# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Burrows, Andrew' _publ_contact_author_name 'Burrows, Andrew' _publ_contact_author_email a.d.burrows@bath.ac.uk _publ_section_title ; Dipyridyl \^I^2^-diketonate complexes: versatile polydentate metalloligands for metal-organic frameworks and hydrogen-bonded networks ; # Attachment '- dppd-strucs.cif' data_compound_1_k05cr2 _database_code_depnum_ccdc_archive 'CCDC 771699' #TrackingRef '- dppd-strucs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C47.75 H37 Al N6 O6' _chemical_formula_weight 817.81 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' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.9780(1) _cell_length_b 12.5850(1) _cell_length_c 14.3390(2) _cell_angle_alpha 87.816(1) _cell_angle_beta 84.052(1) _cell_angle_gamma 79.823(1) _cell_volume 2115.61(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 54895 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 30.034 _exptl_crystal_description Block _exptl_crystal_colour very-pale-straw _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.284 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 853 _exptl_absorpt_coefficient_mu 0.105 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.90 _exptl_absorpt_correction_T_max 0.97 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 KappaCCD _diffrn_measurement_method KappaCCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39978 _diffrn_reflns_av_R_equivalents 0.0539 _diffrn_reflns_av_sigmaI/netI 0.0520 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.56 _diffrn_reflns_theta_max 30.16 _reflns_number_total 12287 _reflns_number_gt 8909 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepack (otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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^)+(0.1087P)^2^+0.9582P] 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 SHELXL _refine_ls_extinction_coef 0.014(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 12287 _refine_ls_number_parameters 572 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0933 _refine_ls_R_factor_gt 0.0633 _refine_ls_wR_factor_ref 0.1945 _refine_ls_wR_factor_gt 0.1713 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.043 _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 Al1 Al 0.87829(4) 0.82748(4) 0.75176(4) 0.02116(13) Uani 1 1 d . . . O1 O 0.89263(11) 0.76591(9) 0.63217(8) 0.0233(3) Uani 1 1 d . . . O2 O 0.89565(11) 0.96115(9) 0.69527(9) 0.0246(3) Uani 1 1 d . . . O3 O 1.03496(10) 0.77958(9) 0.75786(8) 0.0227(3) Uani 1 1 d . . . O4 O 0.86365(10) 0.88873(9) 0.87049(8) 0.0232(3) Uani 1 1 d . . . O5 O 0.85374(10) 0.69334(9) 0.80502(9) 0.0228(3) Uani 1 1 d . . . O6 O 0.71933(11) 0.86676(9) 0.74556(9) 0.0250(3) Uani 1 1 d . . . N1 N 0.84609(19) 0.60883(14) 0.32755(13) 0.0418(4) Uani 1 1 d . . . N2 N 0.85691(16) 1.33312(13) 0.55584(13) 0.0356(4) Uani 1 1 d . . . N3 N 1.42040(15) 0.56929(15) 0.80333(14) 0.0385(4) Uani 1 1 d . . . N4 N 0.80048(16) 0.99035(16) 1.20674(13) 0.0390(4) Uani 1 1 d . . . N5 N 0.82569(15) 0.31378(13) 0.89135(13) 0.0338(4) Uani 1 1 d . . . N6 N 0.35663(15) 0.94953(15) 0.59550(13) 0.0370(4) Uani 1 1 d . . . C1 C 0.86051(15) 0.81503(13) 0.55736(12) 0.0235(3) Uani 1 1 d . . . C2 C 0.83807(17) 0.92804(14) 0.54727(13) 0.0271(4) Uani 1 1 d . . . H2 H 0.8042 0.9600 0.4936 0.033 Uiso 1 1 calc R . . C3 C 0.86453(15) 0.99414(13) 0.61454(12) 0.0241(3) Uani 1 1 d . . . C4 C 0.85223(16) 0.74568(14) 0.47700(12) 0.0249(3) Uani 1 1 d . . . C5 C 0.87006(19) 0.63390(15) 0.48963(14) 0.0338(4) Uani 1 1 d . . . H5 H 0.8847 0.6018 0.5492 0.041 Uiso 1 1 calc R . . C6 C 0.8660(2) 0.57037(16) 0.41367(16) 0.0422(5) Uani 1 1 d . . . H6 H 0.8783 0.4943 0.4234 0.051 Uiso 1 1 calc R . . C7 C 0.8285(2) 0.71638(17) 0.31688(14) 0.0366(5) Uani 1 1 d . . . H7 H 0.8137 0.7460 0.2566 0.044 Uiso 1 1 calc R . . C8 C 0.83037(18) 0.78734(15) 0.38796(13) 0.0308(4) Uani 1 1 d . . . H8 H 0.8170 0.8631 0.3762 0.037 Uiso 1 1 calc R . . C9 C 0.85987(15) 1.11185(13) 0.59330(13) 0.0246(3) Uani 1 1 d . . . C10 C 0.86659(17) 1.15312(15) 0.50193(13) 0.0286(4) Uani 1 1 d . . . H10 H 0.8725 1.1067 0.4502 0.034 Uiso 1 1 calc R . . C11 C 0.86445(17) 1.26316(16) 0.48739(15) 0.0318(4) Uani 1 1 d . . . H11 H 0.8686 1.2901 0.4246 0.038 Uiso 1 1 calc R . . C12 C 0.8511(2) 1.29267(16) 0.64348(16) 0.0374(5) Uani 1 1 d . . . H12 H 0.8460 1.3412 0.6935 0.045 Uiso 1 1 calc R . . C13 C 0.85185(18) 1.18397(15) 0.66595(14) 0.0306(4) Uani 1 1 d . . . H13 H 0.8470 1.1595 0.7295 0.037 Uiso 1 1 calc R . . C14 C 1.08622(14) 0.76444(13) 0.83253(12) 0.0210(3) Uani 1 1 d . . . C15 C 1.03966(15) 0.80245(13) 0.92035(12) 0.0234(3) Uani 1 1 d . . . H15 H 1.0831 0.7853 0.9724 0.028 Uiso 1 1 calc R . . C16 C 0.93096(14) 0.86512(13) 0.93458(11) 0.0205(3) Uani 1 1 d . . . C17 C 1.20356(14) 0.69865(13) 0.82273(12) 0.0226(3) Uani 1 1 d . . . C18 C 1.23220(16) 0.62073(14) 0.75398(13) 0.0269(4) Uani 1 1 d . . . H18 H 1.1783 0.6100 0.7127 0.032 Uiso 1 1 calc R . . C19 C 1.34071(17) 0.55896(16) 0.74660(15) 0.0334(4) Uani 1 1 d . . . H19 H 1.3596 0.5066 0.6989 0.040 Uiso 1 1 calc R . . C20 C 1.39088(18) 0.64363(19) 0.86948(17) 0.0409(5) Uani 1 1 d . . . H20 H 1.4458 0.6514 0.9108 0.049 Uiso 1 1 calc R . . C21 C 1.28557(16) 0.71015(17) 0.88183(15) 0.0326(4) Uani 1 1 d . . . H21 H 1.2696 0.7625 0.9296 0.039 Uiso 1 1 calc R . . C22 C 0.88812(15) 0.90902(13) 1.02943(12) 0.0219(3) Uani 1 1 d . . . C23 C 0.95867(16) 0.91055(14) 1.10067(13) 0.0251(3) Uani 1 1 d . . . H23 H 1.0380 0.8832 1.0905 0.030 Uiso 1 1 calc R . . C24 C 0.91116(18) 0.95271(15) 1.18661(13) 0.0299(4) Uani 1 1 d . . . H24 H 0.9605 0.9549 1.2340 0.036 Uiso 1 1 calc R . . C25 C 0.73369(19) 0.9876(2) 1.13864(16) 0.0424(5) Uani 1 1 d . . . H25 H 0.6544 1.0134 1.1519 0.051 Uiso 1 1 calc R . . C26 C 0.77239(17) 0.94935(17) 1.04937(14) 0.0328(4) Uani 1 1 d . . . H26 H 0.7211 0.9507 1.0029 0.039 Uiso 1 1 calc R . . C27 C 0.77261(14) 0.64385(13) 0.79170(12) 0.0219(3) Uani 1 1 d . . . C28 C 0.67475(15) 0.69112(14) 0.75023(13) 0.0257(4) Uani 1 1 d . . . H28 H 0.6222 0.6472 0.7358 0.031 Uiso 1 1 calc R . . C29 C 0.65271(15) 0.80214(14) 0.72960(12) 0.0232(3) Uani 1 1 d . . . C30 C 0.78852(15) 0.52823(13) 0.82429(12) 0.0225(3) Uani 1 1 d . . . C31 C 0.89753(16) 0.47581(15) 0.84137(14) 0.0277(4) Uani 1 1 d . . . H31 H 0.9610 0.5121 0.8310 0.033 Uiso 1 1 calc R . . C32 C 0.91095(17) 0.36955(16) 0.87389(15) 0.0333(4) Uani 1 1 d . . . H32 H 0.9856 0.3341 0.8844 0.040 Uiso 1 1 calc R . . C33 C 0.72163(17) 0.36530(16) 0.87457(15) 0.0327(4) Uani 1 1 d . . . H33 H 0.6597 0.3272 0.8865 0.039 Uiso 1 1 calc R . . C34 