# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Jian-Ping Lang' _publ_contact_author_email JPLANG@SUDA.EDU.CN _publ_section_title ; Construction of [Ag2X2]-based complexes from reactions of Ag(I) salts with N-diphenylphosphanylmethyl-4-aminopyridine: isolation, structures, and luminescent properties ; loop_ _publ_author_name 'Jian-Ping Lang' 'Ni-Ya Li' 'Hong-Xi Li' 'Dong Liu' 'Zhi-Gang Ren' ; Li-Pei Wei ; 'Ruan-Xin Yuan' 'Liang Zhang' #===END #========================================================================== data_[{Ag2Cl2(dppmapy)2}.0.5MeOH.0.5CH2Cl2]n _database_code_depnum_ccdc_archive 'CCDC 748192' #TrackingRef 'JPLangCIF.cif' #========================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C36 H32 Ag2 Cl2 N4 P2), (C0.50 Cl), (C0.50 O0.50)' _chemical_formula_sum 'C37 H32 Ag2 Cl3 N4 O0.50 P2' _chemical_formula_weight 924.70 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' 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' Cl Cl 0.1484 0.1585 '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 orthorhombic _symmetry_space_group_name_H-M 'P n a 21' _symmetry_space_group_name_HALL 'P 2c -2n' 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' _cell_length_a 19.128(4) _cell_length_b 14.406(3) _cell_length_c 15.244(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4200.7(15) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 14178 _cell_measurement_theta_min 3.0219 _cell_measurement_theta_max 27.5709 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.462 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1844 _exptl_absorpt_coefficient_mu 1.230 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7325 _exptl_absorpt_correction_T_max 0.8766 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'Rigaku MercuryCCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 19395 _diffrn_reflns_av_R_equivalents 0.0979 _diffrn_reflns_av_sigmaI/netI 0.1365 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6254 _reflns_number_gt 4001 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_cell_refinement 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_data_reduction 'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material SHELXL9 _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^)+(0.0952P)^2^+21.2648P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.05(11) _refine_ls_number_reflns 6254 _refine_ls_number_parameters 297 _refine_ls_number_restraints 295 _refine_ls_R_factor_all 0.1555 _refine_ls_R_factor_gt 0.1126 _refine_ls_wR_factor_ref 0.2728 _refine_ls_wR_factor_gt 0.2467 _refine_ls_goodness_of_fit_ref 1.198 _refine_ls_restrained_S_all 1.173 _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 Ag1 Ag 0.62803(7) 0.83967(11) 0.4525(5) 0.0672(5) Uani 1 1 d . . . Ag2 Ag 0.56144(7) 0.66733(13) 0.2940(5) 0.0872(7) Uani 1 1 d . . . P1 P 0.5513(2) 0.9306(4) 0.5397(6) 0.0526(13) Uani 1 1 d . . . P2 P 0.6379(3) 0.5678(5) 0.2144(7) 0.0690(17) Uani 1 1 d . . . Cl1 Cl 0.5660(2) 0.6614(4) 0.4657(7) 0.0729(17) Uani 1 1 d . . . Cl2 Cl 0.6227(2) 0.8427(4) 0.2802(6) 0.0675(15) Uani 1 1 d . . . N1 N 0.2404(8) 0.7103(11) 0.4649(12) 0.077(5) Uani 1 1 d DU . . N2 N 0.4431(9) 0.8137(12) 0.5132(12) 0.063(5) Uani 1 1 d . . . N3 N 0.9503(7) 0.7835(12) 0.2734(13) 0.065(5) Uani 1 1 d . . . N4 N 0.7478(8) 0.6836(12) 0.2405(14) 0.072(6) Uani 1 1 d . . . C1 C 0.3761(10) 0.7818(15) 0.4946(10) 0.058(5) Uani 1 1 d DU . . C2 C 0.3187(10) 0.8404(14) 0.4905(8) 0.061(4) Uani 1 1 d DU . . H2 H 0.3240 0.9048 0.4975 0.073 Uiso 1 1 calc R . . C3 C 0.2534(11) 0.8015(14) 0.4757(9) 0.055(5) Uani 1 1 d DU . . H3 H 0.2151 0.8422 0.4729 0.066 Uiso 1 1 calc R . . C4 C 0.2961(11) 0.6573(15) 0.4692(13) 0.085(7) Uani 1 1 d DU . . H4 H 0.2894 0.5932 0.4619 0.102 Uiso 1 1 calc R . . C5 C 0.3645(12) 0.6880(16) 0.4836(12) 0.075(6) Uani 1 1 d DU . . H5 H 0.4019 0.6456 0.4857 0.090 Uiso 1 1 calc R . . C6 C 0.4555(10) 0.9114(13) 0.5135(17) 0.067(6) Uani 1 1 d U . . H6A H 0.4262 0.9416 0.5577 0.081 Uiso 1 1 calc R . . H6B H 0.4443 0.9378 0.4560 0.081 Uiso 1 1 calc R . . C7 C 0.5595(11) 0.912(2) 0.6574(19) 0.086(3) Uani 1 1 d U . . C8 C 0.6154(12) 0.8581(19) 0.6860(18) 0.086(3) Uani 1 1 d U . . H8 H 0.6460 0.8318 0.6447 0.103 Uiso 1 1 calc R . . C9 C 0.6260(11) 0.8425(17) 0.7740(17) 0.086(3) Uani 1 1 d U . . H9 H 0.6644 0.8075 0.7936 0.103 Uiso 1 1 calc R . . C10 C 0.5783(12) 0.8800(17) 0.8335(17) 0.086(3) Uani 1 1 d U . . H10 H 0.5873 0.8747 0.8939 0.103 Uiso 1 1 calc R . . C11 C 0.5222(11) 0.9218(17) 0.8077(18) 0.086(3) Uani 1 1 d U . . H11 H 0.4879 0.9388 0.8488 0.103 Uiso 1 1 calc R . . C12 C 0.5125(12) 0.9419(18) 0.7190(18) 0.086(3) Uani 1 1 d U . . H12 H 0.4731 0.9762 0.7014 0.103 Uiso 1 1 calc R . . C13 C 0.5594(11) 1.0576(16) 0.5286(12) 0.084(3) Uani 1 1 d DU . . C14 C 0.6171(12) 1.0966(15) 0.5020(11) 0.084(3) Uani 1 1 d DU . . H14 H 0.6540 1.0583 0.4833 0.101 Uiso 1 1 calc R . . C15 C 0.6265(12) 1.1902(15) 0.4999(12) 0.084(3) Uani 1 1 d DU . . H15 H 0.6686 1.2169 0.4804 0.101 Uiso 1 1 calc R . . C16 C 0.5681(11) 1.2467(16) 0.5293(13) 0.084(3) Uani 1 1 d DU . . H16 H 0.5729 1.3116 0.5289 0.101 Uiso 1 1 calc R . . C17 C 0.5100(12) 1.2113(15) 0.5561(14) 0.084(3) Uani 1 1 d DU . . H17 H 0.4730 1.2494 0.5747 0.101 Uiso 1 1 calc R . . C18 C 0.5038(12) 1.1164(15) 0.5566(14) 0.084(3) Uani 1 1 d DU . . H18 H 0.4618 1.0895 0.5761 0.101 Uiso 1 1 calc R . . C19 C 0.8129(10) 0.7136(15) 0.2502(17) 0.071(3) Uani 1 1 d U . . C20 C 0.8735(9) 0.6576(15) 0.2654(16) 0.071(3) Uani 1 1 d U . . H20 H 0.8671 0.5932 0.2705 0.085 Uiso 1 1 calc R . . C21 C 0.9387(10) 0.6908(16) 0.2730(18) 0.071(3) Uani 1 1 d U . . H21 H 0.9766 0.6495 0.2780 0.085 Uiso 1 1 calc R . . C22 C 0.8934(9) 0.8404(15) 0.2660(16) 0.071(3) Uani 1 1 d U . . H22 H 0.9017 0.9046 0.2679 0.085 Uiso 1 1 calc R . . C23 C 0.8274(11) 0.8135(15) 0.2565(19) 0.088(9) Uani 1 1 d U . . H23 H 0.7910 0.8573 0.2538 0.106 Uiso 1 1 calc R . . C24 C 0.7318(8) 0.5868(13) 0.2385(16) 0.066(6) Uani 1 1 d U . . H24A H 0.7434 0.5589 0.2953 0.079 Uiso 1 1 calc R . . H24B H 0.7603 0.5563 0.1934 0.079 Uiso 1 1 calc R . . C25 C 0.6301(14) 0.448(2) 0.2316(18) 0.123(5) Uani 1 1 d DU . . C26 C 0.5750(13) 0.4096(18) 0.2777(16) 0.123(5) Uani 1 1 d DU . . H26 H 0.5413 0.4502 0.3008 0.148 Uiso 1 1 calc R . . C27 C 0.5661(13) 0.3178(18) 0.2920(19) 0.123(5) Uani 1 1 d DU . . H27 H 0.5273 0.2967 0.3240 0.148 Uiso 1 1 calc R . . C28 C 0.6137(12) 0.2558(19) 0.2599(19) 0.123(5) Uani 1 1 d DU . . H28 H 0.6069 0.1921 0.2703 0.148 Uiso 1 1 calc R . . C29 C 0.6712(14) 0.2840(19) 0.2126(19) 0.123(5) Uani 1 1 d DU . . H29 H 0.7042 0.2418 0.1902 0.148 Uiso 1 1 calc R . . C30 C 0.6773(15) 0.382(2) 0.2002(19) 0.123(5) Uani 1 1 d DU . . H30 H 0.7161 0.4034 0.1683 0.148 Uiso 1 1 calc R . . C31 C 0.6309(10) 0.5787(15) 0.0992(19) 0.101(3) Uani 1 1 d DU . . C32 C 0.5689(11) 0.5475(14) 0.0572(16) 0.101(3) Uani 1 1 d DU . . H32 H 0.5345 0.5177 0.0910 0.122 Uiso 1 1 calc R . . C33 C 0.5573(11) 0.5595(14) -0.0311(15) 0.101(3) Uani 1 1 d DU . . H33 H 0.5155 0.5377 -0.0561 0.122 Uiso 1 1 calc R . . C34 C 0.6066(9) 0.6032(14) -0.0842(18) 0.101(3) Uani 1 1 d DU . . H34 H 0.5978 0.6108 -0.1445 0.122 Uiso 1 1 calc R . . C35 C 0.6686(10) 0.6357(14) -0.0481(17) 0.101(3) Uani 1 1 d DU . . H35 H 0.7026 0.6655 -0.0827 0.122 Uiso 1 1 calc R . . C36 C 0.6786(13) 0.6222(14) 0.0425(16) 0.101(3) Uani 1 1 d DU . . H36 H 0.7205 0.6441 0.0671 0.122 Uiso 1 1 calc R . . C38 C 0.725(3) 0.869(4) 0.998(4) 0.14(2) Uiso 0.50 1 d PD . . Cl4 Cl 0.677(3) 0.924(3) 1.080(3) 0.31(2) Uiso 0.50 1 d PD . . Cl3 Cl 0.791(3) 0.937(4) 0.951(5) 0.44(3) Uiso 0.50 1 d PD . . O1 O 0.603(2) 0.559(3) 0.647(3) 0.130(14) Uiso 0.50 1 d PD . . C37 C 0.674(3) 0.575(6) 0.671(5) 0.15(3) Uiso 0.50 1 d PD . . 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 0.0369(7) 0.0762(9) 0.0886(11) -0.0080(13) 0.0031(8) 0.0059(7) Ag2 0.0354(7) 0.0919(12) 0.1342(18) -0.0300(16) 0.0019(9) 0.0103(8) P1 0.032(2) 0.056(3) 0.070(4) -0.001(3) -0.006(2) -0.003(2) P2 0.032(2) 0.078(4) 0.098(5) -0.011(4) 0.005(3) -0.004(3) Cl1 0.040(2) 0.071(3) 0.108(5) 0.013(4) 0.002(3) 0.002(2) Cl2 0.038(2) 0.074(3) 0.090(4) -0.017(4) -0.003(2) 0.001(2) N1 0.043(7) 0.065(7) 0.123(14) 0.002(11) 0.007(10) -0.005(6) N2 0.061(11) 0.074(11) 0.054(11) -0.005(9) -0.020(8) -0.023(9) N3 0.031(7) 0.075(11) 0.090(14) -0.011(11) -0.009(8) 0.005(7) N4 0.024(7) 0.069(11) 0.121(16) -0.020(11) -0.003(9) 0.008(8) C1 0.046(8) 0.080(9) 0.048(11) -0.019(10) -0.013(8) -0.001(7) C2 0.056(8) 0.065(9) 0.061(11) -0.022(10) -0.007(8) 0.002(6) C3 0.053(8) 0.062(7) 0.051(12) -0.005(9) -0.006(8) -0.001(7) C4 0.051(8) 0.061(9) 0.144(19) -0.021(13) -0.002(12) 0.001(6) C5 0.050(8) 0.076(9) 0.099(17) -0.017(12) -0.021(11) 0.009(9) C6 0.037(10) 0.060(12) 0.106(18) -0.001(12) -0.010(10) -0.003(9) C7 0.059(5) 0.109(8) 0.089(7) 0.011(7) -0.009(5) -0.006(5) C8 0.059(5) 0.109(8) 0.089(7) 0.011(7) -0.009(5) -0.006(5) C9 0.059(5) 0.109(8) 0.089(7) 0.011(7) -0.009(5) -0.006(5) C10 0.059(5) 0.109(8) 0.089(7) 0.011(7) -0.009(5) -0.006(5) C11 0.059(5) 0.109(8) 0.089(7) 0.011(7) -0.009(5) -0.006(5) C12 0.059(5) 0.109(8) 0.089(7) 0.011(7) -0.009(5) -0.006(5) C13 0.063(5) 0.065(5) 0.125(8) 0.001(6) -0.004(5) -0.010(4) C14 0.063(5) 0.065(5) 0.125(8) 0.001(6) -0.004(5) -0.010(4) C15 0.063(5) 0.065(5) 0.125(8) 0.001(6) -0.004(5) -0.010(4) C16 0.063(5) 0.065(5) 0.125(8) 0.001(6) -0.004(5) -0.010(4) C17 0.063(5) 0.065(5) 0.125(8) 0.001(6) -0.004(5) -0.010(4) C18 0.063(5) 0.065(5) 0.125(8) 0.001(6) -0.004(5) -0.010(4) C19 0.035(5) 0.075(6) 0.102(9) -0.022(7) -0.004(5) 0.004(5) C20 0.035(5) 0.075(6) 0.102(9) -0.022(7) -0.004(5) 0.004(5) C21 0.035(5) 0.075(6) 0.102(9) -0.022(7) -0.004(5) 0.004(5) C22 0.035(5) 0.075(6) 0.102(9) -0.022(7) -0.004(5) 0.004(5) C23 0.037(9) 0.061(12) 0.17(3) 0.054(15) 0.016(13) 0.012(9) C24 0.013(7) 0.068(12) 0.117(18) 0.007(12) 0.001(9) -0.004(8) C25 0.081(7) 0.086(7) 0.202(13) 0.038(9) 0.028(8) -0.018(5) C26 0.081(7) 0.086(7) 0.202(13) 0.038(9) 0.028(8) -0.018(5) C27 0.081(7) 0.086(7) 0.202(13) 0.038(9) 0.028(8) -0.018(5) C28 0.081(7) 0.086(7) 0.202(13) 0.038(9) 0.028(8) -0.018(5) C29 0.081(7) 0.086(7) 0.202(13) 0.038(9) 0.028(8) -0.018(5) C30 0.081(7) 0.086(7) 0.202(13) 0.038(9) 0.028(8) -0.018(5) C31 0.077(6) 0.126(8) 0.102(8) -0.016(8) -0.008(6) -0.025(6) C32 0.077(6) 0.126(8) 0.102(8) -0.016(8) -0.008(6) -0.025(6) C33 0.077(6) 0.126(8) 0.102(8) -0.016(8) -0.008(6) -0.025(6) C34 0.077(6) 0.126(8) 0.102(8) -0.016(8) -0.008(6) -0.025(6) C35 0.077(6) 0.126(8) 0.102(8) -0.016(8) -0.008(6) -0.025(6) C36 0.077(6) 0.126(8) 0.102(8) -0.016(8) -0.008(6) -0.025(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.274(15) 3_565 ? Ag1 P1 2.374(6) . ? Ag1 Cl2 2.629(7) . ? Ag1 Cl1 2.836(6) . ? Ag2 N3 2.262(14) 3_465 ? Ag2 P2 2.380(6) . ? Ag2 