C8 F5 106.3(2) . . ? F6 C8 F4 107.9(3) . . ? F5 C8 F4 103.7(2) . . ? F6 C8 C5 112.8(2) . . ? F5 C8 C5 112.9(3) . . ? F4 C8 C5 112.6(2) . . ? C4 F1 K 121.69(17) . . ? C8 F5 K 110.34(15) . 2_545 ? C8 F4 K 150.96(17) . 2 ? N3 B N1 110.8(2) . . ? N3 B K 136.47(18) . 1_545 ? N1 B K 111.59(17) . 1_545 ? N3 B H1A 108.5(12) . . ? N1 B H1A 109.5(11) . . ? K B H1A 47.0(12) 1_545 . ? N3 B H1B 108.9(13) . . ? N1 B H1B 107.8(13) . . ? K B H1B 66.4(13) 1_545 . ? H1A B H1B 111.4(18) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 22.49 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.277 _refine_diff_density_min -0.292 _refine_diff_density_rms 0.048 #===END data_dias366s _database_code_depnum_ccdc_archive 'CCDC 649309' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (H2B(3-NO2Pz)2)Ag(PPh3)2 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H36 Ag B N6 O4 P2' _chemical_formula_weight 869.39 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n 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 10.2087(7) _cell_length_b 20.5503(13) _cell_length_c 18.9869(12) _cell_angle_alpha 90.00 _cell_angle_beta 98.871(1) _cell_angle_gamma 90.00 _cell_volume 3935.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6845 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 28.26 _exptl_crystal_description parallelpipe _exptl_crystal_colour colorless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.467 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1776 _exptl_absorpt_coefficient_mu 0.644 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8483 _exptl_absorpt_correction_T_max 0.9084 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28835 _diffrn_reflns_av_R_equivalents 0.0380 _diffrn_reflns_av_sigmaI/netI 0.0345 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7736 _reflns_number_gt 6836 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0438P)^2^+2.2277P] 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 7736 _refine_ls_number_parameters 513 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0374 _refine_ls_R_factor_gt 0.0325 _refine_ls_wR_factor_ref 0.0861 _refine_ls_wR_factor_gt 0.0810 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag Ag 0.763471(16) 0.245334(7) 1.003926(8) 0.02165(7) Uani 1 1 d . . . P1 P 0.75383(5) 0.15066(2) 0.92365(3) 0.01948(12) Uani 1 1 d . . . P2 P 0.85244(5) 0.35414(3) 1.00362(3) 0.01979(12) Uani 1 1 d . . . N3 N 0.71899(19) 0.18155(9) 1.16010(9) 0.0259(4) Uani 1 1 d . . . N6 N 1.01687(19) 0.13861(9) 1.10240(10) 0.0284(4) Uani 1 1 d . . . N2 N 0.52516(19) 0.26004(9) 1.02872(10) 0.0245(4) Uani 1 1 d . . . N5 N 0.39869(19) 0.29233(9) 0.91763(11) 0.0298(4) Uani 1 1 d . . . N4 N 0.80891(17) 0.18888(9) 1.11550(9) 0.0223(4) Uani 1 1 d . . . N1 N 0.50312(18) 0.22253(9) 1.08444(10) 0.0255(4) Uani 1 1 d . . . O2 O 0.48845(17) 0.32994(8) 0.90772(9) 0.0337(4) Uani 1 1 d . . . O3 O 1.02156(16) 0.17002(9) 1.04796(9) 0.0324(4) Uani 1 1 d . . . O4 O 1.10525(19) 0.10112(10) 1.12931(10) 0.0457(5) Uani 1 1 d . . . O1 O 0.29184(17) 0.28802(9) 0.87737(9) 0.0393(4) Uani 1 1 d . . . B B 0.5966(3) 0.22792(15) 1.15764(15) 0.0317(6) Uani 1 1 d . . . C1 C 0.4162(2) 0.25214(10) 0.98049(13) 0.0247(5) Uani 1 1 d . . . C2 C 0.3244(2) 0.21006(11) 1.00261(13) 0.0308(5) Uani 1 1 d . . . H2 H 0.2409 0.1967 0.9775 0.037 Uiso 1 1 calc R . . C3 C 0.3837(2) 0.19247(11) 1.06956(13) 0.0296(5) Uani 1 1 d . . . H3 H 0.3472 0.1638 1.1006 0.035 Uiso 1 1 calc R . . C4 C 0.9027(2) 0.14491(11) 1.13807(12) 0.0256(5) Uani 1 1 d . . . C5 C 0.8766(3) 0.10965(13) 1.19652(13) 0.0387(6) Uani 1 1 d . . . H5 H 0.9283 0.0763 1.2219 0.046 Uiso 1 1 calc R . . C6 C 0.7580(3) 0.13473(13) 1.20868(13) 0.0372(6) Uani 1 1 d . . . H6 H 0.7105 0.1213 1.2455 0.045 Uiso 1 1 calc R . . C7 C 0.7391(2) 0.07703(10) 0.97505(11) 0.0214(4) Uani 1 1 d . . . C8 C 0.6408(2) 0.07762(11) 1.01889(12) 0.0258(5) Uani 1 1 d . . . H8 H 0.5832 0.1140 1.0181 0.031 Uiso 1 1 calc R . . C9 C 0.6267(2) 0.02572(11) 1.06335(13) 0.0303(5) Uani 1 1 d . . . H9 H 0.5596 0.0266 1.0929 0.036 Uiso 1 1 calc R . . C10 C 0.7102(2) -0.02777(11) 1.06496(12) 0.0305(5) Uani 1 1 d . . . H10 H 0.7003 -0.0635 1.0955 0.037 Uiso 1 1 calc R . . C11 C 0.8074(2) -0.02882(12) 1.02206(14) 0.0343(5) Uani 1 1 d . . . H11 H 0.8644 -0.0654 1.0230 0.041 Uiso 1 1 calc R . . C12 C 0.8226(2) 0.02356(11) 0.97732(13) 0.0295(5) Uani 1 1 d . . . H12 H 0.8905 0.0226 0.9483 0.035 Uiso 1 1 calc R . . C13 C 0.6060(2) 0.15019(10) 0.85583(11) 0.0205(4) Uani 1 1 d . . . C14 C 0.5359(2) 0.09375(12) 0.83414(12) 0.0269(5) Uani 1 1 d . . . H14 H 0.5612 0.0535 0.8569 0.032 Uiso 1 1 calc R . . C15 C 0.4290(2) 0.09613(13) 0.77923(12) 0.0333(5) Uani 1 1 d . . . H15 H 0.3817 0.0575 0.7642 0.040 Uiso 1 1 calc R . . C16 C 0.3912(2) 0.15487(14) 0.74639(12) 0.0358(6) Uani 1 1 d . . . H16 H 0.3183 0.1564 0.7087 0.043 Uiso 1 1 calc R . . C17 C 0.4593(2) 0.21102(13) 0.76834(12) 0.0339(6) Uani 1 1 d . . . H17 H 0.4323 0.2513 0.7461 0.041 Uiso 1 1 calc R . . C18 C 0.5672(2) 0.20918(12) 0.82271(12) 0.0282(5) Uani 1 1 d . . . H18 H 0.6144 0.2480 0.8373 0.034 Uiso 1 1 calc R . . C19 C 0.8823(2) 0.13335(10) 0.86890(11) 0.0211(4) Uani 1 1 d . . . C20 C 0.8653(2) 0.08281(11) 0.81920(12) 0.0266(5) Uani 1 1 d . . . H20 H 0.7891 0.0557 0.8160 0.032 Uiso 1 1 calc R . . C21 C 0.9582(2) 0.07168(11) 0.77443(12) 0.0282(5) Uani 1 1 d . . . H21 H 0.9463 0.0368 0.7412 0.034 Uiso 1 1 calc R . . C22 C 1.0683(2) 0.11165(12) 0.77833(12) 0.0294(5) Uani 1 1 d . . . H22 H 1.1313 0.1046 0.7472 0.035 Uiso 1 1 calc R . . C23 C 1.0867(2) 0.16174(12) 0.82738(12) 0.0295(5) Uani 1 1 d . . . H23 H 1.1627 0.1889 0.8301 0.035 Uiso 1 1 calc R . . C24 C 0.9940(2) 0.17256(10) 0.87283(12) 0.0237(4) Uani 1 1 d . . . H24 H 1.0073 0.2069 0.9067 0.028 Uiso 1 1 calc R . . C25 C 0.8395(2) 0.38889(10) 0.91426(11) 0.0218(4) Uani 1 1 d . . . C26 C 0.8496(3) 0.34676(11) 0.85764(13) 0.0315(5) Uani 1 1 d . . . H26 H 0.8625 0.3015 0.8665 0.038 Uiso 1 1 calc R . . C27 C 0.8411(3) 0.37013(12) 0.78865(13) 0.0365(6) Uani 1 1 d . . . H27 H 0.8486 0.3410 0.7506 0.044 Uiso 1 1 calc R . . C28 C 0.8217(2) 0.43611(12) 0.77518(13) 0.0326(5) Uani 1 1 d . . . H28 H 0.8158 0.4523 0.7279 0.039 Uiso 1 1 calc R . . C29 C 0.8111(2) 0.47825(11) 0.83087(12) 0.0278(5) Uani 1 1 d . . . H29 H 0.7980 0.5234 0.8217 0.033 Uiso 1 1 calc R . . C30 C 0.8193(2) 0.45498(10) 0.90023(12) 0.0234(4) Uani 1 1 d . . . H30 H 0.8112 0.4842 0.9381 0.028 Uiso 1 1 calc R . . C31 C 0.7829(2) 0.41748(10) 1.05463(11) 0.0212(4) Uani 1 1 d . . . C32 C 0.6455(2) 0.42138(11) 1.04994(13) 0.0291(5) Uani 1 1 d . . . H32 H 0.5906 0.3903 1.0225 0.035 Uiso 1 1 calc R . . C33 C 0.5885(2) 0.47057(12) 1.08534(13) 0.0319(5) Uani 1 1 d . . . H33 H 0.4948 0.4734 1.0814 0.038 Uiso 1 1 calc R . . C34 C 0.6679(2) 0.51546(11) 1.12643(12) 0.0275(5) Uani 1 1 d . . . H34 H 0.6287 0.5493 1.1501 0.033 Uiso 1 1 calc R . . C35 C 0.8037(2) 