Eelctronic Supplementary Material for CrystEngComm This Journal is © The Royal Society of Chemistry 2004 data_global _publ_contact_author_email MIGUEL.JULVE@UV.ES _publ_contact_author_name 'Miguel Julve' _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_year ? _journal_page_first ? _publ_contact_author_address ; Dept. Química Inorgànica Universitat de Valencia Avda. Dr. Moliner 50 Burjassot (Valencia) 46100 SPAIN ; _publ_section_title ; Preparation and Crystal Structure of the Oxalato-Bridged CrIII-AgI Two-Dimensional Compound {Ag3(H2O)[Cr(dpa)(ox)2]3}n · 2nH2O (dpa == 2,2'-Dipyridylamine) ; loop_ _publ_author_name 'Miguel Julve' 'Fernando S. Delgado' 'Catalina Ruiz-Perez' 'Consuelo Yuste Vivas' data_COMPOUND1 _database_code_depnum_ccdc_archive 'CCDC 224289' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H33 Ag3 Cr3 N9 O27' _chemical_formula_weight 1575.38 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.486(5) _cell_length_b 11.381(5) _cell_length_c 23.904(5) _cell_angle_alpha 94.779(5) _cell_angle_beta 101.094(5) _cell_angle_gamma 91.342(5) _cell_volume 2521.6(18) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description cubes _exptl_crystal_colour 'deep red' _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.075 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1554 _exptl_absorpt_coefficient_mu 1.870 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21379 _diffrn_reflns_av_R_equivalents 0.0295 _diffrn_reflns_av_sigmaI/netI 0.0525 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 30.02 _reflns_number_total 14619 _reflns_number_gt 11283 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0533P)^2^+2.5058P] where P==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14619 _refine_ls_number_parameters 757 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0672 _refine_ls_R_factor_gt 0.0460 _refine_ls_wR_factor_ref 0.1267 _refine_ls_wR_factor_gt 0.1147 _refine_ls_goodness_of_fit_ref 1.102 _refine_ls_restrained_S_all 1.102 _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 0.25551(3) -0.18141(3) 0.206232(12) 0.03890(8) Uani 1 1 d . . . Ag2 Ag 0.68353(4) -0.45818(3) 0.603214(15) 0.04644(9) Uani 1 1 d . . . Ag3 Ag 0.77219(4) -0.00552(3) 0.909572(14) 0.04697(9) Uani 1 1 d . . . Cr1 Cr 0.32287(6) 0.30253(5) 0.93200(2) 0.02326(11) Uani 1 1 d . . . Cr2 Cr 1.11362(6) -0.19865(5) 0.75547(2) 0.02445(11) Uani 1 1 d . . . Cr3 Cr 0.25450(6) -0.23619(5) 0.44260(2) 0.02582(12) Uani 1 1 d . . . C1 C 0.0421(4) 0.2164(3) 0.89343(15) 0.0288(7) Uani 1 1 d . . . C2 C 0.0810(4) 0.2864(3) 0.84480(15) 0.0301(7) Uani 1 1 d . . . C3 C 0.5544(4) 0.3103(3) 0.87879(15) 0.0284(7) Uani 1 1 d . . . C4 C 0.5049(4) 0.1777(3) 0.87399(14) 0.0292(7) Uani 1 1 d . . . C5 C 0.5034(4) 0.1795(3) 1.02402(17) 0.0346(8) Uani 1 1 d . . . H5 H 0.5495 0.1554 0.9943 0.041 Uiso 1 1 calc