C 0.69883(16) 0.47128(15) 0.84066(13) 0.0273(4) Uani 1 1 d . . . H34 H 0.6237 0.5039 0.8290 0.033 Uiso 1 1 calc R . . C35 C 0.54737(15) 0.85203(15) 0.68543(12) 0.0252(4) Uani 1 1 d . . . C36 C 0.5328(2) 0.95861(18) 0.6579(2) 0.0544(7) Uani 1 1 d . . . H36 H 0.5871 1.0019 0.6694 0.065 Uiso 1 1 calc R . . C37 C 0.4372(2) 1.00267(19) 0.6127(2) 0.0577(8) Uani 1 1 d . . . H37 H 0.4297 1.0763 0.5930 0.069 Uiso 1 1 calc R . . C38 C 0.3721(2) 0.8483(2) 0.6233(3) 0.0733(11) Uani 1 1 d . . . H38 H 0.3154 0.8074 0.6123 0.088 Uiso 1 1 calc R . . C39 C 0.4648(2) 0.7960(2) 0.6677(2) 0.0650(9) Uani 1 1 d . . . H39 H 0.4705 0.7219 0.6855 0.078 Uiso 1 1 calc R . . C40 C 0.6323(2) 0.7154(2) 0.08623(18) 0.0470(6) Uani 1 1 d D . . C41 C 0.5849(3) 0.7786(2) 0.0128(2) 0.0566(7) Uani 1 1 d . . . H41 H 0.6207 0.7685 -0.0492 0.068 Uiso 1 1 calc R . . C42 C 0.4878(3) 0.8547(2) 0.0283(3) 0.0672(9) Uani 1 1 d . . . H42 H 0.4580 0.8965 -0.0229 0.081 Uiso 1 1 calc R . . C43 C 0.4327(3) 0.8715(2) 0.1178(3) 0.0649(8) Uani 1 1 d . . . H43 H 0.3660 0.9246 0.1285 0.078 Uiso 1 1 calc R . . C44 C 0.4773(3) 0.8090(2) 0.1912(2) 0.0601(7) Uani 1 1 d . . . H44 H 0.4402 0.8186 0.2529 0.072 Uiso 1 1 calc R . . C45 C 0.5754(2) 0.7325(2) 0.17556(19) 0.0498(6) Uani 1 1 d . . . H45 H 0.6046 0.6906 0.2270 0.060 Uiso 1 1 calc R . . C46 C 0.7391(3) 0.6344(2) 0.0700(2) 0.0586(7) Uani 1 1 d D . . H46A H 0.7757 0.6212 0.1283 0.088 Uiso 1 1 calc R . . H46B H 0.7911 0.6620 0.0214 0.088 Uiso 1 1 calc R . . H46C H 0.7207 0.5667 0.0494 0.088 Uiso 1 1 calc R . . C47 C 0.4642(8) 0.5832(5) 0.4560(7) 0.120(5) Uani 0.50 1 d PD . . C48 C 0.4089(5) 0.5002(5) 0.4601(5) 0.0628(17) Uani 0.50 1 d PD . . H48 H 0.3428 0.5057 0.4276 0.075 Uiso 0.50 1 calc PR . . C49 C 0.5593(6) 0.5853(7) 0.4948(6) 0.133(6) Uani 0.50 1 d PD . . H49 H 0.5989 0.6447 0.4891 0.160 Uiso 0.50 1 calc PR . . C50 C 0.4427(9) 0.6596(15) 0.4072(8) 0.101(7) Uani 0.25 1 d PD A 1 H50A H 0.4565 0.6381 0.3415 0.151 Uiso 0.25 1 calc PR A 1 H50B H 0.4912 0.7120 0.4183 0.151 Uiso 0.25 1 calc PR A 1 H50C H 0.3625 0.6924 0.4212 0.151 Uiso 0.25 1 calc PR A 1 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 Al1 0.0241(3) 0.0185(2) 0.0214(3) 0.00066(18) -0.01009(19) -0.00068(19) O1 0.0286(6) 0.0195(5) 0.0223(6) 0.0017(4) -0.0104(5) -0.0013(5) O2 0.0318(7) 0.0198(5) 0.0238(6) 0.0017(4) -0.0138(5) -0.0032(5) O3 0.0248(6) 0.0230(6) 0.0205(6) 0.0014(4) -0.0083(5) -0.0016(5) O4 0.0247(6) 0.0218(6) 0.0231(6) -0.0008(4) -0.0102(5) 0.0002(5) O5 0.0237(6) 0.0209(5) 0.0246(6) 0.0017(4) -0.0100(5) -0.0022(4) O6 0.0259(6) 0.0213(6) 0.0280(6) -0.0013(5) -0.0111(5) 0.0003(5) N1 0.0660(13) 0.0305(9) 0.0324(9) -0.0053(7) -0.0124(9) -0.0130(8) N2 0.0435(10) 0.0226(7) 0.0410(10) 0.0049(7) -0.0109(8) -0.0040(7) N3 0.0251(8) 0.0388(9) 0.0499(11) -0.0072(8) -0.0073(7) 0.0026(7) N4 0.0413(10) 0.0454(10) 0.0278(9) -0.0053(7) -0.0010(7) -0.0014(8) N5 0.0365(9) 0.0260(8) 0.0394(9) 0.0085(7) -0.0116(7) -0.0042(7) N6 0.0277(8) 0.0459(10) 0.0348(9) 0.0074(7) -0.0112(7) 0.0040(7) C1 0.0262(8) 0.0220(8) 0.0229(8) 0.0008(6) -0.0096(6) -0.0018(6) C2 0.0364(10) 0.0213(8) 0.0247(9) 0.0016(6) -0.0147(7) -0.0014(7) C3 0.0269(8) 0.0208(8) 0.0250(8) 0.0014(6) -0.0105(7) -0.0011(6) C4 0.0299(9) 0.0230(8) 0.0233(8) -0.0022(6) -0.0087(7) -0.0044(7) C5 0.0499(12) 0.0248(9) 0.0294(10) 