0.51075(10) 1.13275(11) 0.0255(5) Uani 1 1 d . . . H35 H 0.8581 0.5410 1.1616 0.031 Uiso 1 1 calc R . . C36 C 0.8620(2) 0.46182(10) 1.09705(11) 0.0234(4) Uani 1 1 d . . . H36 H 0.9558 0.4588 1.1018 0.028 Uiso 1 1 calc R . . C37 C 1.0300(2) 0.35507(10) 1.03836(11) 0.0208(4) Uani 1 1 d . . . C38 C 1.0707(2) 0.32545(11) 1.10409(12) 0.0247(5) Uani 1 1 d . . . H38 H 1.0075 0.3044 1.1281 0.030 Uiso 1 1 calc R . . C39 C 1.2031(2) 0.32656(11) 1.13464(12) 0.0289(5) Uani 1 1 d . . . H39 H 1.2297 0.3074 1.1801 0.035 Uiso 1 1 calc R . . C40 C 1.2970(2) 0.35561(11) 1.09902(13) 0.0285(5) Uani 1 1 d . . . H40 H 1.3877 0.3563 1.1200 0.034 Uiso 1 1 calc R . . C41 C 1.2573(2) 0.38349(11) 1.03275(13) 0.0276(5) Uani 1 1 d . . . H41 H 1.3215 0.4027 1.0079 0.033 Uiso 1 1 calc R . . C42 C 1.1245(2) 0.38361(10) 1.00236(12) 0.0243(4) Uani 1 1 d . . . H42 H 1.0981 0.4031 0.9570 0.029 Uiso 1 1 calc R . . H1B H 0.629(2) 0.2805(12) 1.1648(13) 0.026(6) Uiso 1 1 d . . . H1A H 0.543(2) 0.2107(13) 1.2001(14) 0.035(7) 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 Ag 0.02669(11) 0.01640(10) 0.02219(10) -0.00036(6) 0.00482(7) -0.00305(6) P1 0.0208(3) 0.0167(3) 0.0208(3) -0.0002(2) 0.0025(2) -0.0012(2) P2 0.0217(3) 0.0157(3) 0.0222(3) -0.0006(2) 0.0041(2) -0.0014(2) N3 0.0293(10) 0.0290(10) 0.0201(9) -0.0002(8) 0.0057(7) -0.0031(8) N6 0.0301(10) 0.0288(10) 0.0249(10) -0.0022(8) 0.0000(8) 0.0069(8) N2 0.0223(10) 0.0258(10) 0.0264(10) -0.0059(8) 0.0072(8) -0.0017(7) N5 0.0314(11) 0.0262(10) 0.0320(11) -0.0065(8) 0.0051(8) 0.0014(8) N4 0.0242(9) 0.0228(9) 0.0196(9) -0.0022(7) 0.0022(7) -0.0025(7) N1 0.0243(9) 0.0249(10) 0.0283(10) -0.0029(8) 0.0077(8) -0.0003(8) O2 0.0386(10) 0.0277(9) 0.0358(9) -0.0020(7) 0.0089(7) -0.0030(7) O3 0.0282(9) 0.0391(10) 0.0305(9) 0.0049(8) 0.0062(7) 0.0024(7) O4 0.0448(11) 0.0533(12) 0.0370(10) 0.0041(9) 0.0004(8) 0.0249(9) O1 0.0348(10) 0.0448(11) 0.0351(10) -0.0053(8) -0.0049(8) -0.0001(8) B 0.0318(15) 0.0372(15) 0.0268(14) -0.0067(12) 0.0066(11) 0.0012(12) C1 0.0243(12) 0.0222(11) 0.0277(12) -0.0066(9) 0.0046(9) 0.0004(8) C2 0.0247(12) 0.0294(12) 0.0386(14) -0.0095(10) 0.0060(10) -0.0043(10) C3 0.0270(12) 0.0252(12) 0.0384(13) -0.0038(10) 0.0110(10) -0.0044(9) C4 0.0302(12) 0.0244(11) 0.0215(11) 0.0003(9) 0.0017(9) 0.0026(9) C5 0.0516(16) 0.0346(14) 0.0304(13) 0.0111(11) 0.0077(11) 0.0114(12) C6 0.0469(15) 0.0375(14) 0.0284(13) 0.0108(11) 0.0100(11) 0.0003(12) C7 0.0228(11) 0.0172(10) 0.0231(10) -0.0010(8) -0.0003(8) -0.0050(8) C8 0.0271(12) 0.0215(11) 0.0290(12) -0.0026(9) 0.0050(9) 0.0006(9) C9 0.0348(13) 0.0275(12) 0.0304(12) 0.0009(10) 0.0103(10) -0.0044(10) C10 0.0357(13) 0.0261(12) 0.0297(12) 0.0076(10) 0.0049(10) -0.0034(10) C11 0.0336(13) 0.0235(12) 0.0461(15) 0.0067(11) 0.0077(11) 0.0049(10) C12 0.0302(12) 0.0246(11) 0.0351(13) 0.0041(10) 0.0092(10) 0.0030(9) C13 0.0199(10) 0.0250(11) 0.0173(10) -0.0031(8) 0.0054(8) 0.0012(8) C14 0.0234(11) 0.0323(12) 0.0250(11) 0.0007(9) 0.0041(9) -0.0029(9) C15 0.0254(12) 0.0501(15) 0.0251(12) -0.0064(11) 0.0059(9) -0.0108(11) C16 0.0216(12) 0.0652(18) 0.0207(11) 0.0012(11) 0.0036(9) 0.0033(11) C17 0.0327(13) 0.0447(15) 0.0249(12) 0.0070(11) 0.0063(10) 0.0125(11) C18 0.0309(12) 0.0285(12) 0.0257(12) 0.0001(9) 0.0064(9) 0.0050(10) C19 0.0209(10) 0.0202(10) 0.0219(10) 0.0033(8) 0.0029(8) -0.0003(8) C20 0.0241(11) 0.0257(11) 0.0303(12) -0.0045(9) 0.0054(9) -0.0047(9) C21 0.0261(12) 0.0291(12) 0.0292(12) -0.0047(10) 0.0035(9) -0.0001(9) C22 0.0231(11) 0.0386(13) 0.0274(12) 0.0031(10) 0.0064(9) 0.0014(10) C23 0.0241(11) 0.0321(12) 0.0325(13) 0.0018(10) 0.0050(9) -0.0072(10) C24 0.0248(11) 0.0202(10) 0.0251(11) 0.0017(9) 0.0005(9) -0.0013(9) C25 0.0217(10) 0.0202(10) 0.0233(11) 0.0007(8) 0.0027(8) -0.0022(8) C26 0.0457(14) 0.0200(11) 0.0295(12) 0.0009(9) 0.0082(10) 0.0058(10) C27 0.0571(17) 0.0276(12) 0.0256(12) -0.0013(10) 0.0092(11) 0.0053(11) C28 0.0382(13) 0.0339(13) 0.0244(12) 0.0063(10) 0.0010(10) 0.0018(11) C29 0.0301(12) 0.0202(11) 0.0303(12) 0.0036(9) -0.0050(9) -0.0014(9) C30 0.0237(11) 0.0188(10) 0.0265(11) -0.0026(9) -0.0003(8) -0.0001(8) C31 0.0249(11) 0.0176(10) 0.0216(10) 0.0016(8) 0.0055(8) 0.0003(8) C32 0.0253(12) 0.0254(11) 0.0368(13) -0.0079(10) 0.0052(9) -0.0047(9) C33 0.0252(12) 0.0336(13) 0.0376(13) -0.0040(10) 0.0069(10) 0.0009(10) C34 0.0361(13) 0.0223(11) 0.0255(11) -0.0020(9) 0.0093(9) 0.0032(9) C35 0.0321(12) 0.0212(11) 0.0226(11) -0.0024(9) 0.0026(9) -0.0024(9) C36 0.0247(11) 0.0214(10) 0.0242(11) 0.0000(9) 0.0040(8) -0.0009(9) C37 0.0234(11) 0.0158(10) 0.0235(11) -0.0030(8) 0.0044(8) 0.0004(8) C38 0.0276(11) 0.0223(11) 0.0253(11) 0.0002(9) 0.0078(9) -0.0001(9) C39 0.0313(12) 0.0295(12) 0.0248(11) -0.0020(9) 0.0014(9) 0.0059(10) C40 0.0233(11) 0.0261(12) 0.0353(13) -0.0091(10) 0.0015(9) 0.0029(9) C41 0.0269(12) 0.0229(11) 0.0346(13) -0.0045(10) 0.0097(9) -0.0015(9) C42 0.0268(11) 0.0199(10) 0.0267(11) -0.0005(9) 0.0053(9) -0.0009(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 Ag N4 2.3970(17) . ? Ag P2 2.4138(6) . ? Ag P1 2.4641(6) . ? Ag N2 2.5661(19) . ? P1 C7 1.819(2) . ? P1 C13 1.827(2) . ? P1 C19 1.830(2) . ? P2 C25 1.827(2) . ? P2 C31 1.830(2) . ? P2 C37 1.831(2) . ? N3 C6 1.350(3) . ? N3 N4 1.350(2) . ? N3 B 1.566(3) . ? N6 O3 1.226(2) . ? N6 O4 1.235(2) . ? N6 C4 1.441(3) . ? N2 C1 1.337(3) . ? N2 N1 1.355(3) . ? N5 O1 1.235(2) . ? N5 O2 1.235(3) . ? N5 C1 1.440(3) . ? N4 C4 1.338(3) . ? N1 C3 1.357(3) . ? N1 B 1.564(3) . ? B H1B 1.13(2) . ? B H1A 1.10(3) . ? C1 C2 1.388(3) . ? C2 C3 1.370(3) . ? C2 H2 0.9500 . ? C3 H3 0.9500 . ? C4 C5 1.385(3) . ? C5 C6 1.368(4) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.388(3) . ? C7 C8 1.399(3) . ? C8 C9 1.381(3) . ? C8 H8 0.9500 . ? C9 C10 1.388(3) . ? C9 H9 0.9500 . ? C10 C11 1.378(3) . ? C10 H10 0.9500 . ? C11 C12 1.395(3) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.391(3) . ? C13 C18 1.395(3) . ? C14 C15 1.389(3) . ? C14 H14 0.9500 . ? C15 C16 1.386(4) . ? C15 H15 0.9500 . ? C16 C17 1.378(4) . ? C16 H16 0.9500 . ? C17 C18 1.389(3) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C24 1.389(3) . ? C19 C20 1.396(3) . ? C20 C21 1.387(3) . ? C20 H20 0.9500 . ? C21 C22 1.385(3) . ? C21 H21 0.9500 . ? C22 C23 1.381(3) . ? C22 H22 0.9500 . ? C23 C24 1.394(3) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C30 1.393(3) . ? C25 C26 1.396(3) . ? C26 C27 1.385(3) . ? C26 H26 0.9500 . ? C27 C28 1.388(3) . ? C27 H27 0.9500 . ? C28 C29 1.384(3) . ? C28 H28 0.9500 . ? C29 C30 1.391(3) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C36 1.389(3) . ? C31 C32 1.394(3) . ? C32 C33 1.390(3) . ? C32 H32 0.9500 . ? C33 C34 1.386(3) . ? C33 H33 0.9500 . ? C34 C35 1.376(3) . ? C34 H34 0.9500 . ? C35 C36 1.396(3) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C38 1.393(3) . ? C37 C42 1.395(3) . ? C38 C39 1.386(3) . ? C38 H38 0.9500 . ? C39 C40 1.390(3) . ? C39 H39 0.9500 . ? C40 