Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global #============================================================================== _journal_coden_Cambridge 222 _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? #======================================================================= # 1. SUBMISSION DETAILS #---------------------- _publ_contact_author_name 'Prof Claudio Pettinari' _publ_contact_author_address ; Dipartimento di Scienze Chimiche University of Camerino Via S. Agostino 1 Camerino MC 62032 ITALY ; _publ_contact_author_email CLAUDIO.PETTINARI@UNICAM.IT _publ_contact_letter ; ? #<< contact letter ; _publ_requested_journal ? _publ_requested_category ? _publ_section_title ; Gold derivatives of scorpionates: comparison with the other coinage metal poly(pyrazolyl)borate analogues ; _publ_section_title_footnote ; ? #<< paper footnote text ; loop_ _publ_author_name 'Claudio Pettinari' 'John B. Hanna' 'Giancarlo Gioia Lobbia' 'Maura Pellei' 'Carlo Santini' 'Brian W. Skelton' 'Allan H. White' _publ_section_synopsis ; ? #<< synopsis if FI,CI,CM,CO papers ; _publ_section_abstract ; ? #<< abstract text ; _publ_section_comment ; ? #<< scientific commentary text ; _publ_section_exptl_prep ; ? #<< material & crystal preparation text ; _publ_section_exptl_refinement ; ? #<< crystallographic methods used ; _publ_section_acknowledgements ; ? #<< acknowledgements text ; _publ_section_references ; Sheldrick, G M. (1996). SADABS. Pogram for Empirical Absorption Correction of Area Detector Data. University of Gottingen, Germany. Siemens (1995). SMART and SAINT. Area-Detector Control and Integration Software. Siemens Analytical X-ray Systems Inc., Madison, Wisconsin, USA. Hall, S.R., King, G.S.D., and Stewart., J.M. (1995). The Xtal 3.5 User's Manual. University of Western Australia, Lamb: Perth. ; _publ_section_figure_captions ; ? #<< figure captions ; #======================================================================= # Data block for single structure (one for each study in the paper) #======================================================================= data_cpcutp _database_code_depnum_ccdc_archive 'CCDC 227418' _audit_creation_method Xtal3.6 _audit_creation_date 03-07-27 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C51 H52 B1 Cu1 N6 P2' _chemical_formula_moiety 'C33 H37 B Cu N6 P, C18 H15 P' _chemical_formula_weight 885.32 _chemical_melting_point ? _symmetry_cell_setting cubic _symmetry_space_group_name_H-M P_a_-3 _symmetry_space_group_name_Hall -p_2ac_2ab_3 loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z 1/2-x,-y,1/2+z 1/2+x,1/2-y,-z -x,1/2+y,1/2-z +y,+z,+x 1/2-y,-z,1/2+x 1/2+y,1/2-z,-x -y,1/2+z,1/2-x +z,+x,+y -z,1/2+x,1/2-y 1/2-z,-x,1/2+y 1/2+z,1/2-x,-y -x,-y,-z 1/2+x,+y,1/2-z 1/2-x,1/2+y,+z +x,1/2-y,1/2+z -y,-z,-x 1/2+y,+z,1/2-x 1/2-y,1/2+z,+x +y,1/2-z,1/2+x -z,-x,-y +z,1/2-x,1/2+y 1/2+z,+x,1/2-y 1/2-z,1/2+x,+y _cell_length_a 21.075(4) _cell_length_b 21.075(4) _cell_length_c 21.075(4) _cell_angle_alpha 90.00000 _cell_angle_beta 90.00000 _cell_angle_gamma 90.00000 _cell_volume 9361(5) _cell_formula_units_Z 8 _exptl_crystal_density_diffrn 1.256 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 8497 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 25.5 _cell_measurement_temperature 150(2) _exptl_absorpt_coefficient_mu .576 _exptl_crystal_description plate _exptl_crystal_size_max .18 _exptl_crystal_size_mid .14 _exptl_crystal_size_min .08 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .86 _exptl_absorpt_correction_T_max 1 _diffrn_reflns_number 88102 _reflns_number_total 3206 _reflns_Friedel_coverage 0 _reflns_number_gt 1890 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 26.35 _diffrn_reflns_theta_full 26.35 _diffrn_measured_fraction_theta_max 1.00 _diffrn_measured_fraction_theta_full 1.00 _diffrn_reflns_av_R_equivalents .12 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .097 _refine_ls_wR_factor_ref .158 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_number_reflns 1890 _refine_ls_number_parameters 187 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .02 _refine_diff_density_min -.696 _refine_diff_density_max 1.967 _refine_ls_extinction_method none _refine_ls_extinction_coef ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction xtal _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 408 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 416 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' B ? 0 8 0 .001 'Int Tables Vol IV Tables 2.2B and 2.3.1' Cu ? 0 8 .263 1.266 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 48 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' P ? 0 16 .09 .095 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cu .15662(5) .15662(5) .15662(5) .0491(6) Uani ? ? 1.00000 ? ? B .2390(5) .2390(5) .2390(5) .064(4) Uani ? ? 1.00000 ? ? N1 .2644(3) .1706(3) .2419(3) .059(4) Uani ? ? 1.00000 ? ? N2 .2385(3) .1262(3) .2021(3) .057(4) Uani ? ? 1.00000 ? ? C3 .2694(4) .0719(4) .2108(5) .073(6) Uani ? ? 1.00000 ? ? C31 .2539(6) .0136(5) .1759(6) .105(8) Uani ? ? 1.00000 ? ? C4 .3158(4) .0806(5) .2578(5) .083(7) Uani ? ? 1.00000 ? ? C5 .3105(5) .1436(5) .2768(5) .079(7) Uani ? ? 1.00000 ? ? C51 .3470(5) .1804(7) .3251(6) .102(9) Uani ? ? 1.00000 ? ? P1 .09775(10) .09744(10) .09746(10) .0497(9) Uani ? ? 1.00000 ? ? C11 .1384(3) .0440(4) .0442(4) .057(5) Uani ? ? 1.00000 ? ? C12 .1911(5) .0648(5) .0129(6) .099(8) Uani ? ? 1.00000 ? ? C13 .2230(5) .0259(5) -.0299(6) .114(9) Uani ? ? 1.00000 ? ? C14 .2030(4) -.0320(5) -.0440(5) .084(7) Uani ? ? 1.00000 ? ? C15 .1512(4) -.0570(4) -.0103(4) .065(5) Uani ? ? 1.00000 ? ? C16 .1188(4) -.0186(4) .0314(4) .054(4) Uani ? ? 1.00000 ? ? P2 .39888(10) .10112(10) -.10112(10) .0381(13) Uani ? ? .757(10) ? ? P2' .4816(3) .0184(3) -.0184(3) .038(4) Uiso ? ? .243(10) ? ? C21 .3998(3) .1196(3) -.0182(4) .052(4) Uani ? ? 1.00000 ? ? C22 .3456(4) .1445(4) .0093(5) .068(6) Uani ? ? 1.00000 ? ? C23 .3431(4) .1575(4) .0726(5) .069(6) Uani ? ? 1.00000 ? ? C24 .3901(5) .1433(5) .1114(5) .078(6) Uani ? ? 1.00000 ? ? C25 .4498(5) .1276(5) .0864(4) .074(6) Uani ? ? 1.00000 ? ? C26 .4533(4) .1128(4) .0213(4) .064(5) Uani ? ? 1.00000 ? ? H31a .22971 .02792 .13710 .20306 Uiso ? ? 1.00000 ? ? H31b .23050 -.01090 .20771 .16608 Uiso ? ? 1.00000 ? ? H31c .29107 -.01027 .16479 .16064 Uiso ? ? 1.00000 ? ? H4 .34357 .05297 .27445 .14365 Uiso ? ? 1.00000 ? ? H51a .32178 .19258 .35970 .13542 Uiso ? ? 1.00000 ? ? H51b .36449 .21826 .30870 .19259 Uiso ? ? 1.00000 ? ? H51c .38124 .14980 .34283 .14374 Uiso ? ? 1.00000 ? ? H12 .20954 .10490 .02288 .14189 Uiso ? ? 1.00000 ? ? H13 .25965 .04396 -.04934 .14120 Uiso ? ? 1.00000 ? ? H14 .22463 -.06015 -.07525 .09846 Uiso ? ? 1.00000 ? ? H15 .13229 -.10283 -.01521 .10396 Uiso ? ? 1.00000 ? ? H16 .07899 -.03910 .05676 .08880 Uiso ? ? 1.00000 ? ? H22 .31135 .15909 -.01713 .11280 Uiso ? ? 1.00000 ? ? H23 .30524 .17819 .08997 .09906 Uiso ? ? 1.00000 ? ? H24 .38866 .14467 .15636 .11953 Uiso ? ? 1.00000 ? ? H25 .48939 .12157 .11534 .11234 Uiso ? ? 1.00000 ? ? H26 .49348 .09096 -.00246 .11219 Uiso ? ? 1.00000 ? ? H .26631 .26631 .26631 .08100 Uiso ? ? 1.00000 ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cu .0491(6) .0491(6) .0491(6) .0096(4) .0096(4) .0096(4) B .064(4) .064(4) .064(4) .002(5) .002(5) .002(5) N1 .055(4) .066(4) .057(4) .007(3) .006(3) .016(3) N2 .055(4) .051(4) .064(4) .021(3) .010(3) .018(3) C3 .055(5) .065(5) .100(7) .009(4) .012(5) .021(5) C31 .099(8) .060(6) .156(11) .036(6) .011(8) .007(7) C4 .053(5) .089(7) .106(8) .014(5) -.003(5) .037(6) C5 .058(5) .096(7) .083(7) .016(5) .000(5) .031(6) C51 .068(7) .145(11) .094(8) .010(7) -.018(6) .019(8) P1 .0497(9) .0497(9) .0497(9) .0103(9) .0103(9) .0103(9) C11 .043(4) .065(5) .063(5) .007(4) .012(3) .009(4) C12 .065(6) .073(6) .158(11) -.013(5) .050(7) -.017(7) C13 .102(8) .075(7) .165(12) -.011(6) .100(8) -.032(7) C14 .062(5) .087(7) .102(8) .014(5) .045(5) -.015(6) C15 .067(5) .057(5) .070(5) .014(4) .006(4) .013(4) C16 .051(4) .048(4) .063(5) .005(3) -.001(4) .014(4) P2 .0381(13) .0381(13) .0381(13) .009(3) -.009(3) -.009(3) C21 .048(4) .045(4) .062(5) -.010(3) .012(4) -.007(3) C22 .042(4) .080(6) .081(6) .004(4) -.009(4) -.019(5) C23 .055(5) .073(6) .079(6) .003(4) -.004(5) -.011(5) C24 .088(7) .082(7) .065(6) .010(5) .027(5) -.019(5) C25 .083(6) .083(6) .057(5) .005(5) .006(5) .002(5) C26 .080(6) .065(5) .047(4) .022(4) -.002(4) -.001(4) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Cu N2 . . 