Cl1 2.620(8) . ? Ag2 Cl2 2.793(6) . ? P1 C7 1.82(3) . ? P1 C13 1.84(2) . ? P1 C6 1.895(19) . ? P2 C25 1.75(3) . ? P2 C31 1.77(3) . ? P2 C24 1.853(16) . ? N1 C4 1.31(2) . ? N1 C3 1.35(2) . ? N1 Ag1 2.274(15) 3_465 ? N2 C1 1.39(2) . ? N2 C6 1.43(2) . ? N3 C21 1.35(3) . ? N3 C22 1.37(2) . ? N3 Ag2 2.262(14) 3_565 ? N4 C19 1.33(2) . ? N4 C24 1.43(2) . ? C1 C5 1.38(3) . ? C1 C2 1.38(3) . ? C2 C3 1.39(3) . ? C2 H2 0.9400 . ? C3 H3 0.9400 . ? C4 C5 1.40(3) . ? C4 H4 0.9400 . ? C5 H5 0.9400 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 C12 1.37(3) . ? C7 C8 1.40(3) . ? C8 C9 1.38(3) . ? C8 H8 0.9400 . ? C9 C10 1.39(3) . ? C9 H9 0.9400 . ? C10 C11 1.29(3) . ? C10 H10 0.9400 . ? C11 C12 1.39(3) . ? C11 H11 0.9400 . ? C12 H12 0.9400 . ? C13 C14 1.30(3) . ? C13 C18 1.42(3) . ? C14 C15 1.36(3) . ? C14 H14 0.9400 . ? C15 C16 1.45(3) . ? C15 H15 0.9400 . ? C16 C17 1.29(3) . ? C16 H16 0.9400 . ? C17 C18 1.37(3) . ? C17 H17 0.9400 . ? C18 H18 0.9400 . ? C19 C20 1.43(3) . ? C19 C23 1.47(3) . ? C20 C21 1.34(3) . ? C20 H20 0.9400 . ? C21 H21 0.9400 . ? C22 C23 1.33(3) . ? C22 H22 0.9400 . ? C23 H23 0.9400 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C25 C26 1.38(3) . ? C25 C30 1.40(4) . ? C26 C27 1.35(3) . ? C26 H26 0.9400 . ? C27 C28 1.37(3) . ? C27 H27 0.9400 . ? C28 C29 1.38(3) . ? C28 H28 0.9400 . ? C29 C30 1.43(4) . ? C29 H29 0.9400 . ? C30 H30 0.9400 . ? C31 C36 1.405(17) . ? C31 C32 1.420(16) . ? C32 C33 1.374(16) . ? C32 H32 0.9400 . ? C33 C34 1.392(16) . ? C33 H33 0.9400 . ? C34 C35 1.390(16) . ? C34 H34 0.9400 . ? C35 C36 1.407(17) . ? C35 H35 0.9400 . ? C36 H36 0.9400 . ? C38 Cl4 1.745(19) . ? C38 Cl3 1.76(2) . ? O1 C37 1.40(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 P1 135.4(4) 3_565 . ? N1 Ag1 Cl2 97.2(4) 3_565 . ? P1 Ag1 Cl2 121.72(18) . . ? N1 Ag1 Cl1 95.9(4) 3_565 . ? P1 Ag1 Cl1 101.63(17) . . ? Cl2 Ag1 Cl1 94.0(2) . . ? N3 Ag2 P2 134.0(5) 3_465 . ? N3 Ag2 Cl1 100.4(5) 3_465 . ? P2 Ag2 Cl1 117.9(2) . . ? N3 Ag2 Cl2 95.7(4) 3_465 . ? P2 Ag2 Cl2 104.39(19) . . ? Cl1 Ag2 Cl2 95.21(19) . . ? C7 P1 C13 103.1(11) . . ? C7 P1 C6 105.6(11) . . ? C13 P1 C6 101.9(9) . . ? C7 P1 Ag1 114.8(9) . . ? C13 P1 Ag1 116.4(8) . . ? C6 P1 Ag1 113.5(7) . . ? C25 P2 C31 103.2(12) . . ? C25 P2 C24 101.4(11) . . ? C31 P2 C24 104.9(10) . . ? C25 P2 Ag2 117.7(11) . . ? C31 P2 Ag2 114.0(7) . . ? C24 P2 Ag2 114.0(7) . . ? Ag2 Cl1 Ag1 85.05(19) . . ? Ag1 Cl2 Ag2 85.74(19) . . ? C4 N1 C3 114.2(18) . . ? C4 N1 Ag1 126.0(14) . 3_465 ? C3 N1 Ag1 119.6(13) . 3_465 ? C1 N2 C6 118.7(18) . . ? C21 N3 C22 117.4(17) . . ? C21 N3 Ag2 117.6(12) . 3_565 ? C22 N3 Ag2 124.9(13) . 3_565 ? C19 N4 C24 121.4(16) . . ? C5 C1 C2 118(2) . . ? C5 C1 N2 120(2) . . ? C2 C1 N2 123(2) . . ? C1 C2 C3 118(2) . . ? C1 C2 H2 120.8 . . ? C3 C2 H2 120.8 . . ? N1 C3 C2 125(2) . . ? N1 C3 H3 117.3 . . ? C2 C3 H3 117.3 . . ? N1 C4 C5 126(2) . . ? N1 C4 H4 117.1 . . ? C5 C4 H4 117.1 . . ? C1 C5 C4 119(2) . . ? C1 C5 H5 120.7 . . ? C4 C5 H5 120.7 . . ? N2 C6 P1 107.8(13) . . ? N2 C6 H6A 110.1 . . ? P1 C6 H6A 110.1 . . ? N2 C6 H6B 110.1 . . ? P1 C6 H6B 110.1 . . ? H6A C6 H6B 108.5 . . ? C12 C7 C8 118(3) . . ? C12 C7 P1 125.2(19) . . ? C8 C7 P1 117(2) . . ? C9 C8 C7 121(3) . . ? C9 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? C8 C9 C10 118(2) . . ? C8 C9 H9 120.8 . . ? C10 C9 H9 120.8 . . ? C11 C10 C9 122(3) . . ? C11 C10 H10 119.1 . . ? C9 C10 H10 119.1 . . ? C10 C11 C12 120(3) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C7 C12 C11 121(2) . . ? C7 C12 H12 119.5 . . ? C11 C12 H12 119.5 . . ? C14 C13 C18 118(2) . . ? C14 C13 P1 121.9(19) . . ? C18 C13 P1 120.0(17) . . ? C13 C14 C15 123(2) . . ? C13 C14 H14 118.4 . . ? C15 C14 H14 118.4 . . ? C14 C15 C16 116(2) . . ? C14 C15 H15 121.8 . . ? C16 C15 H15 121.8 . . ? C17 C16 C15 123(2) . . ? C17 C16 H16 118.7 . . ? C15 C16 H16 118.7 . . ? C16 C17 C18 118(2) . . ? C16 C17 H17 121.0 . . ? C18 C17 H17 121.0 . . ? C17 C18 C13 122(2) . . ? C17 C18 H18 119.1 . . ? C13 C18 H18 119.1 . . ? N4 C19 C20 126(2) . . ? N4 C19 C23 120.3(19) . . ? C20 C19 C23 112.8(18) . . ? C21 C20 C19 125(2) . . ? C21 C20 H20 117.7 . . ? C19 C20 H20 117.7 . . ? C20 C21 N3 120.3(19) . . ? C20 C21 H21 119.9 . . ? N3 C21 H21 119.9 . . ? C23 C22 N3 126(2) . . ? C23 C22 H22 116.9 . . ? N3 C22 H22 116.9 . . ? C22 C23 C19 118(2) . . ? C22 C23 H23 120.9 . . ? C19 C23 H23 120.9 . . ? N4 C24 P2 110.8(12) . . ? N4 C24 H24A 109.5 . . ? P2 C24 H24A 109.5 . . ? N4 C24 H24B 109.5 . . ? P2 C24 H24B 109.5 . . ? H24A C24 H24B 108.1 . . ? C26 C25 C30 113(3) . . ? C26 C25 P2 123(2) . . ? C30 C25 P2 125(2) . . ? C27 C26 C25 125(3) . . ? C27 C26 H26 117.5 . . ? C25 C26 H26 117.5 . . ? C26 C27 C28 120(3) . . ? C26 C27 H27 120.1 . . ? C28 C27 H27 120.1 . . ? C27 C28 C29 122(3) . . ? C27 C28 H28 119.1 . . ? C29 C28 H28 119.1 . . ? C28 C29 C30 115(3) . . ? C28 C29 H29 122.4 . . ? C30 C29 H29 122.4 . . ? C25 C30 C29 125(3) . . ? C25 C30 H30 117.4 . . ? C29 C30 H30 117.4 . . ? C36 C31 C32 114(2) . . ? C36 C31 P2 126.9(16) . . ? C32 C31 P2 119.0(17) . . ? C33 C32 C31 122(2) . . ? C33 C32 H32 118.8 . . ? C31 C32 H32 118.8 . . ? C32 C33 C34 121(2) . . ? C32 C33 H33 119.4 . . ? C34 C33 H33 119.4 . . ? C35 C34 C33 120(2) . . ? C35 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? C34 C35 C36 117(2) . . ? C34 C35 H35 121.4 . . ? C36 C35 H35 121.4 . . ? C31 C36 C35 125(2) . . ? C31 C36 H36 117.4 . . ? C35 C36 H36 117.4 . . ? Cl4 C38 Cl3 114(4) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.363 _refine_diff_density_min -0.750 _refine_diff_density_rms 0.180 #===END #========================================================================== data_[{Ag2Br2(dppmapy)2}.2CHCl3]n _database_code_depnum_ccdc_archive 'CCDC 748193' #TrackingRef 'JPLangCIF.cif' #========================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H17 Ag Br N2 P, C H Cl3' _chemical_formula_sum 'C19 H18 Ag Br Cl3 N2 P' _chemical_formula_weight 599.44 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' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 'P 21/c ' _symmetry_space_group_name_Hall '-P 2ybc' 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 14.061(3) _cell_length_b 19.031(4) _cell_length_c 8.7505(18) _cell_angle_alpha 90.00 _cell_angle_beta 105.85(3) _cell_angle_gamma 90.00 _cell_volume 2252.6(9) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 10284 _cell_measurement_theta_min 3.0120 _cell_measurement_theta_max 27.5126 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.768 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1176 _exptl_absorpt_coefficient_mu 3.103 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3357 _exptl_absorpt_correction_T_max 0.5758 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'Rigaku MercuryCCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 12666 _diffrn_reflns_av_R_equivalents 0.0377 _diffrn_reflns_av_sigmaI/netI 0.0683 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.49 _reflns_number_total 5091 _reflns_number_gt 3708 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_cell_refinement 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_data_reduction 'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material SHELXL9 _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^)+(0.0687P)^2^+11.6940P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5091 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0758 _refine_ls_R_factor_gt 0.0616 _refine_ls_wR_factor_ref 0.1847 _refine_ls_wR_factor_gt 0.1782 _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_restrained_S_all 1.104 _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 0.42245(5) 1.00593(3) 0.78838(7) 0.0399(2) Uani 1 1 d . . . Br1 Br 0.39891(6) 1.06493(4) 1.06904(10) 0.0405(2) Uani 1 1 d . . . P1 P 0.30124(14) 0.92457(9) 0.6482(2) 0.0320(4) Uani 1 1 d . . . N1 N 0.5080(5) 0.6072(3) 0.7671(8) 0.0416(16) Uani 1 1 d . . . C1 C 0.5344(6) 0.7283(4) 0.8452(9) 0.0392(18) Uani 1 1 d . . . H1 H 0.5710 0.7613 0.9178 0.047 Uiso 1 1 calc R . . Cl1 Cl 0.1698(4) 0.3694(2) 0.1121(5) 0.1167(15) Uani 1 1 d . . . N2 N 0.4325(5) 0.8203(3) 0.6996(8) 0.0430(16) Uani 1 1 d . . . H2 H 0.4656 0.8485 0.7732 0.052 Uiso 1 1 calc R . . C2 C 0.5587(6) 0.6589(4) 0.8615(9) 0.0413(18) Uani 1 1 d . . . H2A H 0.6143 0.6460 0.9439 0.050 Uiso 1 1 calc R . . Cl2 Cl 0.1099(3) 0.3408(3) 0.3920(4) 0.1067(12) Uani 1 1 d . . . C3 C 0.4312(6) 0.6287(4) 0.6503(10) 0.043(2) Uani 1 1 d . . . H3 H 0.3945 0.5943 0.5823 0.052 Uiso 1 1 calc R . . Cl3 Cl 0.2305(3) 0.24179(18) 0.2806(4) 0.1023(12) Uani 1 1 d . . . C4 C 0.4013(6) 0.6979(4) 0.6213(9) 0.0384(17) Uani 1 1 d . . . H4 H 0.3460 0.7093 0.5368 0.046 Uiso 1 1 calc R . . C5 C 0.4546(5) 0.7506(4) 0.7196(9) 0.0346(16) Uani 1 1 d . . . C6 C 0.3602(6) 0.8518(4) 0.5688(9) 0.0372(16) Uani 1 1 d . . . H6A H 0.3104 0.8169 0.5173 0.045 Uiso 1 1 calc R . . H6B H 0.3920 0.8696 0.4899 0.045 Uiso 1 1 calc R . . C7 C 0.2232(5) 0.8805(4) 0.7556(9) 0.0348(16) Uani 1 1 d . . . C8 C 0.1859(8) 0.8137(5) 0.7169(11) 0.059(3) Uani 1 1 d . . . H8 H 0.2016 0.7888 0.6343 0.071 Uiso 1 1 calc R . . C9 C 0.1249(8) 0.7834(5) 0.8008(12) 0.066(3) Uani 1 1 d . . . H9 H 0.0992 0.7381 0.7734 0.079 Uiso 1 1 calc R . . C10 C 0.1020(7) 0.8188(5) 0.9228(11) 0.052(2) Uani 1 1 d . . . H10 H 0.0593 0.7989 0.9769 0.063 Uiso 1 1 calc R . . C11 C 0.1431(6) 0.8847(5) 0.9644(10) 0.051(2) Uani 1 1 d . . . H11 H 0.1300 0.9085 1.0506 0.061 Uiso 1 1 calc R . . C12 C 0.2029(6) 0.9165(4) 0.8822(10) 0.0400(17) Uani 1 1 d . . . H12 H 0.2293 0.9614 0.9111 0.048 Uiso 1 1 calc R . . C13 C 0.2151(5) 0.9615(3) 0.4716(9) 0.0322(15) Uani 1 1 d . . . C14 C 0.1123(6) 0.9535(5) 0.4360(10) 0.0434(18) Uani 1 1 d . . . H14 H 0.0842 0.9245 0.4989 0.052 Uiso 1 1 calc R . . C15 C 0.0527(7) 0.9891(6) 0.3070(11) 0.056(2) Uani 1 1 d . . . H15 H -0.0163 0.9838 0.2839 0.067 Uiso 1 1 calc R . . C16 C 0.0900(7) 1.0308(6) 0.2138(10) 0.056(2) Uani 1 1 d . . . H16 H 0.0475 1.0549 0.1282 0.067 Uiso 1 1 calc R . . C17 C 0.1936(7) 1.0383(5) 0.2453(10) 0.051(2) Uani 1 1 d . . . H17 H 0.2205 1.0667 0.1797 0.061 Uiso 1 1 calc R . . C18 C 0.2554(6) 1.0032(4) 0.3740(10) 0.0442(19) Uani 1 1 d . . . H18 H 0.3244 1.0076 0.3952 0.053 Uiso 1 1 calc R . . C19 C 0.2021(8) 0.3294(6) 0.2951(13) 0.066(3) Uani 1 1 d . . . H19 H 0.2625 0.3530 0.3599 0.079 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0394(3) 0.0268(3) 0.0486(4) -0.0008(2) 0.0039(3) -0.0079(2) Br1 0.0368(4) 0.0331(4) 0.0482(5) -0.0040(3) 0.0057(3) 0.0002(3) P1 0.0328(9) 0.0232(8) 0.0383(10) -0.0009(7) 0.0071(8) -0.0023(7) N1 0.042(4) 0.026(3) 0.050(4) -0.010(3) 0.002(3) 0.006(3) C1 0.038(4) 0.029(4) 0.045(4) -0.009(3) 0.001(3) 0.002(3) Cl1 0.151(4) 0.109(3) 0.114(3) 0.057(2) 0.076(3) 0.045(3) N2 0.043(4) 0.022(3) 0.052(4) -0.005(3) -0.007(3) -0.001(3) C2 