C41 1.385(3) . ? C40 H40 0.9500 . ? C41 C42 1.389(3) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Ag P2 115.40(4) . . ? N4 Ag P1 98.53(4) . . ? P2 Ag P1 135.158(19) . . ? N4 Ag N2 87.40(6) . . ? P2 Ag N2 105.02(4) . . ? P1 Ag N2 104.95(4) . . ? C7 P1 C13 104.24(10) . . ? C7 P1 C19 105.60(10) . . ? C13 P1 C19 100.69(9) . . ? C7 P1 Ag 108.88(7) . . ? C13 P1 Ag 112.95(7) . . ? C19 P1 Ag 122.76(7) . . ? C25 P2 C31 103.60(10) . . ? C25 P2 C37 104.84(10) . . ? C31 P2 C37 104.19(10) . . ? C25 P2 Ag 113.02(7) . . ? C31 P2 Ag 118.74(7) . . ? C37 P2 Ag 111.15(7) . . ? C6 N3 N4 110.55(19) . . ? C6 N3 B 127.1(2) . . ? N4 N3 B 121.99(19) . . ? O3 N6 O4 123.8(2) . . ? O3 N6 C4 119.24(18) . . ? O4 N6 C4 116.99(19) . . ? C1 N2 N1 104.17(18) . . ? C1 N2 Ag 124.88(15) . . ? N1 N2 Ag 110.64(13) . . ? O1 N5 O2 123.8(2) . . ? O1 N5 C1 117.2(2) . . ? O2 N5 C1 119.01(19) . . ? C4 N4 N3 104.23(18) . . ? C4 N4 Ag 129.90(15) . . ? N3 N4 Ag 123.42(13) . . ? N2 N1 C3 110.38(19) . . ? N2 N1 B 120.07(19) . . ? C3 N1 B 128.5(2) . . ? N1 B N3 110.99(19) . . ? N1 B H1B 107.6(12) . . ? N3 B H1B 110.9(12) . . ? N1 B H1A 108.7(13) . . ? N3 B H1A 105.6(14) . . ? H1B B H1A 113.0(18) . . ? N2 C1 C2 113.4(2) . . ? N2 C1 N5 118.8(2) . . ? C2 C1 N5 127.2(2) . . ? C3 C2 C1 102.8(2) . . ? C3 C2 H2 128.6 . . ? C1 C2 H2 128.6 . . ? N1 C3 C2 109.1(2) . . ? N1 C3 H3 125.4 . . ? C2 C3 H3 125.4 . . ? N4 C4 C5 113.2(2) . . ? N4 C4 N6 120.05(19) . . ? C5 C4 N6 126.8(2) . . ? C6 C5 C4 102.9(2) . . ? C6 C5 H5 128.6 . . ? C4 C5 H5 128.6 . . ? N3 C6 C5 109.2(2) . . ? N3 C6 H6 125.4 . . ? C5 C6 H6 125.4 . . ? C12 C7 C8 118.8(2) . . ? C12 C7 P1 125.03(17) . . ? C8 C7 P1 115.99(16) . . ? C9 C8 C7 120.6(2) . . ? C9 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? C8 C9 C10 120.2(2) . . ? C8 C9 H9 119.9 . . ? C10 C9 H9 119.9 . . ? C11 C10 C9 119.7(2) . . ? C11 C10 H10 120.2 . . ? C9 C10 H10 120.2 . . ? C10 C11 C12 120.4(2) . . ? C10 C11 H11 119.8 . . ? C12 C11 H11 119.8 . . ? C7 C12 C11 120.3(2) . . ? C7 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C14 C13 C18 119.6(2) . . ? C14 C13 P1 122.98(17) . . ? C18 C13 P1 117.36(16) . . ? C15 C14 C13 120.1(2) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C16 C15 C14 120.0(2) . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C17 C16 C15 120.0(2) . . ? C17 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? C16 C17 C18 120.5(2) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C17 C18 C13 119.8(2) . . ? C17 C18 H18 120.1 . . ? C13 C18 H18 120.1 . . ? C24 C19 C20 118.9(2) . . ? C24 C19 P1 120.75(17) . . ? C20 C19 P1 120.20(16) . . ? C21 C20 C19 120.8(2) . . ? C21 C20 H20 119.6 . . ? C19 C20 H20 119.6 . . ? C22 C21 C20 119.7(2) . . ? C22 C21 H21 120.1 . . ? C20 C21 H21 120.1 . . ? C23 C22 C21 120.2(2) . . ? C23 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? C22 C23 C24 120.1(2) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C19 C24 C23 120.3(2) . . ? C19 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C30 C25 C26 118.9(2) . . ? C30 C25 P2 123.09(17) . . ? C26 C25 P2 117.98(16) . . ? C27 C26 C25 120.8(2) . . ? C27 C26 H26 119.6 . . ? C25 C26 H26 119.6 . . ? C26 C27 C28 119.9(2) . . ? C26 C27 H27 120.0 . . ? C28 C27 H27 120.0 . . ? C29 C28 C27 119.7(2) . . ? C29 C28 H28 120.1 . . ? C27 C28 H28 120.1 . . ? C28 C29 C30 120.5(2) . . ? C28 C29 H29 119.7 . . ? C30 C29 H29 119.7 . . ? C29 C30 C25 120.1(2) . . ? C29 C30 H30 119.9 . . ? C25 C30 H30 119.9 . . ? C36 C31 C32 119.2(2) . . ? C36 C31 P2 122.36(16) . . ? C32 C31 P2 118.41(16) . . ? C33 C32 C31 120.2(2) . . ? C33 C32 H32 119.9 . . ? C31 C32 H32 119.9 . . ? C34 C33 C32 120.3(2) . . ? C34 C33 H33 119.8 . . ? C32 C33 H33 119.8 . . ? C35 C34 C33 119.7(2) . . ? C35 C34 H34 120.1 . . ? C33 C34 H34 120.1 . . ? C34 C35 C36 120.5(2) . . ? C34 C35 H35 119.8 . . ? C36 C35 H35 119.8 . . ? C31 C36 C35 120.0(2) . . ? C31 C36 H36 120.0 . . ? C35 C36 H36 120.0 . . ? C38 C37 C42 119.3(2) . . ? C38 C37 P2 117.41(16) . . ? C42 C37 P2 123.32(16) . . ? C39 C38 C37 120.3(2) . . ? C39 C38 H38 119.8 . . ? C37 C38 H38 119.8 . . ? C38 C39 C40 120.3(2) . . ? C38 C39 H39 119.9 . . ? C40 C39 H39 119.9 . . ? C41 C40 C39 119.5(2) . . ? C41 C40 H40 120.2 . . ? C39 C40 H40 120.2 . . ? C40 C41 C42 120.5(2) . . ? C40 C41 H41 119.7 . . ? C42 C41 H41 119.7 . . ? C41 C42 C37 120.0(2) . . ? C41 C42 H42 120.0 . . ? C37 C42 H42 120.0 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.941 _refine_diff_density_min -0.325 _refine_diff_density_rms 0.073 #===END data_dias368s _database_code_depnum_ccdc_archive 'CCDC 649310' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (H2B(3-NO2Pz)2)AgPTol3 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H27 Ag B N6 O4 P' _chemical_formula_weight 649.20 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 35.4543(15) _cell_length_b 10.6701(5) _cell_length_c 15.0076(6) _cell_angle_alpha 90.00 _cell_angle_beta 94.616(1) _cell_angle_gamma 90.00 _cell_volume 5659.0(4) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6722 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 28.41 _exptl_crystal_description parallelpipe _exptl_crystal_colour cream _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.524 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2640 _exptl_absorpt_coefficient_mu 0.813 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8319 _exptl_absorpt_correction_T_max 0.8947 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22606 _diffrn_reflns_av_R_equivalents 0.0151 _diffrn_reflns_av_sigmaI/netI 0.0132 _diffrn_reflns_limit_h_min -44 _diffrn_reflns_limit_h_max 44 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 26.50 _reflns_number_total 5871 _reflns_number_gt 5516 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0379P)^2^+7.5928P] 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 5871 _refine_ls_number_parameters 372 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0268 _refine_ls_R_factor_gt 0.0252 _refine_ls_wR_factor_ref 0.0677 _refine_ls_wR_factor_gt 0.0664 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag Ag 0.618583(4) 0.192673(12) 0.041538(8) 0.02580(6) Uani 1 1 d . . . P P 0.616955(12) 0.33821(4) 0.15880(3) 0.01965(9) Uani 1 1 d . . . N1 N 0.66313(5) 0.17097(16) -0.13493(11) 0.0348(4) Uani 1 1 d . . . N2 N 0.67024(5) 0.16425(15) -0.04556(11) 0.0299(3) Uani 1 1 d . . . N3 N 0.59349(5) 0.11524(16) -0.15561(10) 0.0333(4) Uani 1 1 d . . . N4 N 0.58530(4) 0.09239(14) -0.07069(9) 0.0258(3) Uani 1 1 d . . . N5 N 0.72322(5) 0.10876(18) 0.05595(12) 0.0387(4) Uani 1 1 d . . . N6 N 0.54379(5) -0.04453(16) 0.00130(12) 0.0360(4) Uani 1 1 d . . . O1 O 0.70349(4) 0.1166(2) 0.11904(11) 0.0529(5) Uani 1 1 d . . . O2 O 0.75704(4) 0.0823(2) 0.06332(12) 0.0573(5) Uani 1 1 d . . . O3 O 0.55520(4) -0.00010(16) 0.07403(10) 0.0430(4) Uani 1 1 d . . . O4 O 0.52038(4) -0.12982(15) -0.00901(13) 