2.075(7) ? Cu P1 . . 2.156(2) ? Cu N2 . 5 2.075(7) ? Cu N2 . 9 2.075(7) ? B N1 . . 1.539(13) ? B H . . .996 ? B N1 . 5 1.539(13) ? B N1 . 9 1.539(13) ? N1 N2 . . 1.371(9) ? N1 C5 . . 1.345(12) ? N2 C3 . . 1.329(11) ? C3 C31 . . 1.469(15) ? C3 C4 . . 1.404(14) ? C31 H31a . . 1.009 ? C31 H31b . . .980 ? C31 H31c . . .960 ? C4 C5 . . 1.391(15) ? C4 H4 . . .897 ? C5 C51 . . 1.493(17) ? C51 H51a . . .938 ? C51 H51b . . .945 ? C51 H51c . . 1.038 ? P1 C11 . . 1.806(8) ? P1 C11 . 5 1.813(8) ? P1 C11 . 9 1.814(8) ? C11 C12 . . 1.365(13) ? C11 C16 . . 1.408(11) ? C12 C13 . . 1.392(17) ? C12 H12 . . .953 ? C13 C14 . . 1.325(15) ? C13 H13 . . .953 ? C14 C15 . . 1.406(13) ? C14 H14 . . .997 ? C15 C16 . . 1.375(12) ? C15 H15 . . 1.049 ? C16 H16 . . 1.085 ? P2 C21 . . 1.790(8) ? P2 C21 . '6 554' 1.790(8) ? P2 C21 . 12 1.790(8) ? C21 C22 . . 1.384(11) ? C21 C26 . . 1.410(11) ? C22 C23 . . 1.361(15) ? C22 H22 . . .963 ? C23 C24 . . 1.319(14) ? C23 H23 . . .980 ? C24 C25 . . 1.404(15) ? C24 H24 . . .949 ? C25 C26 . . 1.410(12) ? C25 H25 . . 1.040 ? C26 H26 . . 1.086 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published N2 Cu P1 . . . 124.5(2) ? N2 Cu N2 . . 5 90.9(3) ? N2 Cu N2 . . 9 90.9(3) ? P1 Cu N2 . . 5 124.7(2) ? P1 Cu N2 . . 9 124.6(2) ? N2 Cu N2 5 . 9 90.9(3) ? N1 B H . . . 108.5 ? N1 B N1 . . 5 110.4(7) ? N1 B N1 . . 9 110.4(7) ? H B N1 . . 5 108.5 ? H B N1 . . 9 108.5 ? N1 B N1 5 . 9 110.4(7) ? B N1 N2 . . . 118.6(7) ? B N1 C5 . . . 132.0(8) ? N2 N1 C5 . . . 109.4(7) ? Cu N2 N1 . . . 113.7(5) ? Cu N2 C3 . . . 137.6(6) ? N1 N2 C3 . . . 107.9(7) ? N2 C3 C31 . . . 122.8(9) ? N2 C3 C4 . . . 109.1(8) ? C31 C3 C4 . . . 128.1(9) ? C3 C31 H31a . . . 105.6 ? C3 C31 H31b . . . 102.2 ? C3 C31 H31c . . . 112.2 ? H31a C31 H31b . . . 117.3 ? H31a C31 H31c . . . 111.8 ? H31b C31 H31c . . . 107.5 ? C3 C4 C5 . . . 105.7(9) ? C3 C4 H4 . . . 130.2 ? C5 C4 H4 . . . 124.1 ? N1 C5 C4 . . . 107.8(9) ? N1 C5 C51 . . . 121.7(10) ? C4 C5 C51 . . . 130.5(10) ? C5 C51 H51a . . . 112.4 ? C5 C51 H51b . . . 113.0 ? C5 C51 H51c . . . 106.4 ? H51a C51 H51b . . . 105.9 ? H51a C51 H51c . . . 106.5 ? H51b C51 H51c . . . 112.6 ? Cu P1 C11 . . . 116.6(3) ? Cu P1 C11 . . 5 116.3(3) ? Cu P1 C11 . . 9 116.3(3) ? C11 P1 C11 . . 5 101.9(4) ? C11 P1 C11 . . 9 101.8(4) ? C11 P1 C11 5 . 9 101.6(4) ? P1 C11 C12 . . . 119.0(7) ? P1 C11 C16 . . . 124.4(6) ? C12 C11 C16 . . . 116.6(8) ? C11 C12 C13 . . . 121.1(10) ? C11 C12 H12 . . . 120.7 ? C13 C12 H12 . . . 117.9 ? C12 C13 C14 . . . 122.3(11) ? C12 C13 H13 . . . 115.8 ? C14 C13 H13 . . . 121.9 ? C13 C14 C15 . . . 118.7(10) ? C13 C14 H14 . . . 123.5 ? C15 C14 H14 . . . 117.7 ? C14 C15 C16 . . . 119.1(8) ? C14 C15 H15 . . . 126.2 ? C16 C15 H15 . . . 114.6 ? C11 C16 C15 . . . 121.9(7) ? C11 C16 H16 . . . 120.3 ? C15 C16 H16 . . . 117.7 ? C21 P2 C21 . . '6 554' 101.8(3) ? C21 P2 C21 . . 12 101.8(3) ? C21 P2 C21 '6 554' . 12 101.8(3) ? P2 C21 C22 . . . 118.9(6) ? P2 C21 C26 . . . 124.2(6) ? C22 C21 C26 . . . 116.8(8) ? C21 C22 C23 . . . 121.3(8) ? C21 C22 H22 . . . 119.8 ? C23 C22 H22 . . . 118.3 ? C22 C23 C24 . . . 122.1(9) ? C22 C23 H23 . . . 119.2 ? C24 C23 H23 . . . 118.7 ? C23 C24 C25 . . . 119.7(9) ? C23 C24 H24 . . . 126.1 ? C25 C24 H24 . . . 114.2 ? C24 C25 C26 . . . 117.6(9) ? C24 C25 H25 . . . 121.9 ? C26 C25 H25 . . . 120.1 ? C21 C26 C25 . . . 120.7(8) ? C21 C26 H26 . . . 113.2 ? C25 C26 H26 . . . 125.7 ? _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 3712 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 15 _reflns_limit_k_min 0 _reflns_limit_k_max 26 _reflns_limit_l_min 1 _reflns_limit_l_max 26 _reflns_number_observed ? _reflns_d_resolution_high .801 _reflns_d_resolution_low 12.138 _diffrn_reflns_av_sigmaI/netI .137 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 150(2) _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .168 _refine_ls_wR_factor_all .198 _refine_ls_goodness_of_fit_all 1.039 _refine_ls_shift/su_mean .001 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #===END ######################################## # # # CIF generated by the Xtal System # # # ######################################## data_cpau _database_code_depnum_ccdc_archive 'CCDC 227419' _audit_creation_method Xtal3.6 _audit_creation_date 03-11-10 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C33 H37 Au1 B1 N6 P1' _chemical_formula_moiety 'C33 H37 Au1 B1 N6 P1' _chemical_formula_weight 756.45 _chemical_melting_point ? _symmetry_cell_setting cubic _symmetry_space_group_name_H-M p_21_3 _symmetry_space_group_name_Hall p_2ac_2ab_3 loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z 1/2-x,-y,1/2+z 1/2+x,1/2-y,-z -x,1/2+y,1/2-z +y,+z,+x 1/2-y,-z,1/2+x 1/2+y,1/2-z,-x -y,1/2+z,1/2-x +z,+x,+y -z,1/2+x,1/2-y 1/2-z,-x,1/2+y 1/2+z,1/2-x,-y _cell_length_a 21.603(2) _cell_length_b 21.603(2) _cell_length_c 21.603(2) _cell_angle_alpha 90.00000 _cell_angle_beta 90.00000 _cell_angle_gamma 90.00000 _cell_volume 10082(2) _cell_formula_units_Z 12 _exptl_crystal_density_diffrn 1.495 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 7352 _cell_measurement_theta_min 2.7 _cell_measurement_theta_max 27.4 _cell_measurement_temperature 150(2) _exptl_absorpt_coefficient_mu 4.46 _exptl_crystal_description block _exptl_crystal_size_max .60 _exptl_crystal_size_mid .55 _exptl_crystal_size_min .50 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .34 _exptl_absorpt_correction_T_max .72 _diffrn_reflns_number 109773 _reflns_number_total 4742 _reflns_Friedel_coverage ? _reflns_number_gt 3124 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 28.97 _diffrn_reflns_theta_full 28.97 _diffrn_measured_fraction_theta_max 1.0 _diffrn_measured_fraction_theta_full 1.0 _diffrn_reflns_av_R_equivalents .080 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .047 _refine_ls_wR_factor_ref .02 _refine_ls_goodness_of_fit_ref 1.261 _refine_ls_number_reflns 3089 _refine_ls_number_parameters 381 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .052 _refine_diff_density_min -1.316 _refine_diff_density_max 1.16 _refine_ls_extinction_method Zachariasen _refine_ls_extinction_coef 8513(262) _refine_ls_abs_structure_details 'Flack xabs refined' _refine_ls_abs_structure_Flack -.009(6) # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 396 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 444 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Au ? 0 12 -2.688 8.798 'Int Tables Vol IV Tables 2.2B and 2.3.1' B ? 0 12 0 .001 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 72 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' P ? 0 12 .09 .095 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Au1 .272131(17) .272131(17) .272131(17) .0757(2) Uani ? ? 1.00000 ? ? B1 .3618(4) .3618(4) .3618(4) .044(4) Uani ? ? 1.00000 ? ? N11 .3865(3) .3668(3) .2959(3) .040(4) Uani ? ? 1.00000 ? ? N12 .3597(3) .3322(3) .2496(3) .042(4) Uani ? ? 1.00000 ? ? C13 .3898(4) .3465(3) .1986(4) .043(6) Uani ? ? 1.00000 ? ? C131 .3728(4) .3160(4) .1391(4) .076(7) Uani ? ? 1.00000 ? ? C14 .4362(4) .3886(4) .2101(4) .064(7) Uani ? ? 1.00000 ? ? C15 .4335(4) .3999(4) .2723(5) .058(6) Uani ? ? 1.00000 ? ? C151 .4726(5) .4408(5) .3112(5) .134(10) Uani ? ? 1.00000 ? ? P1 .21398(9) .21399(9) .21399(9) .0439(10) Uani ? ? 1.00000 ? ? C111 .1643(3) .1619(4) .2567(4) .045(6) Uani ? ? 1.00000 ? ? C112 .1433(5) .1796(4) .3142(5) .080(8) Uani ? ? 1.00000 ? ? C113 .1058(5) .1422(6) .3483(5) .100(10) Uani ? ? 1.00000 ? ? C114 .0865(5) .0866(6) .3264(6) .101(10) Uani ? ? 1.00000 ? ? C115 .1078(5) .0672(5) .2712(6) .111(10) Uani ? ? 1.00000 ? ? C116 .1460(5) .1053(5) .2355(4) .092(8) Uani ? ? 1.00000 ? ? Au2 .625004(15) .625004(15) .625004(15) .0591(2) Uani ? ? 1.00000 ? ? B2 .5341(4) .5341(4) .5341(4) .043(5) Uani ? ? 1.00000 ? ? N21 .5039(3) .5367(3) .5990(3) .036(4) Uani ? ? 1.00000 ? ? N22 .5334(3) .5689(3) .6450(3) .041(4) Uani ? ? 1.00000 ? ? C23 .4987(4) .5622(4) .6957(4) .047(6) Uani ? ? 