# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_1^.^CH~2~Cl~2~^.^H~2~O _database_code_depnum_ccdc_archive 'CCDC 865925' #TrackingRef 'cif.cif' #============================================================================== # CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C58 H58 Ag2 Cl2 N4 O8 P4, 2(Cl O4), C H2 Cl2, H2 O' _chemical_formula_sum 'C59 H62 Ag2 Cl6 N4 O17 P4' _chemical_formula_weight 1651.45 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 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 24.496(5) _cell_length_b 15.496(3) _cell_length_c 19.454(4) _cell_angle_alpha 90.00 _cell_angle_beta 112.31(3) _cell_angle_gamma 90.00 _cell_volume 6832(2) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 14883 _cell_measurement_theta_min 3.0000 _cell_measurement_theta_max 27.4849 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.606 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3344 _exptl_absorpt_coefficient_mu 0.971 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7627 _exptl_absorpt_correction_T_max 1.0000 _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 Mercury' _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 30018 _diffrn_reflns_av_R_equivalents 0.0599 _diffrn_reflns_av_sigmaI/netI 0.1447 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 27.48 _reflns_number_total 15343 _reflns_number_gt 10732 _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 'SHELXS-97 (Sheldrick, 1990)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0342P)^2^+19.1949P] 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 15343 _refine_ls_number_parameters 824 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.1590 _refine_ls_R_factor_gt 0.1150 _refine_ls_wR_factor_ref 0.2029 _refine_ls_wR_factor_gt 0.1837 _refine_ls_goodness_of_fit_ref 1.232 _refine_ls_restrained_S_all 1.241 _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 0.34854(3) 0.38600(4) 0.58386(4) 0.03806(17) Uani 1 1 d . . . Ag2 Ag 0.15525(3) 0.27824(4) 0.40855(4) 0.04383(19) Uani 1 1 d . . . P1 P 0.37465(9) 0.53576(13) 0.57526(12) 0.0324(5) Uani 1 1 d . . . P2 P 0.10633(9) 0.39312(14) 0.32422(12) 0.0377(5) Uani 1 1 d . . . P3 P 0.12872(9) 0.12916(14) 0.41771(12) 0.0362(5) Uani 1 1 d . . . P4 P 0.39459(9) 0.27434(13) 0.67317(12) 0.0323(5) Uani 1 1 d . . . N1 N 0.2766(3) 0.5696(4) 0.4503(4) 0.0335(15) Uani 1 1 d . . . N2 N 0.1921(3) 0.5199(4) 0.3733(4) 0.0338(15) Uani 1 1 d . . . N3 N 0.2266(3) 0.0970(4) 0.5440(4) 0.0310(14) Uani 1 1 d . . . N4 N 0.3097(3) 0.1473(4) 0.6240(4) 0.0347(15) Uani 1 1 d . . . C1 C 0.3397(3) 0.5844(5) 0.4821(4) 0.0295(16) Uani 1 1 d . . . H1A H 0.3472 0.6466 0.4857 0.035 Uiso 1 1 calc R . . H1B H 0.3575 0.5599 0.4492 0.035 Uiso 1 1 calc R . . C2 C 0.2336(3) 0.6160(6) 0.4733(5) 0.046(2) Uani 1 1 d . . . H2A H 0.2367 0.6786 0.4683 0.055 Uiso 1 1 calc R . . H2B H 0.2394 0.6024 0.5248 0.055 Uiso 1 1 calc R . . C3 C 0.1737(4) 0.5818(6) 0.4187(6) 0.050(2) Uani 1 1 d . . . H3A H 0.1518 0.5528 0.4449 0.060 Uiso 1 1 calc R . . H3B H 0.1495 0.6283 0.3880 0.060 Uiso 1 1 calc R . . C4 C 0.2497(3) 0.5182(5) 0.3949(4) 0.0326(17) Uani 1 1 d . . . H4 H 0.2696 0.4832 0.3725 0.039 Uiso 1 1 calc R . . C5 C 0.1515(4) 0.4780(5) 0.3062(4) 0.040(2) Uani 1 1 d . . . H5A H 0.1744 0.4527 0.2794 0.048 Uiso 1 1 calc R . . H5B H 0.1253 0.5218 0.2739 0.048 Uiso 1 1 calc R . . C6 C 0.4523(3) 0.5525(5) 0.5953(4) 0.0357(18) Uani 1 1 d . . . C7 C 0.4920(4) 0.4897(6) 0.6338(5) 0.052(2) Uani 1 1 d . . . H7 H 0.4782 0.4398 0.6494 0.063 Uiso 1 1 calc R . . C8 C 0.5526(4) 0.4988(7) 0.6502(6) 0.061(3) Uani 1 1 d . . . H8 H 0.5789 0.4548 0.6757 0.073 Uiso 1 1 calc R . . C9 C 0.5729(4) 0.5712(6) 0.6292(5) 0.049(2) Uani 1 1 d . . . H9 H 0.6136 0.5778 0.6411 0.059 Uiso 1 1 calc R . . C10 C 0.5345(4) 0.6357(6) 0.5904(5) 0.049(2) Uani 1 1 d . . . H10 H 0.5489 0.6853 0.5750 0.058 Uiso 1 1 calc R . . C11 C 0.4749(4) 0.6265(6) 0.5745(5) 0.049(2) Uani 1 1 d . . . H11 H 0.4489 0.6709 0.5492 0.059 Uiso 1 1 calc R . . C12 C 0.3555(3) 0.6048(5) 0.6375(4) 0.0369(18) Uani 1 1 d . . . C13 C 0.3637(4) 0.6950(5) 0.6401(5) 0.046(2) Uani 1 1 d . . . H13 H 0.3787 0.7215 0.6075 0.056 Uiso 1 1 calc R . . C14 C 0.3499(4) 0.7445(7) 0.6898(6) 0.057(3) Uani 1 1 d . . . H14 H 0.3556 0.8046 0.6910 0.069 Uiso 1 1 calc R . . C15 C 0.3279(4) 0.7068(7) 0.7378(6) 0.062(3) Uani 1 1 d . . . H15 H 0.3186 0.7411 0.7717 0.075 Uiso 1 1 calc R . . C16 C 0.3196(4) 0.6198(7) 0.7364(6) 0.058(3) Uani 1 1 d . . . H16 H 0.3046 0.5940 0.7694 0.069 Uiso 1 1 calc R . . C17 C 0.3331(4) 0.5695(6) 0.6865(5) 0.042(2) Uani 1 1 d . . . H17 H 0.3269 0.5096 0.6858 0.051 Uiso 1 1 calc R . . C18 C 0.0719(4) 0.3489(5) 0.2314(5) 0.042(2) Uani 1 1 d . . . C19 C 0.0103(4) 0.3421(6) 0.1955(6) 0.053(3) Uani 1 1 d . . . H19 H -0.0144 0.3635 0.2185 0.064 Uiso 1 1 calc R . . C20 C -0.0141(5) 0.3036(7) 0.1256(6) 0.076(4) Uani 1 1 d . . . H20 H -0.0554 0.3000 0.1018 0.091 Uiso 1 1 calc R . . C21 C 0.0207(6) 0.2710(7) 0.0912(6) 0.072(3) Uani 1 1 d . . . H21 H 0.0038 0.2451 0.0441 0.086 Uiso 1 1 calc R . . C22 C 0.0811(5) 0.2770(6) 0.1268(6) 0.059(3) Uani 1 1 d . . . H22 H 0.1054 0.2552 0.1034 0.071 Uiso 1 1 calc R . . C23 C 0.1065(4) 0.3143(6) 0.1962(5) 0.052(2) Uani 1 1 d . . . H23 H 0.1479 0.3163 0.2199 0.062 Uiso 1 1 calc R . . C24 C 0.0482(4) 0.4486(6) 0.3433(5) 0.041(2) Uani 1 1 d . . . C25 C 0.0320(4) 0.4174(6) 0.3994(5) 0.052(2) Uani 1 1 d . . . H25 H 0.0519 0.3700 0.4280 0.063 Uiso 1 1 calc R . . C26 C -0.0132(5) 0.4558(8) 0.4131(7) 0.071(3) Uani 1 1 d . . . H26 H -0.0259 0.4327 0.4493 0.085 Uiso 1 1 calc R . . C27 C -0.0400(5) 0.5282(8) 0.3739(7) 0.073(4) Uani 1 1 d . . . H27 H -0.0700 0.5556 0.3849 0.088 Uiso 1 1 calc R . . C28 C -0.0241(5) 0.5610(7) 0.3195(6) 0.065(3) Uani 1 1 d . . . H28 H -0.0429 0.6104 0.2930 0.078 Uiso 1 1 calc R . . C29 C 0.0201(4) 0.5208(6) 0.3035(5) 0.051(2) Uani 1 1 d . . . H29 H 0.0311 0.5425 0.2654 0.062 Uiso 1 1 calc R . . C30 C 0.1634(4) 0.0802(5) 0.5115(5) 0.041(2) Uani 1 1 d . . . H30A H 0.1448 0.1038 0.5441 0.049 Uiso 1 1 calc R . . H30B H 0.1567 0.0177 0.5079 0.049 Uiso 1 1 calc R . . C31 C 0.2700(3) 0.0526(5) 0.5215(5) 0.041(2) Uani 1 1 d . . . H31A H 0.2647 0.0674 0.4704 0.050 Uiso 1 1 calc R . . H31B H 0.2672 -0.0102 0.5256 0.050 Uiso 1 1 calc R . . C32 C 0.3294(3) 0.0870(5) 0.5776(4) 0.0367(19) Uani 1 1 d . . . H32A H 0.3538 0.0402 0.6076 0.044 Uiso 1 1 calc R . . H32B H 0.3514 0.1176 0.5523 0.044 Uiso 1 1 calc R . . C33 C 0.2523(3) 0.1459(5) 0.6008(4) 0.0307(17) Uani 1 1 d . . . H33 H 0.2312 0.1780 0.6237 0.037 Uiso 1 1 calc R . . C34 C 0.3485(3) 0.1885(5) 0.6913(4) 0.0374(19) Uani 1 1 d . . . H34A H 0.3744 0.1449 0.7241 0.045 Uiso 1 1 calc R . . H34B H 0.3249 0.2139 0.7170 0.045 Uiso 1 1 calc R . . C35 C 0.0507(3) 0.1141(6) 0.3985(4) 0.0392(19) Uani 1 1 d . . . C36 C 0.0279(4) 0.0417(6) 0.4205(5) 0.048(2) Uani 1 1 d . . . H36 H 0.0530 -0.0031 0.4468 