0.041(4) 0.035(4) 0.041(4) -0.003(3) 0.000(3) 0.011(3) Cl2 0.105(3) 0.144(4) 0.081(2) -0.002(2) 0.043(2) 0.007(2) C3 0.040(4) 0.024(4) 0.057(5) -0.011(3) -0.003(4) 0.004(3) Cl3 0.143(3) 0.0639(18) 0.095(2) 0.0073(16) 0.024(2) 0.010(2) C4 0.038(4) 0.028(4) 0.043(4) -0.006(3) -0.001(3) 0.009(3) C5 0.036(4) 0.028(3) 0.041(4) -0.007(3) 0.011(3) -0.001(3) C6 0.039(4) 0.030(4) 0.041(4) 0.000(3) 0.009(3) 0.004(3) C7 0.031(4) 0.030(4) 0.040(4) -0.001(3) 0.005(3) -0.003(3) C8 0.082(7) 0.049(5) 0.053(5) -0.015(4) 0.031(5) -0.029(5) C9 0.084(7) 0.054(6) 0.061(6) 0.001(5) 0.021(5) -0.033(5) C10 0.045(5) 0.066(6) 0.046(5) 0.013(4) 0.014(4) -0.005(4) C11 0.044(5) 0.068(6) 0.043(5) 0.002(4) 0.017(4) 0.010(4) C12 0.034(4) 0.039(4) 0.045(4) -0.002(3) 0.008(3) 0.005(3) C13 0.037(4) 0.019(3) 0.039(4) -0.003(3) 0.006(3) 0.003(3) C14 0.035(4) 0.048(5) 0.046(5) 0.002(4) 0.010(3) -0.002(4) C15 0.033(4) 0.080(7) 0.050(5) 0.001(5) 0.005(4) 0.006(4) C16 0.046(5) 0.078(7) 0.042(5) 0.014(5) 0.009(4) 0.027(5) C17 0.050(5) 0.057(5) 0.047(5) 0.013(4) 0.015(4) 0.011(4) C18 0.039(4) 0.051(5) 0.042(5) 0.004(4) 0.011(4) 0.000(4) C19 0.066(6) 0.059(6) 0.072(7) -0.005(5) 0.020(5) -0.015(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 Ag1 N1 2.272(6) 2_656 ? Ag1 P1 2.380(2) . ? Ag1 Br1 2.8010(12) . ? Ag1 Br1 2.8236(12) 3_677 ? Br1 Ag1 2.8236(12) 3_677 ? P1 C13 1.824(7) . ? P1 C7 1.831(8) . ? P1 C6 1.845(8) . ? N1 C3 1.333(10) . ? N1 C2 1.356(10) . ? N1 Ag1 2.272(6) 2_646 ? C1 C2 1.361(10) . ? C1 C5 1.405(10) . ? C1 H1 0.9400 . ? Cl1 C19 1.718(12) . ? N2 C5 1.363(9) . ? N2 C6 1.438(9) . ? N2 H2 0.8700 . ? C2 H2A 0.9400 . ? Cl2 C19 1.746(12) . ? C3 C4 1.384(10) . ? C3 H3 0.9400 . ? Cl3 C19 1.727(11) . ? C4 C5 1.397(10) . ? C4 H4 0.9400 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 C8 1.381(11) . ? C7 C12 1.396(11) . ? C8 C9 1.397(13) . ? C8 H8 0.9400 . ? C9 C10 1.373(14) . ? C9 H9 0.9400 . ? C10 C11 1.387(14) . ? C10 H10 0.9400 . ? C11 C12 1.386(12) . ? C11 H11 0.9400 . ? C12 H12 0.9400 . ? C13 C18 1.395(11) . ? C13 C14 1.402(11) . ? C14 C15 1.385(12) . ? C14 H14 0.9400 . ? C15 C16 1.344(14) . ? C15 H15 0.9400 . ? C16 C17 1.413(13) . ? C16 H16 0.9400 . ? C17 C18 1.391(12) . ? C17 H17 0.9400 . ? C18 H18 0.9400 . ? C19 H19 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 P1 136.96(17) 2_656 . ? N1 Ag1 Br1 90.46(19) 2_656 . ? P1 Ag1 Br1 118.24(6) . . ? N1 Ag1 Br1 96.71(17) 2_656 3_677 ? P1 Ag1 Br1 110.02(5) . 3_677 ? Br1 Ag1 Br1 96.19(4) . 3_677 ? Ag1 Br1 Ag1 83.81(4) . 3_677 ? C13 P1 C7 105.0(3) . . ? C13 P1 C6 103.4(3) . . ? C7 P1 C6 104.1(4) . . ? C13 P1 Ag1 113.7(2) . . ? C7 P1 Ag1 118.6(2) . . ? C6 P1 Ag1 110.5(3) . . ? C3 N1 C2 115.1(6) . . ? C3 N1 Ag1 113.8(5) . 2_646 ? C2 N1 Ag1 124.2(5) . 2_646 ? C2 C1 C5 119.9(7) . . ? C2 C1 H1 120.1 . . ? C5 C1 H1 120.1 . . ? C5 N2 C6 126.5(6) . . ? C5 N2 H2 116.8 . . ? C6 N2 H2 116.8 . . ? N1 C2 C1 124.5(7) . . ? N1 C2 H2A 117.8 . . ? C1 C2 H2A 117.8 . . ? N1 C3 C4 125.1(7) . . ? N1 C3 H3 117.4 . . ? C4 C3 H3 117.4 . . ? C3 C4 C5 119.0(7) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? N2 C5 C4 123.6(7) . . ? N2 C5 C1 119.9(7) . . ? C4 C5 C1 116.4(7) . . ? N2 C6 P1 107.8(5) . . ? N2 C6 H6A 110.1 . . ? P1 C6 H6A 110.1 . . ? N2 C6 H6B 110.1 . . ? P1 C6 H6B 110.1 . . ? H6A C6 H6B 108.5 . . ? C8 C7 C12 120.0(8) . . ? C8 C7 P1 122.4(6) . . ? C12 C7 P1 117.6(6) . . ? C7 C8 C9 119.8(9) . . ? C7 C8 H8 120.1 . . ? C9 C8 H8 120.1 . . ? C10 C9 C8 120.9(9) . . ? C10 C9 H9 119.5 . . ? C8 C9 H9 119.5 . . ? C9 C10 C11 118.6(8) . . ? C9 C10 H10 120.7 . . ? C11 C10 H10 120.7 . . ? C12 C11 C10 121.7(8) . . ? C12 C11 H11 119.1 . . ? C10 C11 H11 119.1 . . ? C11 C12 C7 118.9(8) . . ? C11 C12 H12 120.6 . . ? C7 C12 H12 120.6 . . ? C18 C13 C14 119.5(7) . . ? C18 C13 P1 116.8(6) . . ? C14 C13 P1 123.5(6) . . ? C15 C14 C13 119.1(8) . . ? C15 C14 H14 120.5 . . ? C13 C14 H14 120.5 . . ? C16 C15 C14 122.3(9) . . ? C16 C15 H15 118.9 . . ? C14 C15 H15 118.9 . . ? C15 C16 C17 119.5(8) . . ? C15 C16 H16 120.2 . . ? C17 C16 H16 120.2 . . ? C18 C17 C16 119.5(9) . . ? C18 C17 H17 120.2 . . ? C16 C17 H17 120.2 . . ? C17 C18 C13 120.0(8) . . ? C17 C18 H18 120.0 . . ? C13 C18 H18 120.0 . . ? Cl1 C19 Cl3 111.5(6) . . ? Cl1 C19 Cl2 110.8(7) . . ? Cl3 C19 Cl2 111.9(6) . . ? Cl1 C19 H19 107.5 . . ? Cl3 C19 H19 107.5 . . ? Cl2 C19 H19 107.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C19 H19 Br1 0.99 2.75 3.718(11) 166.5 4_575 _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.833 _refine_diff_density_min -0.716 _refine_diff_density_rms 0.150 #===END #========================================================================== data_[Ag2I2(dppmapy)4].3MeOH _database_code_depnum_ccdc_archive 'CCDC 748194' #TrackingRef 'JPLangCIF.cif' #========================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C72 H68 Ag2 I2 N8 P4, C2 O2, C O' _chemical_formula_sum 'C75 H68 Ag2 I2 N8 O3 P4' _chemical_formula_weight 1722.79 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' 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.941(2) _cell_length_b 12.106(2) _cell_length_c 14.236(3) _cell_angle_alpha 101.13(3) _cell_angle_beta 93.39(3) _cell_angle_gamma 105.72(3) _cell_volume 1930.1(7) _cell_formula_units_Z 1 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 7329 _cell_measurement_theta_min 3.0898 _cell_measurement_theta_max 27.5476 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.482 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 858 _exptl_absorpt_coefficient_mu 1.439 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7148 _exptl_absorpt_correction_T_max 0.8694 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.' _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 'Rigaku MercuryCCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 18700 _diffrn_reflns_av_R_equivalents 0.0608 _diffrn_reflns_av_sigmaI/netI 0.0886 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 27.48 _reflns_number_total 8709 _reflns_number_gt 6288 _reflns_threshold_expression >2sigma(I) __computing_data_collection 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_cell_refinement 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_data_reduction 'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material SHELXL97 _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^)+(0.0813P)^2^+0.9375P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8709 _refine_ls_number_parameters 421 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1140 _refine_ls_R_factor_gt 0.0813 _refine_ls_wR_factor_ref 0.2092 _refine_ls_wR_factor_gt 0.1872 _refine_ls_goodness_of_fit_ref 1.132 _refine_ls_restrained_S_all 1.132 _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 I1 I 0.09192(4) 0.38388(4) 0.04080(4) 0.05071(19) Uani 1 1 d . . . Ag1 Ag 0.15335(5) 0.61808(5) -0.00107(5) 0.0493(2) Uani 1 1 d . . . P1 P 0.26921(16) 0.77844(17) 0.13202(16) 0.0433(5) Uani 1 1 d . . . N1 N 0.2053(10) 0.5191(9) 0.5191(7) 0.091(3) Uani 1 1 d . . . C1 C 0.2432(12) 0.6326(10) 0.5170(9) 0.090(3) Uani 1 1 d . . . H1 H 0.2653 0.6874 0.5772 0.108 Uiso 1 1 calc R . . O1 O 0.305(2) 0.234(2) 0.5541(18) 0.149(8) Uiso 0.50 1 d PD A 1 O1A O 0.290(2) 0.114(2) 0.528(2) 0.164(9) Uiso 0.50 1 d PD B 2 P2 P 0.22306(17) 0.60162(18) -0.16293(16) 0.0469(5) Uani 1 1 d . . . N2 N 0.2248(6) 0.6384(5) 0.2607(5) 0.0508(16) Uani 1 1 d . . . H2 H 0.2113 0.5853 0.2063 0.061 Uiso 1 1 calc R . . C2 C 0.2528(9) 0.6768(8) 0.4355(7) 0.067(2) Uani 1 1 d . . . H2A H 0.2834 0.7590 0.4400 0.081 Uiso 1 1 calc R . . O2 O 0.481(2) 0.006(2) 0.4416(17) 0.163(9) Uiso 0.50 1 d PD . . C3 C 0.2174(7) 0.6004(7) 0.3459(6) 0.0502(19) Uani 1 1 d . . . N3 N -0.0803(11) 0.0466(9) -0.4030(11) 0.117(5) Uani 1 1 d . . . N4 N 0.1160(6) 0.3698(6) -0.2284(6) 0.065(2) Uani 1 1 d . . . H4 H 0.1520 0.3693 -0.1728 0.078 Uiso 1 1 calc R . . C4 C 0.1775(7) 0.4793(7) 0.3444(7) 0.054(2) Uani 1 1 d . . . H4A H 0.1541 0.4225 0.2853 0.065 Uiso 1 1 calc R . . C5 C 0.1739(10) 0.4465(9) 0.4321(8) 0.074(3) Uani 1 1 d . . . H5 H 0.1464 0.3648 0.4306 0.088 Uiso 1 1 calc R . . C6 C 0.2534(7) 0.7603(7) 0.2560(6) 0.0484(18) Uani 1 1 d . . . H6A H 0.3276 0.8042 0.2977 0.058 Uiso 1 1 calc R . . H6B H 0.1909 0.7936 0.2804 0.058 Uiso 1 1 calc R . . C7 C 0.2502(6) 0.9237(6) 0.1379(6) 0.0451(17) Uani 1 1 d . . . C8 C 0.3205(8) 1.0219(7) 0.2053(7) 0.057(2) Uani 1 1 d . . . H8 H 0.3807 1.0127 0.2472 0.069 Uiso 1 1 calc R . . C9 C 0.3043(8) 1.1315(7) 0.2121(7) 0.065(2) Uani 1 1 d . . . H9 H 0.3513 1.1968 0.2594 0.079 Uiso 1 1 calc R . . C10 C 0.2198(8) 1.1452(8) 0.1500(8) 0.070(3) Uani 1 1 d . . . H10 H 0.2092 1.2209 0.1539 0.085 Uiso 1 1 calc R . . C11 C 0.1498(8) 1.0511(8) 0.0818(9) 0.078(3) Uani 1 1 d . . . H11 H 0.0905 1.0620 0.0401 0.093 Uiso 1 1 calc R . . C12 C 0.1659(7) 0.9387(7) 0.0741(8) 0.066(3) Uani 1 1 d . . . H12 H 0.1197 0.8740 0.0258 0.079 Uiso 1 1 calc R . . C13 C 0.4243(6) 0.8003(6) 0.1237(6) 0.0438(17) Uani 1 1 d . . . C14 C 0.4912(7) 0.7510(7) 0.1756(6) 0.0510(19) Uani 1 1 d . . . H14 H 0.4574 0.7102 0.2225 0.061 Uiso 1 1 calc R . . C15 C 0.6080(8) 0.7598(8) 0.1608(8) 0.064(2) Uani 1 1 d . . . H15 H 0.6524 0.7239 0.1963 0.077 Uiso 1 1 calc R . . C16 C 0.6573(8) 0.8206(7) 0.0947(7) 0.062(2) Uani 1 1 d . . . H16 H 0.7368 0.8278 0.0853 0.075 Uiso 1 1 calc R . . C17 C 0.5929(7) 0.8721(7) 0.0408(7) 0.064(2) Uani 1 1 d . . . H17 H 0.6276 0.9136 -0.0053 0.077 Uiso 1 1 calc R . . C18 C 0.4769(7) 0.8615(7) 0.0561(7) 0.057(2) Uani 1 1 d . . . H18 H 0.4323 0.8964 0.0199 0.068 Uiso 1 1 calc R . . C19 C -0.0431(12) 0.0585(11) -0.3124(16) 0.114(6) Uani 1 1 d . . . H19 H -0.0637 -0.0098 -0.2862 0.137 Uiso 1 1 calc R . . C20 C 0.0248(8) 0.1636(9) -0.2502(10) 0.086(4) Uani 1 1 d . . . H20 H 0.0502 0.1654 -0.1853 0.103 Uiso 1 1 calc R . . C21 C 0.0538(7) 0.2658(8) -0.2874(8) 0.060(2) Uani 1 1 d . . . C22 C 0.0161(9) 0.2528(8) -0.3824(8) 0.072(3) Uani 1 1 d . . . H22 H 0.0345 0.3187 -0.4117 0.087 Uiso 1 1 calc R . . C23 C -0.0489(11) 0.1440(10) -0.4359(10) 0.100(4) Uani 1 1 d . . . H23 H -0.0729 0.1388 -0.5018 0.120 Uiso 1 1 calc R . . C24 C 0.1246(7) 0.4819(7) -0.2549(6) 0.052(2) Uani 1 1 d . . . H24A H 0.0459 0.4939 -0.2606 0.062 Uiso 1 1 calc R . . H24B H 0.1549 0.4815 -0.3181 0.062 Uiso 1 1 calc R . . C25 C 0.2238(7) 0.7289(7) -0.2137(6) 0.0518(19) Uani 1 1 d . . . C26 C 0.1191(9) 0.7481(9) -0.2404(10) 0.098(4) Uani 1 1 d . . . H26 H 0.0475 0.6940 -0.2332 0.117 Uiso 1 1 calc R . . C27 C 0.1165(10) 0.8445(10) -0.2774(11) 0.102(4) Uani 1 1 d . . . H27 H 0.0435 0.8559 -0.2961 0.122 Uiso 1 1 calc R . . C28 C 0.2175(9) 0.9231(8) -0.2874(8) 0.074(3) Uani 1 1 d . . . H28 H 0.2153 0.9891 -0.3136 0.088 Uiso 1 1 calc R . . C29 C 0.3207(9) 0.9078(7) -0.2604(8) 0.073(3) Uani 1 1 d . . . H29 H 0.3915 0.9637 -0.2666 0.088 Uiso 1 1 calc R . . C30 C 0.3244(8) 0.8108(7) -0.2234(7) 0.061(2) Uani 1 1 d . . . H30 H 0.3982 0.8010 -0.2045 0.074 Uiso 1 1 calc R . . C31 C 0.3657(6) 0.5791(6) -0.1771(6) 0.0415(16) Uani 1 1 d . . . C32 C 0.4401(7) 0.5884(6) -0.0967(6) 0.0508(19) Uani 1 1 d . . . H32 H 0.4144 0.6041 -0.0350 0.061 Uiso 1 1 calc R . . C33 C 0.5526(7) 0.5753(7) -0.1030(7) 0.055(2) Uani 1 1 d . . . H33 H 0.6032 0.5841 -0.0463 0.066 Uiso 1 1 calc R . . C34 C 0.5883(7) 0.5497(7) -0.1912(7) 0.055(2) Uani 1 1 d . . . H34 H 0.6638 0.5391 -0.1963 0.066 Uiso 1 1 calc R . . C35 C 0.5146(8) 0.5388(7) -0.2748(7) 0.061(2) Uani 1 1 d . . . H35 H 0.5408 0.5219 -0.3362 0.073 Uiso 1 1 calc R . . C36 C 0.4023(7) 0.5529(7) -0.2681(6) 0.055(2) Uani 1 1 d . . . H36 H 0.3518 0.5447 -0.3247 0.066 Uiso 1 1 calc R . . C37 C 0.392(2) 0.288(2) 0.4984(18) 0.091(7) Uiso 0.50 1 d PD A 1 C37A C 0.253(4) 0.193(4) 0.477(3) 0.199(19) Uiso 0.50 1 d PD B 2 C38 C 0.511(3) -0.090(2) 0.387(2) 0.135(11) Uiso 0.50 1 d PD . . 