1.00000 ? ? C231 .5176(4) .5935(4) .7549(4) .073(7) Uani ? ? 1.00000 ? ? C24 .4484(3) .5246(4) .6830(4) .057(6) Uani ? ? 1.00000 ? ? C25 .4532(3) .5084(3) .6225(4) .049(6) Uani ? ? 1.00000 ? ? C251 .4106(4) .4697(4) .5832(4) .082(7) Uani ? ? 1.00000 ? ? P2 .68336(9) .68336(9) .68336(9) .0449(11) Uani ? ? 1.00000 ? ? C211 .7287(3) .7411(4) .6420(3) .042(5) Uani ? ? 1.00000 ? ? C212 .7515(4) .7249(4) .5848(4) .074(7) Uani ? ? 1.00000 ? ? C213 .7888(5) .7670(5) .5510(4) .092(9) Uani ? ? 1.00000 ? ? C214 .8002(4) .8248(5) .5754(5) .083(9) Uani ? ? 1.00000 ? ? C215 .7764(5) .8413(4) .6309(5) .078(8) Uani ? ? 1.00000 ? ? C216 .7411(4) .8004(4) .6645(4) .064(7) Uani ? ? 1.00000 ? ? Au3 .931387(19) .931387(19) .931397(19) .1070(3) Uani ? ? 1.00000 ? ? B3 1.0194(6) 1.0194(6) 1.0194(6) .136(11) Uani ? ? 1.00000 ? ? N31 1.0443(4) 1.0238(6) .9530(4) .093(8) Uani ? ? 1.00000 ? ? N32 1.0302(4) .9775(4) .9131(5) .090(7) Uani ? ? 1.00000 ? ? C33 1.0555(5) .9906(7) .8596(7) .098(11) Uani ? ? 1.00000 ? ? C331 1.0509(6) .9511(7) .8054(5) .142(13) Uani ? ? 1.00000 ? ? C34 1.0852(7) 1.0470(10) .8634(7) .129(14) Uani ? ? 1.00000 ? ? C35 1.0775(6) 1.0668(7) .9192(10) .121(13) Uani ? ? 1.00000 ? ? C351 1.0977(5) 1.1259(6) .9550(7) .200(15) Uani ? ? 1.00000 ? ? P3 .87301(10) .87301(10) .87302(10) .0535(10) Uani ? ? 1.00000 ? ? C311 .8154(4) .9156(4) .8285(4) .046(6) Uani ? ? 1.00000 ? ? C312 .8318(4) .9696(5) .8008(5) .087(8) Uani ? ? 1.00000 ? ? C313 .7903(6) 1.0035(5) .7663(6) .103(10) Uani ? ? 1.00000 ? ? C314 .7324(6) .9807(5) .7578(5) .093(9) Uani ? ? 1.00000 ? ? C315 .7145(4) .9264(5) .7843(4) .075(8) Uani ? ? 1.00000 ? ? C316 .7563(4) .8936(3) .8206(4) .056(6) Uani ? ? 1.00000 ? ? H1 .38763 .38763 .38763 .06400 Uiso ? ? 1.00000 ? ? H131a .39224 .27478 .13765 .11100 Uiso ? ? 1.00000 ? ? H131b .39020 .33879 .10516 .11100 Uiso ? ? 1.00000 ? ? H131c .32947 .31206 .13325 .11100 Uiso ? ? 1.00000 ? ? H14 .46371 .40611 .17985 .08400 Uiso ? ? 1.00000 ? ? H151a .50082 .41829 .33734 .18300 Uiso ? ? 1.00000 ? ? H151b .44869 .46767 .33736 .18300 Uiso ? ? 1.00000 ? ? H151c .49741 .46650 .28364 .18300 Uiso ? ? 1.00000 ? ? H112 .15748 .21913 .33173 .09400 Uiso ? ? 1.00000 ? ? H113 .08992 .15566 .38807 .12100 Uiso ? ? 1.00000 ? ? H114 .05757 .06029 .34991 .12200 Uiso ? ? 1.00000 ? ? H115 .09530 .02649 .25734 .14200 Uiso ? ? 1.00000 ? ? H116 .15748 .09230 .19215 .11700 Uiso ? ? 1.00000 ? ? H2 .50925 .50925 .50925 .06300 Uiso ? ? 1.00000 ? ? H231a .48942 .62407 .76741 .11300 Uiso ? ? 1.00000 ? ? H231b .52108 .56287 .78766 .11300 Uiso ? ? 1.00000 ? ? H231c .55807 .61140 .75106 .11300 Uiso ? ? 1.00000 ? ? H24 .41744 .51095 .71166 .07100 Uiso ? ? 1.00000 ? ? H251a .43259 .46204 .54624 .12200 Uiso ? ? 1.00000 ? ? H251b .37690 .49844 .57327 .12200 Uiso ? ? 1.00000 ? ? H251c .40164 .43179 .60494 .12200 Uiso ? ? 1.00000 ? ? H212 .74178 .68483 .56648 .09600 Uiso ? ? 1.00000 ? ? H213 .80713 .75449 .51163 .10900 Uiso ? ? 1.00000 ? ? H214 .82614 .85390 .55178 .10300 Uiso ? ? 1.00000 ? ? H215 .78314 .88258 .64574 .09400 Uiso ? ? 1.00000 ? ? H216 .72483 .81355 .70393 .07400 Uiso ? ? 1.00000 ? ? H3 1.04300 1.04300 1.04300 .17300 Uiso ? ? 1.00000 ? ? H331a 1.08133 .95778 .77531 .18000 Uiso ? ? 1.00000 ? ? H331b 1.01050 .95430 .78660 .18000 Uiso ? ? 1.00000 ? ? H331c 1.05442 .90745 .81869 .18000 Uiso ? ? 1.00000 ? ? H34 1.10981 1.07085 .83286 .15000 Uiso ? ? 1.00000 ? ? H351a 1.08779 1.16459 .93580 .27500 Uiso ? ? 1.00000 ? ? H351b 1.07463 1.13043 .99758 .27500 Uiso ? ? 1.00000 ? ? H351c 1.14117 1.12794 .97004 .27500 Uiso ? ? 1.00000 ? ? H312 .87398 .98504 .80385 .11000 Uiso ? ? 1.00000 ? ? H313 .80028 1.04460 .75011 .12200 Uiso ? ? 1.00000 ? ? H314 .70220 1.00384 .73369 .11500 Uiso ? ? 1.00000 ? ? H315 .67249 .90896 .77594 .09100 Uiso ? ? 1.00000 ? ? H316 .74305 .85627 .84237 .07200 Uiso ? ? 1.00000 ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Au1 .0757(2) .0757(2) .0757(2) -.0225(2) -.0225(2) -.0225(2) B1 .044(4) .044(4) .044(4) -.006(5) -.006(5) -.006(5) N11 .038(4) .039(4) .043(4) -.004(3) -.002(3) .001(4) N12 .045(5) .043(4) .036(4) -.005(3) .009(3) .007(3) C13 .048(6) .037(5) .044(6) .014(4) .009(5) .001(4) C131 .089(7) .093(7) .046(6) .008(6) .016(6) -.003(5) C14 .064(7) .056(7) .070(7) -.014(5) .026(5) .009(5) C15 .053(6) .049(6) .073(7) -.009(5) .011(6) -.005(5) C151 .119(9) .167(11) .115(9) -.109(9) .020(7) -.038(8) P1 .0439(10) .0439(10) .0439(10) -.0038(11) -.0038(11) -.0038(11) C111 .047(6) .040(6) .049(6) .003(4) -.002(5) .001(5) C112 .115(10) .071(7) .055(7) -.006(7) .016(7) .003(6) C113 .105(10) .116(11) .080(9) -.009(8) .026(7) .032(8) C114 .081(9) .102(11) .119(11) -.020(8) .020(8) .060(9) C115 .117(11) .076(8) .141(12) -.049(7) .022(9) .021(9) C116 .121(9) .065(7) .089(8) -.028(6) .032(7) -.015(6) Au2 .0591(2) .0591(2) .0591(2) -.0148(2) -.0148(2) -.0148(2) B2 .043(5) .043(5) .043(5) .003(5) .003(5) .003(5) N21 .030(4) .045(5) .031(4) -.004(3) .004(3) -.006(3) N22 .039(4) .046(4) .040(4) -.003(3) .004(4) -.004(4) C23 .043(6) .060(6) .038(6) .005(5) .000(5) -.001(5) C231 .061(6) .111(8) .045(6) -.015(5) .003(5) -.022(5) C24 .038(6) .070(7) .063(7) -.015(5) .009(5) .002(5) C25 .039(6) .044(5) .064(7) -.011(4) .008(5) .000(5) C251 .067(7) .096(8) .084(7) -.041(6) -.002(6) .002(6) P2 .0449(11) .0449(11) .0449(11) -.0072(11) -.0072(11) -.0072(11) C211 .035(5) .053(6) .038(5) -.004(5) -.007(4) -.001(4) C212 .086(8) .054(6) .081(8) -.007(5) .023(6) -.004(6) C213 .093(9) .098(9) .085(8) .006(8) .049(6) .007(7) C214 .063(7) .075(8) .111(10) -.019(6) .011(7) .028(8) C215 .095(8) .058(7) .080(8) -.021(6) -.004(7) .014(6) C216 .078(7) .060(7) .053(6) -.017(6) -.020(5) .000(5) Au3 .1070(3) .1070(3) .1070(3) -.0284(3) -.0284(3) -.0284(3) B3 .136(11) .136(11) .136(11) -.050(10) -.050(10) -.050(10) N31 .061(7) .103(8) .114(9) -.008(6) -.015(6) .001(8) N32 .080(6) .107(8) .082(8) -.027(5) .011(6) .005(6) C33 .034(7) .128(12) .132(14) .007(7) .006(8) .063(11) C331 .131(12) .229(17) .066(9) .037(11) .004(8) .026(9) C34 .070(10) .178(18) .139(14) .002(10) -.006(10) .055(14) C35 .042(8) .084(11) .24(2) -.026(8) -.038(13) .041(14) C351 .126(12) .132(12) .34(2) -.031(11) -.042(12) .016(14) P3 .0535(10) .0535(10) .0535(10) -.0012(15) -.0012(15) -.0012(15) C311 .038(6) .048(6) .053(6) -.003(5) .008(5) .009(5) C312 .063(7) .076(8) .121(10) -.014(6) .005(6) .043(7) C313 .102(10) .077(9) .131(11) -.013(8) .004(9) .042(7) C314 .090(9) .089(9) .099(9) .034(8) .004(8) .046(7) C315 .047(7) .076(8) .101(9) .014(6) -.003(6) .009(7) C316 .049(6) .041(6) .077(7) .009(5) .011(5) .017(5) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Au1 N12 . . 2.345(6) ? Au1 P1 . . 2.176(2) ? Au1 N12 . 5 2.345(6) ? Au1 N12 . 9 2.345(6) ? B1 N11 . . 1.524(10) ? B1 H1 . . .966 ? B1 N11 . 5 1.523(10) ? B1 N11 . 9 1.523(10) ? N11 N12 . . 1.377(8) ? N11 C15 . . 1.344(10) ? N12 C13 . . 1.317(10) ? C13 C131 . . 1.490(11) ? C13 C14 . . 1.375(12) ? C131 H131a . . .984 ? C131 H131b . . .960 ? C131 H131c . . .948 ? C14 C15 . . 1.366(14) ? C14 H14 . . .962 ? C15 C151 . . 1.483(14) ? C151 H151a . . .963 ? C151 H151b . . .961 ? C151 H151c . . .975 ? P1 C111 . . 1.808(8) ? P1 C111 . 5 1.808(8) ? P1 C111 . 9 1.808(8) ? C111 C112 . . 1.377(13) ? C111 C116 . . 1.365(13) ? C112 C113 . . 1.361(15) ? C112 H112 . . .983 ? C113 C114 . . 1.355(18) ? C113 H113 . . .970 ? C114 C115 . . 1.346(18) ? C114 H114 . . .987 ? C115 C116 . . 1.398(15) ? C115 H115 . . .966 ? C116 H116 . . 1.008 ? Au2 N22 . . 2.360(6) ? Au2 P2 . . 2.184(2) ? Au2 N22 . 5 2.360(6) ? Au2 N22 . 9 2.360(6) ? B2 N21 . . 1.547(11) ? B2 H2 . . .928 ? B2 N21 . 5 1.547(11) ? B2 N21 . 9 1.547(11) ? N21 N22 . . 1.370(8) ? N21 C25 . . 1.354(10) ? N22 C23 . . 1.335(10) ? C23 C231 . . 1.504(11) ? C23 C24 . . 1.384(11) ? C231 H231a . . .938 ? C231 H231b . . .972 ? C231 H231c . . .959 ? C24 C25 . . 1.357(13) ? C24 H24 . . .958 ? C25 C251 . . 1.507(12) ? C251 H251a . . .944 ? C251 H251b . . .980 ? C251 H251c . . .964 ? P2 C211 . . 1.819(8) ? P2 C211 . 5 1.819(8) ? P2 C211 . 9 1.819(8) ? C211 C212 . . 1.377(12) ? C211 C216 . . 1.396(12) ? C212 C213 . . 1.418(14) ? C212 H212 . . .974 ? C213 C214 . . 1.375(15) ? C213 H213 . . .977 ? C214 C215 . . 