R . . C6 C 0.5392(4) 0.1282(4) 1.07440(18) 0.0408(9) Uani 1 1 d . . . H6 H 0.6080 0.0711 1.0788 0.049 Uiso 1 1 calc R . . C7 C 0.4700(5) 0.1638(3) 1.11867(17) 0.0405(9) Uani 1 1 d . . . H7 H 0.4902 0.1290 1.1530 0.049 Uiso 1 1 calc R . . C8 C 0.3706(5) 0.2511(3) 1.11149(16) 0.0370(8) Uani 1 1 d . . . H8 H 0.3243 0.2764 1.1410 0.044 Uiso 1 1 calc R . . C9 C 0.3412(4) 0.3008(3) 1.05882(14) 0.0277(7) Uani 1 1 d . . . C10 C 0.2211(4) 0.4742(3) 1.01666(14) 0.0265(6) Uani 1 1 d . . . C11 C 0.1501(4) 0.5752(3) 1.03150(16) 0.0335(8) Uani 1 1 d . . . H11 H 0.1144 0.5821 1.0652 0.040 Uiso 1 1 calc R . . C12 C 0.1342(4) 0.6636(3) 0.99554(18) 0.0370(8) Uani 1 1 d . . . H12 H 0.0852 0.7305 1.0042 0.044 Uiso 1 1 calc R . . C13 C 0.1910(4) 0.6530(3) 0.94652(17) 0.0373(8) Uani 1 1 d . . . H13 H 0.1851 0.7140 0.9227 0.045 Uiso 1 1 calc R . . C14 C 0.2562(4) 0.5511(3) 0.93357(16) 0.0338(8) Uani 1 1 d . . . H14 H 0.2947 0.5442 0.9005 0.041 Uiso 1 1 calc R . . C15 C 0.9652(4) -0.3214(3) 0.65790(14) 0.0276(7) Uani 1 1 d . . . C16 C 0.9167(4) -0.3769(3) 0.70846(15) 0.0281(7) Uani 1 1 d . . . C17 C 1.0167(4) -0.1276(3) 0.85331(15) 0.0318(7) Uani 1 1 d . . . C18 C 0.8965(4) -0.0997(3) 0.80205(15) 0.0303(7) Uani 1 1 d . . . C19 C 1.1799(5) 0.0563(3) 0.75281(18) 0.0374(8) Uani 1 1 d . . . H19 H 1.0973 0.0611 0.7684 0.045 Uiso 1 1 calc R . . C20 C 1.2406(5) 0.1582(4) 0.74042(18) 0.0420(9) Uani 1 1 d . . . H20 H 1.2007 0.2306 0.7474 0.050 Uiso 1 1 calc R . . C21 C 1.3633(5) 0.1511(4) 0.71713(19) 0.0451(10) Uani 1 1 d . . . H21 H 1.4073 0.2190 0.7081 0.054 Uiso 1 1 calc R . . C22 C 1.4191(5) 0.0432(4) 0.7076(2) 0.0429(9) Uani 1 1 d . . . H22 H 1.5011 0.0374 0.6917 0.052 Uiso 1 1 calc R . . C23 C 1.3530(4) -0.0587(3) 0.72163(15) 0.0319(7) Uani 1 1 d . . . C24 C 1.4040(4) -0.2697(3) 0.73519(15) 0.0312(7) Uani 1 1 d . . . C25 C 1.5096(5) -0.3520(4) 0.72983(19) 0.0423(9) Uani 1 1 d . . . H25 H 1.5819 -0.3358 0.7099 0.051 Uiso 1 1 calc R . . C26 C 1.5053(5) -0.4554(4) 0.7540(2) 0.0462(10) Uani 1 1 d . . . H26 H 1.5741 -0.5110 0.7506 0.055 Uiso 1 1 calc R . . C27 C 1.3967(5) -0.4775(4) 0.78401(19) 0.0436(9) Uani 1 1 d . . . H27 H 1.3935 -0.5469 0.8017 0.052 Uiso 1 1 calc R . . C28 C 1.2960(4) -0.3961(3) 0.78688(16) 0.0358(8) Uani 1 1 d . . . H28 H 1.2233 -0.4117 0.8066 0.043 Uiso 1 1 calc R . . C29 C 0.2482(4) -0.1472(3) 0.33882(15) 0.0290(7) Uani 1 1 d . . . C30 C 0.3086(4) -0.2721(3) 0.33277(15) 0.0289(7) Uani 1 1 d . . . C31 C 0.4192(4) -0.3642(4) 0.52245(16) 0.0348(8) Uani 1 1 d . . . C32 C 0.5179(4) -0.2600(4) 0.51353(16) 0.0350(8) Uani 1 1 d . . . C33 C 0.2599(5) -0.0192(4) 0.51823(17) 0.0393(9) Uani 1 1 d . . . H33 H 0.3318 0.0016 0.4990 0.047 Uiso 1 1 calc R . . C34 C 0.2282(5) 0.0594(4) 0.56029(19) 0.0463(10) Uani 1 1 d . . . H34 H 0.2777 0.1321 0.5695 0.056 Uiso 1 1 calc R . . C35 C 0.1212(6) 0.0283(4) 