0.0019(7) -0.0135(9) -0.0086(8) C6 0.0686(15) 0.0220(9) 0.0398(12) -0.0022(8) -0.0168(11) -0.0110(9) C7 0.0559(13) 0.0323(10) 0.0249(9) -0.0002(7) -0.0139(9) -0.0109(9) C8 0.0444(11) 0.0230(8) 0.0264(9) 0.0000(7) -0.0107(8) -0.0054(8) C9 0.0266(8) 0.0202(8) 0.0278(9) 0.0021(6) -0.0107(7) -0.0017(6) C10 0.0340(10) 0.0265(8) 0.0263(9) 0.0017(7) -0.0111(7) -0.0035(7) C11 0.0349(10) 0.0283(9) 0.0327(10) 0.0086(7) -0.0104(8) -0.0049(7) C12 0.0542(13) 0.0225(9) 0.0358(11) -0.0022(8) -0.0103(9) -0.0040(8) C13 0.0427(11) 0.0226(8) 0.0265(9) 0.0007(7) -0.0093(8) -0.0028(7) C14 0.0221(8) 0.0170(7) 0.0248(8) 0.0014(6) -0.0074(6) -0.0030(6) C15 0.0243(8) 0.0230(8) 0.0226(8) 0.0013(6) -0.0091(6) 0.0001(6) C16 0.0247(8) 0.0173(7) 0.0206(8) 0.0011(6) -0.0071(6) -0.0042(6) C17 0.0214(8) 0.0213(7) 0.0250(8) 0.0025(6) -0.0054(6) -0.0021(6) C18 0.0263(8) 0.0247(8) 0.0301(9) -0.0017(7) -0.0081(7) -0.0022(7) C19 0.0295(9) 0.0290(9) 0.0401(11) -0.0067(8) -0.0026(8) 0.0003(7) C20 0.0240(9) 0.0516(13) 0.0472(13) -0.0099(10) -0.0133(9) 0.0000(9) C21 0.0253(9) 0.0388(10) 0.0343(10) -0.0087(8) -0.0100(7) -0.0014(8) C22 0.0260(8) 0.0182(7) 0.0223(8) 0.0014(6) -0.0050(6) -0.0044(6) C23 0.0290(9) 0.0229(8) 0.0244(8) 0.0004(6) -0.0086(7) -0.0038(7) C24 0.0383(10) 0.0295(9) 0.0232(9) -0.0011(7) -0.0076(7) -0.0066(8) C25 0.0310(10) 0.0583(14) 0.0340(11) -0.0075(10) -0.0006(8) 0.0031(10) C26 0.0282(9) 0.0398(10) 0.0297(10) -0.0045(8) -0.0065(7) -0.0005(8) C27 0.0234(8) 0.0213(7) 0.0205(8) -0.0001(6) -0.0048(6) -0.0009(6) C28 0.0237(8) 0.0243(8) 0.0302(9) 0.0020(7) -0.0103(7) -0.0030(6) C29 0.0229(8) 0.0242(8) 0.0215(8) -0.0011(6) -0.0061(6) 0.0010(6) C30 0.0247(8) 0.0208(7) 0.0213(8) 0.0002(6) -0.0055(6) -0.0005(6) C31 0.0241(8) 0.0244(8) 0.0344(10) 0.0041(7) -0.0079(7) -0.0021(7) C32 0.0277(9) 0.0276(9) 0.0438(11) 0.0083(8) -0.0113(8) -0.0001(7) C33 0.0311(10) 0.0297(9) 0.0388(11) 0.0089(8) -0.0100(8) -0.0081(8) C34 0.0246(8) 0.0264(8) 0.0306(9) 0.0033(7) -0.0076(7) -0.0019(7) C35 0.0220(8) 0.0297(9) 0.0220(8) 0.0018(7) -0.0072(6) 0.0027(7) C36 0.0449(13) 0.0268(10) 0.097(2) 0.0029(12) -0.0421(14) -0.0006(9) C37 0.0524(15) 0.0308(11) 0.092(2) 0.0101(12) -0.0405(15) 0.0046(10) C38 0.0503(15) 0.0608(16) 0.122(3) 0.0463(18) -0.0585(18) -0.0261(13) C39 0.0462(14) 0.0498(14) 0.110(2) 0.0449(15) -0.0507(16) -0.0228(12) C40 0.0620(15) 0.0417(12) 0.0431(13) -0.0038(10) -0.0165(11) -0.0176(11) C41 0.078(2) 0.0530(15) 0.0451(14) -0.0003(11) -0.0201(13) -0.0212(14) C42 0.085(2) 0.0500(15) 0.076(2) 0.0116(14) -0.0438(18) -0.0194(15) C43 0.0666(19) 0.0457(14) 0.085(2) -0.0029(14) -0.0237(17) -0.0072(13) C44 0.0704(19) 0.0479(14) 0.0634(18) -0.0083(13) -0.0083(14) -0.0114(13) C45 0.0622(16) 0.0455(13) 0.0436(13) -0.0003(10) -0.0124(11) -0.0107(12) C46 0.0679(18) 0.0610(16) 0.0465(15) -0.0068(12) -0.0041(13) -0.0096(14) C47 0.149(9) 0.043(3) 0.127(7) -0.011(4) 0.109(7) 0.025(4) C48 0.037(3) 0.061(4) 0.086(4) -0.033(3) 0.011(3) -0.001(3) C49 0.064(5) 0.133(8) 0.205(12) -0.138(9) 0.090(6) -0.057(5) C50 0.038(6) 0.22(2) 0.038(6) -0.016(9) 0.028(5) -0.022(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 O4 1.8744(13) . ? Al1 O2 1.8746(13) . ? Al1 O3 1.8769(13) . ? Al1 O5 1.8842(13) . ? Al1 O1 1.8879(13) . ? Al1 O6 1.8913(13) . ? O1 C1 1.277(2) . ? O2 C3 1.284(2) . ? O3 C14 