1.353(15) ? C214 H214 . . .985 ? C215 C216 . . 1.375(13) ? C215 H215 . . .959 ? C216 H216 . . .964 ? Au3 N32 . . 2.390(8) ? Au3 P3 . . 2.184(2) ? Au3 N32 . 5 2.389(8) ? Au3 N32 . 9 2.390(8) ? B3 N31 . . 1.535(16) ? B3 H3 . . .882 ? B3 N31 . 5 1.535(16) ? B3 N31 . 9 1.535(16) ? N31 N32 . . 1.353(14) ? N31 C35 . . 1.38(2) ? N32 C33 . . 1.311(18) ? C33 C331 . . 1.45(2) ? C33 C34 . . 1.38(2) ? C331 H331a . . .936 ? C331 H331b . . .966 ? C331 H331c . . .988 ? C34 C35 . . 1.29(3) ? C34 H34 . . .990 ? C35 C351 . . 1.56(2) ? C351 H351a . . .958 ? C351 H351b . . 1.051 ? C351 H351c . . .994 ? P3 C311 . . 1.821(8) ? P3 C311 . 5 1.821(8) ? P3 C311 . 9 1.821(8) ? C311 C312 . . 1.359(13) ? C311 C316 . . 1.372(12) ? C312 C313 . . 1.379(15) ? C312 H312 . . .972 ? C313 C314 . . 1.356(17) ? C313 H313 . . .977 ? C314 C315 . . 1.361(15) ? C314 H314 . . .973 ? C315 C316 . . 1.392(12) ? C315 H315 . . .999 ? C316 H316 . . .977 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published N12 Au1 P1 . . . 131.69(16) ? N12 Au1 N12 . . 5 80.6(2) ? N12 Au1 N12 . . 9 80.6(2) ? P1 Au1 N12 . . 5 131.69(16) ? P1 Au1 N12 . . 9 131.69(16) ? N12 Au1 N12 5 . 9 80.6(2) ? N11 B1 H1 . . . 107.3 ? N11 B1 N11 . . 5 111.6 ? N11 B1 N11 . . 9 111.6 ? H1 B1 N11 . . 5 107.3 ? H1 B1 N11 . . 9 107.3 ? N11 B1 N11 5 . 9 111.6(6) ? B1 N11 N12 . . . 119.7(6) ? B1 N11 C15 . . . 131.1(7) ? N12 N11 C15 . . . 109.3(6) ? Au1 N12 N11 . . . 119.2(4) ? Au1 N12 C13 . . . 134.7(5) ? N11 N12 C13 . . . 105.9(6) ? N12 C13 C131 . . . 119.6(7) ? N12 C13 C14 . . . 111.3(7) ? C131 C13 C14 . . . 129.0(8) ? C13 C131 H131a . . . 108.8 ? C13 C131 H131b . . . 109.5 ? C13 C131 H131c . . . 113.5 ? H131a C131 H131b . . . 105.8 ? H131a C131 H131c . . . 109.7 ? H131b C131 H131c . . . 109.3 ? C13 C14 C15 . . . 105.4(8) ? C13 C14 H14 . . . 125.9 ? C15 C14 H14 . . . 128.7 ? N11 C15 C14 . . . 108.1(7) ? N11 C15 C151 . . . 122.2(8) ? C14 C15 C151 . . . 129.7(8) ? C15 C151 H151a . . . 113.2 ? C15 C151 H151b . . . 112.8 ? C15 C151 H151c . . . 107.8 ? H151a C151 H151b . . . 107.5 ? H151a C151 H151c . . . 107.3 ? H151b C151 H151c . . . 108.1 ? Au1 P1 C111 . . . 114.0(3) ? Au1 P1 C111 . . 5 114.0(3) ? Au1 P1 C111 . . 9 114.0(3) ? C111 P1 C111 . . 5 104.5(4) ? C111 P1 C111 . . 9 104.5(4) ? C111 P1 C111 5 . 9 104.5(4) ? P1 C111 C112 . . . 118.9(6) ? P1 C111 C116 . . . 124.0(7) ? C112 C111 C116 . . . 117.1(8) ? C111 C112 C113 . . . 121.3(9) ? C111 C112 H112 . . . 119.1 ? C113 C112 H112 . . . 119.6 ? C112 C113 C114 . . . 121.3(10) ? C112 C113 H113 . . . 120.7 ? C114 C113 H113 . . . 117.9 ? C113 C114 C115 . . . 118.8(11) ? C113 C114 H114 . . . 121.7 ? C115 C114 H114 . . . 119.5 ? C114 C115 C116 . . . 120.4(10) ? C114 C115 H115 . . . 117.6 ? C116 C115 H115 . . . 122.0 ? C111 C116 C115 . . . 121.0(9) ? C111 C116 H116 . . . 119.3 ? C115 C116 H116 . . . 119.6 ? N22 Au2 P2 . . . 132.46(16) ? N22 Au2 N22 . . 5 79.4(2) ? N22 Au2 N22 . . 9 79.4(2) ? P2 Au2 N22 . . 5 132.46(16) ? P2 Au2 N22 . . 9 132.46(16) ? N22 Au2 N22 5 . 9 79.4(2) ? N21 B2 H2 . . . 107.5 ? N21 B2 N21 . . 5 111.3(6) ? N21 B2 N21 . . 9 111.3(6) ? H2 B2 N21 . . 5 107.5 ? H2 B2 N21 . . 9 107.5 ? N21 B2 N21 5 . 9 111.3(6) ? B2 N21 N22 . . . 118.7(6) ? B2 N21 C25 . . . 131.7(7) ? N22 N21 C25 . . . 109.4(6) ? Au2 N22 N21 . . . 121.2(4) ? Au2 N22 C23 . . . 132.5(5) ? N21 N22 C23 . . . 106.2(6) ? N22 C23 C231 . . . 119.8(7) ? N22 C23 C24 . . . 110.0(7) ? C231 C23 C24 . . . 130.2(7) ? C23 C231 H231a . . . 112.6 ? C23 C231 H231b . . . 109.5 ? C23 C231 H231c . . . 110.8 ? H231a C231 H231b . . . 108.7 ? H231a C231 H231c . . . 109.5 ? H231b C231 H231c . . . 105.5 ? C23 C24 C25 . . . 106.4(7) ? C23 C24 H24 . . . 127.0 ? C25 C24 H24 . . . 126.6 ? N21 C25 C24 . . . 107.9(7) ? N21 C25 C251 . . . 122.2(8) ? C24 C25 C251 . . . 129.8(7) ? C25 C251 H251a . . . 105.5 ? C25 C251 H251b . . . 103.0 ? C25 C251 H251c . . . 108.6 ? H251a C251 H251b . . . 107.5 ? H251a C251 H251c . . . 111.3 ? H251b C251 H251c . . . 119.7 ? Au2 P2 C211 . . . 115.0(3) ? Au2 P2 C211 . . 5 115.0(3) ? Au2 P2 C211 . . 9 115.0(3) ? C211 P2 C211 . . 5 103.4(3) ? C211 P2 C211 . . 9 103.4(3) ? C211 P2 C211 5 . 9 103.4(3) ? P2 C211 C212 . . . 117.4(6) ? P2 C211 C216 . . . 124.1(6) ? C212 C211 C216 . . . 118.5(7) ? C211 C212 C213 . . . 120.2(8) ? C211 C212 H212 . . . 120.8 ? C213 C212 H212 . . . 119.0 ? C212 C213 C214 . . . 119.1(9) ? C212 C213 H213 . . . 120.0 ? C214 C213 H213 . . . 120.9 ? C213 C214 C215 . . . 120.7(9) ? C213 C214 H214 . . . 118.8 ? C215 C214 H214 . . . 120.4 ? C214 C215 C216 . . . 120.6(8) ? C214 C215 H215 . . . 119.0 ? C216 C215 H215 . . . 120.4 ? C211 C216 C215 . . . 120.8(8) ? C211 C216 H216 . . . 120.6 ? C215 C216 H216 . . . 118.6 ? N32 Au3 P3 . . . 131.4(3) ? N32 Au3 N32 . . 5 81.0(3) ? N32 Au3 N32 . . 9 81.0(3) ? P3 Au3 N32 . . 5 131.4(3) ? P3 Au3 N32 . . 9 131.4(3) ? N32 Au3 N32 5 . 9 81.0(3) ? N31 B3 H3 . . . 107.6 ? N31 B3 N31 . . 5 111.3(10) ? N31 B3 N31 . . 9 111.3(10) ? H3 B3 N31 . . 5 107.6 ? H3 B3 N31 . . 9 107.6 ? N31 B3 N31 5 . 9 111.3(10) ? B3 N31 N32 . . . 118.1(10) ? B3 N31 C35 . . . 135.8(12) ? N32 N31 C35 . . . 106.1(11) ? Au3 N32 N31 . . . 113.8(6) ? Au3 N32 C33 . . . 127.5(8) ? N31 N32 C33 . . . 108.0(10) ? N32 C33 C331 . . . 123.8(12) ? N32 C33 C34 . . . 109.4(13) ? C331 C33 C34 . . . 126.8(13) ? C33 C331 H331a . . . 114.9 ? C33 C331 H331b . . . 111.1 ? C33 C331 H331c . . . 108.8 ? H331a C331 H331b . . . 109.3 ? H331a C331 H331c . . . 107.1 ? H331b C331 H331c . . . 105.0 ? C33 C34 C35 . . . 106.7(15) ? C33 C34 H34 . . . 132.0 ? C35 C34 H34 . . . 121.3 ? N31 C35 C34 . . . 109.8(14) ? N31 C35 C351 . . . 115.8(15) ? C34 C35 C351 . . . 134.3(16) ? C35 C351 H351a . . . 116.0 ? C35 C351 H351b . . . 112.2 ? C35 C351 H351c . . . 117.7 ? H351a C351 H351b . . . 101.0 ? H351a C351 H351c . . . 108.3 ? H351b C351 H351c . . . 99.1 ? Au3 P3 C311 . . . 114.1(3) ? Au3 P3 C311 . . 5 114.1(3) ? Au3 P3 C311 . . 9 114.1(3) ? C311 P3 C311 . . 5 104.5(4) ? C311 P3 C311 . . 9 104.5(4) ? C311 P3 C311 5 . 9 104.5(4) ? P3 C311 C312 . . . 119.2(6) ? P3 C311 C316 . . . 121.8(6) ? C312 C311 C316 . . . 118.9(8) ? C311 C312 C313 . . . 121.7(9) ? C311 C312 H312 . . . 120.6 ? C313 C312 H312 . . . 117.6 ? C312 C313 C314 . . . 118.7(10) ? C312 C313 H313 . . . 122.2 ? C314 C313 H313 . . . 119.0 ? C313 C314 C315 . . . 121.3(10) ? C313 C314 H314 . . . 120.3 ? C315 C314 H314 . . . 118.4 ? C314 C315 C316 . . . 119.4(8) ? C314 C315 H315 . . . 120.6 ? C316 C315 H315 . . . 120.0 ? C311 C316 C315 . . . 119.9(7) ? C311 C316 H316 . . . 119.9 ? C315 C316 H316 . . . 120.1 ? _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 4512 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 16 _reflns_limit_k_min 0 _reflns_limit_k_max 29 _reflns_limit_l_min 1 _reflns_limit_l_max 29 _reflns_number_observed ? _reflns_d_resolution_high .734 _reflns_d_resolution_low 15.229 _diffrn_reflns_av_sigmaI/netI .116 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 150(2) _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression 'Eq22 p292 "Cryst. Comp." Munksgaard 1970' _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .096 _refine_ls_wR_factor_all .023 _refine_ls_goodness_of_fit_all 1.540 _refine_ls_shift/su_mean .002 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end #===END ######################################## # # # CIF generated by the Xtal System # # # ######################################## data_cpagtp _database_code_depnum_ccdc_archive 'CCDC 227420' _audit_creation_method Xtal3.6 _audit_creation_date 03-07-28 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C35 H40 Ag1 B1 N7 P1' _chemical_formula_moiety 'C33 H37 Ag1 B1 N6 P1, C2 H3 N' _chemical_formula_weight 708.41 _chemical_melting_point ? _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P_-1 _symmetry_space_group_name_Hall -p_1 loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,-y,-z _cell_length_a 10.8780(10) _cell_length_b 19.290(3) _cell_length_c 19.464(3) _cell_angle_alpha 61.793(2) _cell_angle_beta 75.916(2) _cell_angle_gamma 84.230(2) _cell_volume 3490.5(8) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.348 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 8658 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 28.84 _cell_measurement_temperature 150(2) _exptl_absorpt_coefficient_mu .658 _exptl_crystal_description bar _exptl_crystal_size_max .28 _exptl_crystal_size_mid .14 _exptl_crystal_size_min .12 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .89 _exptl_absorpt_correction_T_max 1 _diffrn_reflns_number 31848 _reflns_number_total 16668 _reflns_Friedel_coverage 0 _reflns_number_gt 14023 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 28.96 _diffrn_reflns_theta_full 27.5 _diffrn_measured_fraction_theta_max .90 _diffrn_measured_fraction_theta_full 1.00 _diffrn_reflns_av_R_equivalents .022 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .033 _refine_ls_wR_factor_ref .046 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_number_reflns 14023 _refine_ls_number_parameters 811 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .005 _refine_diff_density_min -.591 _refine_diff_density_max 1.278 _refine_ls_extinction_method none _refine_ls_extinction_coef ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 140 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 160 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Ag ? 