0.057 Uiso 1 1 calc R . . C37 C -0.0329(5) 0.0367(7) 0.4027(6) 0.063(3) Uani 1 1 d . . . H37 H -0.0486 -0.0124 0.4171 0.075 Uiso 1 1 calc R . . C38 C -0.0700(4) 0.1007(8) 0.3654(6) 0.068(3) Uani 1 1 d . . . H38 H -0.1106 0.0966 0.3555 0.081 Uiso 1 1 calc R . . C39 C -0.0482(5) 0.1710(8) 0.3424(7) 0.072(3) Uani 1 1 d . . . H39 H -0.0739 0.2147 0.3150 0.087 Uiso 1 1 calc R . . C40 C 0.0122(4) 0.1782(6) 0.3594(6) 0.056(3) Uani 1 1 d . . . H40 H 0.0271 0.2274 0.3441 0.067 Uiso 1 1 calc R . . C41 C 0.1468(4) 0.0556(6) 0.3567(5) 0.041(2) Uani 1 1 d . . . C42 C 0.1781(4) 0.0879(7) 0.3165(5) 0.053(2) Uani 1 1 d . . . H42 H 0.1889 0.1465 0.3205 0.064 Uiso 1 1 calc R . . C43 C 0.1937(5) 0.0331(9) 0.2697(6) 0.071(3) Uani 1 1 d . . . H43 H 0.2147 0.0543 0.2417 0.085 Uiso 1 1 calc R . . C44 C 0.1778(4) -0.0522(8) 0.2654(6) 0.066(3) Uani 1 1 d . . . H44 H 0.1891 -0.0896 0.2350 0.080 Uiso 1 1 calc R . . C45 C 0.1462(5) -0.0841(7) 0.3038(6) 0.069(3) Uani 1 1 d . . . H45 H 0.1348 -0.1424 0.2988 0.083 Uiso 1 1 calc R . . C46 C 0.1309(4) -0.0301(6) 0.3505(6) 0.056(3) Uani 1 1 d . . . H46 H 0.1095 -0.0520 0.3778 0.067 Uiso 1 1 calc R . . C47 C 0.4514(3) 0.2157(5) 0.6552(4) 0.0338(18) Uani 1 1 d . . . C48 C 0.4654(4) 0.2418(6) 0.5949(5) 0.042(2) Uani 1 1 d . . . H48 H 0.4454 0.2884 0.5649 0.051 Uiso 1 1 calc R . . C49 C 0.5088(4) 0.1987(6) 0.5800(5) 0.051(2) Uani 1 1 d . . . H49 H 0.5191 0.2173 0.5406 0.061 Uiso 1 1 calc R . . C50 C 0.5375(4) 0.1288(6) 0.6219(6) 0.052(2) Uani 1 1 d . . . H50 H 0.5666 0.0994 0.6105 0.062 Uiso 1 1 calc R . . C51 C 0.5233(4) 0.1020(6) 0.6805(5) 0.046(2) Uani 1 1 d . . . H51 H 0.5426 0.0541 0.7090 0.055 Uiso 1 1 calc R . . C52 C 0.4803(4) 0.1455(5) 0.6981(5) 0.043(2) Uani 1 1 d . . . H52 H 0.4711 0.1275 0.7385 0.052 Uiso 1 1 calc R . . C53 C 0.4315(4) 0.3208(5) 0.7654(4) 0.0355(18) Uani 1 1 d . . . C54 C 0.4921(4) 0.3282(6) 0.7967(5) 0.053(3) Uani 1 1 d . . . H54 H 0.5153 0.3057 0.7718 0.064 Uiso 1 1 calc R . . C55 C 0.5188(5) 0.3688(6) 0.8645(6) 0.067(3) Uani 1 1 d . . . H55 H 0.5601 0.3743 0.8852 0.080 Uiso 1 1 calc R . . C56 C 0.4864(6) 0.4007(7) 0.9016(6) 0.071(4) Uani 1 1 d . . . H56 H 0.5052 0.4275 0.9480 0.085 Uiso 1 1 calc R . . C57 C 0.4267(6) 0.3939(6) 0.8715(6) 0.067(3) Uani 1 1 d . . . H57 H 0.4043 0.4153 0.8978 0.080 Uiso 1 1 calc R . . C58 C 0.3983(4) 0.3559(6) 0.8028(5) 0.050(2) Uani 1 1 d . . . H58 H 0.3568 0.3539 0.7815 0.061 Uiso 1 1 calc R . . Cl1 Cl 0.29472(10) 0.28197(15) 0.41260(14) 0.0469(5) Uani 1 1 d . . . Cl2 Cl 0.20511(9) 0.38328(14) 0.57710(12) 0.0424(5) Uani 1 1 d . . . Cl3 Cl 0.32714(11) 0.84994(16) 0.45540(14) 0.0529(6) Uani 1 1 d . . . Cl4 Cl 0.26720(12) -0.03133(15) 0.71929(14) 0.0519(6) Uani 1 1 d . . . O1 O 0.3299(3) 0.3571(4) 0.4464(4) 0.0595(18) Uani 1 1 d U . . O2 O 0.2452(4) 0.3092(5) 0.3497(5) 0.094(3) Uani 1 1 d U . . O3 O 0.3271(5) 0.2206(7) 0.3960(7) 0.140(4) Uani 1 1 d U . . O4 O 0.2706(4) 0.2459(5) 0.4634(5) 0.092(3) Uani 1 1 d U . . O5 O 0.1696(3) 0.3100(4) 0.5427(4) 0.068(2) Uani 1 1 d U . . O6 O 0.2344(3) 0.4108(5) 0.5295(4) 0.071(2) Uani 1 1 d U . . O7 O 0.1700(4) 0.4513(5) 0.5850(5) 0.084(2) Uani 1 1 d U . . O8 O 0.2483(3) 0.3563(4) 0.6471(4) 0.0639(19) Uani 1 1 d U . . O9 O 0.2803(5) 0.8220(11) 0.3970(7) 0.216(7) Uani 1 1 d . . . O10 O 0.3407(6) 0.9316(5) 0.4385(7) 0.150(5) Uani 1 1 d . . . O11 O 0.3129(6) 0.8507(7) 0.5180(6) 0.146(5) Uani 1 1 d . . . O12 O 0.3744(3) 0.7932(5) 0.4681(5) 0.085(3) Uani 1 1 d . . . O13 O 0.2123(5) -0.0490(10) 0.6738(8) 0.203(7) Uani 1 1 d . . . O14 O 0.2828(7) -0.0882(5) 0.7787(6) 0.164(6) Uani 1 1 d . . . O15 O 0.3040(4) -0.0405(5) 0.6794(5) 0.107(4) Uani 1 1 d . . . O16 O 0.2693(4) 0.0529(5) 0.7478(5) 0.089(3) Uani 1 1 d . . . C59 C 0.1889(7) -0.2308(10) 0.5870(8) 0.128(6) Uani 1 1 d . . . H59A H 0.1849 -0.1943 0.6259 0.153 Uiso 1 1 calc R . . H59B H 0.2304 -0.2476 0.6028 0.153 Uiso 1 1 calc R . . Cl5 Cl 0.1694(2) -0.1729(3) 0.5072(3) 0.1398(17) Uani 1 1 d . . . Cl6 Cl 0.1463(3) -0.3230(3) 0.5774(3) 0.168(2) Uani 1 1 d . . . O17 O 0.1926(4) -0.2869(6) 0.2933(5) 0.114(3) Uiso 1 1 d . . . H17A H 0.2045 -0.3389 0.3015 0.172 Uiso 1 1 d R . . H17B H 0.2207 -0.2545 0.3196 0.172 Uiso 1 1 d 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 0.0342(3) 0.0351(3) 0.0412(4) 0.0060(3) 0.0101(3) 0.0011(3) Ag2 0.0395(4) 0.0416(4) 0.0446(4) 0.0065(3) 0.0093(3) -0.0012(3) P1 0.0272(10) 0.0330(11) 0.0336(11) 0.0031(9) 0.0076(9) 0.0000(9) P2 0.0319(11) 0.0414(12) 0.0351(12) 0.0006(10) 0.0073(9) -0.0021(10) P3 0.0312(11) 0.0390(12) 0.0359(12) 0.0007(10) 0.0099(9) -0.0018(9) P4 0.0270(10) 0.0330(11) 0.0333(11) 0.0025(9) 0.0072(9) 0.0009(9) N1 0.027(3) 0.033(4) 0.036(4) 0.001(3) 0.007(3) 0.003(3) N2 0.030(3) 0.037(4) 0.031(4) 0.002(3) 0.008(3) 0.003(3) N3 0.025(3) 0.033(3) 0.030(3) -0.001(3) 0.005(3) -0.005(3) N4 0.024(3) 0.039(4) 0.035(4) -0.001(3) 0.004(3) -0.007(3) C1 0.023(4) 0.034(4) 0.030(4) -0.001(3) 0.009(3) -0.007(3) C2 0.035(5) 0.052(5) 0.050(6) -0.010(5) 0.016(4) 0.001(4) C3 0.036(5) 0.047(5) 0.070(7) -0.008(5) 0.024(5) 0.000(4) C4 0.032(4) 0.030(4) 0.035(4) 0.005(4) 0.012(4) -0.001(3) C5 0.034(4) 0.045(5) 0.030(4) 0.003(4) -0.001(4) -0.004(4) C6 0.032(4) 0.041(5) 0.035(4) -0.001(4) 0.013(4) -0.005(4) C7 0.042(5) 0.050(6) 0.060(6) 0.012(5) 0.015(5) 0.001(4) C8 0.027(5) 0.063(7) 0.081(8) 0.007(6) 0.007(5) 0.015(5) C9 0.022(4) 0.072(6) 0.052(6) -0.013(5) 0.012(4) -0.009(4) C10 0.038(5) 0.061(6) 0.049(6) 0.004(5) 0.019(4) -0.004(4) C11 0.029(4) 0.053(6) 0.057(6) 0.010(5) 0.008(4) 0.004(4) C12 0.031(4) 0.046(5) 0.029(4) 0.002(4) 0.005(3) 0.001(4) C13 0.055(6) 0.039(5) 0.045(5) 0.001(4) 0.018(5) 0.002(4) C14 0.048(6) 0.054(6) 0.069(7) -0.006(5) 0.021(5) 0.008(5) C15 0.045(6) 0.086(8) 0.053(6) -0.016(6) 0.016(5) 0.010(6) C16 0.044(5) 0.077(7) 0.056(6) 0.005(6) 0.023(5) 0.007(5) C17 0.032(4) 0.045(5) 0.045(5) -0.001(4) 0.010(4) 0.000(4) C18 0.043(5) 0.035(4) 0.040(5) 0.001(4) 0.008(4) 0.001(4) C19 0.037(5) 0.054(6) 0.060(6) -0.009(5) 0.007(5) 0.011(4) C20 0.065(7) 0.069(7) 0.063(8) -0.021(6) -0.010(6) 0.004(6) C21 0.092(9) 0.060(7) 0.045(6) -0.020(5) 0.006(6) 0.009(7) C22 0.069(7) 0.052(6) 0.064(7) -0.016(5) 0.032(6) -0.006(5) C23 0.048(5) 0.065(6) 0.036(5) -0.012(5) 0.009(4) -0.006(5) C24 0.039(5) 0.046(5) 0.036(5) -0.002(4) 0.012(4) 0.001(4) C25 0.059(6) 0.063(6) 0.041(5) -0.012(5) 0.025(5) -0.011(5) C26 0.077(8) 0.085(8) 0.070(8) -0.014(7) 0.052(7) -0.010(7) C27 0.041(6) 0.097(9) 0.076(9) -0.033(7) 0.015(6) -0.003(6) C28 0.056(7) 0.077(8) 0.050(6) -0.016(6) 0.006(5) 0.007(6) C29 0.038(5) 0.063(6) 0.046(6) -0.011(5) 0.008(4) 0.002(5) C30 0.039(5) 0.041(5) 0.043(5) 0.000(4) 0.016(4) -0.002(4) C31 0.034(4) 0.044(5) 0.045(5) -0.010(4) 0.013(4) 0.007(4) C32 0.027(4) 0.048(5) 0.031(4) -0.001(4) 0.007(3) 0.008(4) C33 0.036(4) 0.030(4) 0.029(4) 0.001(3) 0.014(3) 0.002(3) C34 0.025(4) 0.047(5) 0.036(5) 0.005(4) 0.006(3) -0.004(4) C35 0.027(4) 0.050(5) 