1.2803(19) . ? O4 C16 1.2771(19) . ? O5 C27 1.277(2) . ? O6 C29 1.277(2) . ? N1 C7 1.338(3) . ? N1 C6 1.338(3) . ? N2 C11 1.329(3) . ? N2 C12 1.338(3) . ? N3 C20 1.335(3) . ? N3 C19 1.342(3) . ? N4 C25 1.330(3) . ? N4 C24 1.332(3) . ? N5 C32 1.336(3) . ? N5 C33 1.340(3) . ? N6 C38 1.307(3) . ? N6 C37 1.315(3) . ? C1 C2 1.405(2) . ? C1 C4 1.493(2) . ? C2 C3 1.393(2) . ? C3 C9 1.493(2) . ? C4 C5 1.393(2) . ? C4 C8 1.394(2) . ? C5 C6 1.385(3) . ? C7 C8 1.385(3) . ? C9 C10 1.391(3) . ? C9 C13 1.392(3) . ? C10 C11 1.389(3) . ? C12 C13 1.392(3) . ? C14 C15 1.390(2) . ? C14 C17 1.496(2) . ? C15 C16 1.398(2) . ? C16 C22 1.494(2) . ? C17 C18 1.391(3) . ? C17 C21 1.391(2) . ? C18 C19 1.388(3) . ? C20 C21 1.384(3) . ? C22 C26 1.393(3) . ? C22 C23 1.394(2) . ? C23 C24 1.386(3) . ? C25 C26 1.389(3) . ? C27 C28 1.397(2) . ? C27 C30 1.497(2) . ? C28 C29 1.401(2) . ? C29 C35 1.498(2) . ? C30 C34 1.389(3) . ? C30 C31 1.396(2) . ? C31 C32 1.387(2) . ? C33 C34 1.393(3) . ? C35 C39 1.361(3) . ? C35 C36 1.370(3) . ? C36 C37 1.392(3) . ? C38 C39 1.388(3) . ? C40 C45 1.393(4) . ? C40 C41 1.401(4) . ? C40 C46 1.492(4) . ? C41 C42 1.375(5) . ? C42 C43 1.386(5) . ? C43 C44 1.383(4) . ? C44 C45 1.386(4) . ? C47 C50 1.173(14) . ? C47 C49 1.323(11) . ? C47 C48 1.329(8) . ? C48 C49 1.255(10) 2_666 ? C49 C48 1.255(10) 2_666 ? 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 O4 Al1 O2 90.10(6) . . ? O4 Al1 O3 91.27(6) . . ? O2 Al1 O3 94.74(6) . . ? O4 Al1 O5 91.47(6) . . ? O2 Al1 O5 176.87(6) . . ? O3 Al1 O5 87.94(5) . . ? O4 Al1 O1 179.85(6) . . ? O2 Al1 O1 89.89(6) . . ? O3 Al1 O1 88.88(6) . . ? O5 Al1 O1 88.54(5) . . ? O4 Al1 O6 90.26(6) . . ? O2 Al1 O6 88.43(6) . . ? O3 Al1 O6 176.48(6) . . ? O5 Al1 O6 88.84(6) . . ? O1 Al1 O6 89.59(6) . . ? C1 O1 Al1 125.67(11) . . ? C3 O2 Al1 125.04(11) . . ? C14 O3 Al1 126.24(11) . . ? C16 O4 Al1 127.17(11) . . ? C27 O5 Al1 126.67(11) . . ? C29 O6 Al1 125.19(11) . . ? C7 N1 C6 115.95(17) . . ? C11 N2 C12 116.49(17) . . ? C20 N3 C19 116.63(17) . . ? C25 N4 C24 116.68(18) . . ? C32 N5 C33 116.57(16) . . ? C38 N6 C37 115.04(19) . . ? O1 C1 C2 123.33(16) . . ? O1 C1 C4 116.41(15) . . ? C2 C1 C4 120.20(15) . . ? C3 C2 C1 121.23(15) . . ? O2 C3 C2 124.67(15) . . ? O2 C3 C9 115.81(15) . . ? C2 C3 C9 119.51(15) . . ? C5 C4 C8 117.65(16) . . ? C5 C4 C1 119.30(16) . . ? C8 C4 C1 123.03(16) . . ? C6 C5 C4 118.71(18) . . ? N1 C6 C5 124.49(18) . . ? N1 C7 C8 124.33(18) . . ? C7 C8 C4 118.86(17) . . ? C10 C9 C13 117.70(16) . . ? C10 C9 C3 122.14(16) . . ? C13 C9 C3 120.13(16) . . ? C11 C10 C9 118.99(18) . . ? N2 C11 C10 124.12(18) . . ? N2 C12 C13 124.10(19) . . ? C12 C13 C9 118.59(18) . . ? O3 C14 C15 124.75(15) . . ? O3 C14 C17 116.26(15) . . ? C15 C14 C17 118.98(15) . . ? C14 C15 C16 122.11(15) . . ? O4 C16 C15 123.98(16) . . ? O4 C16 C22 116.34(15) . . ? C15 C16 C22 119.68(15) . . ? C18 C17 C21 118.01(16) . . ? C18 C17 C14 119.56(16) . . ? C21 C17 C14 122.40(16) . . ? C19 C18 C17 119.02(17) . . ? N3 C19 C18 123.45(19) . . ? N3 C20 C21 124.36(19) . . ? C20 C21 C17 118.52(19) . . ? C26 C22 C23 117.61(17) . . ? C26 C22 C16 119.39(16) . . ? C23 C22 C16 123.00(16) . . ? C24 C23 C22 118.92(17) . . ? N4 C24 C23 123.95(18) . . ? N4 C25 C26 124.3(2) . . ? C25 C26 C22 118.57(18) . . ? O5 C27 C28 124.16(15) . . ? O5 C27 C30 115.05(14) . . ? C28 