0.58865(19) 0.0487(11) Uani 1 1 d . . . H35 H 0.0988 0.0796 0.6178 0.058 Uiso 1 1 calc R . . C36 C 0.0478(5) -0.0787(4) 0.57377(17) 0.0417(9) Uani 1 1 d . . . H36 H -0.0252 -0.1001 0.5924 0.050 Uiso 1 1 calc R . . C37 C 0.0838(4) -0.1545(3) 0.53056(15) 0.0329(8) Uani 1 1 d . . . C38 C -0.0317(4) -0.3182(3) 0.46124(16) 0.0335(8) Uani 1 1 d . . . C39 C -0.1552(5) -0.3936(4) 0.4499(2) 0.0488(11) Uani 1 1 d . . . H39 H -0.2011 -0.4109 0.4794 0.059 Uiso 1 1 calc R . . C40 C -0.2070(5) -0.4410(5) 0.3957(2) 0.0574(13) Uani 1 1 d . . . H40 H -0.2892 -0.4904 0.3876 0.069 Uiso 1 1 calc R . . C41 C -0.1351(5) -0.4147(4) 0.3521(2) 0.0493(11) Uani 1 1 d . . . H41 H -0.1709 -0.4433 0.3143 0.059 Uiso 1 1 calc R . . C42 C -0.0118(4) -0.3465(4) 0.36617(17) 0.0367(8) Uani 1 1 d . . . H42 H 0.0371 -0.3311 0.3372 0.044 Uiso 1 1 calc R . . O1 O 0.1422(3) 0.2194(2) 0.93874(10) 0.0288(5) Uani 1 1 d . . . O2 O 0.2094(3) 0.3330(2) 0.85695(10) 0.0302(5) Uani 1 1 d . . . O3 O -0.0745(3) 0.1648(3) 0.88703(13) 0.0443(7) Uani 1 1 d . . . O4 O -0.0063(3) 0.2913(3) 0.80053(12) 0.0476(7) Uani 1 1 d . . . O5 O 0.4952(3) 0.3763(2) 0.91328(11) 0.0307(5) Uani 1 1 d . . . O6 O 0.3967(3) 0.1582(2) 0.89745(11) 0.0313(5) Uani 1 1 d . . . O7 O 0.6418(3) 0.3427(3) 0.85138(12) 0.0405(6) Uani 1 1 d . . . O8 O 0.5692(3) 0.1033(2) 0.85049(12) 0.0392(6) Uani 1 1 d . . . O9 O 1.0673(3) -0.2430(2) 0.67270(10) 0.0300(5) Uani 1 1 d . . . O10 O 0.9940(3) -0.3423(2) 0.75779(10) 0.0310(5) Uani 1 1 d . . . O11 O 0.9074(3) -0.3538(3) 0.60865(11) 0.0384(6) Uani 1 1 d . . . O12 O 0.8149(3) -0.4469(3) 0.70039(12) 0.0398(6) Uani 1 1 d . . . O13 O 1.1327(3) -0.1630(2) 0.83844(10) 0.0320(5) Uani 1 1 d . . . O14 O 0.9345(3) -0.1136(2) 0.75356(10) 0.0319(5) Uani 1 1 d . . . O15 O 0.9952(3) -0.1158(3) 0.90241(12) 0.0440(7) Uani 1 1 d . . . O16 O 0.7792(3) -0.0662(3) 0.80994(13) 0.0437(7) Uani 1 1 d . . . O17 O 0.2246(3) -0.1150(2) 0.38857(10) 0.0319(5) Uani 1 1 d . . . O18 O 0.3138(3) -0.3276(2) 0.37822(11) 0.0328(5) Uani 1 1 d . . . O19 O 0.2298(3) -0.0877(2) 0.29793(11) 0.0419(7) Uani 1 1 d . . . O20 O 0.3479(3) -0.3080(3) 0.28918(12) 0.0439(7) Uani 1 1 d . . . O21 O 0.2916(3) -0.3673(2) 0.49107(11) 0.0359(6) Uani 1 1 d . . . O22 O 0.4575(3) -0.1929(2) 0.47591(11) 0.0350(6) Uani 1 1 d . . . O23 O 0.4589(3) -0.4366(3) 0.55630(15) 0.0562(9) Uani 1 1 d . . . O24 O 0.6402(3) -0.2475(3) 0.54109(14) 0.0530(8) Uani 1 1 d . . . N1 N 0.4040(3) 0.2639(3) 1.01504(12) 0.0276(6) Uani 1 1 d . . . N2 N 0.2671(3) 0.4597(2) 0.96704(12) 0.0263(6) Uani 1 1 d . . . N3 N 0.2412(3) 0.3874(3) 1.05373(13) 0.0314(6) Uani 1 1 d . . . H3 H 0.1829 0.3869 1.0772 0.038 Uiso 1 1 calc R . . N4 N 1.2334(3) -0.0528(3) 0.74370(13) 0.0293(6) Uani 1 1 d . . . N5 N 1.2963(3) -0.2920(3) 0.76206(12) 0.0282(6) Uani 1 1 d . . . N6 N 1.4155(3) -0.1639(3) 0.71187(15) 0.0364(7) Uani 1 1 d . . . H6A H 1.4707 -0.1639 0.6872 0.044 Uiso 1 1 calc R . . N7 N 0.1905(3) -0.1262(3) 0.50364(13) 0.0315(6) Uani 1 1 d . . . N8 N 0.0434(3) -0.2998(3) 0.41997(13) 0.0295(6) Uani 1 1 d . . . N9 N 0.0090(4) -0.2606(3) 0.51509(14) 0.0388(7) Uani 1 1 d . . . H9 H -0.0154 -0.2955 0.5425 0.047 Uiso 1 1 calc R . . O1W O 0.8047(4) -0.0008(3) 1.00792(13) 0.0521(8) Uani 1 1 d . . . O2W O 0.3355(4) 0.1596(3) 0.33924(14) 0.0535(8) Uani 1 1 d . . . O3W O 0.1441(4) 0.4587(3) 0.15770(14) 0.0615(9) 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 Ag1 0.03867(16) 0.05286(19) 0.02726(14) 0.00581(12) 0.00992(11) 0.00823(13) Ag2 0.03937(17) 0.04300(18) 0.05018(19) 0.00890(14) -0.00950(14) -0.00346(13) Ag3 0.04981(19) 0.0569(2) 0.03954(17) 0.00993(14) 0.01819(14) 0.01415(15) Cr1 0.0230(2) 0.0244(3) 0.0237(2) 0.00382(19) 0.00681(19) 0.00391(19) Cr2 0.0232(2) 0.0281(3) 0.0229(2) 0.0050(2) 0.00525(19) 0.0029(2) Cr3 0.0280(3) 0.0271(3) 0.0235(2) 0.0076(2) 0.0056(2) 0.0011(2) C1 0.0264(16) 0.0285(17) 0.0314(17) -0.0002(13) 0.0062(13) 0.0054(13) C2 0.0327(18) 0.0299(17) 0.0286(17) 0.0003(13) 0.0088(14) 0.0070(14) C3 0.0243(16) 0.0334(18) 0.0289(16) 0.0081(14) 0.0063(13) 0.0052(13) C4 0.0286(17) 0.0349(18) 0.0253(16) 0.0088(13) 0.0047(13) 0.0094(14) C5 0.0275(17) 0.0366(19) 0.039(2) 0.0069(15) 0.0018(15) 0.0067(14) C6 0.039(2) 0.035(2) 0.044(2) 0.0106(17) -0.0057(17) 0.0063(16) C7 0.051(2) 0.0333(19) 0.0305(18) 0.0101(15) -0.0102(17) -0.0045(17) C8 0.047(2) 0.035(2) 0.0275(17) 0.0076(14) 0.0022(16) -0.0018(16) C9 0.0284(16) 0.0272(16) 0.0266(16) 0.0040(13) 0.0025(13) 0.0003(13) C10 0.0244(15) 0.0290(17) 0.0265(16) 0.0032(13) 0.0053(12) 0.0033(13) C11 0.0356(19) 0.0348(19) 0.0325(18) 0.0005(14) 0.0126(15) 0.0080(15) C12 0.037(2) 0.0302(18) 0.043(2) 0.0008(15) 0.0063(16) 0.0087(15) C13 0.046(2) 0.0271(18) 0.039(2) 0.0082(15) 0.0072(17) 0.0072(16) C14 0.041(2) 0.0318(18) 0.0325(18) 0.0102(14) 0.0123(15) 0.0065(15) C15 0.0262(16) 0.0335(18) 0.0248(15) 0.0050(13) 0.0078(13) 0.0054(13) C16 0.0292(17) 0.0297(17) 0.0275(16) 0.0041(13) 0.0095(13) 0.0037(13) C17 0.0374(19) 0.0283(17) 0.0293(17) 0.0016(13) 0.0058(14) 0.0045(14) C18 0.0304(17) 0.0299(17) 0.0327(17) 0.0065(14) 0.0086(14) 0.0077(14) C19 0.041(2) 0.0310(19) 0.043(2) 0.0019(16) 0.0171(17) 0.0027(15) C20 0.054(3) 0.0299(19) 0.043(2) 0.0021(16) 0.0129(19) 0.0013(17) C21 0.048(2) 0.036(2) 0.051(2) 0.0080(18) 0.010(2) -0.0109(18) C22 0.036(2) 0.042(2) 0.053(2) 0.0077(19) 0.0144(18) -0.0054(17) C23 0.0299(17) 0.0358(19) 0.0296(17) 0.0035(14) 0.0050(14) -0.0008(14) C24 0.0295(17) 0.0334(18) 0.0305(17) 0.0014(14) 0.0057(14) 0.0060(14) C25 0.037(2) 0.044(2) 0.049(2) 0.0000(18) 0.0168(18) 0.0117(17) C26 0.043(2) 0.041(2) 0.055(3) 0.0040(19) 0.006(2) 0.0147(18) C27 0.046(2) 0.040(2) 0.044(2) 0.0125(18) 0.0026(18) 0.0129(18) C28 0.037(2) 0.039(2) 0.0314(18) 