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 I1 0.0369(3) 0.0526(3) 0.0680(4) 0.0297(3) 0.0012(2) 0.0111(2) Ag1 0.0416(3) 0.0536(4) 0.0541(4) 0.0211(3) 0.0052(3) 0.0094(3) P1 0.0387(9) 0.0441(10) 0.0504(13) 0.0197(9) 0.0051(9) 0.0107(8) N1 0.122(8) 0.103(7) 0.062(6) 0.043(5) 0.012(6) 0.036(6) C1 0.132(10) 0.081(7) 0.064(7) 0.027(6) 0.015(7) 0.036(7) P2 0.0375(9) 0.0538(11) 0.0555(13) 0.0264(10) 0.0089(9) 0.0123(9) N2 0.062(4) 0.050(4) 0.049(4) 0.020(3) 0.015(3) 0.023(3) C2 0.087(7) 0.070(6) 0.044(5) 0.025(4) 0.004(5) 0.012(5) C3 0.048(4) 0.058(5) 0.054(5) 0.027(4) 0.011(4) 0.020(4) N3 0.105(9) 0.063(6) 0.155(12) -0.021(8) 0.060(9) -0.003(6) N4 0.055(4) 0.067(5) 0.075(6) 0.038(4) -0.006(4) 0.008(4) C4 0.061(5) 0.044(4) 0.065(6) 0.026(4) 0.010(4) 0.017(4) C5 0.092(7) 0.069(6) 0.076(8) 0.044(6) 0.020(6) 0.027(6) C6 0.048(4) 0.050(4) 0.052(5) 0.021(4) 0.010(4) 0.016(4) C7 0.040(4) 0.043(4) 0.049(5) 0.016(3) 0.004(3) 0.002(3) C8 0.064(5) 0.050(4) 0.062(6) 0.022(4) -0.001(4) 0.017(4) C9 0.066(6) 0.050(5) 0.080(7) 0.019(5) 0.002(5) 0.013(4) C10 0.065(6) 0.052(5) 0.113(9) 0.038(6) 0.025(6) 0.030(5) C11 0.048(5) 0.065(6) 0.133(10) 0.049(6) -0.004(6) 0.021(4) C12 0.051(5) 0.053(5) 0.097(8) 0.036(5) 0.000(5) 0.010(4) C13 0.046(4) 0.038(4) 0.053(5) 0.015(3) 0.012(4) 0.016(3) C14 0.053(4) 0.048(4) 0.053(5) 0.016(4) -0.004(4) 0.015(4) C15 0.052(5) 0.067(5) 0.083(7) 0.026(5) 0.006(5) 0.028(4) C16 0.050(5) 0.058(5) 0.078(7) 0.016(5) 0.016(5) 0.013(4) C17 0.054(5) 0.056(5) 0.084(7) 0.021(5) 0.017(5) 0.014(4) C18 0.048(4) 0.051(4) 0.072(6) 0.015(4) 0.008(4) 0.015(4) C19 0.084(9) 0.055(7) 0.215(19) 0.032(10) 0.065(12) 0.026(7) C20 0.059(6) 0.070(6) 0.154(12) 0.057(7) 0.045(7) 0.032(5) C21 0.038(4) 0.060(5) 0.084(7) 0.021(5) 0.013(4) 0.013(4) C22 0.069(6) 0.062(6) 0.075(8) 0.008(5) 0.018(5) 0.005(5) C23 0.102(9) 0.071(7) 0.103(10) -0.011(7) 0.040(8) -0.002(7) C24 0.044(4) 0.062(5) 0.056(5) 0.031(4) 0.003(4) 0.013(4) C25 0.046(4) 0.056(4) 0.059(5) 0.025(4) 0.010(4) 0.014(4) C26 0.055(5) 0.086(7) 0.189(14) 0.096(8) 0.030(7) 0.033(5) C27 0.067(7) 0.095(8) 0.172(14) 0.079(9) 0.021(8) 0.032(6) C28 0.079(7) 0.055(5) 0.092(8) 0.033(5) -0.004(6) 0.019(5) C29 0.076(6) 0.045(5) 0.095(8) 0.028(5) 0.011(6) 0.002(5) C30 0.053(5) 0.057(5) 0.075(7) 0.026(5) 0.004(4) 0.011(4) C31 0.034(3) 0.045(4) 0.046(5) 0.018(3) -0.002(3) 0.008(3) C32 0.049(4) 0.048(4) 0.059(6) 0.019(4) 0.012(4) 0.015(4) C33 0.044(4) 0.062(5) 0.064(6) 0.015(4) -0.002(4) 0.023(4) C34 0.043(4) 0.047(4) 0.082(7) 0.021(4) 0.017(4) 0.016(4) C35 0.058(5) 0.055(5) 0.075(7) 0.017(5) 0.021(5) 0.021(4) C36 0.059(5) 0.062(5) 0.045(5) 0.015(4) 0.003(4) 0.017(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag I1 Ag1 2.9170(10) . ? I1 Ag1 2.9427(10) 2_565 ? Ag1 P1 2.467(2) . ? Ag1 P2 2.486(2) . ? Ag1 I1 2.9427(10) 2_565 ? P1 C13 1.813(7) . ? P1 C7 1.821(8) . ? P1 C6 1.834(8) . ? N1 C1 1.332(13) . ? N1 C5 1.339(13) . ? C1 C2 1.367(14) . ? C1 H1 0.9500 . ? O1 C37 1.432(10) . ? O1A C37A 1.445(10) . ? P2 C31 1.814(7) . ? P2 C25 1.822(8) . ? P2 C24 1.833(9) . ? N2 C3 1.377(10) . ? N2 C6 1.438(9) . ? N2 H2 0.8800 . ? C2 C3 1.389(12) . ? C2 H2A 0.9500 . ? O2 C38 1.418(10) . ? C3 C4 1.408(10) . ? N3 C19 1.31(2) . ? N3 C23 1.320(17) . ? N4 C21 1.362(11) . ? N4 C24 1.456(10) . ? N4 H4 0.8800 . ? C4 C5 1.382(13) . ? C4 H4A 0.9500 . ? C5 H5 0.9500 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C12 1.388(11) . ? C7 C8 1.400(11) . ? C8 C9 1.378(11) . ? C8 H8 0.9500 . ? C9 C10 1.367(13) . ? C9 H9 0.9500 . ? C10 C11 1.378(14) . ? C10 H10 0.9500 . ? C11 C12 1.410(12) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.378(10) . ? C13 C18 1.402(11) . ? C14 C15 1.402(11) . ? C14 H14 0.9500 . ? C15 C16 1.369(12) . ? C15 H15 0.9500 . ? C16 C17 1.393(13) . ? C16 H16 0.9500 . ? C17 C18 1.391(11) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.408(19) . ? C19 H19 0.9500 . ? C20 C21 1.404(12) . ? C20 H20 0.9500 . ? C21 C22 1.364(14) . ? C22 C23 1.381(14) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C30 1.369(10) . ? C25 C26 1.378(12) . ? C26 C27 1.377(13) . ? C26 H26 0.9500 . ? C27 C28 1.353(13) . ? C27 H27 0.9500 . ? C28 C29 1.339(13) . ? C28 H28 0.9500 . ? C29 C30 1.387(12) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.373(11) . ? C31 C36 1.398(11) . ? C32 C33 1.401(10) . ? C32 H32 0.9500 . ? C33 C34 1.356(12) . ? C33 H33 0.9500 . ? C34 C35 1.399(13) . ? C34 H34 0.9500 . ? C35 C36 1.403(11) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Ag1 I1 Ag1 85.96(4) . 2_565 ? P1 Ag1 P2 118.56(7) . . ? P1 Ag1 I1 115.46(6) . . ? P2 Ag1 I1 107.54(6) . . ? P1 Ag1 I1 114.62(6) . 2_565 ? P2 Ag1 I1 103.33(6) . 2_565 ? I1 Ag1 I1 94.04(4) . 2_565 ? C13 P1 C7 104.1(3) . . ? C13 P1 C6 103.6(4) . . ? C7 P1 C6 101.9(4) . . ? C13 P1 Ag1 110.0(3) . . ? C7 P1 Ag1 117.3(3) . . ? C6 P1 Ag1 118.1(3) . . ? C1 N1 C5 114.4(9) . . ? N1 C1 C2 125.4(11) . . ? N1 C1 H1 117.3 . . ? C2 C1 H1 117.3 . . ? C31 P2 C25 105.4(3) . . ? C31 P2 C24 103.4(4) . . ? C25 P2 C24 101.5(4) . . ? C31 P2 Ag1 119.3(3) . . ? C25 P2 Ag1 112.2(3) . . ? C24 P2 Ag1 113.2(3) . . ? C3 N2 C6 123.3(7) . . ? C3 N2 H2 118.3 . . ? C6 N2 H2 118.3 . . ? C1 C2 C3 119.4(9) . . ? C1 C2 H2A 120.3 . . ? C3 C2 H2A 120.3 . . ? N2 C3 C2 122.7(7) . . ? N2 C3 C4 120.0(8) . . ? C2 C3 C4 117.3(8) . . ? C19 N3 C23 114.7(12) . . ? C21 N4 C24 121.7(8) . . ? C21 N4 H4 119.1 . . ? C24 N4 H4 119.1 . . ? C5 C4 C3 117.3(9) . . ? C5 C4 H4A 121.3 . . ? C3 C4 H4A 121.3 . . ? N1 C5 C4 126.2(9) . . ? N1 C5 H5 116.9 . . ? C4 C5 H5 116.9 . . ? N2 C6 P1 111.2(6) . . ? N2 C6 H6A 109.4 . . ? P1 C6 H6A 109.4 . . ? N2 C6 H6B 109.4 . . ? P1 C6 H6B 109.4 . . ? H6A C6 H6B 108.0 . . ? C12 C7 C8 119.0(7) . . ? C12 C7 P1 119.9(6) . . ? C8 C7 P1 121.1(6) . . ? C9 C8 C7 121.4(9) . . ? C9 C8 H8 119.3 . . ? C7 C8 H8 119.3 . . ? C10 C9 C8 119.2(9) . . ? C10 C9 H9 120.4 . . ? C8 C9 H9 120.4 . . ? C9 C10 C11 121.2(8) . . ? C9 C10 H10 119.4 . . ? C11 C10 H10 119.4 . . ? C10 C11 C12 120.1(9) . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C7 C12 C11 119.1(9) . . ? C7 C12 H12 120.5 . . ? C11 C12 H12 120.5 . . ? C14 C13 C18 118.1(7) . . ? C14 C13 P1 122.7(6) . . ? C18 C13 P1 119.0(6) . . ? C13 C14 C15 121.5(8) . . ? C13 C14 H14 119.3 . . ? C15 C14 H14 119.3 . . ? C16 C15 C14 119.2(9) . . ? C16 C15 H15 120.4 . . ? C14 C15 H15 120.4 . . ? C15 C16 C17 121.2(8) . . ? C15 C16 H16 119.4 . . ? C17 C16 H16 119.4 . . ? C18 C17 C16 118.6(9) . . ? C18 C17 H17 120.7 . . ? C16 C17 H17 120.7 . . ? C17 C18 C13 121.4(9) . . ? C17 C18 H18 119.3 . . ? C13 C18 H18 119.3 . . ? N3 C19 C20 125.7(13) . . ? N3 C19 H19 117.1 . . ? C20 C19 H19 117.1 . . ? C21 C20 C19 117.7(13) . . ? C21 C20 H20 121.1 . . ? C19 C20 H20 121.1 . . ? N4 C21 C22 124.3(9) . . ? N4 C21 C20 119.3(10) . . ? C22 C21 C20 116.4(10) . . ? C21 C22 C23 120.1(11) . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? N3 C23 C22 125.4(14) . . ? N3 C23 H23 117.3 . . ? C22 C23 H23 117.3 . . ? N4 C24 P2 109.8(6) . . ? N4 C24 H24A 109.7 . . ? P2 C24 H24A 109.7 . . ? N4 C24 H24B 109.7 . . ? P2 C24 H24B 109.7 . . ? H24A C24 H24B 108.2 . . ? C30 C25 C26 117.3(8) . . ? C30 C25 P2 123.2(6) . . ? C26 C25 P2 119.5(6) . . ? C27 C26 C25 121.0(9) . . ? C27 C26 H26 119.5 . . ? C25 C26 H26 119.5 . . ? C28 C27 C26 120.4(10) . . ? C28 C27 H27 119.8 . . ? C26 C27 H27 119.8 . . ? C29 C28 C27 119.9(9) . . ? C29 C28 H28 120.0 . . ? C27 C28 H28 120.0 . . ? C28 C29 C30 120.3(9) . . ? C28 C29 H29 119.9 . . ? C30 C29 H29 119.9 . . ? C25 C30 C29 121.1(9) . . ? C25 C30 H30 119.4 . . ? C29 C30 H30 119.4 . . ? C32 C31 C36 119.0(7) . . ? C32 C31 P2 119.5(6) . . ? C36 C31 P2 121.5(6) . . ? C31 C32 C33 122.0(8) . . ? C31 C32 H32 119.0 . . ? C33 C32 H32 119.0 . . ? C34 C33 C32 119.1(8) . . ? C34 C33 H33 120.5 . . ? C32 C33 H33 120.5 . . ? C33 C34 C35 120.5(8) . . ? C33 C34 H34 119.8 . . ? C35 C34 H34 119.8 . . ? C34 C35 C36 120.2(8) . . ? C34 C35 H35 119.9 . . ? C36 C35 H35 119.9 . . ? C31 C36 C35 119.2(8) . . ? C31 C36 H36 120.4 . . ? C35 C36 H36 120.4 . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 1.122 _refine_diff_density_min -0.947 _refine_diff_density_rms 0.116 #===END # Attachment 'JPLangCIF.cif' data_[{Ag2(CN)2(dppmapy)}.0.5CHCl3]n _database_code_depnum_ccdc_archive 'CCDC 748195' #TrackingRef 'JPLangCIF.cif' #========================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C20 H17 Ag2 N4 P), 2(C0.50 Cl1.50)' _chemical_formula_sum 'C41 H34 Ag4 Cl3 N8 P2 ' _chemical_formula_weight 1238.53 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' 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' Cl Cl 0.1484 0.1585 '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' 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 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 16.255(3) _cell_length_b 7.3326(15) _cell_length_c 19.528(4) _cell_angle_alpha 90.00 _cell_angle_beta 106.83(3) _cell_angle_gamma 90.00 _cell_volume 2227.9(8) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 8947 _cell_measurement_theta_min 3.0713 _cell_measurement_theta_max 27.5126 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.846 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1210 _exptl_absorpt_coefficient_mu 2.024 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4310 _exptl_absorpt_correction_T_max 0.8232 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'Rigaku MercuryCCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 14257 _diffrn_reflns_av_R_equivalents 0.0383 _diffrn_reflns_av_sigmaI/netI 0.0432 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5037 _reflns_number_gt 4088 _reflns_threshold_expression >2sigma(I) __computing_data_collection 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_cell_refinement 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_data_reduction 