C27 C30 120.78(15) . . ? C27 C28 C29 121.16(16) . . ? O6 C29 C28 123.55(15) . . ? O6 C29 C35 115.72(15) . . ? C28 C29 C35 120.72(16) . . ? C34 C30 C31 118.34(15) . . ? C34 C30 C27 122.80(15) . . ? C31 C30 C27 118.84(16) . . ? C32 C31 C30 118.43(17) . . ? N5 C32 C31 124.22(17) . . ? N5 C33 C34 123.96(18) . . ? C30 C34 C33 118.48(17) . . ? C39 C35 C36 116.83(18) . . ? C39 C35 C29 123.44(17) . . ? C36 C35 C29 119.69(18) . . ? C35 C36 C37 119.1(2) . . ? N6 C37 C36 124.6(2) . . ? N6 C38 C39 125.1(2) . . ? C35 C39 C38 119.3(2) . . ? C45 C40 C41 116.8(3) . . ? C45 C40 C46 121.4(2) . . ? C41 C40 C46 121.8(3) . . ? C42 C41 C40 121.7(3) . . ? C41 C42 C43 120.9(3) . . ? C44 C43 C42 118.4(3) . . ? C43 C44 C45 120.7(3) . . ? C44 C45 C40 121.6(3) . . ? C50 C47 C49 110.5(9) . . ? C50 C47 C48 123.6(11) . . ? C49 C47 C48 125.3(8) . . ? C49 C48 C47 122.5(7) 2_666 . ? C48 C49 C47 112.2(7) 2_666 . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 30.16 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.951 _refine_diff_density_min -0.423 _refine_diff_density_rms 0.122 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.042 0.273 0.001 16397 7095 ' ' _platon_squeeze_details ; ; #===end data_compound_3_anna _database_code_depnum_ccdc_archive 'CCDC 771700' #TrackingRef '- dppd-strucs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C47 H51 Ag3 Al N9 O19 S4' _chemical_formula_weight 1524.80 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.2130 0.2455 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag 0.1306 4.2820 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M R3c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x+y, y, z+1/2' 'x, x-y, z+1/2' '-y, -x, z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' '-x+y+2/3, y+1/3, z+5/6' 'x+2/3, x-y+1/3, z+5/6' '-y+2/3, -x+1/3, z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x+y+1/3, y+2/3, z+7/6' 'x+1/3, x-y+2/3, z+7/6' '-y+1/3, -x+2/3, z+7/6' _cell_length_a 22.4562(3) _cell_length_b 22.4562(3) _cell_length_c 72.1481(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 31508.5(6) _cell_formula_units_Z 18 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 57004 _cell_measurement_theta_min 7.65 _cell_measurement_theta_max 72.39 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.446 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 13788 _exptl_absorpt_coefficient_mu 8.419 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.24 _exptl_absorpt_correction_T_max 0.27 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '135mm CCD detector on \k-goniostat' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 57004 _diffrn_reflns_av_R_equivalents 0.0738 _diffrn_reflns_av_sigmaI/netI 0.0327 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -84 _diffrn_reflns_limit_l_max 85 _diffrn_reflns_theta_min 7.65 _diffrn_reflns_theta_max 72.39 _reflns_number_total 12792 _reflns_number_gt 10519 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Oxford Diffraction Software' _computing_cell_refinement 'Oxford Diffraction Software' _computing_data_reduction 'Oxford Diffraction Software' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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. At some stage, all crystallographers have been confronted with a structure like that