0 4 -1.085 1.101 'Int Tables Vol IV Tables 2.2B and 2.3.1' B ? 0 4 0 .001 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 28 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' P ? 0 4 .09 .095 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ag1 .653346(15) .277304(10) .078134(10) .02309(16) Uani ? ? 1.00000 ? ? Ag2 .636696(15) .259939(10) .523718(10) .02253(16) Uani ? ? 1.00000 ? ? B1 .9287(2) .28478(14) -.04784(14) .019(2) Uani ? ? 1.00000 ? ? N111 .94026(16) .33073(10) -.00240(10) .0196(15) Uani ? ? 1.00000 ? ? N112 .83794(17) .34268(11) .04799(11) .0220(16) Uani ? ? 1.00000 ? ? C113 .8797(2) .38454(13) .07610(13) .025(2) Uani ? ? 1.00000 ? ? C1131 .7908(3) .40926(16) .13248(16) .036(3) Uani ? ? 1.00000 ? ? C114 1.0097(2) .40031(13) .04436(14) .027(2) Uani ? ? 1.00000 ? ? C115 1.0451(2) .36533(13) -.00513(13) .023(2) Uani ? ? 1.00000 ? ? C1151 1.1732(2) .36456(15) -.05524(15) .032(2) Uani ? ? 1.00000 ? ? N121 .89424(16) .19729(10) .01157(10) .0203(16) Uani ? ? 1.00000 ? ? N122 .79707(17) .17689(11) .07809(11) .0224(16) Uani ? ? 1.00000 ? ? C123 .7969(2) .09826(13) .11951(13) .025(2) Uani ? ? 1.00000 ? ? C1231 .7038(3) .05625(16) .19691(16) .040(3) Uani ? ? 1.00000 ? ? C124 .8942(2) .06786(13) .07962(15) .030(2) Uani ? ? 1.00000 ? ? C125 .9533(2) .13171(13) .01142(14) .025(2) Uani ? ? 1.00000 ? ? C1251 1.0608(2) .13394(16) -.05431(16) .035(2) Uani ? ? 1.00000 ? ? N131 .82924(16) .32321(10) -.09944(10) .0199(16) Uani ? ? 1.00000 ? ? N132 .70327(16) .32472(11) -.06497(11) .0220(16) Uani ? ? 1.00000 ? ? C133 .6452(2) .36480(14) -.12533(14) .025(2) Uani ? ? 1.00000 ? ? C1331 .5060(2) .37919(17) -.10965(15) .036(3) Uani ? ? 1.00000 ? ? C134 .7318(2) .38953(15) -.19872(14) .028(2) Uani ? ? 1.00000 ? ? C135 .8478(2) .36189(14) -.18011(13) .025(2) Uani ? ? 1.00000 ? ? C1351 .9750(2) .37008(18) -.23531(15) .040(3) Uani ? ? 1.00000 ? ? P1 .44262(5) .25692(3) .15309(3) .0209(5) Uani ? ? 1.00000 ? ? C141 .3536(2) .20577(13) .12183(13) .023(2) Uani ? ? 1.00000 ? ? C142 .4185(2) .15302(15) .09578(15) .030(2) Uani ? ? 1.00000 ? ? C143 .3532(3) .10606(16) .07983(16) .036(3) Uani ? ? 1.00000 ? ? C144 .2226(3) .11196(15) .08866(15) .034(2) Uani ? ? 1.00000 ? ? C145 .1581(2) .16554(16) .11177(16) .035(2) Uani ? ? 1.00000 ? ? C146 .2232(2) .21255(15) .12808(15) .031(2) Uani ? ? 1.00000 ? ? C151 .3509(2) .34454(13) .14353(13) .0216(19) Uani ? ? 1.00000 ? ? C152 .3813(2) .41404(14) .07202(13) .026(2) Uani ? ? 1.00000 ? ? C153 .3130(2) .48220(14) .06131(15) .030(2) Uani ? ? 1.00000 ? ? C154 .2152(2) .48191(14) .12241(16) .030(2) Uani ? ? 1.00000 ? ? C155 .1859(2) .41360(15) .19407(15) .031(2) Uani ? ? 1.00000 ? ? C156 .2521(2) .34501(14) .20464(13) .027(2) Uani ? ? 1.00000 ? ? C161 .4078(2) .19580(13) .26180(13) .023(2) Uani ? ? 1.00000 ? ? C162 .4566(2) .22021(16) .30742(15) .033(2) Uani ? ? 1.00000 ? ? C163 .4213(3) .18045(18) .39090(16) .040(3) Uani ? ? 1.00000 ? ? C164 .3406(2) .11600(17) .42878(15) .037(2) Uani ? ? 1.00000 ? ? C165 .2950(2) .08971(15) .38473(15) .034(2) Uani ? ? 1.00000 ? ? C166 .3280(2) .12992(14) .30112(14) .029(2) Uani ? ? 1.00000 ? ? B2 .3652(2) .31682(15) .59941(16) .024(2) Uani ? ? 1.00000 ? ? N211 .46192(16) .30769(11) .64980(11) .0227(17) Uani ? ? 1.00000 ? ? N212 .58972(17) .30618(11) .61997(11) .0229(17) Uani ? ? 1.00000 ? ? C213 .6467(2) .29613(13) .67746(14) .024(2) Uani ? ? 1.00000 ? ? C2131 .7879(2) .29382(16) .66425(16) .034(2) Uani ? ? 1.00000 ? ? C214 .5565(2) .29050(14) .74530(14) .028(2) Uani ? ? 1.00000 ? ? C215 .4405(2) .29769(14) .72560(14) .026(2) Uani ? ? 1.00000 ? ? C2151 .3096(3) .2962(2) .77466(17) .044(3) Uani ? ? 1.00000 ? ? N221 .41495(17) .37893(11) .51145(11) .0240(17) Uani ? ? 1.00000 ? ? N222 .50546(19) .36082(12) .45972(12) .0281(18) Uani ? ? 1.00000 ? ? C223 .5306(2) .42696(15) .39051(14) .031(2) Uani ? ? 1.00000 ? ? C2231 .6249(3) .42763(19) .31984(16) .051(3) Uani ? ? 1.00000 ? ? C224 .4564(2) .48828(14) .39687(15) .033(2) Uani ? ? 1.00000 ? ? C225 .3854(2) .45577(14) .47366(15) .028(2) Uani ? ? 1.00000 ? ? C2251 .2891(3) .49392(15) .51430(18) .039(3) Uani ? ? 1.00000 ? ? N231 .34406(17) .23593(11) .60443(11) .0222(17) Uani ? ? 1.00000 ? ? N232 .44598(17) .19133(11) .59280(11) .0225(17) Uani ? ? 1.00000 ? ? C233 .3987(2) .12434(13) .60503(12) .0225(19) Uani ? ? 1.00000 ? ? C2331 .4862(2) .06095(13) .59990(14) .028(2) Uani ? ? 1.00000 ? ? C234 .2659(2) .12500(14) .62413(14) .028(2) Uani ? ? 1.00000 ? ? C235 .2346(2) .19634(14) .62364(13) .025(2) Uani ? ? 1.00000 ? ? C2351 .1057(2) .22749(16) .64251(17) .036(3) Uani ? ? 1.00000 ? ? P2 .83737(5) .22045(3) .47905(3) .0197(5) Uani ? ? 1.00000 ? ? C241 .8473(2) .20492(13) .39240(12) .0212(19) Uani ? ? 1.00000 ? ? C242 .7580(2) .15391(15) .39841(15) .031(2) Uani ? ? 1.00000 ? ? C243 .7529(2) .14494(17) .33230(16) .036(3) Uani ? ? 1.00000 ? ? C244 .8354(2) .18706(16) .25956(15) .035(3) Uani ? ? 1.00000 ? ? C245 .9231(3) .23735(17) .25330(14) .037(2) Uani ? ? 1.00000 ? ? C246 .9308(2) .24584(15) .31944(14) .031(2) Uani ? ? 1.00000 ? ? C251 .8888(2) .12808(12) .55259(13) .0219(19) Uani ? ? 1.00000 ? ? C252 .8379(2) .10576(14) .63355(14) .030(2) Uani ? ? 1.00000 ? ? C253 .8775(3) .03800(15) .69246(14) .037(2) Uani ? ? 1.00000 ? ? C254 .9672(3) -.00873(14) .67145(15) .035(2) Uani ? ? 1.00000 ? ? C255 1.0180(2) .01212(14) .59188(16) .033(2) Uani ? ? 1.00000 ? ? C256 .9794(2) .08014(14) .53220(14) .027(2) Uani ? ? 1.00000 ? ? C261 .9660(2) .29006(13) .44903(13) .0233(19) Uani ? ? 1.00000 ? ? C262 .9335(2) .36610(15) .43504(17) .036(3) Uani ? ? 1.00000 ? ? C263 1.0267(3) .42176(16) .4137(2) .049(3) Uani ? ? 1.00000 ? ? C264 1.1529(3) .40155(18) .40592(17) .044(3) Uani ? ? 1.00000 ? ? C265 1.1864(2) .32584(18) .42043(17) .040(3) Uani ? ? 1.00000 ? ? C266 1.0933(2) .27013(15) .44203(16) .034(2) Uani ? ? 1.00000 ? ? N11 .8309(4) .1007(2) -.1583(2) .089(5) Uani ? ? 1.00000 ? ? C11 .7631(3) .11730(18) -.11418(18) .048(3) Uani ? ? 1.00000 ? ? C12 .6762(3) .13789(18) -.05791(18) .044(3) Uani ? ? 1.00000 ? ? N21 .6126(3) -.06145(19) .08446(18) .065(4) Uani ? ? 1.00000 ? ? C21 .5504(3) -.07740(17) .14621(18) .041(3) Uani ? ? 1.00000 ? ? C22 .4652(3) -.09494(18) .22347(18) .050(3) Uani ? ? 1.00000 ? ? H1 1.01061 .28811 -.08508 .02500 Uiso ? ? 1.00000 ? ? H1131a .82205 .39319 .17943 .05600 Uiso ? ? 1.00000 ? ? H1131b .70867 .38555 .14799 .05600 Uiso ? ? 1.00000 ? ? H1131c .78231 .46492 .10756 .05600 Uiso ? ? 1.00000 ? ? H114 1.06312 .42945 .05473 .03400 Uiso ? ? 1.00000 ? ? H1151a 1.17101 .39171 -.11113 .05000 Uiso ? ? 1.00000 ? ? H1151b 1.20003 .31243 -.04224 .05000 Uiso ? ? 1.00000 ? ? H1151c 1.23366 .39050 -.04710 .05000 Uiso ? ? 1.00000 ? ? H1231a .74929 .02368 .23690 .06100 Uiso ? ? 1.00000 ? ? H1231b .65062 .02345 .19134 .06100 Uiso ? ? 1.00000 ? ? H1231c .65276 .09275 .21076 .06100 Uiso ? ? 1.00000 ? ? H124 .91537 .01371 .09621 .03700 Uiso ? ? 1.00000 ? ? H1251a 1.12921 .16587 -.06150 .05400 Uiso ? ? 1.00000 ? ? H1251b 1.03379 .15520 -.10358 .05400 Uiso ? ? 1.00000 ? ? H1251c 1.09064 .08235 -.04232 .05400 Uiso ? ? 1.00000 ? ? H1331a .46436 .33685 -.06016 .05500 Uiso ? ? 