'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material SHELXL97 _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^)+(0.0942P)^2^+4.1463P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5037 _refine_ls_number_parameters 259 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0873 _refine_ls_R_factor_gt 0.0706 _refine_ls_wR_factor_ref 0.1980 _refine_ls_wR_factor_gt 0.1840 _refine_ls_goodness_of_fit_ref 1.116 _refine_ls_restrained_S_all 1.130 _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 Ag1 Ag 0.80029(3) 0.66496(8) 0.24679(3) 0.0551(2) Uani 1 1 d . . . P1 P 0.70244(10) 0.8072(2) 0.14560(9) 0.0429(4) Uani 1 1 d . . . N1 N 1.0630(3) 1.1068(9) 0.1969(3) 0.0529(14) Uani 1 1 d . . . C1 C 0.9973(5) 1.1479(10) 0.2230(4) 0.0514(17) Uani 1 1 d . . . H1 H 1.0100 1.2094 0.2670 0.062 Uiso 1 1 calc R . . N2 N 0.8101(3) 0.9796(8) 0.0827(3) 0.0450(12) Uani 1 1 d . . . H2 H 0.8041 0.9285 0.0413 0.054 Uiso 1 1 calc R . . C2 C 0.9127(4) 1.1062(10) 0.1897(4) 0.0490(16) Uani 1 1 d . . . H2A H 0.8698 1.1339 0.2116 0.059 Uiso 1 1 calc R . . Ag2 Ag 0.75199(4) -0.02662(9) 0.33006(3) 0.0599(2) Uani 1 1 d . . . C3 C 0.8916(4) 1.0217(9) 0.1224(3) 0.0414(14) Uani 1 1 d . . . N3 N 0.7501(5) 0.3679(10) 0.2596(4) 0.0676(18) Uani 1 1 d . . . C4 C 0.9605(5) 0.9774(10) 0.0955(4) 0.0510(17) Uani 1 1 d . . . H4 H 0.9502 0.9185 0.0510 0.061 Uiso 1 1 calc R . . N4 N 0.7747(5) -0.3798(11) 0.4286(4) 0.0688(18) Uani 1 1 d . . . C5 C 1.0417(5) 1.0201(12) 0.1339(4) 0.060(2) Uani 1 1 d . . . H5 H 1.0865 0.9864 0.1149 0.072 Uiso 1 1 calc R . . C6 C 0.7334(4) 1.0124(9) 0.1032(4) 0.0457(15) Uani 1 1 d . . . H6A H 0.6865 1.0457 0.0608 0.055 Uiso 1 1 calc R . . H6B H 0.7431 1.1148 0.1368 0.055 Uiso 1 1 calc R . . C7 C 0.6868(5) 0.6414(10) 0.0747(4) 0.0535(18) Uani 1 1 d . . . C8 C 0.7556(8) 0.5305(12) 0.0718(5) 0.080(3) Uani 1 1 d . . . H8 H 0.8074 0.5413 0.1087 0.097 Uiso 1 1 calc R . . C9 C 0.7519(10) 0.4081(14) 0.0190(6) 0.098(4) Uani 1 1 d . . . H9 H 0.8009 0.3411 0.0183 0.118 Uiso 1 1 calc R . . C10 C 0.6783(11) 0.3842(17) -0.0316(6) 0.099(4) Uani 1 1 d . . . H10 H 0.6752 0.2957 -0.0671 0.119 Uiso 1 1 calc R . . C11 C 0.6058(9) 0.486(2) -0.0339(6) 0.119(6) Uani 1 1 d . . . H11 H 0.5544 0.4671 -0.0705 0.143 Uiso 1 1 calc R . . C12 C 0.6102(6) 0.6201(17) 0.0204(5) 0.086(3) Uani 1 1 d . . . H12 H 0.5621 0.6924 0.0194 0.103 Uiso 1 1 calc R . . C13 C 0.5961(4) 0.8601(11) 0.1524(3) 0.0497(16) Uani 1 1 d . . . C14 C 0.5436(5) 0.9987(13) 0.1147(5) 0.067(2) Uani 1 1 d . . . H14 H 0.5635 1.0719 0.0833 0.081 Uiso 1 1 calc R . . C15 C 0.4631(5) 1.0312(13) 0.1225(5) 0.070(2) Uani 1 1 d . . . H15 H 0.4291 1.1272 0.0975 0.084 Uiso 1 1 calc R . . C16 C 0.4333(5) 0.9210(14) 0.1675(4) 0.067(2) Uani 1 1 d . . . H16 H 0.3772 0.9373 0.1708 0.081 Uiso 1 1 calc R . . C17 C 0.4841(5) 0.7898(15) 0.2069(5) 0.074(3) Uani 1 1 d . . . H17 H 0.4644 0.7197 0.2393 0.089 Uiso 1 1 calc R . . C18 C 0.5651(5) 0.7588(14) 0.1996(4) 0.063(2) Uani 1 1 d . . . H18 H 0.5998 0.6672 0.2271 0.076 Uiso 1 1 calc R . . C19 C 0.7471(5) 0.2256(12) 0.2817(4) 0.0585(18) Uani 1 1 d . . . C20 C 0.7658(5) -0.2632(11) 0.3889(4) 0.0527(17) Uani 1 1 d . . . C21 C 0.9996(8) 0.9130(12) 0.4744(5) 0.250(4) Uani 0.50 1 d PD . . Cl1 Cl 1.0034(12) 0.990(2) 0.3998(8) 0.250(4) Uani 0.50 1 d PD . . Cl2 Cl 1.0876(10) 0.8162(19) 0.5320(8) 0.250(4) Uani 0.50 1 d PD . . Cl3 Cl 0.9996(8) 0.9130(12) 0.4744(5) 0.250(4) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0393(3) 0.0580(4) 0.0600(4) 0.0038(3) 0.0018(2) 0.0077(2) P1 0.0315(8) 0.0500(10) 0.0445(8) 0.0041(7) 0.0065(6) -0.0027(7) N1 0.030(3) 0.067(4) 0.059(3) -0.012(3) 0.009(2) -0.008(3) C1 0.046(4) 0.059(4) 0.048(3) -0.015(3) 0.010(3) -0.003(3) N2 0.036(3) 0.052(3) 0.047(3) -0.003(2) 0.012(2) -0.006(2) C2 0.041(3) 0.053(4) 0.052(4) -0.002(3) 0.012(3) -0.006(3) Ag2 0.0685(4) 0.0549(4) 0.0605(4) -0.0016(3) 0.0253(3) -0.0019(3) C3 0.039(3) 0.040(3) 0.045(3) 0.002(3) 0.012(3) -0.009(3) N3 0.071(5) 0.052(4) 0.087(5) -0.010(4) 0.034(4) 0.000(3) C4 0.045(4) 0.061(4) 0.048(4) -0.017(3) 0.015(3) -0.008(3) N4 0.074(5) 0.081(5) 0.052(4) 0.005(4) 0.020(3) 0.001(4) C5 0.046(4) 0.078(5) 0.058(4) -0.016(4) 0.019(3) -0.009(4) C6 0.033(3) 0.052(4) 0.051(4) -0.002(3) 0.009(3) -0.005(3) C7 0.065(5) 0.044(4) 0.052(4) 0.007(3) 0.018(3) -0.020(3) C8 0.137(9) 0.048(5) 0.054(5) 0.000(4) 0.024(5) 0.002(5) C9 0.173(12) 0.053(5) 0.074(6) 0.004(5) 0.045(8) 0.008(7) C10 0.146(12) 0.082(7) 0.086(8) -0.014(6) 0.060(8) -0.051(8) C11 0.120(10) 0.179(14) 0.064(6) -0.038(7) 0.036(6) -0.115(11) C12 0.070(6) 0.123(8) 0.064(5) -0.024(6) 0.021(4) -0.052(6) C13 0.034(3) 0.070(5) 0.041(3) 0.007(3) 0.005(3) -0.008(3) C14 0.045(4) 0.089(6) 0.068(5) 0.031(5) 0.016(4) 0.007(4) C15 0.042(4) 0.088(6) 0.077(5) 0.017(5) 0.014(4) 0.018(4) C16 0.041(4) 0.099(7) 0.062(4) -0.018(5) 0.016(3) -0.004(4) C17 0.051(5) 0.107(7) 0.070(5) 0.020(5) 0.026(4) -0.002(5) C18 0.046(4) 0.087(6) 0.055(4) 0.006(4) 0.012(3) -0.009(4) C19 0.061(5) 0.056(5) 0.065(4) -0.015(4) 0.028(4) -0.003(4) C20 0.059(4) 0.059(4) 0.044(3) -0.006(3) 0.020(3) -0.005(4) C21 0.279(10) 0.203(8) 0.221(8) 0.017(5) -0.004(7) -0.100(7) Cl1 0.279(10) 0.203(8) 0.221(8) 0.017(5) -0.004(7) -0.100(7) Cl2 0.279(10) 0.203(8) 0.221(8) 0.017(5) -0.004(7) -0.100(7) Cl3 0.279(10) 0.203(8) 0.221(8) 0.017(5) -0.004(7) -0.100(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.217(5) 2_745 ? Ag1 N3 2.365(7) . ? Ag1 P1 2.3880(19) . ? Ag1 Ag2 3.0189(10) 1_565 ? P1 C7 1.804(8) . ? P1 C13 1.814(7) . ? P1 C6 1.856(7) . ? N1 C5 1.339(9) . ? N1 C1 1.344(9) . ? N1 Ag1 2.217(5) 2_755 ? C1 C2 1.374(9) . ? C1 H1 0.9400 . ? N2 C3 1.362(8) . ? N2 C6 1.436(8) . ? N2 H2 0.8700 . ? C2 C3 1.402(9) . ? C2 H2A 0.9400 . ? Ag2 C20 2.057(8) . ? Ag2 C19 2.067(9) . ? Ag2 Ag1 3.0189(10) 1_545 ? C3 C4 1.407(10) . ? N3 C19 1.136(10) . ? C4 C5 1.352(10) . ? C4 H4 0.9400 . ? N4 C20 1.134(10) . ? C5 H5 0.9400 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 C12 1.391(12) . ? C7 C8 1.396(14) . ? C8 C9 1.356(14) . ? C8 H8 0.9400 . ? C9 C10 1.324(18) . ? C9 H9 0.9400 . ? C10 C11 1.385(19) . ? C10 H10 0.9400 . ? C11 C12 1.433(16) . ? C11 H11 0.9400 . ? C12 H12 0.9400 . ? C13 C18 1.387(11) . ? C13 C14 1.392(11) . ? C14 C15 1.382(11) . ? C14 H14 0.9400 . ? C15 C16 1.380(13) . ? C15 H15 0.9400 . ? C16 C17 1.354(13) . ? C16 H16 0.9400 . ? C17 C18 1.383(11) . ? C17 H17 0.9400 . ? C18 H18 0.9400 . ? C21 Cl1 1.581(11) . ? C21 Cl3 1.620(15) 3_776 ? C21 C21 1.620(15) 3_776 ? C21 Cl2 1.698(11) . ? Cl2 Cl3 2.42(2) 3_776 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N3 95.6(3) 2_745 . ? N1 Ag1 P1 145.72(16) 2_745 . ? N3 Ag1 P1 108.8(2) . . ? N1 Ag1 Ag2 104.88(18) 2_745 1_565 ? N3 Ag1 Ag2 118.77(17) . 1_565 ? P1 Ag1 Ag2 84.47(5) . 1_565 ? C7 P1 C13 105.9(4) . . ? C7 P1 C6 101.5(3) . . ? C13 P1 C6 104.3(3) . . ? C7 P1 Ag1 104.6(3) . . ? C13 P1 Ag1 117.0(2) . . ? C6 P1 Ag1 121.4(2) . . ? C5 N1 C1 115.6(6) . . ? C5 N1 Ag1 120.2(5) . 2_755 ? C1 N1 Ag1 124.2(5) . 2_755 ? N1 C1 C2 124.5(6) . . ? N1 C1 H1 117.7 . . ? C2 C1 H1 117.7 . . ? C3 N2 C6 125.6(6) . . ? C3 N2 H2 117.2 . . ? C6 N2 H2 117.2 . . ? C1 C2 C3 118.8(6) . . ? C1 C2 H2A 120.6 . . ? C3 C2 H2A 120.6 . . ? C20 Ag2 C19 173.2(3) . . ? C20 Ag2 Ag1 70.48(19) . 1_545 ? C19 Ag2 Ag1 113.9(2) . 1_545 ? N2 C3 C2 124.6(6) . . ? N2 C3 C4 118.8(6) . . ? C2 C3 C4 116.5(6) . . ? C19 N3 Ag1 160.2(7) . . ? C5 C4 C3 119.6(6) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? N1 C5 C4 124.8(7) . . ? N1 C5 H5 117.6 . . ? C4 C5 H5 117.6 . . ? N2 C6 P1 111.0(5) . . ? N2 C6 H6A 109.4 . . ? P1 C6 H6A 109.4 . . ? N2 C6 H6B 109.4 . . ? P1 C6 H6B 109.4 . . ? H6A C6 H6B 108.0 . . ? C12 C7 C8 117.0(8) . . ? C12 C7 P1 123.8(8) . . ? C8 C7 P1 119.1(6) . . ? C9 C8 C7 123.8(11) . . ? C9 C8 H8 118.1 . . ? C7 C8 H8 118.1 . . ? C10 C9 C8 119.1(13) . . ? C10 C9 H9 120.4 . . ? C8 C9 H9 120.4 . . ? C9 C10 C11 122.0(11) . . ? C9 C10 H10 119.0 . . ? C11 C10 H10 119.0 . . ? C10 C11 C12 119.1(10) . . ? C10 C11 H11 120.4 . . ? C12 C11 H11 120.4 . . ? C7 C12 C11 118.9(12) . . ? C7 C12 H12 120.6 . . ? C11 C12 H12 120.6 . . ? C18 C13 C14 117.2(7) . . ? C18 C13 P1 118.1(6) . . ? C14 C13 P1 124.6(6) . . ? C15 C14 C13 121.5(8) . . ? C15 C14 H14 119.3 . . ? C13 C14 H14 119.3 . . ? C16 C15 C14 119.2(8) . . ? C16 C15 H15 120.4 . . ? C14 C15 H15 120.4 . . ? C17 C16 C15 120.6(8) . . ? C17 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? C16 C17 C18 120.0(8) . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C17 C18 C13 121.4(8) . . ? C17 C18 H18 119.3 . . ? C13 C18 H18 119.3 . . ? N3 C19 Ag2 174.5(8) . . ? N4 C20 Ag2 171.4(7) . . ? Cl1 C21 Cl3 106.9(12) . 3_776 ? Cl1 C21 C21 106.9(12) . 3_776 ? Cl3 C21 C21 0.0(9) 3_776 3_776 ? Cl1 C21 Cl2 120.7(12) . . ? Cl3 C21 Cl2 93.8(11) 3_776 . ? C21 C21 Cl2 93.8(11) 3_776 . ? C21 Cl2 Cl3 41.9(6) . 3_776 ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 2.456 _refine_diff_density_min -1.682 _refine_diff_density_rms 0.139 #===END #========================================================================== data_[Ag2(dca)2(dppmapy)2]n _database_code_depnum_ccdc_archive 'CCDC 748196' #TrackingRef 'JPLangCIF.cif' #========================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H17 Ag N5 P' _chemical_formula_sum 'C20 H17 Ag N5 P' _chemical_formula_weight 466.23 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' 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 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 8.7081(17) _cell_length_b 12.027(2) _cell_length_c 19.966(4) _cell_angle_alpha 79.33(3) _cell_angle_beta 89.42(3) _cell_angle_gamma 72.74(3) _cell_volume 1960.2(7) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 5842 _cell_measurement_theta_min 3.0032 _cell_measurement_theta_max 27.4507 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.580 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 936 _exptl_absorpt_coefficient_mu 1.124 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6620 _exptl_absorpt_correction_T_max 0.9056 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.' _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 'Rigaku MercuryCCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 13605 _diffrn_reflns_av_R_equivalents 0.0446 _diffrn_reflns_av_sigmaI/netI 0.0790 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 25.50 _reflns_number_total 7123 _reflns_number_gt 5289 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_cell_refinement 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_data_reduction 'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material SHELXL97 _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^)+(0.0489P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7123 _refine_ls_number_parameters 487 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0768 _refine_ls_R_factor_gt 0.0521 _refine_ls_wR_factor_ref 0.1244 _refine_ls_wR_factor_gt 0.1110 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.051 _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 C1 C -0.1228(6) 0.0346(5) 0.9358(3) 0.0299(13) Uani 1 1 d . . . H1 H -0.0908 -0.0475 0.9342 0.036 Uiso 1 1 calc R . . N1 N -0.2348(5) 0.0720(4) 0.9803(2) 0.0315(11) Uani 1 1 d . . . P1 P 0.30131(17) 0.20550(12) 0.85005(7) 0.0287(3) Uani 1 1 d . . . Ag1 Ag 0.33564(5) 0.05311(4) 0.94868(2) 0.03519(14) Uani 1 1 d . . . C2 C -0.0513(6) 0.1049(5) 0.8929(3) 0.0320(13) Uani 1 1 d . . . H2 H 0.0246 0.0718 0.8620 0.038 Uiso 1 1 calc R . . N2 N -0.0252(5) 0.3023(4) 0.8550(2) 0.0342(12) Uani 1 1 d . . . H2A H -0.0587 0.3774 0.8589 0.041 Uiso 1 1 calc R . . P2 P 0.03416(18) 0.21497(12) 0.35287(7) 0.0290(3) Uani 1 1 d . . . Ag2 Ag 0.11880(5) 0.05599(4) 0.44911(2) 0.03467(14) Uani 1 1 d . . . C3 C -0.0907(6) 0.2261(5) 0.8947(3) 0.0278(12) Uani 1 1 d . . . N3 N 0.5832(6) -0.1165(4) 0.9449(3) 0.0430(13) Uani 1 1 d . . . C4 C -0.2073(7) 0.2656(5) 0.9414(3) 0.0338(13) Uani 1 1 d . . . H4 H -0.2403 0.3467 0.9453 0.041 Uiso 1 1 calc R . . N4 N 0.6950(10) -0.2417(6) 0.8646(4) 0.0969(19) Uani 1 1 d U . . C5 C -0.2728(7) 0.1885(5) 0.9809(3) 0.0329(13) Uani 1 1 d . . . H5 H -0.3517 0.2193 1.0113 0.039 Uiso 1 1 calc R . . N5 N 0.8473(8) -0.4466(5) 0.8741(4) 0.0697(19) Uani 1 1 d . . . C6 C 0.0963(6) 0.2685(5) 0.8066(3) 0.0341(13) Uani 1 1 d . . . H6A H 0.0938 0.3387 0.7713 0.041 Uiso 1 1 calc R . . H6B H 0.0726 0.2087 0.7837 0.041 Uiso 1 1 calc R . . N6 N 0.6774(5) 0.0773(4) 0.4820(2) 0.0324(11) Uani 1 1 d . . . C7 C 0.3432(7) 0.3364(5) 0.8691(3) 0.0362(14) Uani 1 1 d . . . N7 N 0.2873(6) 0.3090(4) 0.3570(2) 0.0372(12) Uani 1 1 d . . . H7 H 0.2627 0.3843 0.3600 0.045 Uiso 1 1 calc R . . C8 C 0.2807(9) 0.3800(5) 0.9255(4) 0.0529(18) Uani 1 1 d . . . H8 H 0.2145 0.3424 0.9535 0.064 Uiso 1 1 calc R . . N8 N 0.0055(6) -0.1117(4) 0.4426(2) 0.0353(11) Uani 1 1 d . . . C9 C 0.3124(11) 0.4781(7) 0.9425(5) 0.074(3) Uani 1 1 d . . . H9 H 0.2678 0.5073 0.9817 0.089 Uiso 1 1 calc R . . N9 N -0.0047(8) -0.2401(5) 0.3618(3) 0.071(2) Uani 1 1 d . . . C10 C 0.4080(11) 0.5329(6) 0.9027(5) 0.069(3) Uani 1 1 d . . . H10 H 0.4297 0.6001 0.9142 0.083 Uiso 1 1 calc R . . N10 N 0.1845(9) -0.4309(5) 0.3510(3) 0.074(2) Uani 1 1 d . . . C11 C 0.4725(9) 0.4904(6) 0.8461(4) 0.062(2) Uani 1 1 d . . . H11 H 0.5390 0.5283 0.8185 0.074 Uiso 1 1 calc R . . C12 C 0.4414(8) 0.3929(5) 0.8289(3) 0.0478(17) Uani 1 1 d . . . H12 H 0.4867 0.3639 0.7897 0.057 Uiso 1 1 calc R . . C13 C 0.4343(6) 0.1638(4) 0.7820(3) 0.0290(12) Uani 1 1 d . . . C14 C 0.5937(7) 0.0995(6) 0.8009(3) 0.0465(16) Uani 1 1 d . . . H14 H 0.6268 0.0757 0.8479 0.056 Uiso 1 1 calc R . . C15 C 0.7041(8) 0.0698(6) 0.7524(4) 0.0536(19) Uani 1 1 d . . . H15 H 0.8127 0.0260 0.7660 0.064 Uiso 1 1 calc R . . C16 C 0.6566(8) 0.1038(5) 0.6841(3) 0.0481(17) Uani 1 1 d . . . H16 H 0.7330 0.0836 0.6506 0.058 Uiso 1 1 calc R . . C17 C 0.5008(8) 0.1660(5) 0.6642(3) 0.0444(16) Uani 1 1 d . . . H17 H 0.4691 0.1887 0.6171 0.053 Uiso 1 1 calc R . . C18 C 0.3873(7) 0.1966(5) 0.7130(3) 0.0357(14) Uani 1 1 d . . . H18 H 0.2786 0.2396 0.6991 0.043 Uiso 1 1 calc R . . C19 C 0.6477(12) -0.1817(6) 0.9140(5) 0.083(2) Uani 1 1 d U . . C20 C 0.7831(12) -0.3547(7) 0.8777(5) 0.086(2) Uani 1 1 d U . . C21 C 0.5955(6) 0.0409(4) 0.4382(3) 0.0300(13) Uani 1 1 d . . . H21 H 0.6284 -0.0414 0.4372 0.036 Uiso 1 1 calc R . . C22 C 0.4694(7) 0.1115(5) 0.3951(3) 0.0339(13) Uani 1 1 d . . . H22 H 0.4215 0.0788 0.3642 0.041 Uiso 1 1 calc R . . C23 C 0.4115(7) 0.2325(5) 0.3968(3) 0.0308(13) Uani 1 1 d . . . C24 C 0.4951(7) 0.2729(5) 0.4432(3) 0.0323(13) Uani 1 1 d . . . H24 H 0.4608 0.3540 0.4472 0.039 Uiso 1 1 calc R . . C25 C 0.6244(7) 0.1958(5) 0.4821(3) 0.0342(13) Uani 1 1 d . . . H25 H 0.6807 0.2266 0.5110 0.041 Uiso 1 1 calc R . . C26 C 0.1903(7) 0.2767(5) 0.3090(3) 0.0333(13) Uani 1 1 d . . . H26A H 0.2615 0.2171 0.2853 0.040 Uiso 1 1 calc R . . H26B H 0.1368 0.3478 0.2742 0.040 Uiso 1 1 calc R . . C27 C -0.1095(7) 0.3450(5) 0.3767(3) 0.0342(14) Uani 1 1 d . . . C28 C -0.0799(8) 0.3772(5) 0.4372(3) 0.0441(16) Uani 1 1 d . . . H28 H 0.0158 0.3340 0.4642 0.053 Uiso 1 1 calc R . . C29 C -0.1903(10) 0.4730(6) 0.4590(4) 0.062(2) Uani 1 1 d . . . H29 H -0.1689 0.4960 0.5001 0.074 Uiso 1 1 calc R . . C30 C -0.3289(10) 0.5330(6) 0.4206(4) 0.061(2) Uani 1 1 d . . . H30 H -0.4057 0.5963 0.4361 0.073 Uiso 1 1 calc R . . C31 C -0.3590(9) 0.5030(6) 0.3602(4) 0.059(2) Uani 1 1 d . . . H31 H -0.4553 0.5465 0.3337 0.070 Uiso 1 1 calc R . . C32 C -0.2491(8) 0.4093(5) 0.3373(3) 0.0444(16) Uani 1 1 d . . . H32 H -0.2694 0.3894 0.2950 0.053 Uiso 1 1 calc R . . C33 C -0.0688(6) 0.1815(5) 0.2837(3) 0.0290(12) Uani 1 1 d . . . C34 C -0.0565(7) 0.2259(5) 0.2149(3) 0.0421(15) Uani 1 1 d . . . H34 H 0.0106 0.2751 0.2021 0.050 Uiso 1 1 calc R . . C35 C -0.1424(8) 0.1986(6) 0.1641(3) 0.0493(17) Uani 1 1 d . . . H35 H -0.1333 0.2292 0.1174 0.059 Uiso 1 1 calc R . . C36 C -0.2389(8) 0.1280(5) 0.1823(3) 0.0478(18) Uani 1 1 d . . . H36 H -0.2976 0.1096 0.1483 0.057 Uiso 1 1 calc R . . C37 C -0.2510(8) 0.0833(6) 0.2506(4) 0.0554(19) Uani 1 1 d . . . H37 H -0.3182 0.0342 0.2634 0.067 Uiso 1 1 calc R . . C38 C -0.1657(8) 0.1100(5) 0.3006(3) 0.0448(16) Uani 1 1 d . . . H38 H -0.1746 0.0783 0.3472 0.054 Uiso 1 1 calc R . . C39 C 0.0076(6) -0.1762(5) 0.4061(3) 0.0347(14) Uani 1 1 d . . . C40 C 0.1025(8) -0.3428(6) 0.3590(3) 0.0490(18) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.025(3) 0.022(3) 0.038(3) -0.005(3) -0.005(3) 0.000(2) N1 0.030(3) 0.032(3) 0.030(3) -0.003(2) -0.002(2) -0.007(2) P1 0.0316(8) 0.0284(8) 0.0253(8) -0.0055(6) 0.0000(6) -0.0075(6) Ag1 0.0406(3) 0.0330(3) 0.0304(3) -0.0026(2) 0.0022(2) -0.0109(2) C2 0.030(3) 0.034(3) 0.032(3) -0.011(3) 0.002(2) -0.008(3) N2 0.033(3) 0.021(2) 0.042(3) -0.001(2) 0.008(2) -0.002(2) P2 0.0320(8) 0.0279(8) 0.0261(8) -0.0037(6) -0.0006(6) -0.0081(6) Ag2 0.0376(3) 0.0323(3) 0.0297(3) -0.0022(2) -0.00245(19) -0.0059(2) C3 0.027(3) 0.028(3) 0.025(3) -0.002(2) 0.000(2) -0.004(2) N3 0.045(3) 0.039(3) 0.043(3) -0.013(3) 0.000(3) -0.006(2) C4 0.039(3) 0.024(3) 0.039(4) -0.008(3) 0.005(3) -0.008(3) N4 0.135(5) 0.052(3) 0.091(4) -0.022(3) 0.054(3) -0.005(3) C5 0.034(3) 0.036(3) 0.028(3) -0.010(3) 0.005(2) -0.008(3) N5 0.077(5) 0.043(3) 0.098(5) -0.034(3) 0.036(4) -0.021(3) C6 0.034(3) 0.032(3) 0.034(3) -0.003(3) 0.004(3) -0.009(3) N6 0.029(3) 0.032(3) 0.033(3) -0.001(2) 0.002(2) -0.007(2) C7 0.050(4) 0.031(3) 0.027(3) -0.003(3) -0.011(3) -0.012(3) N7 0.041(3) 0.028(3) 0.041(3) -0.003(2) -0.008(2) -0.010(2) C8 0.067(5) 0.042(4) 0.051(4) -0.017(3) 0.000(4) -0.012(3) N8 0.036(3) 0.034(3) 0.035(3) -0.011(2) 0.001(2) -0.006(2) C9 0.092(7) 0.058(5) 0.074(6) -0.039(5) -0.016(5) -0.007(5) N9 0.074(4) 0.052(4) 0.081(5) -0.040(3) -0.033(4) 0.007(3) C10 0.093(7) 0.036(4) 0.081(6) -0.016(4) -0.027(5) -0.019(4) N10 0.109(6) 0.036(3) 0.071(5) -0.025(3) -0.007(4) -0.004(3) C11 0.080(6) 0.049(4) 0.059(5) 0.014(4) -0.024(4) -0.035(4) C12 0.065(5) 0.038(4) 0.041(4) 0.003(3) -0.013(3) -0.021(3) C13 0.031(3) 0.030(3) 0.028(3) -0.007(3) 0.001(2) -0.012(2) C14 0.038(4) 0.060(4) 0.035(4) -0.003(3) 0.002(3) -0.009(3) C15 0.033(4) 0.067(5) 0.051(5) -0.012(4) 0.009(3) 0.000(3) C16 0.059(5) 0.047(4) 0.045(4) -0.021(3) 0.021(3) -0.020(3) C17 0.065(5) 0.044(4) 0.029(3) -0.013(3) 0.011(3) -0.020(3) C18 0.039(3) 0.036(3) 0.033(3) -0.007(3) -0.001(3) -0.013(3) C19 0.120(5) 0.041(3) 0.084(4) -0.021(3) 0.055(4) -0.015(3) C20 0.123(5) 0.044(3) 0.085(4) -0.021(3) 0.059(4) -0.013(3) C21 0.029(3) 0.019(3) 0.039(3) -0.002(3) -0.002(3) -0.004(2) C22 0.035(3) 0.034(3) 0.035(3) -0.013(3) -0.003(3) -0.009(3) C23 0.033(3) 0.030(3) 0.028(3) 0.000(3) 0.004(2) -0.011(3) C24 0.039(3) 0.028(3) 0.031(3) -0.008(3) 0.001(3) -0.011(3) C25 0.035(3) 0.035(3) 0.035(3) -0.014(3) 0.005(3) -0.009(3) C26 0.033(3) 0.030(3) 0.029(3) 0.003(3) -0.007(3) -0.003(3) C27 0.044(4) 0.026(3) 0.028(3) -0.001(3) 0.005(3) -0.005(3) C28 0.055(4) 0.035(3) 0.038(4) -0.007(3) -0.003(3) -0.008(3) C29 0.098(6) 0.043(4) 0.043(4) -0.018(4) 0.014(4) -0.014(4) C30 0.078(6) 0.037(4) 0.049(5) -0.009(4) 0.014(4) 0.010(4) C31 0.065(5) 0.046(4) 0.044(4) 0.001(4) 0.004(4) 0.009(4) C32 0.052(4) 0.038(3) 0.033(4) -0.005(3) -0.001(3) 0.000(3) C33 0.025(3) 0.028(3) 0.029(3) -0.007(3) -0.001(2) 0.000(2) C34 0.044(4) 0.050(4) 0.033(4) -0.007(3) -0.001(3) -0.016(3) C35 0.051(4) 0.064(4) 0.029(4) -0.012(3) -0.001(3) -0.009(4) C36 0.048(4) 0.045(4) 0.049(4) -0.021(3) -0.017(3) -0.003(3) C37 0.062(5) 0.057(4) 0.056(5) -0.010(4) -0.011(4) -0.031(4) C38 0.057(4) 0.040(4) 0.040(4) -0.001(3) -0.007(3) -0.021(3) C39 0.024(3) 0.031(3) 0.041(4) 0.002(3) -0.004(3) 0.000(3) C40 0.060(5) 0.039(4) 0.047(4) -0.018(3) -0.011(3) -0.009(3) _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 C1 N1 1.345(7) . ? C1 C2 1.368(7) . ? C1 H1 0.9500 . ? N1 C5 1.343(6) . ? N1 Ag1 2.240(5) 2_557 ? P1 C13 1.821(6) . ? P1 C7 1.822(6) . ? P1 C6 1.871(6) . ? P1 Ag1 2.3825(18) . ? Ag1 N1 2.240(5) 2_557 ? Ag1 N3 2.502(5) . ? Ag1 N3 2.558(5) 2_657 ? Ag1 Ag1 3.3176(15) 2_657 ? C2 C3 1.403(7) . ? C2 H2 0.9500 . ? N2 C3 1.351(7) . ? N2 C6 1.446(7) . ? N2 H2A 0.8800 . ? P2 C33 1.821(5) . ? P2 C27 1.828(6) . ? P2 C26 1.871(6) . ? P2 Ag2 2.3924(18) . ? Ag2 N6 2.271(4) 2_656 ? Ag2 N8 2.518(5) . ? Ag2 N8 2.522(5) 2_556 ? Ag2 Ag2 3.2830(13) 2_556 ? C3 C4 1.409(7) . ? N3 C19 1.107(8) . ? N3 Ag1 2.558(5) 2_657 ? C4 C5 1.356(8) . ? C4 H4 0.9500 . ? N4 C19 1.319(10) . ? N4 C20 1.326(9) . ? C5 H5 0.9500 . ? N5 C20 1.096(8) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? N6 C21 1.343(7) . ? N6 C25 1.362(6) . ? N6 Ag2 2.271(4) 2_656 ? C7 C8 1.370(8) . ? C7 C12 1.402(9) . ? N7 C23 1.344(7) . ? N7 C26 1.459(7) . ? N7 H7 0.8800 . ? C8 C9 1.388(9) . ? C8 H8 0.9500 . ? N8 C39 1.154(7) . ? N8 Ag2 2.522(5) 2_556 ? C9 C10 1.370(12) . ? C9 H9 0.9500 . ? N9 C39 1.298(8) . ? N9 C40 1.320(8) . ? C10 C11 1.373(11) . ? C10 H10 0.9500 . ? N10 C40 1.127(7) . ? C11 C12 1.380(9) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.390(8) . ? C13 C18 1.391(7) . ? C14 C15 1.376(8) . ? C14 H14 0.9500 . ? C15 C16 1.380(9) . ? C15 H15 0.9500 . ? C16 C17 1.362(9) . ? C16 H16 0.9500 . ? C17 C18 1.399(8) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C21 C22 1.366(7) . ? C21 H21 0.9500 . ? C22 C23 1.399(7) . ? C22 H22 0.9500 . ? C23 C24 1.419(7) . ? C24 C25 1.365(7) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.384(8) . ? C27 C32 1.390(8) . ? C28 C29 1.401(8) . ? C28 H28 0.9500 . ? C29 C30 1.364(10) . ? C29 H29 0.9500 . ? C30 C31 1.371(9) . ? C30 H30 0.9500 . ? C31 C32 1.392(8) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C38 1.372(8) . ? C33 C34 1.395(8) . ? C34 C35 1.407(8) . ? C34 H34 0.9500 . ? C35 C36 1.364(9) . ? C35 H35 0.9500 . ? C36 C37 1.386(9) . ? C36 H36 0.9500 . ? C37 C38 1.387(8) . ? C37 H37 0.9500 . ? C38 H38 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 N1 C1 C2 125.5(5) . . ? N1 C1 H1 117.3 . . ? C2 C1 H1 117.3 . . ? C5 N1 C1 114.3(5) . . ? C5 N1 Ag1 123.5(4) . 