0.033(4) -0.009(4) 0.003(3) -0.003(4) C36 0.038(5) 0.066(6) 0.044(5) -0.008(5) 0.021(4) -0.011(5) C37 0.052(6) 0.088(8) 0.055(7) -0.017(6) 0.028(5) -0.029(6) C38 0.033(5) 0.108(9) 0.063(7) -0.030(7) 0.019(5) -0.013(6) C39 0.046(6) 0.085(8) 0.077(8) -0.020(7) 0.013(6) 0.010(6) C40 0.036(5) 0.052(6) 0.072(7) -0.017(5) 0.011(5) -0.001(4) C41 0.031(4) 0.055(5) 0.033(5) 0.002(4) 0.009(4) 0.002(4) C42 0.039(5) 0.080(7) 0.040(5) -0.002(5) 0.014(4) -0.008(5) C43 0.052(6) 0.119(10) 0.049(6) -0.005(7) 0.027(5) 0.002(7) C44 0.047(6) 0.092(9) 0.055(7) -0.027(6) 0.014(5) 0.010(6) C45 0.056(7) 0.069(7) 0.079(8) -0.026(6) 0.021(6) 0.006(6) C46 0.053(6) 0.050(6) 0.069(7) 0.001(5) 0.029(5) 0.000(5) C47 0.020(3) 0.038(4) 0.031(4) -0.002(4) -0.004(3) -0.001(3) C48 0.033(4) 0.047(5) 0.047(5) -0.001(4) 0.014(4) 0.003(4) C49 0.052(6) 0.061(6) 0.046(6) -0.001(5) 0.026(5) -0.003(5) C50 0.038(5) 0.053(6) 0.067(7) -0.009(5) 0.023(5) 0.007(4) C51 0.034(5) 0.040(5) 0.053(6) 0.002(4) 0.005(4) 0.013(4) C52 0.033(4) 0.039(5) 0.051(6) 0.007(4) 0.010(4) 0.005(4) C53 0.037(4) 0.034(4) 0.031(4) 0.005(4) 0.007(4) 0.000(4) C54 0.045(5) 0.044(5) 0.052(6) -0.007(5) -0.003(5) 0.004(4) C55 0.062(7) 0.047(6) 0.051(7) 0.002(5) -0.024(5) -0.005(5) C56 0.116(11) 0.051(6) 0.031(5) -0.006(5) 0.012(6) -0.028(7) C57 0.106(10) 0.052(6) 0.051(7) -0.006(5) 0.039(7) -0.026(7) C58 0.055(6) 0.055(6) 0.050(6) -0.010(5) 0.029(5) -0.013(5) Cl1 0.0374(11) 0.0474(13) 0.0545(14) -0.0025(11) 0.0158(10) 0.0043(10) Cl2 0.0370(11) 0.0478(12) 0.0429(12) -0.0023(10) 0.0157(9) 0.0026(10) Cl3 0.0532(14) 0.0542(14) 0.0534(15) 0.0120(12) 0.0225(12) 0.0153(12) Cl4 0.0709(16) 0.0471(13) 0.0496(14) -0.0057(11) 0.0362(13) -0.0096(12) O1 0.060(3) 0.060(3) 0.059(4) 0.000(3) 0.023(3) -0.014(3) O2 0.084(4) 0.089(4) 0.087(4) 0.021(4) 0.007(3) -0.011(4) O3 0.131(6) 0.139(6) 0.156(6) -0.032(4) 0.060(4) 0.017(4) O4 0.101(4) 0.094(4) 0.085(4) 0.020(3) 0.042(4) -0.017(4) O5 0.072(4) 0.064(4) 0.065(4) -0.001(3) 0.022(3) -0.022(3) O6 0.064(4) 0.089(4) 0.070(4) 0.014(3) 0.038(3) 0.003(3) O7 0.085(4) 0.081(4) 0.087(4) -0.008(3) 0.034(3) 0.028(3) O8 0.057(3) 0.068(4) 0.055(3) 0.001(3) 0.008(3) 0.006(3) O9 0.102(9) 0.32(2) 0.140(12) -0.011(12) -0.050(8) -0.016(11) O10 0.229(13) 0.053(5) 0.251(14) 0.051(7) 0.182(12) 0.035(7) O11 0.243(13) 0.143(9) 0.116(8) 0.064(7) 0.140(9) 0.110(9) O12 0.072(5) 0.064(5) 0.129(8) 0.024(5) 0.051(5) 0.024(4) O13 0.071(7) 0.332(19) 0.187(14) -0.119(13) 0.026(8) -0.089(10) O14 0.375(19) 0.068(6) 0.128(9) 0.041(6) 0.185(12) 0.058(9) O15 0.170(10) 0.085(6) 0.124(8) 0.036(5) 0.122(8) 0.053(6) O16 0.152(9) 0.056(5) 0.095(7) -0.006(4) 0.086(6) -0.011(5) C59 0.133(14) 0.110(12) 0.100(13) -0.004(10) -0.001(11) 0.040(11) Cl5 0.142(4) 0.121(3) 0.128(4) 0.015(3) 0.019(3) 0.005(3) Cl6 0.225(6) 0.126(4) 0.203(6) -0.009(4) 0.136(5) -0.020(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 Ag1 P4 2.408(2) . ? Ag1 P1 2.430(2) . ? Ag1 O1 2.575(7) . ? Ag2 P2 2.409(2) . ? Ag2 P3 2.425(2) . ? Ag2 O5 2.546(7) . ? P1 C12 1.806(8) . ? P1 C6 1.808(8) . ? P1 C1 1.845(7) . ? P2 C18 1.812(9) . ? P2 C24 1.818(9) . ? P2 C5 1.837(8) . ? P3 C35 1.818(8) . ? P3 C41 1.818(9) . ? P3 C30 1.858(9) . ? P4 C47 1.804(8) . ? P4 C53 1.824(8) . ? P4 C34 1.862(8) . ? N1 C4 1.300(9) . ? N1 C1 1.447(9) . ? N1 C2 1.478(9) . ? N2 C4 1.312(9) . ? N2 C5 1.459(9) . ? N2 C3 1.483(10) . ? N3 C33 1.289(9) . ? N3 C30 1.457(9) . ? N3 C31 1.465(9) . ? N4 C33 1.304(9) . ? N4 C34 1.443(9) . ? N4 C32 1.501(9) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C2 C3 1.543(11) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C4 H4 0.9400 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 C7 1.379(11) . ? C6 C11 1.398(11) . ? C7 C8 1.401(11) . ? C7 H7 0.9400 . ? C8 C9 1.352(13) . ? C8 H8 0.9400 . ? C9 C10 1.383(12) . ? C9 H9 0.9400 . ? C10 C11 1.381(11) . ? C10 H10 0.9400 . ? C11 H11 0.9400 . ? C12 C17 1.381(11) . ? C12 C13 1.411(11) . ? C13 C14 1.372(12) . ? C13 H13 0.9400 . ? C14 C15 1.373(13) . ? C14 H14 0.9400 . ? C15 C16 1.363(14) . ? C15 H15 0.9400 . ? C16 C17 1.379(12) . ? C16 H16 0.9400 . ? C17 H17 0.9400 . ? C18 C23 1.385(12) . ? C18 C19 1.405(11) . ? C19 C20 1.393(13) . ? C19 H19 0.9400 . ? C20 C21 1.366(15) . ? C20 H20 0.9400 . ? C21 C22 1.378(14) . ? C21 H21 0.9400 . ? C22 C23 1.382(12) . ? C22 H22 0.9400 . ? C23 H23 0.9400 . ? C24 C25 1.382(11) . ? C24 C29 1.387(12) . ? C25 C26 1.370(13) . ? C25 H25 0.9400 . ? C26 C27 1.376(15) . ? C26 H26 0.9400 . ? C27 C28 1.357(15) . ? C27 H27 0.9400 . ? C28 C29 1.383(13) . ? C28 H28 0.9400 . ? C29 H29 0.9400 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C31 C32 1.543(10) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C33 H33 0.9400 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C35 C40 1.381(12) . ? C35 C36 1.391(11) . ? C36 C37 1.398(12) . ? C36 H36 0.9400 . ? C37 C38 1.354(15) . ? C37 H37 0.9400 . ? C38 C39 1.361(15) . ? C38 H38 0.9400 . ? C39 C40 1.394(13) . ? C39 H39 0.9400 . ? C40 H40 0.9400 . ? C41 C46 1.376(12) . ? C41 C42 1.381(11) . ? C42 C43 1.399(13) . ? C42 H42 0.9400 . ? C43 C44 1.371(15) . ? C43 H43 0.9400 . ? C44 C45 1.357(15) . ? C44 H44 0.9400 . ? C45 C46 1.388(13) . ? C45 H45 0.9400 . ? C46 H46 0.9400 . ? C47 C52 1.391(11) . ? C47 C48 1.402(11) . ? C48 C49 1.376(11) . ? C48 H48 0.9400 . ? C49 C50 1.376(12) . ? C49 H49 0.9400 . ? C50 C51 1.377(12) . ? C50 H50 0.9400 . ? C51 C52 1.396(11) . ? C51 H51 0.9400 . ? C52 H52 0.9400 . ? C53 C54 1.380(11) . ? C53 C58 1.391(11) . ? C54 C55 1.381(12) . ? C54 H54 0.9400 . ? C55 C56 1.353(15) . ? C55 H55 0.9400 . ? C56 C57 1.359(15) . ? C56 H56 0.9400 . ? C57 C58 1.383(13) . ? C57 H57 0.9400 . ? C58 H58 0.9400 . ? Cl1 O3 1.353(10) . ? Cl1 O2 1.420(8) . ? Cl1 O4 1.443(8) . ? Cl1 O1 1.450(7) . ? Cl2 O7 1.405(7) . ? Cl2 O8 1.432(7) . ? Cl2 O5 1.433(7) . ? Cl2 O6 1.436(7) . ? Cl3 O9 1.343(11) . ? Cl3 O10 1.379(8) . ? Cl3 O11 1.387(8) . ? Cl3 O12 1.399(7) . ? Cl4 O13 1.328(10) . ? Cl4 O14 1.387(9) . ? Cl4 O15 1.402(7) . ? Cl4 O16 1.411(7) . ? C59 Cl5 1.696(15) . ? C59 Cl6 1.737(16) . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? O17 H17A 0.8503 . ? O17 H17B 0.8496 . ? 