1.00000 ? ? H1331b .47140 .38290 -.15144 .05500 Uiso ? ? 1.00000 ? ? H1331c .49048 .42696 -.10537 .05500 Uiso ? ? 1.00000 ? ? H134 .71575 .42010 -.25155 .03600 Uiso ? ? 1.00000 ? ? H1351a 1.00828 .31980 -.22595 .06000 Uiso ? ? 1.00000 ? ? H1351b 1.03253 .39837 -.22731 .06000 Uiso ? ? 1.00000 ? ? H1351c .96687 .39863 -.28971 .06000 Uiso ? ? 1.00000 ? ? H142 .50859 .14896 .08937 .03700 Uiso ? ? 1.00000 ? ? H143 .39811 .06952 .06302 .04500 Uiso ? ? 1.00000 ? ? H144 .17654 .07870 .07958 .04200 Uiso ? ? 1.00000 ? ? H145 .06862 .17015 .11606 .04400 Uiso ? ? 1.00000 ? ? H146 .17835 .24982 .14402 .04000 Uiso ? ? 1.00000 ? ? H152 .44876 .41448 .02964 .03300 Uiso ? ? 1.00000 ? ? H153 .33360 .52953 .01175 .03800 Uiso ? ? 1.00000 ? ? H154 .16929 .52875 .11542 .03700 Uiso ? ? 1.00000 ? ? H155 .12004 .41355 .23664 .03800 Uiso ? ? 1.00000 ? ? H156 .22895 .29735 .25445 .03400 Uiso ? ? 1.00000 ? ? H162 .51446 .26484 .28060 .04200 Uiso ? ? 1.00000 ? ? H163 .45514 .19881 .42118 .05100 Uiso ? ? 1.00000 ? ? H164 .31521 .08888 .48637 .04700 Uiso ? ? 1.00000 ? ? H165 .23942 .04360 .41179 .04400 Uiso ? ? 1.00000 ? ? H166 .29576 .11215 .27020 .03600 Uiso ? ? 1.00000 ? ? H2 .28392 .33373 .62218 .03100 Uiso ? ? 1.00000 ? ? H2131a .82314 .28337 .62028 .05200 Uiso ? ? 1.00000 ? ? H2131b .81162 .25283 .71103 .05200 Uiso ? ? 1.00000 ? ? H2131c .82049 .34255 .65356 .05200 Uiso ? ? 1.00000 ? ? H214 .57211 .28304 .79483 .03500 Uiso ? ? 1.00000 ? ? H2151a .27100 .34600 .75211 .06800 Uiso ? ? 1.00000 ? ? H2151b .31296 .28277 .82839 .06800 Uiso ? ? 1.00000 ? ? H2151c .25706 .25763 .77727 .06800 Uiso ? ? 1.00000 ? ? H2231a .65791 .37629 .33412 .07800 Uiso ? ? 1.00000 ? ? H2231b .69255 .46338 .30484 .07800 Uiso ? ? 1.00000 ? ? H2231c .58508 .44324 .27651 .07800 Uiso ? ? 1.00000 ? ? H224 .45523 .54119 .35605 .04000 Uiso ? ? 1.00000 ? ? H2251a .28922 .54918 .47958 .05900 Uiso ? ? 1.00000 ? ? H2251b .31124 .48543 .56202 .05900 Uiso ? ? 1.00000 ? ? H2251c .20730 .47196 .52703 .05900 Uiso ? ? 1.00000 ? ? H2331a .45438 .01114 .64246 .04300 Uiso ? ? 1.00000 ? ? H2331b .56813 .06995 .60389 .04300 Uiso ? ? 1.00000 ? ? H2331c .49250 .06102 .55017 .04300 Uiso ? ? 1.00000 ? ? H234 .20878 .08446 .63496 .03500 Uiso ? ? 1.00000 ? ? H2351a .09699 .23231 .68978 .05700 Uiso ? ? 1.00000 ? ? H2351b .04336 .19111 .65120 .05700 Uiso ? ? 1.00000 ? ? H2351c .09541 .27694 .59891 .05700 Uiso ? ? 1.00000 ? ? H242 .70024 .12508 .44864 .03900 Uiso ? ? 1.00000 ? ? H243 .69213 .10876 .33741 .04600 Uiso ? ? 1.00000 ? ? H244 .83147 .18133 .21390 .04400 Uiso ? ? 1.00000 ? ? H245 .97936 .26795 .20268 .04800 Uiso ? ? 1.00000 ? ? H246 .99359 .28061 .31418 .04100 Uiso ? ? 1.00000 ? ? H252 .77432 .13786 .64852 .03700 Uiso ? ? 1.00000 ? ? H253 .84260 .02346 .74777 .04700 Uiso ? ? 1.00000 ? ? H254 .99353 -.05654 .71212 .04400 Uiso ? ? 1.00000 ? ? H255 1.08175 -.01990 .57742 .04100 Uiso ? ? 1.00000 ? ? H256 1.01273 .09375 .47717 .03400 Uiso ? ? 1.00000 ? ? H262 .84624 .38029 .44063 .04600 Uiso ? ? 1.00000 ? ? H263 1.00163 .47400 .40400 .06300 Uiso ? ? 1.00000 ? ? H264 1.21689 .43984 .39124 .05500 Uiso ? ? 1.00000 ? ? H265 1.27437 .31168 .41549 .04900 Uiso ? ? 1.00000 ? ? H266 1.11772 .21731 .45155 .04300 Uiso ? ? 1.00000 ? ? H12a .69449 .19024 -.06937 .06700 Uiso ? ? 1.00000 ? ? H12b .68601 .10268 -.00496 .06700 Uiso ? ? 1.00000 ? ? H12c .59180 .13488 -.06125 .06700 Uiso ? ? 1.00000 ? ? H22a .50725 -.12837 .26562 .07600 Uiso ? ? 1.00000 ? ? H22b .39113 -.12164 .22985 .07600 Uiso ? ? 1.00000 ? ? H22c .44273 -.04765 .22725 .07600 Uiso ? ? 1.00000 ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ag1 .01528(8) .02789(9) .02621(9) .00067(6) -.00020(6) -.01479(7) Ag2 .01592(8) .02584(9) .02720(9) .00476(6) -.00200(6) -.01555(7) B1 .0156(11) .0209(11) .0212(11) .0006(9) -.0022(9) -.0108(9) N111 .0146(8) .0221(9) .0224(9) .0016(7) -.0030(7) -.0113(7) N112 .0183(9) .0231(9) .0262(9) .0019(7) -.0023(7) -.0142(8) C113 .0280(12) .0222(11) .0273(11) .0017(9) -.0068(9) -.0135(9) C1131 .0391(14) .0386(14) .0406(14) .0019(11) -.0058(11) -.0279(12) C114 .0274(12) .0260(11) .0309(12) -.0014(9) -.0096(9) -.0143(10) C115 .0210(11) .0216(11) .0264(11) -.0007(8) -.0074(9) -.0096(9) C1151 .0201(11) .0349(13) .0396(14) -.0050(10) -.0024(10) -.0169(11) N121 .0180(9) .0213(9) .0212(8) .0022(7) -.0027(7) -.0108(7) N122 .0217(9) .0221(9) .0230(9) .0012(7) -.0031(7) -.0112(7) C123 .0292(12) .0216(11) .0272(11) .0008(9) -.0087(9) -.0116(9) C1231 .0478(16) .0300(13) .0324(13) -.0073(12) -.0025(12) -.0091(11) C124 .0352(13) .0215(11) .0376(13) .0063(9) -.0126(11) -.0167(10) C125 .0254(11) .0246(11) .0321(12) .0062(9) -.0109(9) -.0185(10) C1251 .0332(13) .0363(14) .0393(14) .0090(11) -.0033(11) -.0246(12) N131 .0170(8) .0236(9) .0201(8) .0006(7) -.0023(7) -.0118(7) N132 .0151(8) .0269(10) .0250(9) .0016(7) -.0035(7) -.0136(8) C133 .0198(11) .0309(12) .0295(11) .0038(9) -.0077(9) -.0184(10) C1331 .0252(12) .0540(17) .0361(13) .0118(11) -.0124(10) -.0273(13) C134 .0275(12) .0354(13) .0259(11) .0031(10) -.0106(9) -.0153(10) C135 .0249(11) .0302(12) .0229(10) -.0001(9) -.0050(9) -.0143(9) C1351 .0272(13) .0615(18) .0252(12) -.0019(12) .0004(10) -.0183(12) P1 .0159(3) .0243(3) .0227(3) .0017(2) -.0018(2) -.0126(2) C141 .0223(11) .0234(11) .0239(10) .0021(8) -.0055(9) -.0112(9) C142 .0238(12) .0362(13) .0355(13) .0037(10) -.0043(10) -.0226(11) C143 .0395(15) .0362(14) .0418(14) .0061(11) -.0108(12) -.0259(12) C144 .0420(15) .0303(13) .0342(13) -.0029(11) -.0167(11) -.0130(11) C145 .0258(12) .0401(14) .0434(14) .0033(10) -.0151(11) -.0203(12) C146 .0243(12) .0333(13) .0403(13) .0077(10) -.0109(10) -.0216(11) C151 .0188(10) .0233(11) .0254(10) .0002(8) -.0037(8) -.0140(9) C152 .0242(11) .0283(12) .0242(11) -.0024(9) -.0023(9) -.0111(9) C153 .0292(12) .0260(12) .0319(12) -.0010(9) -.0090(10) -.0094(10) C154 .0298(12) .0252(12) .0444(14) .0044(9) -.0145(11) -.0211(11) C155 .0274(12) .0330(13) .0341(13) .0054(10) -.0019(10) -.0203(11) C156 .0249(11) .0272(12) .0249(11) .0023(9) -.0023(9) -.0117(9) C161 .0189(10) .0257(11) .0231(10) .0074(8) -.0041(8) -.0109(9) C162 .0283(13) .0399(14) .0333(13) .0031(10) -.0100(10) -.0178(11) C163 .0350(14) .0556(18) .0349(14) .0098(13) -.0156(11) -.0246(13) C164 .0293(13) .0480(16) .0252(12) .0123(11) -.0063(10) -.0120(11) C165 .0284(13) .0347(14) .0291(12) .0048(10) -.0025(10) -.0091(11) C166 .0248(12) .0305(12) .0293(12) .0048(9) -.0049(9) -.0146(10) B2 .0157(11) .0259(13) .0336(13) .0051(9) -.0040(10) -.0180(11) N211 .0159(9) .0276(10) .0285(9) .0029(7) -.0021(7) -.0179(8) N212 .0156(9) .0271(10) .0283(9) .0031(7) -.0015(7) -.0169(8) C213 .0207(11) .0233(11) .0325(12) .0011(8) -.0075(9) -.0150(9) C2131 .0216(12) .0479(15) .0406(14) .0044(10) -.0092(10) -.0265(12) C214 .0280(12) .0315(12) .0278(11) -.0006(9) -.0048(9) -.0175(10) C215 .0234(11) .0309(12) .0270(11) -.0019(9) -.0008(9) -.0170(10) C2151 .0279(13) .072(2) .0401(15) -.0017(13) .0036(11) -.0370(15) N221 .0194(9) .0247(9) .0312(10) .0058(7) -.0079(8) -.0156(8) N222 .0257(10) .0299(11) .0283(10) .0078(8) -.0056(8) -.0148(8) C223 .0302(13) .0312(13) .0286(12) .0029(10) -.0091(10) -.0102(10) C2231 .0552(19) .0498(18) .0290(14) .0077(15) -.0011(13) -.0093(13) C224 .0318(13) .0253(12) .0394(13) .0031(10) -.0148(11) -.0110(10) C225 .0243(12) .0262(12) .0410(13) .0057(9) -.0159(10) -.0179(10) C2251 .0357(14) .0307(14) .0566(17) .0110(11) -.0138(13) -.0246(13) N231 .0172(9) .0268(10) .0263(9) .0039(7) -.0045(7) -.0160(8) N232 .0155(9) .0239(9) .0287(9) .0038(7) -.0039(7) -.0137(8) C233 .0243(11) .0232(11) .0197(10) .0003(8) -.0047(8) -.0099(8) C2331 .0294(12) .0233(11) .0309(12) .0024(9) -.0044(10) -.0131(10) C234 .0238(11) .0293(12) .0295(12) -.0050(9) -.0054(9) -.0124(10) C235 .0183(10) .0314(12) .0253(11) .0010(9) -.0055(8) -.0128(9) C2351 .0166(11) .0455(15) .0497(15) .0023(10) -.0055(10) -.0264(13) P2 .0156(2) .0209(3) .0225(3) .0026(2) -.0015(2) -.0117(2) C241 .0187(10) .0239(11) .0228(10) .0058(8) -.0046(8) -.0134(9) C242 .0272(12) .0381(14) .0302(12) -.0031(10) -.0018(10) -.0187(11) C243 .0324(13) .0462(16) .0424(15) .0052(11) -.0126(11) -.0289(13) C244 .0364(14) .0476(16) .0309(12) .0176(12) -.0160(11) -.0260(12) C245 .0342(14) .0491(16) .0233(12) .0036(12) -.0005(10) -.0155(11) C246 .0237(12) .0392(14) .0291(12) -.0020(10) -.0009(9) -.0158(11) C251 .0203(10) .0188(10) .0274(11) .0015(8) -.0059(8) -.0113(9) C252 .0310(13) .0286(12) .0289(12) .0036(10) -.0018(10) -.0145(10) C253 .0450(15) .0324(14) .0237(12) .0006(11) -.0037(11) -.0072(10) C254 .0426(15) .0213(12) .0368(13) .0029(10) -.0155(11) -.0074(10) C255 .0337(13) .0254(12) .0445(14) .0089(10) -.0135(11) -.0194(11) C256 .0247(11) .0291(12) .0286(11) .0041(9) -.0052(9) -.0162(10) C261 .0209(11) .0239(11) .0230(10) -.0016(8) -.0024(8) -.0100(9) C262 .0319(13) .0268(13) .0488(15) .0012(10) -.0041(11) -.0187(12) C263 .0485(18) .0272(14) .065(2) -.0086(12) -.0008(15) -.0203(14) C264 .0461(17) .0467(17) .0401(15) -.0218(13) -.0011(13) -.0201(13) C265 .0245(13) .0502(17) .0435(15) -.0085(11) -.0070(11) -.0187(13) C266 .0226(12) .0340(13) .0445(14) .0010(10) -.0074(10) -.0185(12) N11 .109(3) .102(3) .066(2) .013(2) -.005(2) -.056(2) C11 .065(2) .0419(16) .0437(16) .0008(14) -.0178(15) -.0229(14) C12 .0454(17) .0517(18) .0486(16) .0016(13) -.0167(14) -.0312(14) N21 .063(2) .072(2) .0611(19) -.0027(16) .0030(15) -.0394(17) C21 .0447(16) .0391(15) .0461(16) .0019(12) -.0152(13) -.0230(13) C22 .069(2) .0432(17) .0376(15) -.0135(15) -.0072(14) -.0183(13) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Ag1 N112 . . 2.281(2) ? Ag1 N122 . . 2.364(2) ? Ag1 N132 . . 2.418(2) ? Ag1 P1 . . 2.3556(6) ? Ag2 N212 . . 2.364(3) ? Ag2 N222 . . 2.322(2) ? Ag2 N232 . . 2.3186(17) ? Ag2 P2 . . 2.3387(6) ? B1 N111 . . 1.550(4) ? B1 N121 . . 1.548(3) ? B1 N131 . . 1.547(3) ? B1 H1 . . .988 ? N111 N112 . . 1.373(3) ? N111 C115 . . 1.356(3) ? N112 C113 . . 1.331(4) ? C113 C1131 . . 1.501(4) ? C113 C114 . . 1.399(3) ? C1131 H1131a . . .953 ? C1131 H1131b . . .959 ? C1131 H1131c . . .952 ? C114 C115 . . 1.383(4) ? C114 H114 . . .962 ? C115 C1151 . . 1.497(3) ? C1151 H1151a . . .964 ? C1151 H1151b . . .947 ? C1151 H1151c . . .949 ? N121 N122 . . 1.373(2) ? N121 C125 . . 1.361(3) ? N122 C123 . . 1.340(3) ? C123 C1231 . . 1.490(3) ? C123 C124 . . 1.404(4) ? C1231 H1231a . . .953 ? C1231 H1231b . . .957 ? C1231 H1231c . . .951 ? C124 C125 . . 1.375(3) ? C124 H124 . . .958 ? C125 C1251 . . 1.495(4) ? C1251 H1251a . . .955 ? C1251 H1251b . . .957 ? C1251 H1251c . . .950 ? N131 N132 . . 1.375(2) ? N131 C135 . . 1.353(3) ? N132 C133 . . 1.335(3) ? C133 C1331 . . 1.495(3) ? C133 C134 . . 1.395(3) ? C1331 H1331a . . .958 ? C1331 H1331b . . .947 ? C1331 H1331c . . .959 ? C134 C135 . . 1.384(3) ? C134 H134 . . .964 ? C135 C1351 . . 1.501(3) ? C1351 H1351a . . .948 ? C1351 H1351b . . .954 ? C1351 H1351c . . .958 ? P1 C141 . . 1.825(3) ? P1 C151 . . 1.828(2) ? P1 C161 . . 1.831(2) ? C141 C142 . . 1.400(4) ? C141 C146 . . 1.392(3) ? C142 C143 . . 1.387(5) ? C142 H142 . . .957 ? C143 C144 . . 1.389(4) ? C143 H143 . . .956 ? C144 C145 . . 1.379(5) ? C144 H144 . . .953 ? C145 C146 . . 1.391(5) ? C145 H145 . . .955 ? C146 H146 . . .958 ? C151 C152 . . 1.395(3) ? C151 C156 . . 1.398(3) ? C152 C153 . . 1.394(4) ? C152 H152 . . .959 ? C153 C154 . . 1.387(4) ? C153 H153 . . .958 ? C154 C155 . . 1.384(3) ? C154 H154 . . .954 ? C155 C156 . . 1.391(4) ? C155 H155 . . .954 ? C156 H156 . . .9663 ? C161 C162 . . 1.402(5) ? C161 C166 . . 1.390(3) ? C162 C163 . . 1.398(4) ? C162 H162 . . .967 ? C163 C164 . . 1.378(4) ? C163 H163 . . .968 ? C164 C165 . . 1.381(5) ? C164 H164 . . .965 ? C165 C166 . . 1.399(3) ? C165 H165 . . .972 ? C166 H166 . . .962 ? B2 N211 . . 1.549(4) ? B2 N221 . . 1.549(3) ? B2 N231 . . 1.554(4) ? B2 H2 . . .986 ? N211 N212 . . 1.373(2) ? N211 C215 . . 1.357(4) ? N212 C213 . . 1.335(4) ? C213 C2131 . . 1.495(3) ? C213 C214 . . 1.405(3) ? C2131 H2131a . . .953 ? C2131 H2131b . . .956 ? C2131 H2131c . . .948 ? C214 C215 . . 1.381(4) ? C214 H214 . . .961 ? C215 C2151 . . 1.503(3) ? C2151 H2151a . . .950 ? C2151 H2151b . . .961 ? C2151 H2151c . . .958 ? N221 N222 . . 1.373(3) ? N221 C225 . . 1.353(3) ? N222 C223 . . 1.335(3) ? C223 C2231 . . 1.498(4) ? C223 C224 . . 1.401(4) ? C2231 H2231a . . .951 ? C2231 H2231b . . .953 ? C2231 H2231c . . .950 ? C224 C225 . . 1.369(3) ? C224 H224 . . .953 ? C225 C2251 . . 1.502(4) ? C2251 H2251a . . .955 ? C2251 H2251b . . .951 ? C2251 H2251c . . .950 ? N231 N232 . . 1.375(3) ? N231 C235 . . 1.355(3) ? N232 C233 . . 1.332(3) ? C233 C2331 . . 1.499(4) ? C233 C234 . . 1.402(3) ? C2331 H2331a . . .951 ? C2331 H2331b . . .953 ? C2331 H2331c . . .953 ? C234 C235 . . 1.380(4) ? C234 H234 . . .959 ? C235 C2351 . . 1.501(3) ? C2351 H2351a . . .949 ? C2351 H2351b . . .953 ? C2351 H2351c . . .950 ? P2 C241 . . 1.824(3) ? P2 C251 . . 1.821(2) ? P2 C261 . . 1.828(3) ? C241 C242 . . 1.398(4) ? C241 C246 . . 1.386(3) ? C242 C243 . . 1.391(5) ? C242 H242 . . .958 ? C243 C244 . . 1.382(3) ? C243 H243 . . .964 ? C244 C245 . . 1.372(5) ? C244 H244 . . .957 ? C245 C246 . . 1.395(5) ? C245 H245 . . .961 ? C246 H246 . . .959 ? C251 C252 . . 1.399(3) ? C251 C256 . . 1.399(4) ? C252 C253 . . 1.385(3) ? C252 H252 . . .966 ? C253 C254 . . 1.382(4) ? C253 H253 . . .958 ? C254 C255 . . 1.380(4) ? C254 H254 . . .963 ? C255 C256 . . 1.391(3) ? C255 H255 . . .962 ? C256 H256 . . .955 ? C261 C262 . . 1.384(4) ? C261 C266 . . 1.391(3) ? C262 C263 . . 1.394(4) ? C262 H262 . . .956 ? C263 C264 . . 1.381(4) ? C263 H263 . . .957 ? C264 C265 . . 1.378(5) ? C264 H264 . . .959 ? C265 C266 . . 1.393(4) ? C265 H265 . . .963 ? C266 H266 . . .966 ? N11 C11 . . 1.136(6) ? C11 C12 . . 1.443(5) ? C12 H12a . . .956 ? C12 H12b . . .955 ? C12 H12c . . .946 ? N21 C21 . . 1.137(4) ? C21 C22 . . 1.462(4) ? C22 H22a . . .960 ? C22 H22b . . .951 ? C22 H22c . . .952 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published N112 Ag1 N122 . . . 81.28(7) ? N112 Ag1 N132 . . . 81.88(7) ? N112 Ag1 P1 . . . 143.26(6) ? N122 Ag1 N132 . . . 83.90(6) ? N122 Ag1 P1 . . . 125.32(4) ? N132 Ag1 P1 . . . 121.85(5) ? N212 Ag2 N222 . . . 83.67(8) ? N212 Ag2 N232 . . . 84.11(8) ? N212 Ag2 P2 . . . 124.44(5) ? N222 Ag2 N232 . . . 82.82(6) ? N222 Ag2 P2 . . . 132.80(5) ? N232 Ag2 P2 . . . 131.71(5) ? N111 B1 N121 . . . 110.53(18) ? N111 B1 N131 . . . 110.2(2) ? N111 B1 H1 . . . 109.1 ? N121 B1 N131 . . . 111.0(2) ? N121 B1 H1 . . . 109.2 ? N131 B1 H1 . . . 106.7 ? B1 N111 N112 . . . 122.20(19) ? B1 N111 C115 . . . 128.15(19) ? N112 N111 C115 . . . 109.6(2) ? Ag1 N112 N111 . . . 117.70(18) ? Ag1 N112 C113 . . . 134.71(15) ? N111 N112 C113 . . . 106.91(19) ? N112 C113 C1131 . . . 120.9(2) ? N112 C113 C114 . . . 110.2(2) ? C1131 C113 C114 . . . 129.0(3) ? C113 C1131 H1131a . . . 110.2 ? C113 C1131 H1131b . . . 110.3 ? C113 C1131 H1131c . . . 110.4 ? H1131a C1131 H1131b . . . 108.4 ? H1131a C1131 H1131c . . . 108.9 ? H1131b C1131 H1131c . . . 108.5 ? C113 C114 C115 . . . 105.6(3) ? C113 C114 H114 . . . 127.2 ? C115 C114 H114 . . . 127.2 ? N111 C115 C114 . . . 107.7(2) ? N111 C115 C1151 . . . 123.7(3) ? C114 C115 C1151 . . . 128.6(3) ? C115 C1151 H1151a . . . 110.1 ? C115 C1151 H1151b . . . 111.2 ? C115 C1151 H1151c . . . 110.2 ? H1151a C1151 H1151b . . . 108.5 ? H1151a C1151 H1151c . . . 108.2 ? H1151b C1151 H1151c . . . 108.6 ? B1 N121 N122 . . . 120.81(19) ? B1 N121 C125 . . . 128.83(17) ? N122 N121 C125 . . . 110.24(15) ? Ag1 N122 N121 . . . 116.34(12) ? Ag1 N122 C123 . . . 135.67(14) ? N121 N122 C123 . . . 106.37(19) ? N122 C123 C1231 . . . 120.5(2) ? N122 C123 C124 . . . 109.92(17) ? C1231 C123 C124 . . . 129.6(2) ? C123 C1231 H1231a . . . 108.4 ? C123 C1231 H1231b . . . 108.5 ? C123 C1231 H1231c . . . 110.6 ? H1231a C1231 H1231b . . . 108.6 ? H1231a C1231 H1231c . . . 111.4 ? H1231b C1231 H1231c . . . 109.2 ? C123 C124 C125 . . . 106.1(2) ? C123 C124 H124 . . . 127.3 ? C125 C124 H124 . . . 126.7 ? N121 C125 C124 . . . 107.4(2) ? N121 C125 C1251 . . . 123.35(18) ? C124 C125 C1251 . . . 129.3(2) ? C125 C1251 H1251a . . . 110.7 ? C125 C1251 H1251b . . . 110.4 ? C125 C1251 H1251c . . . 110.4 ? H1251a C1251 H1251b . . . 108.4 ? H1251a C1251 H1251c . . . 108.9 ? H1251b C1251 H1251c . . . 108.0 ? B1 N131 N132 . . . 121.29(16) ? B1 N131 C135 . . . 128.55(17) ? N132 N131 C135 . . . 110.10(18) ? Ag1 N132 N131 . . . 115.69(14) ? Ag1 N132 C133 . . . 137.19(15) ? N131 N132 C133 . . . 