0.0509(4) Uani 1 1 d . . . B B 0.62346(8) 0.2151(3) -0.17613(17) 0.0418(6) Uani 1 1 d . . . C1 C 0.70639(5) 0.12925(17) -0.03333(14) 0.0313(4) Uani 1 1 d . . . C2 C 0.72346(6) 0.11397(18) -0.11265(14) 0.0364(4) Uani 1 1 d . . . H2 H 0.7488 0.0908 -0.1209 0.044 Uiso 1 1 calc R . . C3 C 0.69452(7) 0.1407(2) -0.17618(15) 0.0413(5) Uani 1 1 d . . . H3 H 0.6962 0.1383 -0.2390 0.050 Uiso 1 1 calc R . . C4 C 0.55864(5) 0.00419(18) -0.07795(13) 0.0313(4) Uani 1 1 d . . . C5 C 0.54911(7) -0.0308(2) -0.16602(16) 0.0462(6) Uani 1 1 d . . . H5 H 0.5310 -0.0911 -0.1882 0.055 Uiso 1 1 calc R . . C6 C 0.57190(7) 0.0421(2) -0.21278(14) 0.0464(6) Uani 1 1 d . . . H6 H 0.5726 0.0417 -0.2759 0.056 Uiso 1 1 calc R . . C7 C 0.65522(5) 0.45151(16) 0.15419(11) 0.0219(3) Uani 1 1 d . . . C8 C 0.66422(5) 0.49400(17) 0.07017(12) 0.0269(4) Uani 1 1 d . . . H8 H 0.6507 0.4625 0.0176 0.032 Uiso 1 1 calc R . . C9 C 0.69265(5) 0.58164(18) 0.06331(13) 0.0313(4) Uani 1 1 d . . . H9 H 0.6980 0.6110 0.0059 0.038 Uiso 1 1 calc R . . C10 C 0.71349(5) 0.62745(18) 0.13874(14) 0.0309(4) Uani 1 1 d . . . C11 C 0.70519(5) 0.58225(18) 0.22184(14) 0.0311(4) Uani 1 1 d . . . H11 H 0.7196 0.6107 0.2741 0.037 Uiso 1 1 calc R . . C12 C 0.67622(5) 0.49632(17) 0.22991(12) 0.0271(4) Uani 1 1 d . . . H12 H 0.6707 0.4680 0.2874 0.032 Uiso 1 1 calc R . . C13 C 0.74477(6) 0.7222(2) 0.13125(18) 0.0442(5) Uani 1 1 d . . . H13A H 0.7620 0.6925 0.0879 0.066 Uiso 1 1 calc R . . H13B H 0.7588 0.7329 0.1897 0.066 Uiso 1 1 calc R . . H13C H 0.7338 0.8027 0.1112 0.066 Uiso 1 1 calc R . . C14 C 0.62067(5) 0.28477(16) 0.27396(11) 0.0207(3) Uani 1 1 d . . . C15 C 0.64588(5) 0.18747(15) 0.29799(12) 0.0242(4) Uani 1 1 d . . . H15 H 0.6597 0.1482 0.2540 0.029 Uiso 1 1 calc R . . C16 C 0.65066(5) 0.14831(17) 0.38680(12) 0.0262(4) Uani 1 1 d . . . H16 H 0.6681 0.0831 0.4028 0.031 Uiso 1 1 calc R . . C17 C 0.63051(5) 0.20225(16) 0.45244(12) 0.0263(4) Uani 1 1 d . . . C18 C 0.60520(5) 0.29857(17) 0.42771(12) 0.0277(4) Uani 1 1 d . . . H18 H 0.5911 0.3365 0.4716 0.033 Uiso 1 1 calc R . . C19 C 0.60037(5) 0.33993(17) 0.33939(12) 0.0255(3) Uani 1 1 d . . . H19 H 0.5831 0.4060 0.3237 0.031 Uiso 1 1 calc R . . C20 C 0.63616(6) 0.1578(2) 0.54805(13) 0.0358(4) Uani 1 1 d . . . H20A H 0.6163 0.1930 0.5824 0.054 Uiso 1 1 calc R . . H20B H 0.6610 0.1855 0.5743 0.054 Uiso 1 1 calc R . . H20C H 0.6349 0.0661 0.5496 0.054 Uiso 1 1 calc R . . C21 C 0.57360(5) 0.42986(16) 0.14695(10) 0.0208(3) Uani 1 1 d . . . C22 C 0.57308(5) 0.55959(17) 0.15507(11) 0.0259(4) Uani 1 1 d . . . H22 H 0.5960 0.6041 0.1689 0.031 Uiso 1 1 calc R . . C23 C 0.53900(5) 0.62433(18) 0.14297(13) 0.0303(4) Uani 1 1 d . . . H23 H 0.5390 0.7131 0.1481 0.036 Uiso 1 1 calc R . . C24 C 0.50501(5) 0.56199(19) 0.12359(12) 0.0294(4) Uani 1 1 d . . . C25 C 0.50570(5) 0.4322(2) 0.11612(13) 0.0314(4) Uani 1 1 d . . . H25 H 0.4827 0.3878 0.1035 0.038 Uiso 1 1 calc R . . C26 C 0.53962(5) 0.36626(18) 0.12678(12) 0.0278(4) Uani 1 1 d . . . H26 H 0.5396 0.2777 0.1203 0.033 Uiso 1 1 calc R . . C27 C 0.46822(6) 0.6331(2) 0.11083(15) 0.0403(5) Uani 1 1 d . . . H27A H 0.4515 0.5919 0.0646 0.061 Uiso 1 1 calc R . . H27B H 0.4732 0.7192 0.0924 0.061 Uiso 1 1 calc R . . H27C H 0.4561 0.6343 0.1672 0.061 Uiso 1 1 calc R . . H1A H 0.6234(7) 0.219(3) -0.2503(19) 0.052(7) Uiso 1 1 d . . . H1B H 0.6161(8) 0.305(2) -0.145(2) 0.054(8) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag 0.03349(9) 0.02432(9) 0.01986(8) -0.00404(4) 0.00385(6) 0.00505(5) P 0.0214(2) 0.0208(2) 0.0168(2) -0.00107(15) 0.00216(15) 0.00266(16) N1 0.0455(10) 0.0305(8) 0.0308(9) 0.0104(7) 0.0170(7) 0.0143(7) N2 0.0345(8) 0.0264(8) 0.0302(8) -0.0019(6) 0.0106(7) 0.0020(6) N3 0.0450(9) 0.0366(9) 0.0180(7) 0.0026(6) 0.0008(6) 0.0205(7) N4 0.0322(8) 0.0266(8) 0.0183(7) 0.0006(6) -0.0005(6) 0.0104(6) N5 0.0305(9) 0.0451(10) 0.0408(10) -0.0175(8) 0.0049(7) -0.0029(7) N6 0.0274(8) 0.0344(9) 0.0447(10) 0.0091(7) -0.0066(7) 0.0045(7) O1 0.0356(8) 0.0900(14) 0.0338(8) -0.0127(8) 0.0064(6) 0.0054(8) O2 0.0293(8) 0.0893(14) 0.0529(10) -0.0311(10) 0.0002(7) 0.0055(8) O3 0.0355(7) 0.0602(10) 0.0323(8) 0.0136(7) -0.0028(6) -0.0025(7) O4 0.0338(8) 0.0328(8) 0.0844(13) 0.0072(8) -0.0051(8) -0.0028(6) B 0.0540(15) 0.0426(13) 0.0310(12) 0.0145(10) 0.0167(11) 0.0244(11) C1 0.0333(9) 0.0233(9) 0.0388(10) -0.0035(8) 0.0122(8) -0.0012(7) C2 0.0405(11) 0.0271(9) 0.0444(12) 0.0039(8) 0.0213(9) 0.0062(8) C3 0.0540(13) 0.0357(11) 0.0381(11) 0.0151(9) 0.0268(10) 0.0183(10) C4 0.0307(9) 0.0285(9) 0.0329(10) -0.0008(8) -0.0079(7) 0.0088(7) C5 0.0481(12) 0.0439(12) 0.0425(12) -0.0147(10) -0.0216(10) 0.0155(10) C6 0.0602(14) 0.0548(14) 0.0217(9) -0.0092(9) -0.0123(9) 0.0265(12) C7 0.0209(7) 0.0215(8) 0.0234(8) 0.0017(6) 0.0027(6) 0.0037(6) C8 0.0280(9) 0.0289(9) 0.0240(8) 0.0027(7) 0.0044(7) 0.0062(7) C9 0.0303(9) 0.0307(10) 0.0346(10) 0.0092(8) 0.0120(8) 0.0068(7) C10 0.0204(8) 0.0262(9) 0.0469(11) 0.0065(8) 0.0073(7) 0.0052(7) C11 0.0259(9) 0.0297(9) 0.0368(10) 0.0019(8) -0.0030(7) 0.0013(7) C12 0.0287(9) 0.0277(9) 0.0246(8) 0.0024(7) 0.0011(7) 0.0015(7) C13 0.0273(10) 0.0392(11) 0.0672(16) 0.0079(11) 0.0105(10) -0.0024(9) C14 0.0226(8) 0.0215(8) 0.0179(8) 0.0005(6) 0.0012(6) -0.0023(6) C15 0.0236(8) 0.0217(8) 0.0273(9) 0.0009(6) 0.0025(7) 0.0002(6) C16 0.0285(9) 0.0215(8) 0.0278(9) 0.0044(7) -0.0032(7) -0.0022(7) C17 0.0327(9) 0.0241(9) 0.0211(9) 0.0029(6) -0.0040(7) -0.0103(7) C18 0.0334(9) 0.0298(9) 0.0202(8) -0.0018(7) 0.0050(7) -0.0044(7) C19 0.0279(8) 0.0261(8) 0.0227(8) -0.0006(7) 0.0034(7) 0.0023(7) C20 0.0516(12) 0.0328(10) 0.0218(9) 0.0053(8) -0.0037(8) -0.0127(9) C21 0.0238(8) 0.0245(8) 0.0142(7) -0.0001(6) 0.0017(6) 0.0045(6) C22 0.0275(8) 0.0270(9) 0.0232(8) -0.0025(7) 0.0016(7) 0.0033(7) C23 0.0350(10) 0.0273(9) 0.0291(9) 0.0019(7) 0.0054(7) 0.0090(7) C24 0.0264(9) 0.0424(11) 0.0199(8) 0.0067(7) 0.0055(7) 0.0113(8) C25 0.0214(8) 0.0424(11) 0.0304(9) 0.0015(8) 0.0022(7) 0.0012(8) C26 0.0269(9) 0.0283(9) 0.0283(9) -0.0012(7) 0.0021(7) 0.0013(7) C27 0.0299(10) 0.0547(13) 0.0374(11) 0.0121(10) 0.0088(8) 0.0167(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 Ag N4 2.2481(15) . ? Ag P 2.3512(4) . ? Ag N2 2.3539(15) . ? P C14 1.8147(17) . ? P C21 1.8183(17) . ? P C7 1.8226(17) . ? N1 N2 1.346(2) . ? N1 C3 1.355(3) . ? N1 B 1.563(3) . ? N2 C1 1.333(3) . ? N3 C6 1.351(3) . ? N3 N4 1.352(2) . ? N3 B 1.553(3) . ? N4 C4 1.332(3) . ? N5 O1 1.225(2) . ? N5 O2 1.228(2) . ? N5 C1 1.439(3) . ? N6 O3 1.228(2) . ? N6 O4 1.233(2) . ? N6 C4 1.436(3) . ? B H1A 1.11(3) . ? B H1B 1.11(3) . ? C1 C2 1.388(3) . ? C2 C3 1.373(3) . ? C2 H2 0.9500 . ? C3 H3 0.9500 . ? C4 C5 1.389(3) . ? C5 C6 1.357(4) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.392(2) . ? C7 C8 1.401(2) . ? C8 C9 1.385(3) . ? C8 H8 0.9500 . ? C9 C10 1.390(3) . ? C9 H9 0.9500 . ? C10 C11 1.391(3) . ? C10 C13 1.512(3) . ? C11 C12 