0.0119(15) 0.0019(15) 0.0070(16) C29 0.0295(17) 0.0299(17) 0.0288(16) 0.0058(13) 0.0073(13) 0.0011(13) C30 0.0286(17) 0.0278(17) 0.0331(17) 0.0037(13) 0.0129(14) -0.0001(13) C31 0.0289(18) 0.046(2) 0.0316(18) 0.0115(16) 0.0069(14) 0.0039(15) C32 0.0320(19) 0.043(2) 0.0291(17) 0.0007(15) 0.0060(15) 0.0027(15) C33 0.043(2) 0.036(2) 0.037(2) 0.0052(16) 0.0036(17) -0.0002(17) C34 0.058(3) 0.036(2) 0.042(2) -0.0009(17) 0.002(2) 0.0062(19) C35 0.066(3) 0.044(2) 0.035(2) 0.0008(18) 0.006(2) 0.018(2) C36 0.049(2) 0.049(2) 0.0303(19) 0.0096(17) 0.0121(17) 0.0116(19) C37 0.040(2) 0.0363(19) 0.0240(16) 0.0086(14) 0.0077(14) 0.0035(15) C38 0.0359(19) 0.0304(18) 0.0368(19) 0.0087(15) 0.0115(15) 0.0004(14) C39 0.042(2) 0.046(2) 0.061(3) 0.002(2) 0.021(2) -0.0118(19) C40 0.043(3) 0.056(3) 0.072(3) -0.006(2) 0.016(2) -0.020(2) C41 0.040(2) 0.054(3) 0.050(3) -0.005(2) 0.0036(19) -0.0071(19) C42 0.037(2) 0.041(2) 0.0320(18) 0.0060(15) 0.0060(15) 0.0020(16) O1 0.0269(12) 0.0333(13) 0.0279(12) 0.0061(10) 0.0080(10) -0.0004(10) O2 0.0322(13) 0.0340(13) 0.0250(11) 0.0075(10) 0.0047(10) 0.0013(10) O3 0.0334(14) 0.0497(17) 0.0481(17) 0.0082(13) 0.0038(12) -0.0101(12) O4 0.0342(15) 0.072(2) 0.0342(15) 0.0130(14) -0.0026(12) 0.0022(14) O5 0.0291(12) 0.0291(12) 0.0360(13) 0.0028(10) 0.0114(10) 0.0026(10) O6 0.0350(13) 0.0261(12) 0.0352(13) 0.0021(10) 0.0128(11) 0.0035(10) O7 0.0400(15) 0.0455(16) 0.0415(15) 0.0078(12) 0.0199(12) 0.0029(12) O8 0.0436(16) 0.0358(14) 0.0426(15) 0.0025(12) 0.0184(13) 0.0151(12) O9 0.0307(12) 0.0350(13) 0.0258(12) 0.0059(10) 0.0081(10) -0.0037(10) O10 0.0308(13) 0.0369(14) 0.0260(12) 0.0080(10) 0.0058(10) -0.0024(10) O11 0.0394(15) 0.0498(16) 0.0251(12) 0.0047(11) 0.0044(11) -0.0064(12) O12 0.0367(15) 0.0448(16) 0.0371(14) 0.0056(12) 0.0062(12) -0.0118(12) O13 0.0292(12) 0.0411(14) 0.0247(12) 0.0025(10) 0.0023(10) 0.0084(10) O14 0.0277(12) 0.0403(14) 0.0293(12) 0.0091(10) 0.0063(10) 0.0104(10) O15 0.0530(18) 0.0534(18) 0.0272(13) 0.0015(12) 0.0118(12) 0.0143(14) O16 0.0377(15) 0.0548(18) 0.0433(16) 0.0110(13) 0.0153(13) 0.0157(13) O17 0.0430(14) 0.0273(12) 0.0293(12) 0.0083(10) 0.0138(11) 0.0069(10) O18 0.0417(14) 0.0259(12) 0.0335(13) 0.0074(10) 0.0115(11) 0.0059(10) O19 0.0626(19) 0.0370(15) 0.0304(13) 0.0133(11) 0.0140(13) 0.0113(13) O20 0.0604(19) 0.0386(15) 0.0402(15) 0.0023(12) 0.0282(14) 0.0090(13) O21 0.0353(14) 0.0381(14) 0.0352(14) 0.0178(11) 0.0034(11) -0.0006(11) O22 0.0297(13) 0.0375(14) 0.0374(14) 0.0080(11) 0.0040(11) -0.0037(11) O23 0.0376(16) 0.074(2) 0.059(2) 0.0424(18) -0.0015(14) 0.0053(15) O24 0.0343(16) 0.070(2) 0.0502(18) 0.0118(16) -0.0037(13) -0.0049(14) N1 0.0263(14) 0.0285(14) 0.0278(14) 0.0049(11) 0.0032(11) 0.0031(11) N2 0.0302(14) 0.0239(13) 0.0266(13) 0.0043(11) 0.0090(11) 0.0051(11) N3 0.0348(16) 0.0359(16) 0.0272(14) 0.0081(12) 0.0125(12) 0.0071(13) N4 