2_557 ? C1 N1 Ag1 122.2(4) . 2_557 ? C13 P1 C7 104.5(3) . . ? C13 P1 C6 104.2(3) . . ? C7 P1 C6 102.7(3) . . ? C13 P1 Ag1 114.33(18) . . ? C7 P1 Ag1 112.11(19) . . ? C6 P1 Ag1 117.54(19) . . ? N1 Ag1 P1 149.34(12) 2_557 . ? N1 Ag1 N3 88.40(17) 2_557 . ? P1 Ag1 N3 111.73(13) . . ? N1 Ag1 N3 86.68(17) 2_557 2_657 ? P1 Ag1 N3 111.75(12) . 2_657 ? N3 Ag1 N3 98.07(15) . 2_657 ? N1 Ag1 Ag1 86.23(11) 2_557 2_657 ? P1 Ag1 Ag1 124.40(5) . 2_657 ? N3 Ag1 Ag1 49.77(12) . 2_657 ? N3 Ag1 Ag1 48.29(11) 2_657 2_657 ? C1 C2 C3 119.6(5) . . ? C1 C2 H2 120.2 . . ? C3 C2 H2 120.2 . . ? C3 N2 C6 124.2(4) . . ? C3 N2 H2A 117.9 . . ? C6 N2 H2A 117.9 . . ? C33 P2 C27 104.9(3) . . ? C33 P2 C26 103.7(3) . . ? C27 P2 C26 103.0(3) . . ? C33 P2 Ag2 114.47(18) . . ? C27 P2 Ag2 111.18(19) . . ? C26 P2 Ag2 118.19(18) . . ? N6 Ag2 P2 148.80(12) 2_656 . ? N6 Ag2 N8 87.79(16) 2_656 . ? P2 Ag2 N8 112.50(12) . . ? N6 Ag2 N8 86.01(16) 2_656 2_556 ? P2 Ag2 N8 112.46(11) . 2_556 ? N8 Ag2 N8 98.70(14) . 2_556 ? N6 Ag2 Ag2 85.24(12) 2_656 2_556 ? P2 Ag2 Ag2 125.94(5) . 2_556 ? N8 Ag2 Ag2 49.40(11) . 2_556 ? N8 Ag2 Ag2 49.30(11) 2_556 2_556 ? N2 C3 C2 124.0(5) . . ? N2 C3 C4 120.9(5) . . ? C2 C3 C4 115.1(5) . . ? C19 N3 Ag1 144.3(7) . . ? C19 N3 Ag1 133.3(7) . 2_657 ? Ag1 N3 Ag1 81.93(15) . 2_657 ? C5 C4 C3 120.4(5) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? C19 N4 C20 121.5(8) . . ? N1 C5 C4 125.1(5) . . ? N1 C5 H5 117.4 . . ? C4 C5 H5 117.4 . . ? N2 C6 P1 110.9(4) . . ? N2 C6 H6A 109.5 . . ? P1 C6 H6A 109.5 . . ? N2 C6 H6B 109.5 . . ? P1 C6 H6B 109.5 . . ? H6A C6 H6B 108.0 . . ? C21 N6 C25 114.7(5) . . ? C21 N6 Ag2 120.2(3) . 2_656 ? C25 N6 Ag2 125.1(4) . 2_656 ? C8 C7 C12 118.3(6) . . ? C8 C7 P1 119.4(5) . . ? C12 C7 P1 122.3(5) . . ? C23 N7 C26 125.0(5) . . ? C23 N7 H7 117.5 . . ? C26 N7 H7 117.5 . . ? C7 C8 C9 121.1(8) . . ? C7 C8 H8 119.4 . . ? C9 C8 H8 119.4 . . ? C39 N8 Ag2 137.9(5) . . ? C39 N8 Ag2 140.8(5) . 2_556 ? Ag2 N8 Ag2 81.30(14) . 2_556 ? C10 C9 C8 120.1(8) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C39 N9 C40 122.7(6) . . ? C9 C10 C11 119.8(7) . . ? C9 C10 H10 120.1 . . ? C11 C10 H10 120.1 . . ? C10 C11 C12 120.5(8) . . ? C10 C11 H11 119.8 . . ? C12 C11 H11 119.8 . . ? C11 C12 C7 120.2(7) . . ? C11 C12 H12 119.9 . . ? C7 C12 H12 119.9 . . ? C14 C13 C18 118.9(6) . . ? C14 C13 P1 117.1(4) . . ? C18 C13 P1 123.9(4) . . ? C15 C14 C13 120.8(6) . . ? C15 C14 H14 119.6 . . ? C13 C14 H14 119.6 . . ? C14 C15 C16 119.9(6) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? C17 C16 C15 120.4(6) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C16 C17 C18 120.3(6) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C13 C18 C17 119.7(6) . . ? C13 C18 H18 120.2 . . ? C17 C18 H18 120.2 . . ? N3 C19 N4 164.7(11) . . ? N5 C20 N4 164.5(11) . . ? N6 C21 C22 125.9(5) . . ? N6 C21 H21 117.0 . . ? C22 C21 H21 117.0 . . ? C21 C22 C23 119.3(5) . . ? C21 C22 H22 120.3 . . ? C23 C22 H22 120.3 . . ? N7 C23 C22 123.8(5) . . ? N7 C23 C24 120.4(5) . . ? C22 C23 C24 115.7(5) . . ? C25 C24 C23 120.3(5) . . ? C25 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? N6 C25 C24 123.8(5) . . ? N6 C25 H25 118.1 . . ? C24 C25 H25 118.1 . . ? N7 C26 P2 111.9(4) . . ? N7 C26 H26A 109.2 . . ? P2 C26 H26A 109.2 . . ? N7 C26 H26B 109.2 . . ? P2 C26 H26B 109.2 . . ? H26A C26 H26B 107.9 . . ? C28 C27 C32 119.5(5) . . ? C28 C27 P2 118.4(4) . . ? C32 C27 P2 122.0(5) . . ? C27 C28 C29 120.4(6) . . ? C27 C28 H28 119.8 . . ? C29 C28 H28 119.8 . . ? C30 C29 C28 119.4(7) . . ? C30 C29 H29 120.3 . . ? C28 C29 H29 120.3 . . ? C29 C30 C31 120.9(6) . . ? C29 C30 H30 119.5 . . ? C31 C30 H30 119.5 . . ? C30 C31 C32 120.4(7) . . ? C30 C31 H31 119.8 . . ? C32 C31 H31 119.8 . . ? C27 C32 C31 119.4(6) . . ? C27 C32 H32 120.3 . . ? C31 C32 H32 120.3 . . ? C38 C33 C34 118.4(6) . . ? C38 C33 P2 117.9(5) . . ? C34 C33 P2 123.7(5) . . ? C33 C34 C35 120.6(6) . . ? C33 C34 H34 119.7 . . ? C35 C34 H34 119.7 . . ? C36 C35 C34 119.8(6) . . ? C36 C35 H35 120.1 . . ? C34 C35 H35 120.1 . . ? C35 C36 C37 119.7(6) . . ? C35 C36 H36 120.1 . . ? C37 C36 H36 120.1 . . ? C36 C37 C38 120.4(7) . . ? C36 C37 H37 119.8 . . ? C38 C37 H37 119.8 . . ? C33 C38 C37 121.0(6) . . ? C33 C38 H38 119.5 . . ? C37 C38 H38 119.5 . . ? N8 C39 N9 173.6(6) . . ? N10 C40 N9 172.7(7) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2A N5 0.88 2.11 2.987(7) 175.1 1_465 N7 H7 N10 0.88 2.10 2.967(7) 170.4 1_565 _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 1.245 _refine_diff_density_min -1.288 _refine_diff_density_rms 0.110 #==END #========================================================================== data_[Ag2(SCN)2(dppmapy)2]n _database_code_depnum_ccdc_archive 'CCDC 748197' #TrackingRef 'JPLangCIF.cif' #========================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H17 Ag N3 P S' _chemical_formula_sum 'C19 H17 Ag N3 P S' _chemical_formula_weight 458.27 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' 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 10.096(2) _cell_length_b 12.572(3) _cell_length_c 15.349(3) _cell_angle_alpha 100.99(3) _cell_angle_beta 99.51(3) _cell_angle_gamma 90.38(3) _cell_volume 1884.7(7) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 7332 _cell_measurement_theta_min 3.1328 _cell_measurement_theta_max 27.4855 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.615 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 920 _exptl_absorpt_coefficient_mu 1.271 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7501 _exptl_absorpt_correction_T_max 0.9392 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'Rigaku MercuryCCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 17270 _diffrn_reflns_av_R_equivalents 0.0371 _diffrn_reflns_av_sigmaI/netI 0.0676 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 27.48 _reflns_number_total 8453 _reflns_number_gt 5919 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_cell_refinement 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_data_reduction 'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material SHELXL97 _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^)+(0.0715P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8453 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0872 _refine_ls_R_factor_gt 0.0555 _refine_ls_wR_factor_ref 0.1385 _refine_ls_wR_factor_gt 0.1227 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _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 C1 C -0.6202(5) -0.0581(4) 0.1551(4) 0.0402(12) Uani 1 1 d . . . H1 H -0.6640 -0.1132 0.1745 0.048 Uiso 1 1 calc R . . N1 N -0.6961(4) 0.0052(4) 0.1071(3) 0.0395(10) Uani 1 1 d . . . P1 P -0.01300(12) 0.02726(10) 0.23498(8) 0.0295(3) Uani 1 1 d . . . S1 S 0.02789(13) 0.17399(11) 0.01552(9) 0.0367(3) Uani 1 1 d . . . Ag1 Ag 0.07643(4) 0.00071(3) 0.09542(2) 0.03799(13) Uani 1 1 d . . . C2 C -0.4810(5) -0.0472(4) 0.1776(3) 0.0353(11) Uani 1 1 d . . . H2A H -0.4334 -0.0925 0.2129 0.042 Uiso 1 1 calc R . . N2 N -0.2785(4) 0.0501(4) 0.1693(3) 0.0382(10) Uani 1 1 d . . . H2 H -0.2421 0.0976 0.1450 0.046 Uiso 1 1 calc R . . P2 P 0.36493(12) 0.48174(10) 0.76340(8) 0.0298(3) Uani 1 1 d . . . S2 S 0.51724(13) 0.32727(10) 0.97538(9) 0.0363(3) Uani 1 1 d . . . Ag2 Ag 0.52435(4) 0.51040(3) 0.90325(2) 0.03701(13) Uani 1 1 d . . . C3 C -0.4131(4) 0.0312(4) 0.1476(3) 0.0317(11) Uani 1 1 d . . . N3 N -0.2547(4) 0.5040(4) 0.8887(3) 0.0383(10) Uani 1 1 d . . . C4 C -0.4916(5) 0.0952(4) 0.0946(3) 0.0336(11) Uani 1 1 d . . . H4A H -0.4503 0.1485 0.0717 0.040 Uiso 1 1 calc R . . N4 N 0.1317(4) 0.4568(3) 0.8279(3) 0.0387(10) Uani 1 1 d . . . H4 H 0.1801 0.4095 0.8520 0.046 Uiso 1 1 calc R . . C5 C -0.6272(5) 0.0795(4) 0.0768(3) 0.0359(11) Uani 1 1 d . . . H5 H -0.6769 0.1232 0.0410 0.043 Uiso 1 1 calc R . . N5 N -0.1894(5) 0.2454(4) 0.1037(3) 0.0483(12) Uani 1 1 d . . . C6 C -0.1918(5) -0.0040(4) 0.2302(3) 0.0341(11) Uani 1 1 d . . . H6A H -0.2089 -0.0825 0.2113 0.041 Uiso 1 1 calc R . . H6B H -0.2141 0.0174 0.2907 0.041 Uiso 1 1 calc R . . N6 N 0.2531(5) 0.2585(4) 0.8876(3) 0.0476(11) Uani 1 1 d . . . C7 C 0.0559(4) -0.0642(4) 0.3078(3) 0.0309(10) Uani 1 1 d . . . C8 C 0.0936(6) -0.0337(5) 0.4011(4) 0.0465(14) Uani 1 1 d . . . H8 H 0.0864 0.0387 0.4295 0.056 Uiso 1 1 calc R . . C9 C 0.1414(7) -0.1092(5) 0.4516(4) 0.0564(17) Uani 1 1 d . . . H9 H 0.1659 -0.0874 0.5144 0.068 Uiso 1 1 calc R . . C10 C 0.1541(6) -0.2149(5) 0.4127(4) 0.0481(14) Uani 1 1 d . . . H10 H 0.1863 -0.2655 0.4482 0.058 Uiso 1 1 calc R . . C11 C 0.1190(6) -0.2462(5) 0.3208(4) 0.0500(14) Uani 1 1 d . . . H11 H 0.1276 -0.3187 0.2932 0.060 Uiso 1 1 calc R . . C12 C 0.0713(6) -0.1718(4) 0.2689(4) 0.0463(13) Uani 1 1 d . . . H12 H 0.0489 -0.1942 0.2061 0.056 Uiso 1 1 calc R . . C13 C 0.0209(5) 0.1607(4) 0.3054(3) 0.0316(10) Uani 1 1 d . . . C14 C 0.1520(6) 0.2051(5) 0.3188(4) 0.0461(14) Uani 1 1 d . . . H14 H 0.2178 0.1665 0.2906 0.055 Uiso 1 1 calc R . . C15 C 0.1846(6) 0.3059(5) 0.3734(4) 0.0551(16) Uani 1 1 d . . . H15 H 0.2734 0.3344 0.3837 0.066 Uiso 1 1 calc R . . C16 C 0.0872(6) 0.3654(5) 0.4132(4) 0.0518(15) Uani 1 1 d . . . H16 H 0.1100 0.4338 0.4502 0.062 Uiso 1 1 calc R . . C17 C -0.0409(6) 0.3243(5) 0.3984(4) 0.0456(14) Uani 1 1 d . . . H17 H -0.1070 0.3650 0.4246 0.055 Uiso 1 1 calc R . . C18 C -0.0751(5) 0.2224(4) 0.3448(4) 0.0397(12) Uani 1 1 d . . . H18 H -0.1643 0.1949 0.3351 0.048 Uiso 1 1 calc R . . C19 C -0.2011(5) 0.5645(4) 0.8405(4) 0.0430(13) Uani 1 1 d . . . H19 H -0.2536 0.6193 0.8204 0.052 Uiso 1 1 calc R . . C20 C -0.0744(5) 0.5537(4) 0.8175(3) 0.0353(11) Uani 1 1 d . . . H20 H -0.0439 0.5977 0.7812 0.042 Uiso 1 1 calc R . . C21 C 0.0068(5) 0.4753(4) 0.8498(3) 0.0322(11) Uani 1 1 d . . . C22 C -0.0450(5) 0.4129(4) 0.9022(3) 0.0338(11) Uani 1 1 d . . . H22 H 0.0076 0.3601 0.9257 0.041 Uiso 1 1 calc R . . C23 C -0.1729(5) 0.4280(4) 0.9201(3) 0.0355(11) Uani 1 1 d . . . H23 H -0.2061 0.3842 0.9556 0.043 Uiso 1 1 calc R . . C24 C 0.1878(5) 0.5120(4) 0.7667(3) 0.0337(11) Uani 1 1 d . . . H24A H 0.1804 0.5904 0.7855 0.040 Uiso 1 1 calc R . . H24B H 0.1354 0.4900 0.7060 0.040 Uiso 1 1 calc R . . C25 C 0.3653(5) 0.3468(4) 0.6954(3) 0.0324(11) Uani 1 1 d . . . C26 C 0.2496(6) 0.2871(5) 0.6495(4) 0.0480(14) Uani 1 1 d . . . H26 H 0.1650 0.3170 0.6526 0.058 Uiso 1 1 calc R . . C27 C 0.2580(7) 0.1839(6) 0.5994(4) 0.0628(18) Uani 1 1 d . . . H27 H 0.1787 0.1442 0.5699 0.075 Uiso 1 1 calc R . . C28 C 0.3796(8) 0.1391(5) 0.5923(4) 