1.389(3) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C19 1.394(2) . ? C14 C15 1.398(2) . ? C15 C16 1.394(3) . ? C15 H15 0.9500 . ? C16 C17 1.388(3) . ? C16 H16 0.9500 . ? C17 C18 1.395(3) . ? C17 C20 1.509(2) . ? C18 C19 1.394(3) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.390(2) . ? C21 C26 1.395(2) . ? C22 C23 1.391(3) . ? C22 H22 0.9500 . ? C23 C24 1.387(3) . ? C23 H23 0.9500 . ? C24 C25 1.390(3) . ? C24 C27 1.508(2) . ? C25 C26 1.391(3) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 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 N4 Ag P 146.31(4) . . ? N4 Ag N2 84.70(6) . . ? P Ag N2 124.60(4) . . ? C14 P C21 104.96(7) . . ? C14 P C7 104.32(8) . . ? C21 P C7 105.40(8) . . ? C14 P Ag 120.07(6) . . ? C21 P Ag 110.70(5) . . ? C7 P Ag 110.27(6) . . ? N2 N1 C3 110.34(18) . . ? N2 N1 B 120.04(16) . . ? C3 N1 B 129.56(18) . . ? C1 N2 N1 104.65(15) . . ? C1 N2 Ag 137.89(14) . . ? N1 N2 Ag 117.04(12) . . ? C6 N3 N4 109.92(19) . . ? C6 N3 B 129.21(19) . . ? N4 N3 B 120.86(17) . . ? C4 N4 N3 104.77(15) . . ? C4 N4 Ag 136.37(13) . . ? N3 N4 Ag 118.74(12) . . ? O1 N5 O2 124.09(19) . . ? O1 N5 C1 119.32(17) . . ? O2 N5 C1 116.59(17) . . ? O3 N6 O4 124.51(19) . . ? O3 N6 C4 118.68(17) . . ? O4 N6 C4 116.81(18) . . ? N3 B N1 108.86(16) . . ? N3 B H1A 106.0(14) . . ? N1 B H1A 109.6(14) . . ? N3 B H1B 108.8(15) . . ? N1 B H1B 109.1(15) . . ? H1A B H1B 114(2) . . ? N2 C1 C2 113.30(19) . . ? N2 C1 N5 119.53(17) . . ? C2 C1 N5 127.15(18) . . ? C3 C2 C1 102.59(17) . . ? C3 C2 H2 128.7 . . ? C1 C2 H2 128.7 . . ? N1 C3 C2 109.11(18) . . ? N1 C3 H3 125.4 . . ? C2 C3 H3 125.4 . . ? N4 C4 C5 112.6(2) . . ? N4 C4 N6 119.52(17) . . ? C5 C4 N6 127.9(2) . . ? C6 C5 C4 103.2(2) . . ? C6 C5 H5 128.4 . . ? C4 C5 H5 128.4 . . ? N3 C6 C5 109.46(19) . . ? N3 C6 H6 125.3 . . ? C5 C6 H6 125.3 . . ? C12 C7 C8 118.56(16) . . ? C12 C7 P 123.21(13) . . ? C8 C7 P 118.23(13) . . ? C9 C8 C7 120.36(17) . . ? C9 C8 H8 119.8 . . ? C7 C8 H8 119.8 . . ? C8 C9 C10 121.28(17) . . ? C8 C9 H9 119.4 . . ? C10 C9 H9 119.4 . . ? C9 C10 C11 118.13(17) . . ? C9 C10 C13 121.32(19) . . ? C11 C10 C13 120.6(2) . . ? C12 C11 C10 121.23(18) . . ? C12 C11 H11 119.4 . . ? C10 C11 H11 119.4 . . ? C11 C12 C7 120.40(17) . . ? C11 C12 H12 119.8 . . ? C7 C12 H12 119.8 . . ? C10 C13 H13A 109.5 . . ? C10 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C10 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C19 C14 C15 119.18(16) . . ? C19 C14 P 122.43(13) . . ? C15 C14 P 118.35(13) . . ? C16 C15 C14 119.67(17) . . ? C16 C15 H15 120.2 . . ? C14 C15 H15 120.2 . . ? C17 C16 C15 121.64(17) . . ? C17 C16 H16 119.2 . . ? C15 C16 H16 119.2 . . ? C16 C17 C18 118.27(16) . . ? C16 C17 C20 120.54(17) . . ? C18 C17 C20 121.19(18) . . ? C19 C18 C17 120.88(17) . . ? C19 C18 H18 119.6 . . ? C17 C18 H18 119.6 . . ? C14 C19 C18 120.34(17) . . ? C14 C19 H19 119.8 . . ? C18 C19 H19 119.8 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 C26 119.09(16) . . ? C22 C21 P 122.97(13) . . ? C26 C21 P 117.92(13) . . ? C21 C22 C23 120.05(17) . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C24 C23 C22 121.34(18) . . ? C24 C23 H23 119.3 . . ? C22 C23 H23 119.3 . . ? C23 C24 C25 118.32(17) . . ? C23 C24 C27 120.92(19) . . ? C25 C24 C27 120.77(19) . . ? C24 C25 C26 121.01(18) . . ? C24 C25 H25 119.5 . . ? C26 C25 H25 119.5 . . ? C25 C26 C21 120.17(17) . . ? C25 C26 H26 119.9 . . ? C21 C26 H26 119.9 . . ? C24 C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C24 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.585 _refine_diff_density_min -0.359 _refine_diff_density_rms 0.065 #===END data_dias452s _database_code_depnum_ccdc_archive 'CCDC 649311' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (H2B(3-(CF3)Pz)2)AgPPh3 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H21 Ag B F6 N4 P' _chemical_formula_weight 653.12 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.8365(6) _cell_length_b 15.3387(9) _cell_length_c 18.2405(11) _cell_angle_alpha 68.022(1) _cell_angle_beta 82.255(1) _cell_angle_gamma 70.454(1) _cell_volume 2649.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8176 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 28.35 _exptl_crystal_description blocks _exptl_crystal_colour colorless _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.637 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1304 _exptl_absorpt_coefficient_mu 0.887 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7135 _exptl_absorpt_correction_T_max 0.8495 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19101 _diffrn_reflns_av_R_equivalents 0.0200 _diffrn_reflns_av_sigmaI/netI 0.0309 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 26.00 _reflns_number_total 10115 _reflns_number_gt 9072 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0553P)^2^+2.9065P] 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 10115 _refine_ls_number_parameters 747 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0416 _refine_ls_R_factor_gt 0.0378 _refine_ls_wR_factor_ref 0.1017 _refine_ls_wR_factor_gt 0.0971 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.283618(19) 0.349125(14) 0.086548(11) 0.02484(7) Uani 1 1 d . . . Ag2 Ag 0.80838(2) 0.360338(15) 0.579327(12) 0.02710(8) Uani 1 1 d . . . B1 B 0.0187(3) 0.4810(3) 0.1324(2) 0.0305(7) Uani 1 1 d . . . B2 B 0.5379(3) 0.4824(2) 0.63697(19) 0.0284(7) Uani 1 1 d . . . N1 N 0.1065(2) 0.43594(17) 0.20622(13) 0.0255(5) Uani 1 1 d . . . N2 N 0.2236(2) 0.36529(16) 0.20829(13) 0.0246(5) Uani 1 1 d . . . N3 N 0.0787(2) 0.55333(17) 0.06344(14) 0.0266(5) Uani 1 1 d . . . N4 N 0.1913(2) 0.51572(16) 0.02788(13) 0.0249(5) Uani 1 1 d . . . N5 N 0.6354(2) 0.43811(16) 0.70660(13) 0.0232(5) Uani 1 1 d . . . N6 N 0.7521(2) 0.36865(16) 0.70466(13) 0.0233(5) Uani 1 1 d . . . N7 N 0.5875(2) 0.55699(17) 0.56434(14) 0.0264(5) Uani 1 1 d . . . N8 N 0.6989(2) 0.52355(17) 0.52561(13) 0.0273(5) Uani 1 1 d . . . P1 P 0.38062(6) 0.20707(5) 0.05173(4) 0.02022(14) Uani 1 1 d . . . P2 P 0.89602(6) 0.21811(5) 0.54313(4) 0.02041(14) Uani 1 1 d . . . C1 C 0.2718(3) 0.3380(2) 0.28006(16) 0.0258(6) Uani 1 1 d . . . C2 C 0.1872(3) 0.3898(2) 0.32537(17) 0.0307(6) Uani 1 1 d . . . H2 H 0.1984 0.3842 0.3779 0.037 Uiso 1 1 calc R . . C3 C 0.0838(3) 0.4509(2) 0.27562(17) 0.0309(6) Uani 1 1 d . . . H3 H 0.0081 0.4965 0.2883 0.037 Uiso 1 1 calc R . . C4 C 0.3999(3) 0.2604(2) 0.30362(17) 0.0332(6) Uani 1 1 d . . . C5 C 0.2171(3) 0.5945(2) -0.02872(16) 0.0290(6) Uani 1 1 d . . . C6 C 0.1215(3) 0.6824(2) -0.02922(19) 0.0362(7) Uani 1 1 d . . . H6 H 0.1167 0.7479 -0.0630 0.043 Uiso 1 1 calc R . . C7 C 0.0358(3) 0.6525(2) 0.03028(18) 0.0341(7) Uani 1 1 d . . . H7 H -0.0410 0.6949 0.0455 0.041 Uiso 1 1 calc R . . C8 C 0.3340(3) 0.5823(2) -0.07989(18) 0.0378(7) Uani 1 1 d . . . C9 C 0.4320(3) 0.22828(19) -0.05111(15) 0.0222(5) Uani 1 1 d . . . C10 C 0.5501(3) 0.1717(2) -0.07339(16) 