0.0280(14) 0.0285(15) 0.0324(15) 0.0025(12) 0.0087(12) -0.0006(11) N5 0.0256(14) 0.0339(15) 0.0251(13) 0.0023(11) 0.0042(11) 0.0050(11) N6 0.0335(16) 0.0357(17) 0.0464(19) 0.0080(14) 0.0211(14) 0.0059(13) N7 0.0351(16) 0.0333(16) 0.0275(14) 0.0040(12) 0.0089(12) 0.0009(12) N8 0.0291(15) 0.0314(15) 0.0287(14) 0.0072(12) 0.0052(12) 0.0022(12) N9 0.048(2) 0.0414(18) 0.0322(16) 0.0086(14) 0.0195(15) -0.0026(15) O1W 0.065(2) 0.0522(19) 0.0374(16) 0.0097(13) 0.0037(15) -0.0073(16) O2W 0.0455(18) 0.062(2) 0.0544(19) -0.0061(16) 0.0207(15) -0.0105(15) O3W 0.084(3) 0.064(2) 0.0437(18) 0.0036(16) 0.0304(18) 0.0024(19) _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 O19 2.415(3) . ? Ag1 O8 2.528(3) 2_656 ? Ag1 O7 2.529(3) 2_656 ? Ag1 O3 2.562(3) 2_556 ? Ag1 O20 2.577(3) . ? Ag2 O23 2.238(3) . ? Ag2 O11 2.385(3) . ? Ag2 O12 2.407(3) . ? Ag2 O18 2.514(3) 2_646 ? Ag3 O1W 2.307(3) . ? Ag3 O16 2.438(3) . ? Ag3 O15 2.512(3) . ? Ag3 O3 2.550(3) 1_655 ? Ag3 O8 2.568(3) . ? Cr1 O5 1.964(3) . ? Cr1 O2 1.969(2) . ? Cr1 O1 1.978(3) . ? Cr1 O6 1.980(3) . ? Cr1 N2 2.036(3) . ? Cr1 N1 2.073(3) . ? Cr2 O9 1.962(2) . ? Cr2 O13 1.963(2) . ? Cr2 O14 1.970(3) . ? Cr2 O10 1.979(3) . ? Cr2 N5 2.041(3) . ? Cr2 N4 2.058(3) . ? Cr3 O17 1.956(2) . ? Cr3 O21 1.962(3) . ? Cr3 O18 1.965(3) . ? Cr3 O22 1.971(3) . ? Cr3 N7 2.034(3) . ? Cr3 N8 2.068(3) . ? C1 O3 1.218(4) . ? C1 O1 1.293(4) . ? C1 C2 1.559(5) . ? C2 O4 1.218(5) . ? C2 O2 1.287(4) . ? C3 O7 1.220(4) . ? C3 O5 1.287(4) . ? C3 C4 1.558(5) . ? C4 O8 1.217(4) . ? C4 O6 1.284(4) . ? C5 N1 1.363(5) . ? C5 C6 1.369(5) . ? C6 C7 1.387(6) . ? C7 C8 1.384(6) . ? C8 C9 1.405(5) . ? C9 N1 1.343(4) . ? C9 N3 1.381(5) . ? C10 N2 1.339(4) . ? C10 N3 1.373(4) . ? C10 C11 1.401(5) . ? C11 C12 1.369(5) . ? C12 C13 1.379(6) . ? C13 C14 1.368(5) . ? C14 N2 1.359(4) . ? C15 O11 1.221(4) . ? C15 O9 1.278(4) . ? C15 C16 1.549(5) . ? C16 O12 1.213(4) . ? C16 O10 1.289(4) . ? C17 O15 1.226(4) . ? C17 O13 1.283(4) . ? C17 C18 1.564(5) . ? C18 O16 1.228(4) . ? C18 O14 1.277(4) . ? C19 C20 1.363(6) . ? C19 N4 1.369(5) . ? C20 C21 1.385(6) . ? C21 C22 1.368(6) . ? C22 C23 1.401(5) . ? C23 N4 1.341(5) . ? C23 N6 1.371(5) . ? C24 N5 1.337(5) . ? C24 N6 1.379(5) . ? C24 C25 1.404(5) . ? C25 C26 1.356(6) . ? C26 C27 1.393(6) . ? C27 C28 1.352(6) . ? C28 N5 1.369(5) . ? C29 O19 1.222(4) . ? C29 O17 1.277(4) . ? C29 C30 1.552(5) . ? C30 O20 1.215(4) . ? C30 O18 1.295(4) . ? C31 O23 1.218(5) . ? C31 O21 1.293(5) . ? C31 C32 1.548(6) . ? C32 O24 1.217(5) . ? C32 O22 1.287(5) . ? C33 N7 1.357(5) . ? C33 C34 1.371(6) . ? C34 C35 1.380(7) . ? C35 C36 1.373(7) . ? C36 C37 1.389(5) . ? C37 N7 1.346(5) . ? C37 N9 1.372(5) . ? C38 N8 1.350(5) . ? C38 N9 1.376(5) . ? C38 C39 1.404(6) . ? C39 C40 1.355(7) . ? C40 C41 1.399(7) . ? C41 C42 1.359(6) . ? C42 N8 1.351(5) . ? O3 Ag3 2.550(3) 1_455 ? O3 Ag1 2.562(3) 2_556 ? O7 Ag1 2.529(3) 2_656 ? O8 Ag1 2.528(3) 2_656 ? O18 Ag2 2.514(3) 2_646 ? 