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 P4 Ag1 P1 132.27(8) . . ? P4 Ag1 O1 118.31(16) . . ? P1 Ag1 O1 92.40(15) . . ? P2 Ag2 P3 132.55(8) . . ? P2 Ag2 O5 113.26(17) . . ? P3 Ag2 O5 92.59(16) . . ? C12 P1 C6 106.9(4) . . ? C12 P1 C1 105.9(4) . . ? C6 P1 C1 102.2(3) . . ? C12 P1 Ag1 112.2(3) . . ? C6 P1 Ag1 113.9(3) . . ? C1 P1 Ag1 114.9(2) . . ? C18 P2 C24 106.1(4) . . ? C18 P2 C5 99.6(4) . . ? C24 P2 C5 106.0(4) . . ? C18 P2 Ag2 108.8(3) . . ? C24 P2 Ag2 115.8(3) . . ? C5 P2 Ag2 118.6(3) . . ? C35 P3 C41 106.5(4) . . ? C35 P3 C30 101.7(4) . . ? C41 P3 C30 104.5(4) . . ? C35 P3 Ag2 113.4(3) . . ? C41 P3 Ag2 114.3(3) . . ? C30 P3 Ag2 115.2(3) . . ? C47 P4 C53 105.0(4) . . ? C47 P4 C34 104.1(4) . . ? C53 P4 C34 101.9(4) . . ? C47 P4 Ag1 114.0(3) . . ? C53 P4 Ag1 110.3(3) . . ? C34 P4 Ag1 119.9(3) . . ? C4 N1 C1 125.0(7) . . ? C4 N1 C2 110.7(7) . . ? C1 N1 C2 124.1(6) . . ? C4 N2 C5 124.1(7) . . ? C4 N2 C3 110.8(7) . . ? C5 N2 C3 124.3(7) . . ? C33 N3 C30 124.6(7) . . ? C33 N3 C31 111.1(6) . . ? C30 N3 C31 123.9(6) . . ? C33 N4 C34 125.0(7) . . ? C33 N4 C32 109.4(6) . . ? C34 N4 C32 124.7(6) . . ? N1 C1 P1 112.2(5) . . ? N1 C1 H1A 109.2 . . ? P1 C1 H1A 109.2 . . ? N1 C1 H1B 109.2 . . ? P1 C1 H1B 109.2 . . ? H1A C1 H1B 107.9 . . ? N1 C2 C3 102.9(6) . . ? N1 C2 H2A 111.2 . . ? C3 C2 H2A 111.2 . . ? N1 C2 H2B 111.2 . . ? C3 C2 H2B 111.2 . . ? H2A C2 H2B 109.1 . . ? N2 C3 C2 102.1(6) . . ? N2 C3 H3A 111.4 . . ? C2 C3 H3A 111.4 . . ? N2 C3 H3B 111.4 . . ? C2 C3 H3B 111.4 . . ? H3A C3 H3B 109.2 . . ? N1 C4 N2 113.4(7) . . ? N1 C4 H4 123.3 . . ? N2 C4 H4 123.3 . . ? N2 C5 P2 113.7(6) . . ? N2 C5 H5A 108.8 . . ? P2 C5 H5A 108.8 . . ? N2 C5 H5B 108.8 . . ? P2 C5 H5B 108.8 . . ? H5A C5 H5B 107.7 . . ? C7 C6 C11 117.4(8) . . ? C7 C6 P1 118.9(6) . . ? C11 C6 P1 123.7(6) . . ? C6 C7 C8 121.4(9) . . ? C6 C7 H7 119.3 . . ? C8 C7 H7 119.3 . . ? C9 C8 C7 119.6(9) . . ? C9 C8 H8 120.2 . . ? C7 C8 H8 120.2 . . ? C8 C9 C10 120.9(8) . . ? C8 C9 H9 119.6 . . ? C10 C9 H9 119.6 . . ? C11 C10 C9 119.3(9) . . ? C11 C10 H10 120.4 . . ? C9 C10 H10 120.4 . . ? C10 C11 C6 121.5(8) . . ? C10 C11 H11 119.3 . . ? C6 C11 H11 119.3 . . ? C17 C12 C13 117.1(8) . . ? C17 C12 P1 120.1(7) . . ? C13 C12 P1 122.8(7) . . ? C14 C13 C12 120.7(9) . . ? C14 C13 H13 119.7 . . ? C12 C13 H13 119.7 . . ? C13 C14 C15 120.3(10) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C16 C15 C14 120.2(10) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C15 C16 C17 119.9(10) . . ? C15 C16 H16 120.1 . . ? C17 C16 H16 120.1 . . ? C16 C17 C12 121.8(9) . . ? C16 C17 H17 119.1 . . ? C12 C17 H17 119.1 . . ? C23 C18 C19 118.0(8) . . ? C23 C18 P2 119.8(7) . . ? C19 C18 P2 122.0(7) . . ? C20 C19 C18 120.0(10) . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C21 C20 C19 121.4(11) . . ? C21 C20 H20 119.3 . . ? C19 C20 H20 119.3 . . ? C20 C21 C22 118.7(10) . . ? C20 C21 H21 120.7 . . ? C22 C21 H21 120.7 . . ? C21 C22 C23 121.3(10) . . ? C21 C22 H22 119.4 . . ? C23 C22 H22 119.4 . . ? C22 C23 C18 120.8(9) . . ? C22 C23 H23 119.6 . . ? C18 C23 H23 119.6 . . ? C25 C24 C29 119.5(9) . . ? C25 C24 P2 118.6(7) . . ? C29 C24 P2 121.9(7) . . ? C26 C25 C24 119.9(10) . . ? C26 C25 H25 120.0 . . ? C24 C25 H25 120.0 . . ? C25 C26 C27 119.7(11) . . ? C25 C26 H26 120.1 . . ? C27 C26 H26 120.1 . . ? C28 C27 C26 121.3(11) . . ? C28 C27 H27 119.3 . . ? C26 C27 H27 119.3 . . ? C27 C28 C29 119.2(11) . . ? C27 C28 H28 120.4 . . ? C29 C28 H28 120.4 . . ? C28 C29 C24 120.2(10) . . ? C28 C29 H29 119.9 . . ? C24 C29 H29 119.9 . . ? N3 C30 P3 111.5(5) . . ? N3 C30 H30A 109.3 . . ? P3 C30 H30A 109.3 . . ? N3 C30 H30B 109.3 . . ? P3 C30 H30B 109.3 . . ? H30A C30 H30B 108.0 . . ? N3 C31 C32 102.8(6) . . ? N3 C31 H31A 111.2 . . ? C32 C31 H31A 111.2 . . ? N3 C31 H31B 111.2 . . ? C32 C31 H31B 111.2 . . ? H31A C31 H31B 109.1 . . ? N4 C32 C31 102.0(6) . . ? N4 C32 H32A 111.4 . . ? C31 C32 H32A 111.4 . . ? N4 C32 H32B 111.4 . . ? C31 C32 H32B 111.4 . . ? H32A C32 H32B 109.2 . . ? N3 C33 N4 114.6(7) . . ? N3 C33 H33 122.7 . . ? N4 C33 H33 122.7 . . ? N4 C34 P4 112.5(5) . . ? N4 C34 H34A 109.1 . . ? P4 C34 H34A 109.1 . . ? N4 C34 H34B 109.1 . . ? P4 C34 H34B 109.1 . . ? H34A C34 H34B 107.8 . . ? C40 C35 C36 118.7(8) . . ? C40 C35 P3 117.7(7) . . ? C36 C35 P3 123.6(7) . . ? C35 C36 C37 118.9(9) . . ? C35 C36 H36 120.5 . . ? C37 C36 H36 120.5 . . ? C38 C37 C36 121.7(10) . . ? C38 C37 H37 119.1 . . ? C36 C37 H37 119.1 . . ? C37 C38 C39 119.8(10) . . ? C37 C38 H38 120.1 . . ? C39 C38 H38 120.1 . . ? C38 C39 C40 119.9(11) . . ? C38 C39 H39 120.0 . . ? C40 C39 H39 120.0 . . ? C35 C40 C39 120.9(10) . . ? C35 C40 H40 119.5 . . ? C39 C40 H40 119.5 . . ? C46 C41 C42 120.0(9) . . ? C46 C41 P3 122.1(7) . . ? C42 C41 P3 117.9(7) . . ? C41 C42 C43 119.6(10) . . ? C41 C42 H42 120.2 . . ? C43 C42 H42 120.2 . . ? C44 C43 C42 119.0(10) . . ? C44 C43 H43 120.5 . . ? C42 C43 H43 120.5 . . ? C45 C44 C43 121.6(10) . . ? C45 C44 H44 119.2 . . ? C43 C44 H44 119.2 . . ? C44 C45 C46 119.6(11) . . ? C44 C45 H45 120.2 . . ? C46 C45 H45 120.2 . . ? C41 C46 C45 120.1(10) . . ? C41 C46 H46 120.0 . . ? C45 C46 H46 120.0 . . ? C52 C47 C48 119.8(8) . . ? C52 C47 P4 122.2(7) . . ? C48 C47 P4 118.0(6) . . ? C49 C48 C47 119.3(8) . . ? C49 C48 H48 120.3 . . ? C47 C48 H48 120.3 . . ? C50 C49 C48 121.3(9) . . ? C50 C49 H49 119.4 . . ? C48 C49 H49 119.4 . . ? C49 C50 C51 119.7(8) . . ? C49 C50 H50 120.2 . . ? C51 C50 H50 120.2 . . ? C50 C51 C52 120.6(8) . . ? C50 C51 H51 119.7 . . ? C52 C51 H51 119.7 . . ? C47 C52 C51 119.4(9) . . ? C47 C52 H52 120.3 . . ? C51 C52 H52 120.3 . . ? C54 C53 C58 118.9(9) . . ? C54 C53 P4 121.0(7) . . ? C58 C53 P4 119.9(7) . . ? C53 C54 C55 119.8(10) . . ? C53 C54 H54 120.1 . . ? C55 C54 H54 120.1 . . ? C56 C55 C54 121.1(11) . . ? C56 C55 H55 119.5 . . ? C54 C55 H55 119.5 . . ? C55 C56 C57 119.7(10) . . ? C55 C56 H56 120.1 . . ? C57 C56 H56 120.1 . . ? C56 C57 C58 120.9(11) . . ? C56 C57 H57 119.5 . . ? C58 C57 H57 119.5 . . ? C57 C58 C53 119.5(10) . . ? C57 C58 H58 120.2 . . ? C53 C58 H58 120.2 . . ? O3 Cl1 O2 112.8(7) . . ? O3 Cl1 O4 108.7(6) . . ? O2 Cl1 O4 105.5(5) . . ? O3 Cl1 O1 111.8(6) . . ? O2 Cl1 O1 108.6(5) . . ? O4 Cl1 O1 109.2(5) . . ? O7 Cl2 O8 112.1(5) . . ? O7 Cl2 O5 111.0(5) . . ? O8 Cl2 O5 108.1(4) . . ? O7 Cl2 O6 108.9(5) . . ? O8 Cl2 O6 109.3(4) . . ? O5 Cl2 O6 107.3(5) . . ? O9 Cl3 O10 107.4(9) . . ? O9 Cl3 O11 109.0(9) . . ? O10 Cl3 O11 111.4(7) . . ? O9 Cl3 O12 109.3(8) . . ? O10 Cl3 O12 111.2(6) . . ? O11 Cl3 O12 108.5(6) . . ? O13 Cl4 O14 108.3(9) . . ? O13 Cl4 O15 108.1(8) . . ? O14 Cl4 O15 111.4(6) . . ? O13 Cl4 O16 109.3(8) . . ? O14 Cl4 O16 107.6(5) . . ? O15 Cl4 O16 112.1(5) . . ? Cl1 O1 Ag1 116.8(4) . . ? Cl2 O5 Ag2 117.0(4) . . ? Cl5 C59 Cl6 112.8(9) . . ? Cl5 C59 H59A 109.0 . . ? Cl6 C59 H59A 109.0 . . ? Cl5 C59 H59B 109.0 . . ? Cl6 C59 H59B 109.0 . . ? H59A C59 H59B 107.8 . . ? H17A O17 H17B 107.7 . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.888 _refine_diff_density_min -0.741 _refine_diff_density_rms 0.105 data_2^.^2CH~2~Cl~2~^.^2H~2~O _database_code_depnum_ccdc_archive 'CCDC 865926' #TrackingRef 'cif.cif' #============================================================================== # CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C58 H58 Ag2 Cl2 N4 P4, 2(Cl O4), 2(C H2 Cl2), 2(H2 O)' _chemical_formula_sum 'C60 H66 Ag2 Cl8 N4 O10 P4' _chemical_formula_weight 1626.