0.0590(17) Uani 1 1 d . . . H28 H 0.3844 0.0701 0.5565 0.071 Uiso 1 1 calc R . . C29 C 0.4958(7) 0.1967(5) 0.6386(4) 0.0552(17) Uani 1 1 d . . . H29 H 0.5798 0.1661 0.6347 0.066 Uiso 1 1 calc R . . C30 C 0.4890(6) 0.2995(4) 0.6909(4) 0.0432(13) Uani 1 1 d . . . H30 H 0.5682 0.3370 0.7233 0.052 Uiso 1 1 calc R . . C31 C 0.3969(5) 0.5713(4) 0.6876(3) 0.0320(11) Uani 1 1 d . . . C32 C 0.3811(5) 0.5395(5) 0.5942(3) 0.0395(12) Uani 1 1 d . . . H32 H 0.3550 0.4673 0.5671 0.047 Uiso 1 1 calc R . . C33 C 0.4033(6) 0.6127(5) 0.5410(4) 0.0489(15) Uani 1 1 d . . . H33 H 0.3920 0.5898 0.4781 0.059 Uiso 1 1 calc R . . C34 C 0.4416(6) 0.7181(5) 0.5787(4) 0.0503(16) Uani 1 1 d . . . H34 H 0.4561 0.7675 0.5421 0.060 Uiso 1 1 calc R . . C35 C 0.4589(6) 0.7519(5) 0.6723(4) 0.0474(14) Uani 1 1 d . . . H35 H 0.4854 0.8241 0.6991 0.057 Uiso 1 1 calc R . . C36 C 0.4366(6) 0.6776(5) 0.7252(4) 0.0428(13) Uani 1 1 d . . . H36 H 0.4488 0.7004 0.7881 0.051 Uiso 1 1 calc R . . C37 C -0.1012(5) 0.2147(4) 0.0673(4) 0.0388(12) Uani 1 1 d . . . C38 C 0.3601(6) 0.2884(4) 0.9240(4) 0.0362(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.027(3) 0.042(3) 0.055(3) 0.018(3) 0.007(2) 0.003(2) N1 0.025(2) 0.044(3) 0.048(3) 0.008(2) 0.0029(19) 0.0073(19) P1 0.0252(6) 0.0346(7) 0.0278(6) 0.0058(5) 0.0019(5) 0.0015(5) S1 0.0348(7) 0.0353(7) 0.0419(7) 0.0105(6) 0.0083(6) 0.0017(5) Ag1 0.0296(2) 0.0506(3) 0.0346(2) 0.00928(18) 0.00630(16) 0.00679(18) C2 0.027(3) 0.036(3) 0.041(3) 0.006(2) 0.002(2) 0.004(2) N2 0.024(2) 0.043(3) 0.050(3) 0.020(2) 0.0021(19) 0.0008(19) P2 0.0256(6) 0.0342(7) 0.0289(6) 0.0034(5) 0.0056(5) 0.0006(5) S2 0.0340(7) 0.0339(7) 0.0416(7) 0.0084(6) 0.0064(6) 0.0033(5) Ag2 0.0289(2) 0.0477(3) 0.0341(2) 0.00780(18) 0.00471(16) -0.00193(17) C3 0.019(2) 0.037(3) 0.044(3) 0.018(2) 0.005(2) 0.002(2) N3 0.022(2) 0.048(3) 0.048(3) 0.014(2) 0.0091(19) 0.0026(19) C4 0.026(3) 0.040(3) 0.037(3) 0.012(2) 0.005(2) 0.004(2) N4 0.030(2) 0.040(2) 0.053(3) 0.019(2) 0.015(2) 0.0075(19) C5 0.031(3) 0.037(3) 0.039(3) 0.009(2) 0.003(2) 0.008(2) N5 0.041(3) 0.038(3) 0.068(3) 0.010(2) 0.016(3) -0.002(2) C6 0.027(3) 0.036(3) 0.041(3) 0.013(2) 0.003(2) 0.001(2) N6 0.041(3) 0.041(3) 0.058(3) 0.010(2) 0.001(2) 0.002(2) C7 0.017(2) 0.039(3) 0.030(2) -0.003(2) -0.0015(19) -0.005(2) C8 0.058(4) 0.042(3) 0.038(3) 0.006(2) 0.004(3) 0.009(3) C9 0.069(4) 0.066(4) 0.031(3) 0.011(3) -0.004(3) 0.014(3) C10 0.047(3) 0.049(3) 0.050(3) 0.020(3) 0.000(3) 0.006(3) C11 0.053(4) 0.036(3) 0.056(4) 0.009(3) -0.003(3) 0.005(3) C12 0.049(3) 0.040(3) 0.041(3) 0.003(2) -0.009(3) -0.001(3) C13 0.027(3) 0.034(3) 0.032(2) 0.004(2) 0.001(2) 0.002(2) C14 0.038(3) 0.040(3) 0.061(4) 0.004(3) 0.016(3) 0.004(3) C15 0.041(3) 0.044(3) 0.074(4) 0.006(3) -0.003(3) -0.004(3) C16 0.059(4) 0.038(3) 0.051(3) 0.003(3) -0.006(3) 0.005(3) C17 0.048(4) 0.039(3) 0.048(3) 0.004(3) 0.009(3) 0.012(3) C18 0.029(3) 0.049(3) 0.046(3) 0.017(3) 0.010(2) 0.005(2) C19 0.030(3) 0.041(3) 0.061(4) 0.015(3) 0.009(3) 0.009(2) C20 0.032(3) 0.036(3) 0.043(3) 0.016(2) 0.013(2) 0.002(2) C21 0.025(2) 0.028(2) 0.046(3) 0.005(2) 0.014(2) 0.003(2) C22 0.030(3) 0.038(3) 0.037(3) 0.016(2) 0.005(2) 0.003(2) C23 0.029(3) 0.038(3) 0.043(3) 0.016(2) 0.008(2) -0.003(2) C24 0.026(2) 0.041(3) 0.038(3) 0.012(2) 0.014(2) 0.005(2) C25 0.034(3) 0.037(3) 0.027(2) 0.008(2) 0.006(2) -0.002(2) C26 0.038(3) 0.049(3) 0.052(3) 0.000(3) 0.006(3) -0.001(3) C27 0.070(5) 0.056(4) 0.054(4) -0.012(3) 0.012(3) -0.020(3) C28 0.087(5) 0.042(3) 0.048(3) -0.001(3) 0.024(4) 0.000(4) C29 0.064(4) 0.042(3) 0.066(4) 0.010(3) 0.029(3) 0.018(3) C30 0.040(3) 0.041(3) 0.052(3) 0.013(3) 0.015(3) 0.004(3) C31 0.024(2) 0.036(3) 0.039(3) 0.011(2) 0.007(2) 0.004(2) C32 0.040(3) 0.046(3) 0.031(3) 0.005(2) 0.004(2) 0.007(2) C33 0.051(4) 0.060(4) 0.042(3) 0.017(3) 0.018(3) 0.018(3) C34 0.049(4) 0.054(4) 0.061(4) 0.030(3) 0.025(3) 0.013(3) C35 0.045(3) 0.040(3) 0.061(4) 0.015(3) 0.015(3) 0.000(3) C36 0.046(3) 0.044(3) 0.041(3) 0.011(2) 0.012(3) 0.000(3) C37 0.036(3) 0.032(3) 0.050(3) 0.016(2) 0.004(3) -0.006(2) C38 0.038(3) 0.031(3) 0.041(3) 0.007(2) 0.008(2) 0.003(2) _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 C1 N1 1.344(6) . ? C1 C2 1.390(7) . ? C1 H1 0.9400 . ? N1 C5 1.354(7) . ? N1 Ag1 2.274(4) 1_455 ? P1 C13 1.810(5) . ? P1 C7 1.816(5) . ? P1 C6 1.832(5) . ? P1 Ag1 2.4260(13) . ? S1 C37 1.670(5) . ? S1 Ag1 2.6045(18) 2 ? S1 Ag1 2.7064(15) . ? Ag1 N1 2.274(4) 1_655 ? Ag1 S1 2.6045(18) 2 ? Ag1 Ag1 3.0738(12) 2 ? C2 C3 1.387(7) . ? C2 H2A 0.9400 . ? N2 C3 1.353(6) . ? N2 C6 1.443(6) . ? N2 H2 0.8700 . ? P2 C25 1.815(5) . ? P2 C31 1.829(5) . ? P2 C24 1.838(5) . ? P2 Ag2 2.4256(16) . ? S2 C38 1.676(6) . ? S2 Ag2 2.5754(16) 2_667 ? S2 Ag2 2.7436(15) . ? Ag2 N3 2.278(4) 1_655 ? Ag2 S2 2.5754(16) 2_667 ? Ag2 Ag2 3.1477(10) 2_667 ? C3 C4 1.407(6) . ? N3 C19 1.326(7) . ? N3 C23 1.372(6) . ? N3 Ag2 2.278(4) 1_455 ? C4 C5 1.357(7) . ? C4 H4A 0.9400 . ? N4 C21 1.368(6) . ? N4 C24 1.451(6) . ? N4 H4 0.8700 . ? C5 H5 0.9400 . ? N5 C37 1.157(6) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? N6 C38 1.155(7) . ? C7 C12 1.392(7) . ? C7 C8 1.396(7) . ? C8 C9 1.378(8) . ? C8 H8 0.9400 . ? C9 C10 1.366(8) . ? C9 H9 0.9400 . ? C10 C11 1.375(8) . ? C10 H10 0.9400 . ? C11 C12 1.380(7) . ? C11 H11 0.9400 . ? C12 H12 0.9400 . ? C13 C18 1.391(6) . ? C13 C14 1.400(7) . ? C14 C15 1.384(8) . ? C14 H14 0.9400 . ? C15 C16 1.390(8) . ? C15 H15 0.9400 . ? C16 C17 1.356(9) . ? C16 H16 0.9400 . ? C17 C18 1.392(8) . ? C17 H17 0.9400 . ? C18 H18 0.9400 . ? C19 C20 1.383(7) . ? C19 H19 0.9400 . ? C20 C21 1.396(6) . ? C20 H20 0.9400 . ? C21 C22 1.383(6) . ? C22 C23 1.371(6) . ? C22 H22 0.9400 . ? C23 H23 0.9400 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C25 C26 1.392(8) . ? C25 C30 1.394(7) . ? C26 C27 1.386(8) . ? C26 H26 0.9400 . ? C27 C28 1.367(9) . ? C27 H27 0.9400 . ? C28 C29 1.386(10) . ? C28 H28 0.9400 . ? C29 C30 1.394(8) . ? C29 H29 0.9400 . ? C30 H30 0.9400 . ? C31 C36 1.379(7) . ? C31 C32 1.394(7) . ? C32 C33 1.382(8) . ? C32 H32 0.9400 . ? C33 C34 1.366(9) . ? C33 H33 0.9400 . ? C34 C35 1.399(8) . ? C34 H34 0.9400 . ? C35 C36 1.388(7) . ? C35 H35 0.9400 . ? C36 H36 0.9400 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 124.1(5) . . ? N1 C1 H1 117.9 . . ? C2 C1 H1 117.9 . . ? C1 N1 C5 115.4(4) . . ? C1 N1 Ag1 121.0(3) . 1_455 ? C5 N1 Ag1 123.1(3) . 1_455 ? C13 P1 C7 104.0(2) . . ? C13 P1 C6 105.8(2) . . ? C7 P1 C6 98.4(2) . . ? C13 P1 Ag1 115.08(16) . . ? C7 P1 Ag1 112.62(15) . . ? C6 P1 Ag1 118.75(17) . . ? C37 S1 Ag1 101.3(2) . 2 ? C37 S1 Ag1 94.96(18) . . ? Ag1 S1 Ag1 70.70(4) 2 . ? N1 Ag1 P1 116.90(12) 1_655 . ? N1 Ag1 S1 110.19(12) 1_655 2 ? P1 Ag1 S1 111.51(5) . 2 ? N1 Ag1 S1 97.83(12) 1_655 . ? P1 Ag1 S1 110.17(5) . . ? S1 Ag1 S1 109.30(4) 2 . ? N1 Ag1 Ag1 114.35(11) 1_655 2 ? P1 Ag1 Ag1 127.90(4) . 2 ? S1 Ag1 Ag1 56.20(4) 2 2 ? S1 Ag1 Ag1 53.10(4) . 2 ? C3 C2 C1 119.3(5) . . ? C3 C2 H2A 120.3 . . ? C1 C2 H2A 120.3 . . ? C3 N2 C6 123.8(4) . . ? C3 N2 H2 118.1 . . ? C6 N2 H2 118.1 . . ? C25 P2 C31 103.7(2) . . ? C25 P2 C24 106.4(2) . . ? C31 P2 C24 98.0(2) . . ? C25 P2 Ag2 113.95(16) . . ? C31 P2 Ag2 113.52(18) . . ? C24 P2 Ag2 119.15(17) . . ? C38 S2 Ag2 101.56(17) . 2_667 ? C38 S2 Ag2 94.73(18) . . ? Ag2 S2 Ag2 72.49(4) 2_667 . ? N3 Ag2 P2 115.67(12) 1_655 . ? N3 Ag2 S2 111.32(12) 1_655 2_667 ? P2 Ag2 S2 115.90(5) . 2_667 ? N3 Ag2 S2 96.24(11) 1_655 . ? P2 Ag2 S2 107.97(5) . . ? S2 Ag2 S2 107.51(4) 2_667 . ? N3 Ag2 Ag2 113.09(11) 1_655 2_667 ? P2 Ag2 Ag2 128.77(4) . 2_667 ? S2 Ag2 Ag2 56.22(4) 2_667 2_667 ? S2 Ag2 Ag2 51.28(4) . 2_667 ? N2 C3 C2 123.2(4) . . ? N2 C3 C4 120.0(4) . . ? C2 C3 C4 116.8(4) . . ? C19 N3 C23 115.5(4) . . ? C19 N3 Ag2 122.3(3) . 1_455 ? C23 N3 Ag2 121.8(3) . 1_455 ? C5 C4 C3 119.7(5) . . ? C5 C4 H4A 120.1 . . ? C3 C4 H4A 120.1 . . ? C21 N4 C24 123.4(4) . . ? C21 N4 H4 118.3 . . ? C24 N4 H4 118.3 . . ? N1 C5 C4 124.5(4) . . ? N1 C5 H5 117.7 . . ? C4 C5 H5 117.7 . . ? N2 C6 P1 113.1(3) . . ? N2 C6 H6A 109.0 . . ? P1 C6 H6A 109.0 . . ? N2 C6 H6B 109.0 . . ? P1 C6 H6B 109.0 . . ? H6A C6 H6B 107.8 . . ? C12 C7 C8 117.5(5) . . ? C12 C7 P1 118.4(4) . . ? C8 C7 P1 124.2(4) . . ? C9 C8 C7 120.3(5) . . ? C9 C8 H8 119.8 . . ? C7 C8 H8 119.8 . . ? C10 C9 C8 121.5(5) . . ? C10 C9 H9 119.2 . . ? C8 C9 H9 119.2 . . ? C9 C10 C11 119.0(5) . . ? C9 C10 H10 120.5 . . ? C11 C10 H10 120.5 . . ? C10 C11 C12 120.4(5) . . ? C10 C11 H11 119.8 . . ? C12 C11 H11 119.8 . . ? C11 C12 C7 121.3(5) . . ? C11 C12 H12 119.4 . . ? C7 C12 H12 119.4 . . ? C18 C13 C14 118.3(5) . . ? C18 C13 P1 124.3(4) . . ? C14 C13 P1 117.4(4) . . ? C15 C14 C13 120.1(5) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C14 C15 C16 120.5(6) . . ? C14 C15 H15 119.7 . . ? C16 C15 H15 119.7 . . ? C17 C16 C15 119.8(6) . . ? C17 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? C16 C17 C18 120.5(5) . . ? C16 C17 H17 119.7 . . ? C18 C17 H17 119.7 . . ? C13 C18 C17 120.8(5) . . ? C13 C18 H18 119.6 . . ? C17 C18 H18 119.6 . . ? N3 C19 C20 125.5(5) . . ? N3 C19 H19 117.3 . . ? C20 C19 H19 117.3 . . ? C19 C20 C21 118.0(4) . . ? C19 C20 H20 121.0 . . ? C21 C20 H20 121.0 . . ? N4 C21 C22 120.2(4) . . ? N4 C21 C20 121.8(4) . . ? C22 C21 C20 117.9(4) . . ? C23 C22 C21 120.0(4) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C22 C23 N3 123.1(4) . . ? C22 C23 H23 118.4 . . ? N3 C23 H23 118.4 . . ? N4 C24 P2 112.2(3) . . ? N4 C24 H24A 109.2 . . ? P2 C24 H24A 109.2 . . ? N4 C24 H24B 109.2 . . ? P2 C24 H24B 109.2 . . ? H24A C24 H24B 107.9 . . ? C26 C25 C30 118.3(5) . . ? C26 C25 P2 124.0(4) . . ? C30 C25 P2 117.7(4) . . ? C27 C26 C25 120.6(6) . . ? C27 C26 H26 119.7 . . ? C25 C26 H26 119.7 . . ? C28 C27 C26 121.1(6) . . ? C28 C27 H27 119.5 . . ? C26 C27 H27 119.5 . . ? C27 C28 C29 119.1(6) . . ? C27 C28 H28 120.4 . . ? C29 C28 H28 120.4 . . ? C28 C29 C30 120.6(6) . . ? C28 C29 H29 119.7 . . ? C30 C29 H29 119.7 . . ? C25 C30 C29 120.3(6) . . ? C25 C30 H30 119.9 . . ? C29 C30 H30 119.9 . . ? C36 C31 C32 118.0(5) . . ? C36 C31 P2 117.8(4) . . ? C32 C31 P2 124.2(4) . . ? C33 C32 C31 120.9(5) . . ? C33 C32 H32 119.6 . . ? C31 C32 H32 119.6 . . ? C34 C33 C32 120.7(5) . . ? C34 C33 H33 119.7 . . ? C32 C33 H33 119.7 . . ? C33 C34 C35 119.5(5) . . ? C33 C34 H34 120.2 . . ? C35 C34 H34 120.2 . . ? C36 C35 C34 119.3(6) . . ? C36 C35 H35 120.3 . . ? C34 C35 H35 120.3 . . ? C31 C36 C35 121.5(5) . . ? C31 C36 H36 119.2 . . ? C35 C36 H36 119.2 . . ? N5 C37 S1 178.4(5) . . ? N6 C38 S2 177.9(5) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2 N5 0.87 2.16 3.010(6) 163.9 . N4 H4 N6 0.87 2.17 3.016(6) 162.8 . N2 H2 N5 0.87 2.16 3.010(6) 163.9 . N4 H4 N6 0.87 2.17 3.016(6) 162.8 . _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 2.447 _refine_diff_density_min -0.806 _refine_diff_density_rms 0.121