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 O19 Ag1 O8 122.42(10) . 2_656 ? O19 Ag1 O7 149.61(9) . 2_656 ? O8 Ag1 O7 67.02(9) 2_656 2_656 ? O19 Ag1 O3 123.77(10) . 2_556 ? O8 Ag1 O3 82.76(10) 2_656 2_556 ? O7 Ag1 O3 84.55(10) 2_656 2_556 ? O19 Ag1 O20 67.55(9) . . ? O8 Ag1 O20 119.30(10) 2_656 . ? O7 Ag1 O20 82.62(9) 2_656 . ? O3 Ag1 O20 146.83(10) 2_556 . ? O23 Ag2 O11 134.06(11) . . ? O23 Ag2 O12 138.65(12) . . ? O11 Ag2 O12 71.21(9) . . ? O23 Ag2 O18 103.58(11) . 2_646 ? O11 Ag2 O18 118.53(10) . 2_646 ? O12 Ag2 O18 78.85(9) . 2_646 ? O1W Ag3 O16 162.13(11) . . ? O1W Ag3 O15 95.06(11) . . ? O16 Ag3 O15 69.30(9) . . ? O1W Ag3 O3 107.13(11) . 1_655 ? O16 Ag3 O3 79.91(10) . 1_655 ? O15 Ag3 O3 81.74(11) . 1_655 ? O1W Ag3 O8 121.95(11) . . ? O16 Ag3 O8 74.75(9) . . ? O15 Ag3 O8 142.60(9) . . ? O3 Ag3 O8 82.22(10) 1_655 . ? O5 Cr1 O2 90.71(11) . . ? O5 Cr1 O1 171.52(11) . . ? O2 Cr1 O1 82.41(11) . . ? O5 Cr1 O6 82.61(11) . . ? O2 Cr1 O6 90.60(11) . . ? O1 Cr1 O6 92.46(11) . . ? O5 Cr1 N2 91.38(11) . . ? O2 Cr1 N2 90.41(11) . . ? O1 Cr1 N2 93.63(11) . . ? O6 Cr1 N2 173.91(11) . . ? O5 Cr1 N1 100.05(12) . . ? O2 Cr1 N1 168.90(11) . . ? O1 Cr1 N1 87.08(11) . . ? O6 Cr1 N1 93.43(11) . . ? N2 Cr1 N1 86.67(11) . . ? O9 Cr2 O13 171.93(11) . . ? O9 Cr2 O14 92.29(11) . . ? O13 Cr2 O14 82.59(10) . . ? O9 Cr2 O10 82.76(10) . . ? O13 Cr2 O10 90.60(11) . . ? O14 Cr2 O10 85.57(12) . . ? O9 Cr2 N5 90.33(11) . . ? O13 Cr2 N5 94.49(11) . . ? O14 Cr2 N5 176.18(11) . . ? O10 Cr2 N5 92.00(12) . . ? O9 Cr2 N4 91.12(11) . . ? O13 Cr2 N4 95.49(12) . . ? O14 Cr2 N4 94.57(12) . . ? O10 Cr2 N4 173.88(11) . . ? N5 Cr2 N4 88.16(13) . . ? O17 Cr3 O21 174.40(11) . . ? O17 Cr3 O18 82.71(10) . . ? O21 Cr3 O18 91.71(11) . . ? O17 Cr3 O22 97.00(11) . . ? O21 Cr3 O22 82.61(11) . . ? O18 Cr3 O22 89.97(12) . . ? O17 Cr3 N7 90.89(12) . . ? O21 Cr3 N7 94.69(12) . . ? O18 Cr3 N7 173.59(11) . . ? O22 Cr3 N7 90.43(12) . . ? O17 Cr3 N8 93.07(12) . . ? O21 Cr3 N8 87.59(11) . . ? O18 Cr3 N8 93.58(12) . . ? O22 Cr3 N8 169.67(11) . . ? N7 Cr3 N8 87.12(13) . . ? O3 C1 O1 125.3(3) . . ? O3 C1 C2 120.3(3) . . ? O1 C1 C2 114.4(3) . . ? O4 C2 O2 126.8(3) . . ? O4 C2 C1 120.0(3) . . ? O2 C2 C1 113.2(3) . . ? O7 C3 O5 126.1(3) . . ? O7 C3 C4 120.3(3) . . ? O5 C3 C4 113.6(3) . . ? O8 C4 O6 126.0(3) . . ? O8 C4 C3 120.1(3) . . ? O6 C4 C3 113.9(3) . . ? N1 C5 C6 123.7(4) . . ? C5 C6 C7 118.2(4) . . ? C8 C7 C6 119.7(4) . . ? C7 C8 C9 118.8(4) . . ? N1 C9 N3 121.5(3) . . ? N1 C9 C8 121.9(3) . . ? N3 C9 C8 116.6(3) . . ? N2 C10 N3 119.7(3) . . ? N2 C10 C11 121.6(3) . . ? N3 C10 C11 118.7(3) . . ? C12 C11 C10 118.8(3) . . ? C11 C12 C13 119.7(3) . . ? C14 C13 C12 118.8(4) . . ? N2 C14 C13 122.6(3) . . ? O11 C15 O9 125.3(3) . . ? O11 C15 C16 