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 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 13.601(3) _cell_length_b 14.615(3) _cell_length_c 17.145(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.03(3) _cell_angle_gamma 90.00 _cell_volume 3408.1(12) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 15087 _cell_measurement_theta_min 3.0301 _cell_measurement_theta_max 27.5049 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.585 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1648 _exptl_absorpt_coefficient_mu 1.040 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6266 _exptl_absorpt_correction_T_max 1.0000 _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 Mercury' _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 30416 _diffrn_reflns_av_R_equivalents 0.0563 _diffrn_reflns_av_sigmaI/netI 0.0544 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 27.51 _reflns_number_total 7801 _reflns_number_gt 6913 _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 'SHELXS-97 (Sheldrick, 1990)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0444P)^2^+7.2445P] 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 7801 _refine_ls_number_parameters 397 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0857 _refine_ls_R_factor_gt 0.0745 _refine_ls_wR_factor_ref 0.1569 _refine_ls_wR_factor_gt 0.1512 _refine_ls_goodness_of_fit_ref 1.218 _refine_ls_restrained_S_all 1.218 _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 0.39806(3) 0.44207(3) 0.55438(2) 0.03793(13) Uani 1 1 d . . . P1 P 0.42987(9) 0.34688(9) 0.67089(7) 0.0333(3) Uani 1 1 d . . . P2 P 0.78007(9) 0.54993(9) 0.47513(7) 0.0317(3) Uani 1 1 d . . . Cl1 Cl 0.49981(11) 0.59595(9) 0.57061(8) 0.0466(3) Uani 1 1 d . . . Cl2 Cl 0.23051(11) 0.79890(11) 0.64417(9) 0.0562(4) Uani 1 1 d . . . O1 O 0.1522(4) 0.8595(4) 0.6588(4) 0.111(2) Uani 1 1 d . . . O2 O 0.2058(3) 0.7415(3) 0.5799(3) 0.0637(12) Uani 1 1 d . . . O3 O 0.3163(4) 0.8513(4) 0.6256(3) 0.0857(17) Uani 1 1 d . . . O4 O 0.2473(6) 0.7445(5) 0.7112(4) 0.135(3) Uani 1 1 d . . . N1 N 0.6302(3) 0.3666(3) 0.6621(2) 0.0350(9) Uani 1 1 d . . . N2 N 0.7475(3) 0.4320(3) 0.5961(2) 0.0359(9) Uani 1 1 d . . . C1 C 0.5553(4) 0.2989(4) 0.6821(3) 0.0400(12) Uani 1 1 d . . . H1A H 0.5648 0.2788 0.7361 0.048 Uiso 1 1 calc R . . H1B H 0.5624 0.2454 0.6481 0.048 Uiso 1 1 calc R . . C2 C 0.6465(4) 0.4522(3) 0.7054(3) 0.0387(12) Uani 1 1 d . . . H2A H 0.6620 0.4401 0.7603 0.046 Uiso 1 1 calc R . . H2B H 0.5888 0.4923 0.7025 0.046 Uiso 1 1 calc R . . C3 C 0.7341(4) 0.4937(4) 0.6629(3) 0.0442(13) Uani 1 1 d . . . H3A H 0.7198 0.5562 0.6456 0.053 Uiso 1 1 calc R . . H3B H 0.7926 0.4945 0.6963 0.053 Uiso 1 1 calc R . . C4 C 0.6867(3) 0.3633(3) 0.6008(3) 0.0344(10) Uani 1 1 d . . . H4 H 0.6839 0.3161 0.5636 0.041 Uiso 1 1 calc R . . C5 C 0.8165(4) 0.4478(3) 0.5330(3) 0.0345(11) Uani 1 1 d . . . H5A H 0.8184 0.3939 0.4990 0.041 Uiso 1 1 calc R . . H5B H 0.8825 0.4570 0.5546 0.041 Uiso 1 1 calc R . . C6 C 0.3535(4) 0.2447(3) 0.6735(3) 0.0348(11) Uani 1 1 d . . . C7 C 0.2618(4) 0.2478(4) 0.7095(3) 0.0472(13) Uani 1 1 d . . . H7 H 0.2438 0.2992 0.7391 0.057 Uiso 1 1 calc R . . C8 C 0.1965(5) 0.1746(4) 0.7017(4) 0.0594(17) Uani 1 1 d . . . H8 H 0.1347 0.1770 0.7262 0.071 Uiso 1 1 calc R . . C9 C 0.2220(5) 0.0989(4) 0.6583(4) 0.0578(16) Uani 1 1 d . . . H9 H 0.1776 0.0501 0.6526 0.069 Uiso 1 1 calc R . . C10 C 0.3131(5) 0.0952(4) 0.6233(4) 0.0549(15) Uani 1 1 d . . . H10 H 0.3312 0.0431 0.5946 0.066 Uiso 1 1 calc R . . C11 C 0.3783(4) 0.1675(4) 0.6301(3) 0.0460(13) Uani 1 1 d . . . H11 H 0.4398 0.1644 0.6053 0.055 Uiso 1 1 calc R . . C12 C 0.4093(4) 0.4064(4) 0.7627(3) 0.0362(11) Uani 1 1 d . . . C13 C 0.4332(4) 0.3704(4) 0.8343(3) 0.0492(14) Uani 1 1 d . . . H13 H 0.4572 0.3102 0.8376 0.059 Uiso 1 1 calc R . . C14 C 0.4225(5) 0.4220(5) 0.9023(4) 0.0611(17) Uani 1 1 d . . . H14 H 0.4411 0.3976 0.9509 0.073 Uiso 1 1 calc R . . C15 C 0.3842(5) 0.5090(5) 0.8972(4) 0.0668(19) Uani 1 1 d . . . H15 H 0.3757 0.5439 0.9428 0.080 Uiso 1 1 calc R . . C16 C 0.3585(5) 0.5450(4) 0.8270(4) 0.0648(19) Uani 1 1 d . . . H16 H 0.3316 0.6042 0.8243 0.078 Uiso 1 1 calc R . . C17 C 0.3718(4) 0.4949(4) 0.7600(3) 0.0478(13) Uani 1 1 d . . . H17 H 0.3552 0.5209 0.7115 0.057 Uiso 1 1 calc R . . C18 C 0.8281(3) 0.6455(3) 0.5306(3) 0.0332(10) Uani 1 1 d . . . C19 C 0.9186(4) 0.6433(4) 0.5692(3) 0.0427(12) Uani 1 1 d . . . H19 H 0.9574 0.5901 0.5671 0.051 Uiso 1 1 calc R . . C20 C 0.9515(4) 0.7180(4) 0.6101(3) 0.0501(14) Uani 1 1 d . . . H20 H 1.0115 0.7151 0.6372 0.060 Uiso 1 1 calc R . . C21 C 0.8966(5) 0.7971(4) 0.6115(4) 0.0546(16) Uani 1 1 d . . . H21 H 0.9203 0.8487 0.6382 0.066 Uiso 1 1 calc R . . C22 C 0.8070(5) 0.8010(4) 0.5739(4) 0.0614(17) Uani 1 1 d . . . H22 H 0.7691 0.8548 0.5757 0.074 Uiso 1 1 calc R . . C23 C 0.7734(4) 0.7253(4) 0.5337(3) 0.0469(13) Uani 1 1 d . . . H23 H 0.7123 0.7280 0.5080 0.056 Uiso 1 1 calc R . . C24 C 0.8633(3) 0.5390(3) 0.3922(3) 0.0346(11) Uani 1 1 d . . . C25 C 0.8522(4) 0.4640(4) 0.3437(3) 0.0459(13) Uani 1 1 d . . . H25 H 0.8050 0.4191 0.3555 0.055 Uiso 1 1 calc R . . C26 C 0.9103(5) 0.4548(4) 0.2778(3) 0.0538(15) Uani 1 1 d . . . H26 H 0.9032 0.4032 0.2456 0.065 Uiso 1 1 calc R . . C27 C 0.9785(5) 0.5209(5) 0.2594(3) 0.0542(16) Uani 1 1 d . . . H27 H 1.0170 0.5146 0.2142 0.065 Uiso 1 1 calc R . . C28 C 0.9905(4) 0.5959(5) 0.3065(3) 0.0511(15) Uani 1 1 d . . . H28 H 1.0375 0.6407 0.2939 0.061 Uiso 1 1 calc R . . C29 C 0.9330(4) 0.6054(4) 0.3730(3) 0.0431(12) Uani 1 1 d . . . H29 H 0.9411 0.6569 0.4053 0.052 Uiso 1 1 calc R . . C30 C 0.0689(8) 0.8649(6) 0.4601(5) 0.101(3) Uani 1 1 d . . . H30A H -0.0020 0.8712 0.4513 0.122 Uiso 1 1 calc R . . H30B H 0.0784 0.8390 0.5122 0.122 Uiso 1 1 calc R . . Cl3 Cl 0.1214(3) 0.9704(2) 0.4571(2) 0.1619(15) Uani 1 1 d . . . Cl4 Cl 0.1164(2) 0.79031(16) 0.39202(14) 0.1056(8) Uani 1 1 d . . . O5 O 0.4254(3) 0.7815(3) 0.4962(2) 0.0628(12) Uani 1 1 d . . . H1O5 H 0.4571 0.7372 0.5163 0.075 Uiso 1 1 d R . . H2O5 H 0.3908 0.8045 0.5326 0.075 Uiso 1 1 d 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 0.0303(2) 0.0439(2) 0.0396(2) 0.00764(17) -0.00178(16) -0.00300(16) P1 0.0316(7) 0.0346(6) 0.0336(6) 0.0054(5) 0.0000(5) -0.0012(5) P2 0.0256(6) 0.0349(6) 0.0346(6) 0.0011(5) 0.0005(5) -0.0010(5) Cl1 0.0511(8) 0.0411(7) 0.0475(7) -0.0029(6) 0.0108(6) -0.0072(6) Cl2 0.0506(9) 0.0585(9) 0.0597(9) -0.0174(7) 0.0009(7) -0.0156(7) O1 0.068(4) 0.104(5) 0.160(6) -0.068(4) 0.033(4) -0.001(3) O2 0.071(3) 0.053(3) 0.067(3) -0.020(2) -0.014(2) -0.008(2) O3 0.069(3) 0.090(4) 0.098(4) -0.042(3) 0.025(3) -0.036(3) O4 0.191(8) 0.136(6) 0.078(4) 0.021(4) -0.049(5) -0.066(6) N1 0.031(2) 0.039(2) 0.035(2) 0.0057(18) 0.0018(18) 0.0004(18) N2 0.036(2) 0.039(2) 0.032(2) 0.0016(17) 0.0032(18) -0.0026(18) C1 0.034(3) 0.040(3) 0.046(3) 0.009(2) 0.001(2) 0.000(2) C2 0.045(3) 0.041(3) 0.030(2) 0.000(2) 0.002(2) 0.001(2) C3 0.043(3) 0.050(3) 0.039(3) -0.004(2) 0.003(2) -0.011(3) C4 0.030(2) 0.036(3) 0.037(3) 0.002(2) -0.004(2) -0.004(2) C5 0.033(3) 0.035(3) 0.036(3) 0.000(2) 0.007(2) 0.000(2) C6 0.034(3) 0.040(3) 