of compound anna, which exhibits high symmetry and considerable disorder. Several data collections inevitably ensue, in an effort to be completely certain about the space group assignment, and to model the disorder if possible. Ultimately, in this eighth instance an excellent data set (Rint = 0.0275, Rsigma = 0.0189, prior to SQUEEZE) was collected, which afforded good statistics and, equally importantly, bore none of the usual signs of merohedral/pseudo-merohedral twinning. The space groups possible were R-3c and R3c. The former did not afford a credible solution which, when the structure was solved, could be easily rationalised as there is no centre of inversion present either in the Al(L3) moieties or in the gross structure. The asymmetric unit then, as presented, consists of three Al1/3(L-Ag) fragments, three nitrates and some disordered solvent of recrystallisation. (We rationalised that, as the crystals lost solvent on exposure to air it was safe to assume that there is some lattice solvent present). The nitrates were hopelessly disordered, which suggests that they do not bind in any periodic way to the silvers, if indeed they bind at all. Thus, the anions and the disordered solvent were treated with the PLATON SQUEEZE routine and given the diffuse nature of the solvent and the available volume, four molecules of DMSO have been included per every 3 silvers in the unit cell. A correction for racemic twinning was also included in the refinement. ; _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^)+(0.1516P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.478(9) _refine_ls_number_reflns 12792 _refine_ls_number_parameters 497 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0767 _refine_ls_R_factor_gt 0.0719 _refine_ls_wR_factor_ref 0.1945 _refine_ls_wR_factor_gt 0.1893 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.14571(4) 0.30312(4) 0.148380(9) 0.1053(3) Uani 1 1 d . . . Al1 Al 0.3333 0.6667 0.22339(3) 0.0333(4) Uani 1 3 d S . . O1 O 0.25710(16) 0.63207(15) 0.23894(4) 0.0382(7) Uani 1 1 d . . . C1 C 0.2103(3) 0.5707(3) 0.24094(7) 0.0532(12) Uani 1 1 d . . . O2 O 0.28739(16) 0.58788(17) 0.20831(4) 0.0411(7) Uani 1 1 d . . . C2 C 0.1962(3) 0.5170(3) 0.22913(6) 0.0637(15) Uani 1 1 d . . . H2 H 0.1610 0.4716 0.2321 0.076 Uiso 1 1 calc R . . C3 C 0.2345(3) 0.5301(3) 0.21266(6) 0.0481(11) Uani 1 1 d . . . C4 C 0.1678(3) 0.5532(3) 0.25874(7) 0.0565(12) Uani 1 1 d . . . C5 C 0.1935(5) 0.5986(4) 0.27288(13) 0.108(4) Uani 1 1 d . . . H5 H 0.2360 0.6403 0.2716 0.129 Uiso 1 1 calc R . . C6 C 0.1558(6) 0.5826(6) 0.28950(14) 0.127(4) Uani 1 1 d . . . H6 H 0.1775 0.6066 0.3006 0.153 Uiso 1 1 calc R . . N7 N 0.0886(4) 0.5330(4) 0.28978(10) 0.111(3) Uani 1 1 d . . . C8 C 0.0682(5) 0.4900(4) 0.27705(15) 0.113(4) Uani 1 1 d . . . H8 H 0.0259 0.4484 0.2788 0.135 Uiso 1 1 calc R . . C9 C 0.1029(4) 0.4986(4) 0.26036(9) 0.0787(19) Uani 1 1 d . . . H9 H 0.0819 0.4673 0.2504 0.094 Uiso 1 1 calc R . . C10 C 0.2168(3) 0.4760(3) 0.19838(7) 0.0540(11) Uani 1 1 d . . . C11 C 0.1684(5) 0.4066(4) 0.20202(10) 0.096(3) Uani 1 1 d . . . H11 H 0.1474 0.3925 0.2139 0.115 Uiso 1 1 calc R . . C12 C 0.1526(4) 0.3604(4) 0.18792(13) 0.086(2) Uani 1 1 d . . . H12 H 0.1227 0.3132 0.1907 0.103 Uiso 1 1 calc R . . N13 N 0.1757(4) 0.3759(4) 0.17045(9) 