0.0266(6) Uani 1 1 d . . . H10 H 0.6086 0.1201 -0.0342 0.032 Uiso 1 1 calc R . . C11 C 0.5824(3) 0.1909(2) -0.15343(17) 0.0314(6) Uani 1 1 d . . . H11 H 0.6637 0.1530 -0.1686 0.038 Uiso 1 1 calc R . . C12 C 0.4961(3) 0.2651(2) -0.21081(17) 0.0340(7) Uani 1 1 d . . . H12 H 0.5172 0.2767 -0.2652 0.041 Uiso 1 1 calc R . . C13 C 0.3788(3) 0.3227(2) -0.18861(17) 0.0334(6) Uani 1 1 d . . . H13 H 0.3200 0.3737 -0.2279 0.040 Uiso 1 1 calc R . . C14 C 0.3477(3) 0.3056(2) -0.10924(16) 0.0279(6) Uani 1 1 d . . . H14 H 0.2689 0.3465 -0.0943 0.033 Uiso 1 1 calc R . . C15 C 0.2640(3) 0.13831(19) 0.06841(16) 0.0242(5) Uani 1 1 d . . . C16 C 0.2427(3) 0.1016(2) 0.01386(17) 0.0282(6) Uani 1 1 d . . . H16 H 0.2903 0.1119 -0.0347 0.034 Uiso 1 1 calc R . . C17 C 0.1524(3) 0.0499(2) 0.0294(2) 0.0363(7) Uani 1 1 d . . . H17 H 0.1376 0.0260 -0.0087 0.044 Uiso 1 1 calc R . . C18 C 0.0839(3) 0.0335(2) 0.1010(2) 0.0379(7) Uani 1 1 d . . . H18 H 0.0228 -0.0023 0.1123 0.045 Uiso 1 1 calc R . . C19 C 0.1053(3) 0.0695(2) 0.15557(19) 0.0399(7) Uani 1 1 d . . . H19 H 0.0590 0.0579 0.2046 0.048 Uiso 1 1 calc R . . C20 C 0.1938(3) 0.1226(2) 0.13962(17) 0.0330(6) Uani 1 1 d . . . H20 H 0.2064 0.1481 0.1772 0.040 Uiso 1 1 calc R . . C21 C 0.5238(3) 0.11657(19) 0.10766(15) 0.0223(5) Uani 1 1 d . . . C22 C 0.6148(3) 0.1508(2) 0.12644(18) 0.0329(6) Uani 1 1 d . . . H22 H 0.6002 0.2199 0.1104 0.040 Uiso 1 1 calc R . . C23 C 0.7268(3) 0.0846(2) 0.1685(2) 0.0400(7) Uani 1 1 d . . . H23 H 0.7887 0.1088 0.1806 0.048 Uiso 1 1 calc R . . C24 C 0.7485(3) -0.0165(2) 0.19285(18) 0.0372(7) Uani 1 1 d . . . H24 H 0.8247 -0.0614 0.2220 0.045 Uiso 1 1 calc R . . C25 C 0.6588(3) -0.0516(2) 0.17462(16) 0.0304(6) Uani 1 1 d . . . H25 H 0.6736 -0.1208 0.1912 0.037 Uiso 1 1 calc R . . C26 C 0.5468(3) 0.01449(19) 0.13189(15) 0.0245(5) Uani 1 1 d . . . H26 H 0.4858 -0.0099 0.1192 0.029 Uiso 1 1 calc R . . C27 C 0.8059(3) 0.3388(2) 0.77568(16) 0.0265(6) Uani 1 1 d . . . C28 C 0.7250(3) 0.3876(2) 0.82413(17) 0.0292(6) Uani 1 1 d . . . H28 H 0.7401 0.3796 0.8767 0.035 Uiso 1 1 calc R . . C29 C 0.6180(3) 0.4500(2) 0.77722(16) 0.0276(6) Uani 1 1 d . . . H29 H 0.5437 0.4945 0.7923 0.033 Uiso 1 1 calc R . . C30 C 0.9341(3) 0.2608(2) 0.79541(18) 0.0350(7) Uani 1 1 d . . . C31 C 0.7083(3) 0.6028(2) 0.46340(17) 0.0350(7) Uani 1 1 d . A . C32 C 0.6033(4) 0.6862(2) 0.46156(19) 0.0428(8) Uani 1 1 d . . . H32 H 0.5864 0.7512 0.4235 0.051 Uiso 1 1 calc R . . C33 C 0.5298(3) 0.6532(2) 0.52712(18) 0.0363(7) Uani 1 1 d . . . H33 H 0.4508 0.6925 0.5433 0.044 Uiso 1 1 calc R . . C34 C 0.8177(4) 0.5944(3) 0.4064(2) 0.0509(10) Uani 1 1 d . . . C35 C 0.9143(3) 0.23726(19) 0.43784(15) 0.0225(5) Uani 1 1 d . . . C36 C 1.0146(3) 0.1749(2) 0.40724(17) 0.0276(6) Uani 1 1 d . . . H36 H 1.0762 0.1191 0.4418 0.033 Uiso 1 1 calc R . . C37 C 1.0247(3) 0.1943(2) 0.32610(17) 0.0325(6) Uani 1 1 d . . . H37 H 1.0943 0.1526 0.3055 0.039 Uiso 1 1 calc R . . C38 C 0.9340(3) 0.2739(2) 0.27541(17) 0.0359(7) Uani 1 1 d . . . H38 H 0.9403 0.2859 0.2202 0.043 Uiso 1 1 calc R . . C39 C 0.8336(3) 0.3362(2) 0.30513(17) 0.0351(7) Uani 1 1 d . . . H39 H 0.7709 0.3907 0.2703 0.042 Uiso 1 1 calc R . . C40 C 0.8248(3) 0.3190(2) 0.38596(16) 0.0272(6) Uani 1 1 d . . . H40 H 0.7575 0.3629 0.4059 0.033 Uiso 1 1 calc R . . C41 C 0.7826(2) 0.14620(19) 0.58141(16) 0.0236(5) Uani 1 1 d . . . C42 C 0.7268(3) 0.1409(2) 0.65576(17) 0.0316(6) Uani 1 1 d . . . H42 H 0.7445 0.1777 0.6828 0.038 Uiso 1 1 calc R . . C43 C 0.6457(3) 0.0826(2) 0.69083(18) 0.0361(7) Uani 1 1 d . . . H43 H 0.6098 0.0785 0.7421 0.043 Uiso 1 1 calc R . . C44 C 0.6171(3) 0.0310(2) 0.65141(19) 0.0348(7) Uani 1 1 d . . . H44 H 0.5617 -0.0089 0.6755 0.042 Uiso 1 1 calc R . . C45 C 0.6692(3) 0.0369(2) 0.57653(19) 0.0353(7) Uani 1 1 d . . . H45 H 0.6487 0.0015 0.5494 0.042 Uiso 1 1 calc R . . C46 C 0.7518(3) 0.0949(2) 0.54085(18) 0.0297(6) Uani 1 1 d . . . H46 H 0.7868 0.0994 0.4894 0.036 Uiso 1 1 calc R . . C47 C 1.0537(3) 0.1284(2) 0.58114(16) 0.0244(5) Uani 1 1 d . . . C48 C 1.1644(3) 0.1608(2) 0.56189(19) 0.0342(7) Uani 1 1 d . . . H48 H 1.1544 0.2292 0.5361 0.041 Uiso 1 1 calc R . . C49 C 1.2888(3) 0.0931(2) 0.5803(2) 0.0407(7) Uani 1 1 d . . . H49 H 1.3636 0.1153 0.5662 0.049 Uiso 1 1 calc R . . C50 C 1.3041(3) -0.0070(2) 0.6193(2) 0.0412(8) Uani 1 1 d . . . H50 H 1.3892 -0.0532 0.6317 0.049 Uiso 1 1 calc R . . C51 C 1.1941(3) -0.0394(2) 0.64016(18) 0.0346(7) Uani 1 1 d . . . H51 H 1.2041 -0.1075 0.6681 0.041 Uiso 1 1 calc R . . C52 C 1.0697(3) 0.0276(2) 0.62015(16) 0.0263(6) Uani 1 1 d . . . H52 H 0.9953 0.0049 0.6330 0.032 Uiso 1 1 calc R . . F1 F 0.4998(2) 0.29615(18) 0.29242(18) 0.0764(8) Uani 1 1 d . . . F2 F 0.4305(2) 0.19776(17) 0.26521(14) 0.0692(8) Uani 1 1 d . . . F3 F 0.4033(2) 0.20581(17) 0.38042(12) 0.0605(6) Uani 1 1 d . . . F4 F 0.3778(3) 0.49575(18) -0.08776(16) 0.0705(8) Uani 1 1 d . . . F5 F 0.43548(19) 0.59444(15) -0.05384(12) 0.0457(5) Uani 1 1 d . . . F6 F 0.3092(2) 0.65424(19) -0.15230(12) 0.0615(6) Uani 1 1 d . . . F7 F 1.0331(2) 0.29659(17) 0.79145(15) 0.0612(6) Uani 1 1 d . . . F8 F 0.9662(3) 0.20723(19) 0.74926(16) 0.0839(10) Uani 1 1 d . . . F9 F 0.9370(2) 0.19787(15) 0.86997(12) 0.0535(5) Uani 1 1 d . . . F10 F 0.8204(6) 0.5345(4) 0.3732(3) 0.074(2) Uani 0.642(7) 1 d P A 1 F11 F 0.9209(5) 0.5849(4) 0.4347(3) 0.0615(17) Uani 0.642(7) 1 d P A 1 F12 F 0.7863(4) 0.6874(3) 0.3437(2) 0.0564(12) Uani 0.642(7) 1 d P A 1 F10A F 0.9243(7) 0.4890(5) 0.4323(4) 0.067(3) Uani 0.358(7) 1 d P A 2 F12A F 0.8075(9) 0.5979(15) 0.3404(6) 0.136(8) Uani 0.358(7) 1 d P A 2 F11A F 0.9138(12) 0.6330(10) 0.4033(9) 0.112(6) Uani 0.358(7) 1 d P A 2 H2A H 0.533(3) 0.417(2) 0.6174(18) 0.028(8) Uiso 1 1 d . . . H1A H 0.015(3) 0.419(2) 0.1120(19) 0.035(9) Uiso 1 1 d . . . H2B H 0.445(4) 0.525(3) 0.654(2) 0.042(10) Uiso 1 1 d . . . H1B H -0.081(4) 0.527(3) 0.146(2) 0.046(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 Ag1 0.02611(12) 0.02189(12) 0.02577(12) -0.01174(9) 0.00043(8) -0.00295(8) Ag2 0.02699(12) 0.02721(12) 0.03004(13) -0.01681(9) 0.00314(8) -0.00571(9) B1 0.0233(16) 0.0326(17) 0.0327(17) -0.0107(14) 0.0006(13) -0.0065(13) B2 0.0226(15) 0.0279(16) 0.0273(16) -0.0057(13) -0.0001(12) -0.0030(12) N1 0.0233(11) 0.0245(11) 0.0269(12) -0.0107(9) 0.0036(9) -0.0048(9) N2 0.0269(12) 0.0203(11) 0.0226(11) -0.0071(9) 0.0019(9) -0.0038(9) N3 0.0250(12) 0.0225(11) 0.0287(12) -0.0094(10) -0.0043(9) -0.0008(9) N4 0.0266(12) 0.0226(11) 0.0237(11) -0.0075(9) -0.0023(9) -0.0052(9) N5 0.0238(11) 0.0210(11) 0.0218(11) -0.0079(9) 0.0016(9) -0.0034(9) N6 0.0229(11) 0.0219(11) 0.0212(11) -0.0075(9) 0.0002(9) -0.0024(9) N7 0.0288(12) 0.0221(11) 0.0247(12) -0.0085(9) -0.0023(9) -0.0025(9) N8 0.0343(13) 0.0245(12) 0.0240(12) -0.0096(9) 0.0024(10) -0.0101(10) P1 0.0205(3) 0.0188(3) 0.0194(3) -0.0076(2) -0.0001(2) -0.0027(3) P2 0.0206(3) 0.0210(3) 0.0190(3) -0.0088(3) -0.0005(2) -0.0035(3) C1 