0.030(2) 0.006(2) -0.001(2) -0.001(2) C7 0.042(3) 0.049(3) 0.051(3) -0.002(3) 0.010(3) -0.003(3) C8 0.055(4) 0.057(4) 0.067(4) -0.006(3) 0.021(3) -0.021(3) C9 0.064(4) 0.056(4) 0.053(4) 0.003(3) 0.004(3) -0.027(3) C10 0.068(4) 0.039(3) 0.057(4) -0.004(3) 0.007(3) -0.010(3) C11 0.046(3) 0.046(3) 0.046(3) -0.003(2) 0.010(3) -0.006(3) C12 0.030(2) 0.040(3) 0.038(3) 0.002(2) -0.001(2) -0.003(2) C13 0.050(3) 0.057(4) 0.041(3) 0.005(3) -0.001(3) 0.005(3) C14 0.060(4) 0.086(5) 0.037(3) -0.005(3) -0.001(3) -0.005(4) C15 0.070(5) 0.072(5) 0.058(4) -0.027(4) 0.005(4) -0.016(4) C16 0.070(5) 0.044(3) 0.080(5) -0.018(3) 0.008(4) -0.005(3) C17 0.049(3) 0.049(3) 0.046(3) -0.002(3) -0.001(3) -0.003(3) C18 0.029(2) 0.035(2) 0.036(2) 0.002(2) 0.003(2) -0.001(2) C19 0.035(3) 0.046(3) 0.047(3) 0.001(2) 0.000(2) -0.005(2) C20 0.045(3) 0.054(4) 0.051(3) -0.001(3) -0.011(3) -0.014(3) C21 0.060(4) 0.051(4) 0.052(4) -0.014(3) 0.004(3) -0.017(3) C22 0.062(4) 0.040(3) 0.082(5) -0.013(3) -0.006(4) 0.009(3) C23 0.041(3) 0.041(3) 0.059(4) -0.005(3) -0.005(3) 0.006(2) C24 0.026(2) 0.042(3) 0.036(3) 0.006(2) 0.000(2) 0.008(2) C25 0.046(3) 0.047(3) 0.045(3) 0.000(2) -0.005(3) 0.000(3) C26 0.066(4) 0.055(4) 0.041(3) -0.002(3) 0.006(3) 0.010(3) C27 0.050(4) 0.077(4) 0.036(3) 0.006(3) 0.010(3) 0.018(3) C28 0.038(3) 0.066(4) 0.049(3) 0.015(3) 0.004(3) -0.003(3) C29 0.037(3) 0.048(3) 0.045(3) 0.008(2) 0.005(2) -0.001(2) C30 0.120(8) 0.081(6) 0.103(7) 0.015(5) 0.036(6) -0.001(5) Cl3 0.223(4) 0.091(2) 0.172(3) -0.004(2) 0.054(3) -0.025(2) Cl4 0.146(2) 0.0781(14) 0.0929(16) 0.0057(12) -0.0067(15) 0.0080(14) O5 0.078(3) 0.059(3) 0.051(2) 0.000(2) 0.008(2) 0.001(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 Ag1 P1 2.4723(14) . ? Ag1 P2 2.4775(14) 3_666 ? Ag1 Cl1 2.6140(15) 3_666 ? Ag1 Cl1 2.6551(15) . ? P1 C6 1.819(5) . ? P1 C12 1.820(5) . ? P1 C1 1.854(5) . ? P2 C18 1.811(5) . ? P2 C24 1.824(5) . ? P2 C5 1.860(5) . ? P2 Ag1 2.4775(14) 3_666 ? Cl1 Ag1 2.6140(15) 3_666 ? Cl2 O1 1.408(6) . ? Cl2 O4 1.416(6) . ? Cl2 O2 1.425(4) . ? Cl2 O3 1.432(5) . ? N1 C4 1.304(6) . ? N1 C1 1.461(6) . ? N1 C2 1.471(6) . ? N2 C4 1.303(6) . ? N2 C5 1.450(6) . ? N2 C3 1.469(6) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C2 C3 1.524(7) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C4 H4 0.9400 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 C7 1.393(7) . ? C6 C11 1.394(7) . ? C7 C8 1.396(8) . ? C7 H7 0.9400 . ? C8 C9 1.378(9) . ? C8 H8 0.9400 . ? C9 C10 1.378(9) . ? C9 H9 0.9400 . ? C10 C11 1.384(8) . ? C10 H10 0.9400 . ? C11 H11 0.9400 . ? C12 C13 1.376(7) . ? C12 C17 1.392(8) . ? C13 C14 1.396(8) . ? C13 H13 0.9400 . ? C14 C15 1.378(10) . ? C14 H14 0.9400 . ? C15 C16 1.360(10) . ? C15 H15 0.9400 . ? C16 C17 1.374(8) . ? C16 H16 0.9400 . ? C17 H17 0.9400 . ? C18 C23 1.385(7) . ? C18 C19 1.398(7) . ? C19 C20 1.372(8) . ? C19 H19 0.9400 . ? C20 C21 1.376(9) . ? C20 H20 0.9400 . ? C21 C22 1.380(9) . ? C21 H21 0.9400 . ? C22 C23 1.381(8) . ? C22 H22 0.9400 . ? C23 H23 0.9400 . ? C24 C25 1.385(7) . ? C24 C29 1.396(7) . ? C25 C26 1.386(8) . ? C25 H25 0.9400 . ? C26 C27 1.375(9) . ? C26 H26 0.9400 . ? C27 C28 1.372(9) . ? C27 H27 0.9400 . ? C28 C29 1.391(7) . ? C28 H28 0.9400 . ? C29 H29 0.9400 . ? C30 Cl3 1.699(9) . ? C30 Cl4 1.723(9) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? O5 H1O5 0.8500 . ? O5 H2O5 0.8500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Ag1 P2 111.24(5) . 3_666 ? P1 Ag1 Cl1 116.74(5) . 3_666 ? P2 Ag1 Cl1 111.26(5) 3_666 3_666 ? P1 Ag1 Cl1 107.51(5) . . ? P2 Ag1 Cl1 119.41(5) 3_666 . ? Cl1 Ag1 Cl1 89.36(5) 3_666 . ? C6 P1 C12 106.4(2) . . ? C6 P1 C1 102.2(2) . . ? C12 P1 C1 103.5(2) . . ? C6 P1 Ag1 112.47(16) . . ? C12 P1 Ag1 113.75(17) . . ? C1 P1 Ag1 117.20(17) . . ? C18 P2 C24 104.6(2) . . ? C18 P2 C5 104.1(2) . . ? C24 P2 C5 100.4(2) . . ? C18 P2 Ag1 115.04(16) . 3_666 ? C24 P2 Ag1 116.86(17) . 3_666 ? C5 P2 Ag1 114.01(16) . 3_666 ? Ag1 Cl1 Ag1 90.64(4) 3_666 . ? O1 Cl2 O4 109.3(5) . . ? O1 Cl2 O2 109.3(3) . . ? O4 Cl2 O2 109.6(4) . . ? O1 Cl2 O3 108.7(4) . . ? O4 Cl2 O3 110.5(4) . . ? O2 Cl2 O3 109.6(3) . . ? C4 N1 C1 125.1(4) . . ? C4 N1 C2 110.5(4) . . ? C1 N1 C2 124.2(4) . . ? C4 N2 C5 125.4(4) . . ? C4 N2 C3 110.2(4) . . ? C5 N2 C3 124.3(4) . . ? N1 C1 P1 111.2(3) . . ? N1 C1 H1A 109.4 . . ? P1 C1 H1A 109.4 . . ? N1 C1 H1B 109.4 . . ? P1 C1 H1B 109.4 . . ? H1A C1 H1B 108.0 . . ? N1 C2 C3 102.4(4) . . ? N1 C2 H2A 111.3 . . ? C3 C2 H2A 111.3 . . ? N1 C2 H2B 111.3 . . ? C3 C2 H2B 111.3 . . ? H2A C2 H2B 109.2 . . ? N2 C3 C2 103.0(4) . . ? N2 C3 H3A 111.2 . . ? C2 C3 H3A 111.2 . . ? N2 C3 H3B 111.2 . . ? C2 C3 H3B 111.2 . . ? H3A C3 H3B 109.1 . . ? N2 C4 N1 113.3(5) . . ? N2 C4 H4 123.3 . . ? N1 C4 H4 123.3 . . ? N2 C5 P2 110.7(3) . . ? N2 C5 H5A 109.5 . . ? P2 C5 H5A 109.5 . . ? N2 C5 H5B 109.5 . . ? P2 C5 H5B 109.5 . . ? H5A C5 H5B 108.1 . . ? C7 C6 C11 118.7(5) . . ? C7 C6 P1 119.7(4) . . ? C11 C6 P1 120.9(4) . . ? C6 C7 C8 120.2(5) . . ? C6 C7 H7 119.9 . . ? C8 C7 H7 119.9 . . ? C9 C8 C7 120.4(6) . . ? C9 C8 H8 119.8 . . ? C7 C8 H8 119.8 . . ? C8 C9 C10 119.5(6) . . ? C8 C9 H9 120.2 . . ? C10 C9 H9 120.2 . . ? C9 C10 C11 120.7(6) . . ? C9 C10 H10 119.7 . . ? C11 C10 H10 119.7 . . ? C10 C11 C6 120.5(5) . . ? C10 C11 H11 119.7 . . ? C6 C11 H11 119.7 . . ? C13 C12 C17 118.2(5) . . ? C13 C12 P1 123.6(4) . . ? C17 C12 P1 118.2(4) . . ? C12 C13 C14 121.0(6) . . ? C12 C13 H13 119.5 . . ? C14 C13 H13 119.5 . . ? C15 C14 C13 119.0(6) . . ? C15 C14 H14 120.5 . . ? C13 C14 H14 120.5 . . ? C16 C15 C14 120.7(6) . . ? C16 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? C15 C16 C17 120.0(6) . . ? C15 C16 H16 120.0 . . ? C17 C16 H16 120.0 . . ? C16 C17 C12 121.0(6) . . ? C16 C17 H17 119.5 . . ? C12 C17 H17 119.5 . . ? C23 C18 C19 118.3(5) . . ? C23 C18 P2 118.4(4) . . ? C19 C18 P2 123.3(4) . . ? C20 C19 C18 120.7(5) . . ? C20 C19 H19 119.6 . . ? C18 C19 H19 119.6 . . ? C19 C20 C21 120.0(6) . . ? C19 C20 H20 120.0 . . ? C21 C20 H20 120.0 . . ? C20 C21 C22 120.4(6) . . ? C20 C21 H21 119.8 . . ? C22 C21 H21 119.8 . . ? C21 C22 C23 119.4(6) . . ? C21 C22 H22 120.3 . . ? C23 C22 H22 120.3 . . ? C22 C23 C18 121.1(6) . . ? C22 C23 H23 119.5 . . ? C18 C23 H23 119.5 . . ? C25 C24 C29 118.9(5) . . ? C25 C24 P2 118.0(4) . . ? C29 C24 P2 123.0(4) . . ? C24 C25 C26 120.3(6) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? C27 C26 C25 120.3(6) . . ? C27 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? C28 C27 C26 120.4(5) . . ? C28 C27 H27 119.8 . . ? C26 C27 H27 119.8 . . ? C27 C28 C29 119.7(6) . . ? C27 C28 H28 120.1 . . ? C29 C28 H28 120.1 . . ? C28 C29 C24 120.4(6) . . ? C28 C29 H29 119.8 . . ? C24 C29 H29 119.8 . . ? Cl3 C30 Cl4 113.3(5) . . ? Cl3 C30 H30A 108.9 . . ? Cl4 C30 H30A 108.9 . . ? Cl3 C30 H30B 108.9 . . ? Cl4 C30 H30B 108.9 . . ? H30A C30 H30B 107.7 . . ? H1O5 O5 H2O5 106.6 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.896 _refine_diff_density_min -1.118 _refine_diff_density_rms 0.095 data_3^.