106.11(17) ? N132 C133 C1331 . . . 120.8(2) ? N132 C133 C134 . . . 110.7(2) ? C1331 C133 C134 . . . 128.5(2) ? C133 C1331 H1331a . . . 109.8 ? C133 C1331 H1331b . . . 110.5 ? C133 C1331 H1331c . . . 110.1 ? H1331a C1331 H1331b . . . 109.1 ? H1331a C1331 H1331c . . . 108.1 ? H1331b C1331 H1331c . . . 109.3 ? C133 C134 C135 . . . 105.4(2) ? C133 C134 H134 . . . 128.0 ? C135 C134 H134 . . . 126.5 ? N131 C135 C134 . . . 107.67(19) ? N131 C135 C1351 . . . 123.3(2) ? C134 C135 C1351 . . . 129.1(2) ? C135 C1351 H1351a . . . 110.4 ? C135 C1351 H1351b . . . 110.2 ? C135 C1351 H1351c . . . 109.7 ? H1351a C1351 H1351b . . . 109.3 ? H1351a C1351 H1351c . . . 109.0 ? H1351b C1351 H1351c . . . 108.3 ? Ag1 P1 C141 . . . 109.21(8) ? Ag1 P1 C151 . . . 116.95(6) ? Ag1 P1 C161 . . . 120.43(7) ? C141 P1 C151 . . . 104.96(12) ? C141 P1 C161 . . . 102.01(11) ? C151 P1 C161 . . . 101.33(11) ? P1 C141 C142 . . . 118.06(19) ? P1 C141 C146 . . . 123.1(2) ? C142 C141 C146 . . . 118.7(3) ? C141 C142 C143 . . . 120.5(2) ? C141 C142 H142 . . . 119.8 ? C143 C142 H142 . . . 119.7 ? C142 C143 C144 . . . 119.9(3) ? C142 C143 H143 . . . 120.0 ? C144 C143 H143 . . . 120.1 ? C143 C144 C145 . . . 120.0(3) ? C143 C144 H144 . . . 120.6 ? C145 C144 H144 . . . 119.4 ? C144 C145 C146 . . . 120.2(3) ? C144 C145 H145 . . . 119.2 ? C146 C145 H145 . . . 120.6 ? C141 C146 C145 . . . 120.5(3) ? C141 C146 H146 . . . 119.4 ? C145 C146 H146 . . . 120.1 ? P1 C151 C152 . . . 118.33(18) ? P1 C151 C156 . . . 123.00(14) ? C152 C151 C156 . . . 118.7(2) ? C151 C152 C153 . . . 120.6(2) ? C151 C152 H152 . . . 119.5 ? C153 C152 H152 . . . 119.94 ? C152 C153 C154 . . . 120.20(19) ? C152 C153 H153 . . . 120.1 ? C154 C153 H153 . . . 119.7 ? C153 C154 C155 . . . 119.6(2) ? C153 C154 H154 . . . 120.3 ? C155 C154 H154 . . . 120.1 ? C154 C155 C156 . . . 120.5(2) ? C154 C155 H155 . . . 119.8 ? C156 C155 H155 . . . 119.7 ? C151 C156 C155 . . . 120.45(18) ? C151 C156 H156 . . . 120.0 ? C155 C156 H156 . . . 119.6 ? P1 C161 C162 . . . 118.10(16) ? P1 C161 C166 . . . 122.9(2) ? C162 C161 C166 . . . 118.8(2) ? C161 C162 C163 . . . 120.2(3) ? C161 C162 H162 . . . 119.4 ? C163 C162 H162 . . . 120.4 ? C162 C163 C164 . . . 120.1(3) ? C162 C163 H163 . . . 118.8 ? C164 C163 H163 . . . 121.1 ? C163 C164 C165 . . . 120.4(2) ? C163 C164 H164 . . . 120.3 ? C165 C164 H164 . . . 119.4 ? C164 C165 C166 . . . 119.9(2) ? C164 C165 H165 . . . 120.0 ? C166 C165 H165 . . . 120.1 ? C161 C166 C165 . . . 120.5(3) ? C161 C166 H166 . . . 119.3 ? C165 C166 H166 . . . 120.2 ? N211 B2 N221 . . . 109.86(18) ? N211 B2 N231 . . . 109.26(18) ? N211 B2 H2 . . . 108.6 ? N221 B2 N231 . . . 110.6(2) ? N221 B2 H2 . . . 109.9 ? N231 B2 H2 . . . 108.6 ? B2 N211 N212 . . . 120.8(2) ? B2 N211 C215 . . . 129.22(18) ? N212 N211 C215 . . . 110.0(2) ? Ag2 N212 N211 . . . 112.89(17) ? Ag2 N212 C213 . . . 132.10(16) ? N211 N212 C213 . . . 106.4(2) ? N212 C213 C2131 . . . 120.7(2) ? N212 C213 C214 . . . 110.5(2) ? C2131 C213 C214 . . . 128.8(3) ? C213 C2131 H2131a . . . 109.8 ? C213 C2131 H2131b . . . 109.41 ? C213 C2131 H2131c . . . 110.2 ? H2131a C2131 H2131b . . . 108.8 ? H2131a C2131 H2131c . . . 109.4 ? H2131b C2131 H2131c . . . 109.2 ? C213 C214 C215 . . . 105.2(2) ? C213 C214 H214 . . . 127.4 ? C215 C214 H214 . . . 127.4 ? N211 C215 C214 . . . 107.9(2) ? N211 C215 C2151 . . . 122.7(2) ? C214 C215 C2151 . . . 129.4(3) ? C215 C2151 H2151a . . . 110.9 ? C215 C2151 H2151b . . . 110.5 ? C215 C2151 H2151c . . . 110.5 ? H2151a C2151 H2151b . . . 108.6 ? H2151a C2151 H2151c . . . 108.4 ? H2151b C2151 H2151c . . . 107.8 ? B2 N221 N222 . . . 121.37(18) ? B2 N221 C225 . . . 129.2(2) ? N222 N221 C225 . . . 109.39(17) ? Ag2 N222 N221 . . . 113.22(13) ? Ag2 N222 C223 . . . 131.05(16) ? N221 N222 C223 . . . 106.5(2) ? N222 C223 C2231 . . . 120.5(2) ? N222 C223 C224 . . . 110.2(2) ? C2231 C223 C224 . . . 129.3(2) ? C223 C2231 H2231a . . . 109.1 ? C223 C2231 H2231b . . . 109.1 ? C223 C2231 H2231c . . . 109.8 ? H2231a C2231 H2231b . . . 109.1 ? H2231a C2231 H2231c . . . 109.6 ? H2231b C2231 H2231c . . . 110.0 ? C223 C224 C225 . . . 105.3(2) ? C223 C224 H224 . . . 127.1 ? C225 C224 H224 . . . 127.5 ? N221 C225 C224 . . . 108.6(2) ? N221 C225 C2251 . . . 122.4(2) ? C224 C225 C2251 . . . 129.0(2) ? C225 C2251 H2251a . . . 109.2 ? C225 C2251 H2251b . . . 109.2 ? C225 C2251 H2251c . . . 110.0 ? H2251a C2251 H2251b . . . 109.0 ? H2251a C2251 H2251c . . . 109.9 ? H2251b C2251 H2251c . . . 109.5 ? B2 N231 N232 . . . 120.28(18) ? B2 N231 C235 . . . 129.7(2) ? N232 N231 C235 . . . 109.9(2) ? Ag2 N232 N231 . . . 115.29(13) ? Ag2 N232 C233 . . . 134.80(16) ? N231 N232 C233 . . . 106.58(18) ? N232 C233 C2331 . . . 120.0(2) ? N232 C233 C234 . . . 110.2(2) ? C2331 C233 C234 . . . 129.7(2) ? C233 C2331 H2331a . . . 109.7 ? C233 C2331 H2331b . . . 109.6 ? C233 C2331 H2331c . . . 109.9 ? H2331a C2331 H2331b . . . 109.2 ? H2331a C2331 H2331c . . . 109.2 ? H2331b C2331 H2331c . . . 109.3 ? C233 C234 C235 . . . 105.5(2) ? C233 C234 H234 . . . 127.2 ? C235 C234 H234 . . . 127.3 ? N231 C235 C234 . . . 107.8(2) ? N231 C235 C2351 . . . 123.5(3) ? C234 C235 C2351 . . . 128.7(2) ? C235 C2351 H2351a . . . 109.0 ? C235 C2351 H2351b . . . 108.7 ? C235 C2351 H2351c . . . 109.7 ? H2351a C2351 H2351b . . . 109.3 ? H2351a C2351 H2351c . . . 110.8 ? H2351b C2351 H2351c . . . 109.4 ? Ag2 P2 C241 . . . 113.02(7) ? Ag2 P2 C251 . . . 114.40(7) ? Ag2 P2 C261 . . . 114.59(8) ? C241 P2 C251 . . . 104.47(12) ? C241 P2 C261 . . . 105.13(11) ? C251 P2 C261 . . . 104.14(11) ? P2 C241 C242 . . . 117.57(16) ? P2 C241 C246 . . . 123.6(2) ? C242 C241 C246 . . . 118.6(3) ? C241 C242 C243 . . . 120.5(2) ? C241 C242 H242 . . . 119.2 ? C243 C242 H242 . . . 120.3 ? C242 C243 C244 . . . 120.3(3) ? C242 C243 H243 . . . 119.8 ? C244 C243 H243 . . . 119.9 ? C243 C244 C245 . . . 119.4(3) ? C243 C244 H244 . . . 120.4 ? C245 C244 H244 . . . 120.2 ? C244 C245 C246 . . . 120.9(2) ? C244 C245 H245 . . . 120.1 ? C246 C245 H245 . . . 119.0 ? C241 C246 C245 . . . 120.3(3) ? C241 C246 H246 . . . 119.9 ? C245 C246 H246 . . . 119.8 ? P2 C251 C252 . . . 117.88(18) ? P2 C251 C256 . . . 123.35(17) ? C252 C251 C256 . . . 118.73(19) ? C251 C252 C253 . . . 120.7(2) ? C251 C252 H252 . . . 119.7 ? C253 C252 H252 . . . 119.7 ? C252 C253 C254 . . . 120.0(2) ? C252 C253 H253 . . . 120.1 ? C254 C253 H253 . . . 120.0 ? C253 C254 C255 . . . 120.2(2) ? C253 C254 H254 . . . 120.3 ? C255 C254 H254 . . . 119.5 ? C254 C255 C256 . . . 120.4(3) ? C254 C255 H255 . . . 120.0 ? C256 C255 H255 . . . 119.6 ? C251 C256 C255 . . . 120.0(2) ? C251 C256 H256 . . . 119.6 ? C255 C256 H256 . . . 120.4 ? P2 C261 C262 . . . 117.64(18) ? P2 C261 C266 . . . 123.7(2) ? C262 C261 C266 . . . 118.6(2) ? C261 C262 C263 . . . 120.7(2) ? C261 C262 H262 . . . 119.5 ? C263 C262 H262 . . . 119.9 ? C262 C263 C264 . . . 120.2(3) ? C262 C263 H263 . . . 118.9 ? C264 C263 H263 . . . 120.9 ? C263 C264 C265 . . . 119.7(3) ? C263 C264 H264 . . . 120.2 ? C265 C264 H264 . . . 120.1 ? C264 C265 C266 . . . 120.1(3) ? C264 C265 H265 . . . 119.7 ? C266 C265 H265 . . . 120.2 ? C261 C266 C265 . . . 120.7(3) ? C261 C266 H266 . . . 119.8 ? C265 C266 H266 . . . 119.5 ? N11 C11 C12 . . . 179.5(4) ? C11 C12 H12a . . . 109.7 ? C11 C12 H12b . . . 109.5 ? C11 C12 H12c . . . 110.2 ? H12a C12 H12b . . . 108.5 ? H12a C12 H12c . . . 109.3 ? H12b C12 H12c . . . 109.6 ? N21 C21 C22 . . . 176.9(3) ? C21 C22 H22a . . . 109.4 ? C21 C22 H22b . . . 109.9 ? C21 C22 H22c . . . 110.3 ? H22a C22 H22b . . . 108.6 ? H22a C22 H22c . . . 108.6 ? H22b C22 H22c . . . 110.1 ? 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 1464 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 14 _reflns_limit_k_min -25 _reflns_limit_k_max 26 _reflns_limit_l_min -24 _reflns_limit_l_max 26 _reflns_number_observed ? _reflns_d_resolution_high .734 _reflns_d_resolution_low 16.939 _diffrn_reflns_av_sigmaI/netI .039 _diffrn_reflns_theta_min 1.2 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 150(2) _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .043 _refine_ls_wR_factor_all .049 _refine_ls_goodness_of_fit_all 1.028 _refine_ls_shift/su_mean .0002 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end #===END