0.0333(15) 0.0217(13) 0.0208(13) -0.0064(10) 0.0017(11) -0.0089(11) C2 0.0400(17) 0.0283(14) 0.0256(14) -0.0124(12) 0.0046(12) -0.0113(13) C3 0.0327(15) 0.0290(14) 0.0310(15) -0.0157(12) 0.0101(12) -0.0079(12) C4 0.0394(17) 0.0274(15) 0.0273(15) -0.0081(12) -0.0048(12) -0.0035(13) C5 0.0376(16) 0.0279(14) 0.0230(14) -0.0065(11) -0.0048(11) -0.0130(12) C6 0.0518(19) 0.0209(14) 0.0336(16) -0.0048(12) -0.0141(14) -0.0084(13) C7 0.0392(17) 0.0209(14) 0.0357(16) -0.0086(12) -0.0129(13) 0.0018(12) C8 0.0500(19) 0.0391(17) 0.0275(15) -0.0074(13) -0.0004(13) -0.0228(15) C9 0.0270(13) 0.0209(12) 0.0201(12) -0.0076(10) 0.0021(10) -0.0098(10) C10 0.0271(14) 0.0230(13) 0.0276(14) -0.0076(11) 0.0021(11) -0.0074(11) C11 0.0369(16) 0.0318(15) 0.0303(15) -0.0155(12) 0.0116(12) -0.0160(13) C12 0.0498(18) 0.0336(16) 0.0240(14) -0.0103(12) 0.0075(13) -0.0226(14) C13 0.0434(17) 0.0299(15) 0.0254(15) -0.0046(12) -0.0043(12) -0.0139(13) C14 0.0280(14) 0.0252(14) 0.0267(14) -0.0077(11) -0.0016(11) -0.0048(11) C15 0.0200(12) 0.0203(12) 0.0261(13) -0.0051(10) -0.0018(10) -0.0014(10) C16 0.0247(14) 0.0263(14) 0.0331(15) -0.0119(12) 0.0013(11) -0.0060(11) C17 0.0310(15) 0.0322(16) 0.0478(18) -0.0171(14) -0.0025(13) -0.0081(12) C18 0.0294(15) 0.0322(16) 0.0488(19) -0.0065(14) -0.0036(13) -0.0132(13) C19 0.0329(16) 0.0475(19) 0.0326(16) -0.0032(14) 0.0035(13) -0.0178(14) C20 0.0289(15) 0.0413(17) 0.0264(15) -0.0090(12) 0.0013(11) -0.0118(13) C21 0.0214(13) 0.0228(13) 0.0204(12) -0.0081(10) -0.0002(10) -0.0034(10) C22 0.0344(16) 0.0280(15) 0.0370(16) -0.0095(12) -0.0046(12) -0.0112(12) C23 0.0301(16) 0.0422(18) 0.0475(19) -0.0140(15) -0.0090(13) -0.0096(13) C24 0.0280(15) 0.0395(17) 0.0354(16) -0.0102(13) -0.0047(12) -0.0014(13) C25 0.0325(15) 0.0239(14) 0.0274(14) -0.0068(11) -0.0003(11) -0.0019(11) C26 0.0268(14) 0.0235(13) 0.0207(13) -0.0069(10) 0.0008(10) -0.0059(11) C27 0.0304(14) 0.0235(13) 0.0249(14) -0.0093(11) -0.0011(11) -0.0063(11) C28 0.0366(16) 0.0317(15) 0.0229(14) -0.0130(11) 0.0021(11) -0.0121(12) C29 0.0290(14) 0.0265(14) 0.0275(14) -0.0127(11) 0.0066(11) -0.0079(11) C30 0.0382(17) 0.0326(16) 0.0300(15) -0.0123(13) -0.0085(13) -0.0013(13) C31 0.0544(19) 0.0362(16) 0.0250(15) -0.0133(12) 0.0027(13) -0.0257(15) C32 0.072(2) 0.0232(15) 0.0332(17) -0.0035(13) -0.0115(16) -0.0175(15) C33 0.0476(18) 0.0249(15) 0.0332(16) -0.0099(12) -0.0088(14) -0.0043(13) C34 0.076(3) 0.064(2) 0.0348(19) -0.0219(17) 0.0159(18) -0.050(2) C35 0.0255(13) 0.0239(13) 0.0196(12) -0.0083(10) 0.0005(10) -0.0092(11) C36 0.0283(14) 0.0277(14) 0.0281(14) -0.0128(11) 0.0039(11) -0.0084(11) C37 0.0381(16) 0.0347(16) 0.0288(15) -0.0153(12) 0.0100(12) -0.0157(13) C38 0.0538(19) 0.0399(17) 0.0193(14) -0.0088(12) 0.0044(13) -0.0248(15) C39 0.0425(17) 0.0330(16) 0.0252(15) -0.0035(12) -0.0062(12) -0.0116(13) C40 0.0263(14) 0.0265(14) 0.0258(14) -0.0090(11) -0.0009(11) -0.0045(11) C41 0.0179(12) 0.0216(13) 0.0275(14) -0.0078(10) 0.0000(10) -0.0025(10) C42 0.0340(15) 0.0349(15) 0.0275(14) -0.0112(12) 0.0028(12) -0.0137(12) C43 0.0349(16) 0.0428(17) 0.0292(15) -0.0094(13) 0.0076(12) -0.0168(14) C44 0.0268(15) 0.0351(16) 0.0408(17) -0.0073(13) -0.0006(12) -0.0141(12) C45 0.0327(16) 0.0357(16) 0.0436(18) -0.0186(14) 0.0001(13) -0.0130(13) C46 0.0247(14) 0.0321(15) 0.0349(16) -0.0168(12) 0.0019(11) -0.0073(12) C47 0.0241(13) 0.0250(13) 0.0247(13) -0.0105(11) -0.0062(10) -0.0045(11) C48 0.0305(15) 0.0284(15) 0.0440(18) -0.0126(13) -0.0064(13) -0.0072(12) C49 0.0288(16) 0.0388(17) 0.057(2) -0.0175(15) -0.0088(14) -0.0093(13) C50 0.0335(16) 0.0353(17) 0.054(2) -0.0166(15) -0.0173(15) -0.0025(13) C51 0.0367(16) 0.0267(15) 0.0396(17) -0.0111(13) -0.0150(13) -0.0039(12) C52 0.0313(14) 0.0257(14) 0.0215(13) -0.0090(11) -0.0044(11) -0.0058(11) F1 0.0349(12) 0.0495(14) 0.114(2) -0.0001(14) -0.0086(13) -0.0050(10) F2 0.0782(16) 0.0527(13) 0.0601(14) -0.0377(12) -0.0351(12) 0.0339(12) F3 0.0663(14) 0.0562(13) 0.0277(10) -0.0004(9) -0.0111(9) 0.0075(11) F4 0.0856(18) 0.0637(15) 0.0908(18) -0.0556(14) 0.0577(15) -0.0488(14) F5 0.0393(10) 0.0410(11) 0.0517(12) -0.0085(9) -0.0052(9) -0.0130(8) F6 0.0643(15) 0.0816(17) 0.0312(11) 0.0012(10) -0.0019(10) -0.0369(13) F7 0.0304(10) 0.0542(13) 0.0787(16) -0.0066(12) -0.0045(10) -0.0055(9) F8 0.0805(17) 0.0773(17) 0.0788(17) -0.0603(15) -0.0513(14) 0.0510(14) F9 0.0542(13) 0.0405(11) 0.0442(12) 0.0040(9) -0.0166(10) -0.0033(9) F10 0.094(4) 0.081(3) 0.090(5) -0.073(3) 0.064(4) -0.059(3) F11 0.032(2) 0.091(4) 0.049(2) -0.009(2) 0.0062(17) -0.023(2) F12 0.076(3) 0.052(2) 0.0310(18) -0.0036(15) 0.0191(17) -0.0262(19) F10A 0.060(5) 0.051(4) 0.053(4) -0.008(3) 0.033(3) 0.004(3) F12A 0.034(4) 0.32(2) 0.046(6) -0.080(10) -0.001(4) -0.025(9) F11A 0.090(8) 0.147(11) 0.196(14) -0.149(11) 0.114(10) -0.101(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 Ag1 N4 2.282(2) . ? Ag1 N2 2.309(2) . ? Ag1 P1 2.3621(7) . ? Ag2 N8 2.264(2) . ? Ag2 N6 2.325(2) . ? Ag2 P2 2.3706(7) . ? B1 N1 1.551(4) . ? B1 N3 1.566(4) . ? B1 H1A 1.16(3) . ? B1 H1B 1.13(4) . ? B2 N5 1.558(4) . ? B2 N7 1.562(4) . ? B2 H2A 1.20(3) . ? B2 H2B 1.07(4) . ? N1 C3 1.346(4) . ? N1 N2 1.359(3) . ? N2 C1 1.338(4) . ? N3 C7 1.345(4) . ? N3 N4 1.356(3) . ? N4 C5 1.349(4) . ? N5 C29 1.348(4) . ? N5 N6 1.360(3) . ? N6 C27 1.345(3) . ? N7 C33 1.333(4) . ? N7 N8 1.359(3) . ? N8 C31 1.340(4) . ? P1 C21 1.817(3) . ? P1 C9 1.821(3) . ? P1 C15 1.830(3) . ? P2 C41 1.821(3) . ? P2 C47 1.823(3) . ? P2 C35 1.824(3) . ? C1 C2 1.399(4) . ? C1 C4 1.483(4) . ? C2 C3 1.375(4) . ? C2 H2 0.9500 . ? C3 H3 0.9500 . ? C4 F2 1.324(4) . ? C4 F1 1.330(4) . ? C4 F3 1.334(4) . ? C5 C6 1.395(4) . ? C5 C8 1.472(5) . ? C6 C7 1.375(5) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 F4 1.308(4) . ? C8 F5 1.346(4) . ? C8 F6 1.357(4) . ? C9 C10 1.391(4) . ? C9 C14 1.400(4) . ? C10 C11 1.397(4) . ? C10 H10 0.9500 . ? C11 C12 1.388(4) . ? C11 H11 0.9500 . ? C12 C13 1.392(4) . ? C12 H12 0.9500 . ? C13 C14 1.387(4) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C16 1.388(4) . ? C15 C20 1.395(4) . ? C16 C17 1.395(4) . ? C16 H16 0.9500 . ? C17 C18 1.392(5) . ? C17 H17 0.9500 . ? C18 C19 1.382(5) . ? C18 H18 0.9500 . ? C19 C20 1.393(4) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C22 1.391(4) . ? C21 C26 1.400(4) . ? C22 C23 1.391(4) . ? C22 H22 0.9500 . ? C23 C24 1.388(5) . ? C23 H23 0.9500 . ? C24 C25 1.385(4) . ? C24 H24 0.9500 . ? C25 C26 1.396(4) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C28 1.399(4) . ? C27 C30 1.481(4) . ? C28 C29 1.381(4) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? C30 F8 1.324(4) . ? C30 F9 1.338(4) . ? C30 F7 1.341(4) . ? C31 C32 1.391(5) . ? C31 C34 1.473(5) . ? C32 C33 1.371(5) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 F12A 1.204(9) . ? C34 F11 1.236(6) . ? C34 F10 1.267(5) . ? C34 F11A 1.344(10) . ? C34 F12 1.420(5) . ? C34 F10A 