^2CH^3^OH _database_code_depnum_ccdc_archive 'CCDC 865927' #TrackingRef 'cif.cif' #============================================================================== # CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C58 H60 Ag2 Cl2 N4 P4, 2(C H4 O)' _chemical_formula_sum 'C60 H68 Ag2 Cl2 N4 O2 P4' _chemical_formula_weight 1287.70 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 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 9.814(2) _cell_length_b 11.780(2) _cell_length_c 13.337(3) _cell_angle_alpha 109.74(3) _cell_angle_beta 98.42(3) _cell_angle_gamma 91.44(3) _cell_volume 1431.0(5) _cell_formula_units_Z 1 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 6668 _cell_measurement_theta_min 3.1682 _cell_measurement_theta_max 27.4971 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.494 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 660 _exptl_absorpt_coefficient_mu 0.936 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7447 _exptl_absorpt_correction_T_max 1.0000 _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 Mercury' _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 13124 _diffrn_reflns_av_R_equivalents 0.0251 _diffrn_reflns_av_sigmaI/netI 0.0418 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.29 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6420 _reflns_number_gt 5471 _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 'SHELXS-97 (Sheldrick, 1990)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0398P)^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 6420 _refine_ls_number_parameters 335 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0456 _refine_ls_R_factor_gt 0.0346 _refine_ls_wR_factor_ref 0.0796 _refine_ls_wR_factor_gt 0.0755 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _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 0.536443(18) 0.633722(17) 0.624361(14) 0.03023(7) Uani 1 1 d . . . P1 P 0.76537(6) 0.67467(6) 0.73935(5) 0.02553(14) Uani 1 1 d . . . P2 P 0.65153(6) 0.23178(6) 0.33481(5) 0.02676(14) Uani 1 1 d . . . Cl1 Cl 0.38466(6) 0.42452(5) 0.56974(4) 0.03262(14) Uani 1 1 d . . . N1 N 0.8607(2) 0.44926(19) 0.69100(15) 0.0299(5) Uani 1 1 d . . . N2 N 0.8506(2) 0.2955(2) 0.51843(15) 0.0329(5) Uani 1 1 d . . . C1 C 0.8974(2) 0.5708(2) 0.69039(19) 0.0295(5) Uani 1 1 d . . . H1A H 0.9060 0.5659 0.6168 0.035 Uiso 1 1 calc R . . H1B H 0.9870 0.6023 0.7366 0.035 Uiso 1 1 calc R . . C2 C 0.9824(3) 0.3777(3) 0.6884(2) 0.0410(7) Uani 1 1 d . . . H2A H 0.9675 0.3120 0.7161 0.049 Uiso 1 1 calc R . . H2B H 1.0652 0.4289 0.7316 0.049 Uiso 1 1 calc R . . C3 C 0.9969(3) 0.3279(3) 0.5706(2) 0.0429(7) Uani 1 1 d . . . H3A H 1.0401 0.3890 0.5479 0.052 Uiso 1 1 calc R . . H3B H 1.0506 0.2567 0.5551 0.052 Uiso 1 1 calc R . . C4 C 0.7665(3) 0.3750(2) 0.59125(19) 0.0335(6) Uani 1 1 d . . . H4A H 0.6972 0.3265 0.6088 0.040 Uiso 1 1 calc R . . H4B H 0.7185 0.4274 0.5566 0.040 Uiso 1 1 calc R . . C5 C 0.8278(3) 0.2922(3) 0.40795(19) 0.0344(6) Uani 1 1 d . . . H5A H 0.8949 0.2420 0.3694 0.041 Uiso 1 1 calc R . . H5B H 0.8447 0.3743 0.4075 0.041 Uiso 1 1 calc R . . C6 C 0.8464(2) 0.8182(2) 0.74357(19) 0.0293(5) Uani 1 1 d . . . C7 C 0.9390(3) 0.8919(3) 0.8321(2) 0.0403(6) Uani 1 1 d . . . H7 H 0.9664 0.8661 0.8909 0.048 Uiso 1 1 calc R . . C8 C 0.9911(3) 1.0027(3) 0.8345(2) 0.0503(8) Uani 1 1 d . . . H8 H 1.0534 1.0520 0.8950 0.060 Uiso 1 1 calc R . . C9 C 0.9526(3) 1.0416(3) 0.7489(2) 0.0508(8) Uani 1 1 d . . . H9 H 0.9867 1.1180 0.7515 0.061 Uiso 1 1 calc R . . C10 C 0.8637(3) 0.9677(3) 0.6591(2) 0.0503(8) Uani 1 1 d . . . H10 H 0.8391 0.9929 0.5996 0.060 Uiso 1 1 calc R . . C11 C 0.8108(3) 0.8569(3) 0.6567(2) 0.0387(6) Uani 1 1 d . . . H11 H 0.7501 0.8072 0.5954 0.046 Uiso 1 1 calc R . . C12 C 0.7788(2) 0.6900(2) 0.88124(18) 0.0284(5) Uani 1 1 d . . . C13 C 0.6747(3) 0.7440(2) 0.9361(2) 0.0348(6) Uani 1 1 d . . . H13 H 0.6012 0.7722 0.8997 0.042 Uiso 1 1 calc R . . C14 C 0.6769(3) 0.7572(3) 1.0438(2) 0.0424(7) Uani 1 1 d . . . H14 H 0.6068 0.7957 1.0805 0.051 Uiso 1 1 calc R . . C15 C 0.7839(3) 0.7130(3) 1.0967(2) 0.0426(7) Uani 1 1 d . . . H15 H 0.7847 0.7191 1.1689 0.051 Uiso 1 1 calc R . . C16 C 0.8878(3) 0.6607(3) 1.0440(2) 0.0438(7) Uani 1 1 d . . . H16 H 0.9606 0.6321 1.0807 0.053 Uiso 1 1 calc R . . C17 C 0.8872(3) 0.6492(3) 0.9367(2) 0.0360(6) Uani 1 1 d . . . H17 H 0.9599 0.6139 0.9015 0.043 Uiso 1 1 calc R . . C18 C 0.6339(3) 0.0792(2) 0.33739(19) 0.0344(6) Uani 1 1 d . . . C19 C 0.5023(4) 0.0193(3) 0.3051(3) 0.0648(10) Uani 1 1 d . . . H19 H 0.4280 0.0574 0.2808 0.078 Uiso 1 1 calc R . . C20 C 0.4793(5) -0.0961(4) 0.3085(4) 0.0846(13) Uani 1 1 d . . . H20 H 0.3906 -0.1367 0.2847 0.102 Uiso 1 1 calc R . . C21 C 0.5864(6) -0.1505(3) 0.3467(3) 0.0790(13) Uani 1 1 d . . . H21 H 0.5700 -0.2260 0.3540 0.095 Uiso 1 1 calc R . . C22 C 0.7153(5) -0.0957(3) 0.3739(3) 0.0739(12) Uani 1 1 d . . . H22 H 0.7892 -0.1353 0.3967 0.089 Uiso 1 1 calc R . . C23 C 0.7405(4) 0.0193(3) 0.3686(3) 0.0573(9) Uani 1 1 d . . . H23 H 0.8312 0.0557 0.3865 0.069 Uiso 1 1 calc R . . C24 C 0.6809(2) 0.2162(2) 0.19884(19) 0.0309(5) Uani 1 1 d . . . C25 C 0.6805(3) 0.1055(3) 0.1171(2) 0.0443(7) Uani 1 1 d . . . H25 H 0.6655 0.0332 0.1305 0.053 Uiso 1 1 calc R . . C26 C 0.7021(4) 0.1016(3) 0.0152(2) 0.0579(9) Uani 1 1 d . . . H26 H 0.6997 0.0266 -0.0404 0.069 Uiso 1 1 calc R . . C27 C 0.7270(3) 0.2065(3) -0.0045(2) 0.0551(9) Uani 1 1 d . . . H27 H 0.7446 0.2028 -0.0729 0.066 Uiso 1 1 calc R . . C28 C 0.7264(3) 0.3173(3) 0.0752(2) 0.0476(7) Uani 1 1 d . . . H28 H 0.7426 0.3890 0.0611 0.057 Uiso 1 1 calc R . . C29 C 0.7017(3) 0.3227(3) 0.1768(2) 0.0378(6) Uani 1 1 d . . . H29 H 0.6990 0.3982 0.2308 0.045 Uiso 1 1 calc R . . C30 C 0.5970(4) 0.4183(4) 0.8552(3) 0.0675(10) Uani 1 1 d . . . H30A H 0.6140 0.4964 0.9128 0.101 Uiso 1 1 calc R . . H30B H 0.5401 0.3644 0.8762 0.101 Uiso 1 1 calc R . . H30C H 0.5496 0.4283 0.7900 0.101 Uiso 1 1 calc R . . O1 O 0.7242(3) 0.3686(2) 0.83597(18) 0.0672(7) Uani 1 1 d . . . H1O1 H 0.7569 0.4058 0.7991 0.101 Uiso 1 1 d 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 0.02795(11) 0.02773(11) 0.03111(11) 0.00684(8) 0.00056(7) 0.00296(8) P1 0.0255(3) 0.0247(3) 0.0249(3) 0.0083(2) 0.0004(2) 0.0006(2) P2 0.0277(3) 0.0249(3) 0.0262(3) 0.0080(2) 0.0017(2) 0.0042(3) Cl1 0.0402(3) 0.0265(3) 0.0303(3) 0.0092(2) 0.0058(3) -0.0027(3) N1 0.0362(11) 0.0273(12) 0.0260(10) 0.0103(9) 0.0010(9) 0.0045(9) N2 0.0353(11) 0.0337(12) 0.0261(10) 0.0075(9) -0.0005(9) 0.0081(10) C1 0.0296(12) 0.0311(14) 0.0287(12) 0.0120(10) 0.0038(10) 0.0028(10) C2 0.0473(16) 0.0347(16) 0.0361(14) 0.0116(12) -0.0083(12) 0.0115(13) C3 0.0349(14) 0.0481(18) 0.0373(14) 0.0072(13) -0.0046(12) 0.0180(13) C4 0.0315(13) 0.0348(15) 0.0291(12) 0.0062(11) 0.0009(10) 0.0043(11) C5 0.0281(13) 0.0408(16) 