120.2(3) . . ? O9 C15 C16 114.6(3) . . ? O12 C16 O10 125.0(3) . . ? O12 C16 C15 121.1(3) . . ? O10 C16 C15 113.9(3) . . ? O15 C17 O13 125.7(4) . . ? O15 C17 C18 120.3(3) . . ? O13 C17 C18 114.0(3) . . ? O16 C18 O14 125.4(3) . . ? O16 C18 C17 121.0(3) . . ? O14 C18 C17 113.5(3) . . ? C20 C19 N4 123.8(4) . . ? C19 C20 C21 118.2(4) . . ? C22 C21 C20 119.3(4) . . ? C21 C22 C23 120.1(4) . . ? N4 C23 N6 121.6(3) . . ? N4 C23 C22 121.0(4) . . ? N6 C23 C22 117.3(3) . . ? N5 C24 N6 120.8(3) . . ? N5 C24 C25 121.7(4) . . ? N6 C24 C25 117.5(3) . . ? C26 C25 C24 119.3(4) . . ? C25 C26 C27 119.4(4) . . ? C28 C27 C26 118.8(4) . . ? C27 C28 N5 123.1(4) . . ? O19 C29 O17 125.6(3) . . ? O19 C29 C30 119.7(3) . . ? O17 C29 C30 114.6(3) . . ? O20 C30 O18 126.5(3) . . ? O20 C30 C29 120.6(3) . . ? O18 C30 C29 112.9(3) . . ? O23 C31 O21 123.2(4) . . ? O23 C31 C32 122.5(4) . . ? O21 C31 C32 114.2(3) . . ? O24 C32 O22 126.2(4) . . ? O24 C32 C31 120.1(4) . . ? O22 C32 C31 113.7(3) . . ? N7 C33 C34 122.6(4) . . ? C33 C34 C35 118.5(4) . . ? C36 C35 C34 119.8(4) . . ? C35 C36 C37 119.2(4) . . ? N7 C37 N9 119.4(3) . . ? N7 C37 C36 121.4(4) . . ? N9 C37 C36 119.2(4) . . ? N8 C38 N9 120.4(3) . . ? N8 C38 C39 121.0(4) . . ? N9 C38 C39 118.5(4) . . ? C40 C39 C38 119.7(4) . . ? C39 C40 C41 119.1(4) . . ? C42 C41 C40 118.5(4) . . ? N8 C42 C41 123.5(4) . . ? C1 O1 Cr1 114.2(2) . . ? C2 O2 Cr1 115.6(2) . . ? C1 O3 Ag3 149.2(3) . 1_455 ? C1 O3 Ag1 118.3(2) . 2_556 ? Ag3 O3 Ag1 89.63(9) 1_455 2_556 ? C3 O5 Cr1 113.6(2) . . ? C4 O6 Cr1 113.9(2) . . ? C3 O7 Ag1 115.8(2) . 2_656 ? C4 O8 Ag1 115.6(2) . 2_656 ? C4 O8 Ag3 120.1(2) . . ? Ag1 O8 Ag3 89.99(9) 2_656 . ? C15 O9 Cr2 113.4(2) . . ? C16 O10 Cr2 112.2(2) . . ? C15 O11 Ag2 112.3(2) . . ? C16 O12 Ag2 112.0(2) . . ? C17 O13 Cr2 113.6(2) . . ? C18 O14 Cr2 113.7(2) . . ? C17 O15 Ag3 112.3(2) . . ? C18 O16 Ag3 114.3(3) . . ? C29 O17 Cr3 114.7(2) . . ? C30 O18 Cr3 114.8(2) . . ? C30 O18 Ag2 134.0(2) . 2_646 ? Cr3 O18 Ag2 108.74(11) . 2_646 ? C29 O19 Ag1 117.8(2) . . ? C30 O20 Ag1 111.6(2) . . ? C31 O21 Cr3 114.5(2) . . ? C32 O22 Cr3 114.8(2) . . ? C31 O23 Ag2 126.9(3) . . ? C9 N1 C5 117.7(3) . . ? C9 N1 Cr1 121.7(2) . . ? C5 N1 Cr1 119.1(2) . . ? C10 N2 C14 118.1(3) . . ? C10 N2 Cr1 124.4(2) . . ? C14 N2 Cr1 116.8(2) . . ? C10 N3 C9 129.4(3) . . ? C23 N4 C19 117.6(3) . . ? C23 N4 Cr2 123.7(2) . . ? C19 N4 Cr2 118.3(2) . . ? C24 N5 C28 117.6(3) . . ? C24 N5 Cr2 124.3(2) . . ? C28 N5 Cr2 117.0(2) . . ? C23 N6 C24 130.4(3) . . ? C37 N7 C33 118.4(3) . . ? C37 N7 Cr3 123.4(3) . . ? C33 N7 Cr3 118.2(3) . . ? C38 N8 C42 117.8(3) . . ? C38 N8 Cr3 119.6(3) . . ? C42 N8 Cr3 121.1(2) . . ? C37 N9 C38 128.2(3) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 30.02 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.897 _refine_diff_density_min -1.389 _refine_diff_density_rms 0.185