1.581(8) . ? C35 C36 1.396(4) . ? C35 C40 1.398(4) . ? C36 C37 1.393(4) . ? C36 H36 0.9500 . ? C37 C38 1.381(4) . ? C37 H37 0.9500 . ? C38 C39 1.387(5) . ? C38 H38 0.9500 . ? C39 C40 1.393(4) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C41 C42 1.393(4) . ? C41 C46 1.398(4) . ? C42 C43 1.389(4) . ? C42 H42 0.9500 . ? C43 C44 1.375(4) . ? C43 H43 0.9500 . ? C44 C45 1.388(5) . ? C44 H44 0.9500 . ? C45 C46 1.399(4) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C47 C52 1.399(4) . ? C47 C48 1.401(4) . ? C48 C49 1.390(4) . ? C48 H48 0.9500 . ? C49 C50 1.392(5) . ? C49 H49 0.9500 . ? C50 C51 1.395(5) . ? C50 H50 0.9500 . ? C51 C52 1.389(4) . ? C51 H51 0.9500 . ? C52 H52 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Ag1 N2 89.05(8) . . ? N4 Ag1 P1 139.73(6) . . ? N2 Ag1 P1 130.93(6) . . ? N8 Ag2 N6 89.44(8) . . ? N8 Ag2 P2 140.12(6) . . ? N6 Ag2 P2 128.52(6) . . ? N1 B1 N3 109.2(2) . . ? N1 B1 H1A 109.9(16) . . ? N3 B1 H1A 108.3(17) . . ? N1 B1 H1B 109.6(19) . . ? N3 B1 H1B 106.6(19) . . ? H1A B1 H1B 113(2) . . ? N5 B2 N7 109.8(2) . . ? N5 B2 H2A 109.2(15) . . ? N7 B2 H2A 107.8(15) . . ? N5 B2 H2B 109.2(19) . . ? N7 B2 H2B 105.8(19) . . ? H2A B2 H2B 115(2) . . ? C3 N1 N2 109.9(2) . . ? C3 N1 B1 130.2(2) . . ? N2 N1 B1 119.8(2) . . ? C1 N2 N1 105.6(2) . . ? C1 N2 Ag1 141.36(19) . . ? N1 N2 Ag1 112.29(16) . . ? C7 N3 N4 110.5(2) . . ? C7 N3 B1 130.3(3) . . ? N4 N3 B1 119.2(2) . . ? C5 N4 N3 105.5(2) . . ? C5 N4 Ag1 140.53(19) . . ? N3 N4 Ag1 113.68(16) . . ? C29 N5 N6 110.1(2) . . ? C29 N5 B2 129.3(2) . . ? N6 N5 B2 120.2(2) . . ? C27 N6 N5 105.4(2) . . ? C27 N6 Ag2 140.37(18) . . ? N5 N6 Ag2 113.05(15) . . ? C33 N7 N8 110.7(2) . . ? C33 N7 B2 129.3(3) . . ? N8 N7 B2 119.7(2) . . ? C31 N8 N7 105.2(2) . . ? C31 N8 Ag2 139.2(2) . . ? N7 N8 Ag2 115.61(16) . . ? C21 P1 C9 104.13(12) . . ? C21 P1 C15 104.24(12) . . ? C9 P1 C15 104.45(12) . . ? C21 P1 Ag1 116.25(9) . . ? C9 P1 Ag1 116.43(9) . . ? C15 P1 Ag1 110.03(9) . . ? C41 P2 C47 103.29(12) . . ? C41 P2 C35 105.64(12) . . ? C47 P2 C35 101.79(12) . . ? C41 P2 Ag2 106.50(9) . . ? C47 P2 Ag2 120.47(9) . . ? C35 P2 Ag2 117.49(9) . . ? N2 C1 C2 111.8(2) . . ? N2 C1 C4 120.5(2) . . ? C2 C1 C4 127.7(3) . . ? C3 C2 C1 103.3(2) . . ? C3 C2 H2 128.3 . . ? C1 C2 H2 128.3 . . ? N1 C3 C2 109.5(2) . . ? N1 C3 H3 125.3 . . ? C2 C3 H3 125.3 . . ? F2 C4 F1 106.3(3) . . ? F2 C4 F3 106.3(3) . . ? F1 C4 F3 104.6(3) . . ? F2 C4 C1 113.1(2) . . ? F1 C4 C1 113.6(3) . . ? F3 C4 C1 112.4(3) . . ? N4 C5 C6 111.0(3) . . ? N4 C5 C8 121.1(3) . . ? C6 C5 C8 127.9(3) . . ? C7 C6 C5 104.3(3) . . ? C7 C6 H6 127.9 . . ? C5 C6 H6 127.9 . . ? N3 C7 C6 108.7(3) . . ? N3 C7 H7 125.6 . . ? C6 C7 H7 125.6 . . ? F4 C8 F5 106.2(3) . . ? F4 C8 F6 109.4(3) . . ? F5 C8 F6 103.9(2) . . ? F4 C8 C5 113.9(3) . . ? F5 C8 C5 112.9(3) . . ? F6 C8 C5 110.0(3) . . ? C10 C9 C14 119.6(2) . . ? C10 C9 P1 122.9(2) . . ? C14 C9 P1 117.5(2) . . ? C9 C10 C11 119.9(3) . . ? C9 C10 H10 120.0 . . ? C11 C10 H10 120.0 . . ? C12 C11 C10 120.2(3) . . ? C12 C11 H11 119.9 . . ? C10 C11 H11 119.9 . . ? C11 C12 C13 120.0(3) . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? C14 C13 C12 120.1(3) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C13 C14 C9 120.1(3) . . ? C13 C14 H14 119.9 . . ? C9 C14 H14 119.9 . . ? C16 C15 C20 119.1(3) . . ? C16 C15 P1 123.2(2) . . ? C20 C15 P1 117.7(2) . . ? C15 C16 C17 120.9(3) . . ? C15 C16 H16 119.6 . . ? C17 C16 H16 119.6 . . ? C18 C17 C16 119.7(3) . . ? C18 C17 H17 120.1 . . ? C16 C17 H17 120.1 . . ? C19 C18 C17 119.6(3) . . ? C19 C18 H18 120.2 . . ? C17 C18 H18 120.2 . . ? C18 C19 C20 120.8(3) . . ? C18 C19 H19 119.6 . . ? C20 C19 H19 119.6 . . ? C19 C20 C15 119.9(3) . . ? C19 C20 H20 120.0 . . ? C15 C20 H20 120.0 . . ? C22 C21 C26 118.9(2) . . ? C22 C21 P1 118.2(2) . . ? C26 C21 P1 122.9(2) . . ? C23 C22 C21 120.5(3) . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C24 C23 C22 120.3(3) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C25 C24 C23 119.8(3) . . ? C25 C24 H24 120.1 . . ? C23 C24 H24 120.1 . . ? C24 C25 C26 120.1(3) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? C25 C26 C21 120.3(3) . . ? C25 C26 H26 119.8 . . ? C21 C26 H26 119.8 . . ? N6 C27 C28 111.8(2) . . ? N6 C27 C30 120.4(2) . . ? C28 C27 C30 127.8(3) . . ? C29 C28 C27 103.4(2) . . ? C29 C28 H28 128.3 . . ? C27 C28 H28 128.3 . . ? N5 C29 C28 109.3(2) . . ? N5 C29 H29 125.3 . . ? C28 C29 H29 125.3 . . ? F8 C30 F9 106.9(3) . . ? F8 C30 F7 107.2(3) . . ? F9 C30 F7 104.0(2) . . ? F8 C30 C27 113.0(2) . . ? F9 C30 C27 112.0(3) . . ? F7 C30 C27 113.1(3) . . ? N8 C31 C32 111.2(3) . . ? N8 C31 C34 120.7(3) . . ? C32 C31 C34 128.1(3) . . ? C33 C32 C31 104.3(3) . . ? C33 C32 H32 127.9 . . ? C31 C32 H32 127.9 . . ? N7 C33 C32 108.7(3) . . ? N7 C33 H33 125.6 . . ? C32 C33 H33 125.6 . . ? F12A C34 F11 124.4(6) . . ? F12A C34 F10 42.9(9) . . ? F11 C34 F10 117.6(6) . . ? F12A C34 F11A 106.3(9) . . ? F11 C34 F11A 32.6(7) . . ? F10 C34 F11A 125.6(5) . . ? F12A C34 F12 60.6(10) . . ? F11 C34 F12 106.1(4) . . ? F10 C34 F12 103.4(4) . . ? F11A C34 F12 73.5(8) . . ? F12A C34 C31 124.3(6) . . ? F11 C34 C31 111.2(4) . . ? F10 C34 C31 112.1(3) . . ? F11A C34 C31 121.2(5) . . ? F12 C34 C31 105.1(4) . . ? F12A C34 F10A 94.7(9) . . ? F11 C34 F10A 61.9(5) . . ? F10 C34 F10A 60.8(5) . . ? F11A C34 F10A 87.9(7) . . ? F12 C34 F10A 141.6(4) . . ? C31 C34 F10A 113.2(3) . . ? C36 C35 C40 119.1(2) . . ? C36 C35 P2 122.8(2) . . ? C40 C35 P2 118.1(2) . . ? C37 C36 C35 120.1(3) . . ? C37 C36 H36 120.0 . . ? C35 C36 H36 120.0 . . ? C38 C37 C36 120.5(3) . . ? C38 C37 H37 119.8 . . ? C36 C37 H37 119.8 . . ? C37 C38 C39 120.0(3) . . ? C37 C38 H38 120.0 . . ? C39 C38 H38 120.0 . . ? C38 C39 C40 120.0(3) . . ? C38 C39 H39 120.0 . . ? C40 C39 H39 120.0 . . ? C39 C40 C35 120.4(3) . . ? C39 C40 H40 119.8 . . ? C35 C40 H40 119.8 . . ? C42 C41 C46 119.1(3) . . ? C42 C41 P2 117.5(2) . . ? C46 C41 P2 123.3(2) . . ? C43 C42 C41 120.8(3) . . ? C43 C42 H42 119.6 . . ? C41 C42 H42 119.6 . . ? C44 C43 C42 120.0(3) . . ? C44 C43 H43 120.0 . . ? C42 C43 H43 120.0 . . ? C43 C44 C45 120.1(3) . . ? C43 C44 H44 119.9 . . ? C45 C44 H44 119.9 . . ? C44 C45 C46 120.3(3) . . ? C44 C45 H45 119.8 . . ? C46 C45 H45 119.8 . . ? C41 C46 C45 119.6(3) . . ? C41 C46 H46 120.2 . . ? C45 C46 H46 120.2 . . ? C52 C47 C48 119.2(3) . . ? C52 C47 P2 122.4(2) . . ? C48 C47 P2 117.9(2) . . ? C49 C48 C47 120.3(3) . . ? C49 C48 H48 119.9 . . ? C47 C48 H48 119.9 . . ? C48 C49 C50 120.2(3) . . ? C48 C49 H49 119.9 . . ? C50 C49 H49 119.9 . . ? C49 C50 C51 119.8(3) . . ? C49 C50 H50 120.1 . . ? C51 C50 H50 120.1 . . ? C52 C51 C50 120.2(3) . . ? C52 C51 H51 119.9 . . ? C50 C51 H51 119.9 . . ? C51 C52 C47 120.3(3) . . ? C51 C52 H52 119.9 . . ? C47 C52 H52 119.9 . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 1.993 _refine_diff_density_min -0.693 _refine_diff_density_rms 0.094 #===END