0.0306(12) 0.0091(11) 0.0012(10) 0.0012(11) C6 0.0294(13) 0.0257(13) 0.0322(12) 0.0097(10) 0.0047(10) 0.0013(10) C7 0.0464(16) 0.0349(16) 0.0364(14) 0.0131(12) -0.0033(12) -0.0066(13) C8 0.0586(19) 0.0402(18) 0.0428(15) 0.0111(13) -0.0090(14) -0.0180(15) C9 0.0584(19) 0.0336(17) 0.0591(18) 0.0201(14) -0.0015(15) -0.0113(14) C10 0.0604(19) 0.0449(19) 0.0513(17) 0.0291(15) -0.0017(15) -0.0061(15) C11 0.0414(15) 0.0367(16) 0.0350(13) 0.0131(12) -0.0032(12) -0.0064(12) C12 0.0298(12) 0.0255(13) 0.0267(11) 0.0076(10) -0.0010(10) -0.0038(10) C13 0.0333(13) 0.0351(15) 0.0343(13) 0.0111(11) 0.0021(11) 0.0012(11) C14 0.0448(16) 0.0402(17) 0.0377(14) 0.0048(12) 0.0149(12) -0.0019(13) C15 0.0570(18) 0.0426(17) 0.0253(12) 0.0097(12) 0.0047(12) -0.0050(14) C16 0.0520(17) 0.0462(18) 0.0292(13) 0.0129(12) -0.0052(12) 0.0035(14) C17 0.0368(14) 0.0390(16) 0.0292(12) 0.0093(11) 0.0014(11) 0.0042(12) C18 0.0474(16) 0.0265(14) 0.0289(12) 0.0086(10) 0.0063(11) 0.0104(12) C19 0.056(2) 0.0378(19) 0.106(3) 0.0313(19) 0.0117(19) 0.0043(16) C20 0.092(3) 0.041(2) 0.129(4) 0.036(2) 0.028(3) -0.003(2) C21 0.146(4) 0.035(2) 0.064(2) 0.0241(17) 0.024(3) 0.012(2) C22 0.121(4) 0.041(2) 0.0498(19) 0.0139(16) -0.015(2) 0.034(2) C23 0.070(2) 0.0376(19) 0.0551(18) 0.0104(14) -0.0075(16) 0.0204(16) C24 0.0260(12) 0.0365(15) 0.0296(12) 0.0112(11) 0.0022(10) 0.0067(11) C25 0.0611(19) 0.0365(17) 0.0343(14) 0.0096(12) 0.0098(13) 0.0134(14) C26 0.082(2) 0.053(2) 0.0338(15) 0.0054(14) 0.0172(15) 0.0194(18) C27 0.063(2) 0.076(3) 0.0349(15) 0.0277(16) 0.0130(14) 0.0105(18) C28 0.0443(16) 0.059(2) 0.0462(16) 0.0286(16) 0.0034(13) -0.0017(15) C29 0.0405(15) 0.0398(16) 0.0328(13) 0.0139(12) 0.0016(11) 0.0005(12) C30 0.079(3) 0.060(2) 0.066(2) 0.0284(19) 0.0079(19) -0.018(2) O1 0.095(2) 0.0562(16) 0.0622(14) 0.0340(12) 0.0187(13) -0.0030(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 P1 2.4633(11) . ? Ag1 P2 2.4634(10) 2_666 ? Ag1 Cl1 2.6660(11) . ? Ag1 Cl1 2.6807(9) 2_666 ? P1 C12 1.824(2) . ? P1 C6 1.830(3) . ? P1 C1 1.841(3) . ? P2 C18 1.813(3) . ? P2 C24 1.827(2) . ? P2 C5 1.850(2) . ? P2 Ag1 2.4634(10) 2_666 ? Cl1 Ag1 2.6807(9) 2_666 ? N1 C1 1.470(3) . ? N1 C2 1.478(3) . ? N1 C4 1.484(3) . ? N2 C5 1.444(3) . ? N2 C4 1.470(3) . ? N2 C3 1.481(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C2 C3 1.509(4) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 C11 1.385(3) . ? C6 C7 1.389(3) . ? C7 C8 1.378(4) . ? C7 H7 0.9400 . ? C8 C9 1.375(4) . ? C8 H8 0.9400 . ? C9 C10 1.380(4) . ? C9 H9 0.9400 . ? C10 C11 1.381(4) . ? C10 H10 0.9400 . ? C11 H11 0.9400 . ? C12 C13 1.386(4) . ? C12 C17 1.395(3) . ? C13 C14 1.389(4) . ? C13 H13 0.9400 . ? C14 C15 1.390(4) . ? C14 H14 0.9400 . ? C15 C16 1.364(4) . ? C15 H15 0.9400 . ? C16 C17 1.391(4) . ? C16 H16 0.9400 . ? C17 H17 0.9400 . ? C18 C23 1.368(4) . ? C18 C19 1.392(4) . ? C19 C20 1.390(5) . ? C19 H19 0.9400 . ? C20 C21 1.368(6) . ? C20 H20 0.9400 . ? C21 C22 1.347(6) . ? C21 H21 0.9400 . ? C22 C23 1.398(5) . ? C22 H22 0.9400 . ? C23 H23 0.9400 . ? C24 C25 1.388(4) . ? C24 C29 1.399(4) . ? C25 C26 1.391(4) . ? C25 H25 0.9400 . ? C26 C27 1.371(5) . ? C26 H26 0.9400 . ? C27 C28 1.379(5) . ? C27 H27 0.9400 . ? C28 C29 1.391(4) . ? C28 H28 0.9400 . ? C29 H29 0.9400 . ? C30 O1 1.414(5) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C30 H30C 0.9700 . ? O1 H1O1 0.8500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Ag1 P2 122.79(3) . 2_666 ? P1 Ag1 Cl1 122.47(3) . . ? P2 Ag1 Cl1 97.38(3) 2_666 . ? P1 Ag1 Cl1 99.39(3) . 2_666 ? P2 Ag1 Cl1 119.36(3) 2_666 2_666 ? Cl1 Ag1 Cl1 92.89(4) . 2_666 ? C12 P1 C6 103.82(11) . . ? C12 P1 C1 104.00(12) . . ? C6 P1 C1 101.04(11) . . ? C12 P1 Ag1 119.61(8) . . ? C6 P1 Ag1 109.45(8) . . ? C1 P1 Ag1 116.68(8) . . ? C18 P2 C24 106.04(12) . . ? C18 P2 C5 104.88(13) . . ? C24 P2 C5 98.22(11) . . ? C18 P2 Ag1 120.27(9) . 2_666 ? C24 P2 Ag1 107.33(9) . 2_666 ? C5 P2 Ag1 117.37(10) . 2_666 ? Ag1 Cl1 Ag1 87.11(4) . 2_666 ? C1 N1 C2 111.5(2) . . ? C1 N1 C4 112.17(18) . . ? C2 N1 C4 102.5(2) . . ? C5 N2 C4 116.5(2) . . ? C5 N2 C3 112.7(2) . . ? C4 N2 C3 107.21(19) . . ? N1 C1 P1 110.94(16) . . ? N1 C1 H1A 109.5 . . ? P1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? P1 C1 H1B 109.5 . . ? H1A C1 H1B 108.0 . . ? N1 C2 C3 104.59(19) . . ? N1 C2 H2A 110.8 . . ? C3 C2 H2A 110.8 . . ? N1 C2 H2B 110.8 . . ? C3 C2 H2B 110.8 . . ? H2A C2 H2B 108.9 . . ? N2 C3 C2 101.3(2) . . ? N2 C3 H3A 111.5 . . ? C2 C3 H3A 111.5 . . ? N2 C3 H3B 111.5 . . ? C2 C3 H3B 111.5 . . ? H3A C3 H3B 109.3 . . ? N2 C4 N1 107.79(19) . . ? N2 C4 H4A 110.1 . . ? N1 C4 H4A 110.1 . . ? N2 C4 H4B 110.1 . . ? N1 C4 H4B 110.1 . . ? H4A C4 H4B 108.5 . . ? N2 C5 P2 113.70(18) . . ? N2 C5 H5A 108.8 . . ? P2 C5 H5A 108.8 . . ? N2 C5 H5B 108.8 . . ? P2 C5 H5B 108.8 . . ? H5A C5 H5B 107.7 . . ? C11 C6 C7 118.6(2) . . ? C11 C6 P1 118.90(18) . . ? C7 C6 P1 122.51(19) . . ? C8 C7 C6 120.5(2) . . ? C8 C7 H7 119.7 . . ? C6 C7 H7 119.7 . . ? C9 C8 C7 120.5(3) . . ? C9 C8 H8 119.8 . . ? C7 C8 H8 119.8 . . ? C8 C9 C10 119.6(3) . . ? C8 C9 H9 120.2 . . ? C10 C9 H9 120.2 . . ? C9 C10 C11 120.1(3) . . ? C9 C10 H10 120.0 . . ? C11 C10 H10 120.0 . . ? C10 C11 C6 120.7(2) . . ? C10 C11 H11 119.6 . . ? C6 C11 H11 119.6 . . ? C13 C12 C17 118.6(2) . . ? C13 C12 P1 117.95(18) . . ? C17 C12 P1 123.5(2) . . ? C12 C13 C14 121.2(2) . . ? C12 C13 H13 119.4 . . ? C14 C13 H13 119.4 . . ? C13 C14 C15 119.3(3) . . ? C13 C14 H14 120.3 . . ? C15 C14 H14 120.3 . . ? C16 C15 C14 120.1(2) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C15 C16 C17 120.7(3) . . ? C15 C16 H16 119.6 . . ? C17 C16 H16 119.6 . . ? C16 C17 C12 120.1(3) . . ? C16 C17 H17 120.0 . . ? C12 C17 H17 120.0 . . ? C23 C18 C19 118.0(3) . . ? C23 C18 P2 124.7(2) . . ? C19 C18 P2 117.3(2) . . ? C20 C19 C18 120.8(3) . . ? C20 C19 H19 119.6 . . ? C18 C19 H19 119.6 . . ? C21 C20 C19 119.8(4) . . ? C21 C20 H20 120.1 . . ? C19 C20 H20 120.1 . . ? C22 C21 C20 120.0(4) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C21 C22 C23 120.8(4) . . ? C21 C22 H22 119.6 . . ? C23 C22 H22 119.6 . . ? C18 C23 C22 120.5(4) . . ? C18 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C25 C24 C29 119.1(2) . . ? C25 C24 P2 123.6(2) . . ? C29 C24 P2 117.2(2) . . ? C24 C25 C26 120.0(3) . . ? C24 C25 H25 120.0 . . ? C26 C25 H25 120.0 . . ? C27 C26 C25 120.5(3) . . ? C27 C26 H26 119.8 . . ? C25 C26 H26 119.8 . . ? C26 C27 C28 120.4(3) . . ? C26 C27 H27 119.8 . . ? C28 C27 H27 119.8 . . ? C27 C28 C29 119.8(3) . . ? C27 C28 H28 120.1 . . ? C29 C28 H28 120.1 . . ? C28 C29 C24 120.2(3) . . ? C28 C29 H29 119.9 . . ? C24 C29 H29 119.9 . . ? O1 C30 H30A 109.5 . . ? O1 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? O1 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C30 O1 H1O1 104.6 . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.555 _refine_diff_density_min -0.442 _refine_diff_density_rms 0.097 #===END