0.094(2) Uani 1 1 d . . . C14 C 0.2202(3) 0.4400(4) 0.16716(7) 0.0637(16) Uani 1 1 d . . . H14 H 0.2410 0.4525 0.1553 0.076 Uiso 1 1 calc R . . C15 C 0.2386(3) 0.4912(3) 0.18053(7) 0.0506(11) Uani 1 1 d . . . H15 H 0.2670 0.5380 0.1771 0.061 Uiso 1 1 calc R . . Ag1A Ag 0.14269(4) 0.33850(3) 0.051842(8) 0.0933(2) Uani 1 1 d . . . Al1A Al 0.3333 0.6666 0.13610(3) 0.0538(6) Uani 1 3 d S . . O1A O 0.2566(2) 0.6306(2) 0.15158(5) 0.0563(9) Uani 1 1 d . . . C1A C 0.1971(3) 0.5765(3) 0.14964(7) 0.0616(14) Uani 1 1 d . . . O2A O 0.2908(2) 0.5899(2) 0.12040(6) 0.0611(10) Uani 1 1 d . . . C2A C 0.1802(3) 0.5294(3) 0.13494(8) 0.0641(14) Uani 1 1 d . . . H2A H 0.1348 0.4914 0.1339 0.077 Uiso 1 1 calc R . . C3A C 0.2289(4) 0.5380(4) 0.12207(9) 0.0687(15) Uani 1 1 d . . . C4A C 0.1475(3) 0.5612(4) 0.16506(8) 0.0708(17) Uani 1 1 d . . . C5A C 0.1720(3) 0.5936(3) 0.18177(7) 0.0544(12) Uani 1 1 d . . . H5A H 0.2199 0.6237 0.1836 0.065 Uiso 1 1 calc R . . C6A C 0.1257(4) 0.5814(4) 0.19591(9) 0.0748(18) Uani 1 1 d . . . H6A H 0.1424 0.6061 0.2072 0.090 Uiso 1 1 calc R . . N7A N 0.0604(3) 0.5377(4) 0.19444(8) 0.0845(19) Uani 1 1 d . . . C8A C 0.0366(4) 0.5057(8) 0.17802(12) 0.143(6) Uani 1 1 d . . . H8A H -0.0117 0.4771 0.1766 0.171 Uiso 1 1 calc R . . C9A C 0.0760(4) 0.5114(6) 0.16372(11) 0.108(4) Uani 1 1 d . . . H9A H 0.0575 0.4836 0.1530 0.129 Uiso 1 1 calc R . . C10A C 0.2108(4) 0.4891(4) 0.10656(7) 0.0682(15) Uani 1 1 d . . . C11A C 0.1540(5) 0.4240(3) 0.10645(8) 0.080(2) Uani 1 1 d . . . H11A H 0.1276 0.4064 0.1174 0.096 Uiso 1 1 calc R . . C12A C 0.1346(5) 0.3833(4) 0.09045(10) 0.088(2) Uani 1 1 d . . . H12A H 0.0907 0.3428 0.0899 0.105 Uiso 1 1 calc R . . N13A N 0.1774(3) 0.4009(4) 0.07574(8) 0.0792(16) Uani 1 1 d . . . C14A C 0.2298(5) 0.4612(5) 0.07499(13) 0.099(3) Uani 1 1 d . . . H14A H 0.2566 0.4745 0.0640 0.118 Uiso 1 1 calc R . . C15A C 0.2507(4) 0.5108(5) 0.09000(10) 0.084(2) Uani 1 1 d . . . H15A H 0.2893 0.5557 0.0888 0.101 Uiso 1 1 calc R . . Ag1B Ag 0.19621(4) 0.36404(4) -0.050232(7) 0.1010(2) Uani 1 1 d . . . Al1B Al 0.3333 0.6666 0.04145(3) 0.0421(5) Uani 1 3 d S . . O1B O 0.25476(18) 0.61824(19) 0.05626(4) 0.0477(8) Uani 1 1 d . . . C1B C 0.1976(3) 0.5643(3) 0.05207(7) 0.0584(13) Uani 1 1 d . . . O2B O 0.30165(18) 0.59022(19) 0.02530(4) 0.0463(8) Uani 1 1 d . . . C2B C 0.1847(3) 0.5274(3) 0.03532(8) 0.0613(14) Uani 1 1 d . . . H2B H 0.1391 0.4934 0.0322 0.074 Uiso 1 1 calc R . . C3B C 0.2407(3) 0.5414(3) 0.02301(6) 0.0523(12) Uani 1 1 d . . . C4B C 0.1405(3) 0.5414(3) 0.06590(7) 0.0635(15) Uani 1 1 d . . . C5B C 0.1554(5) 0.5781(4) 0.08290(10) 0.089(3) Uani 1 1 d . . . H5B H 0.2003 0.6154 0.0853 0.107 Uiso 1 1 calc R . . C6B C 0.1064(4) 0.5599(4) 0.09536(11) 0.089(2) Uani 1 1 d . . . H6B H 0.1168 0.5851 0.1066 0.107 Uiso 1 1 calc R . . N7B N 0.0404(3) 0.5057(3) 0.09266(9) 0.0729(16) Uani 1 1 d . . . C8B C 0.0272(5) 0.4688(5) 0.07773(10) 0.095(3) Uani 1 1 d . . . H8B H -0.0170 0.4296 0.0760 0.114 Uiso 1 1 calc R . . C9B C 0.0780(5) 0.4871(5) 0.06438(11) 0.096(3) Uani 1 1 d . . . H9B H 0.0674 0.4593 0.0536 0.115 Uiso 1 1 calc R . . C10B C 0.2301(4) 0.4981(3) 0.00702(9) 0.0661(15) Uani 1 1 d . . . C11B C 0.1650(4) 0.4616(5) -0.00220(9) 0.086(2) Uani 1 1 d . . . H11B H 0.1246 0.4554 0.0038 0.103 Uiso 1 1 calc R . . C12B C 0.1613(4) 0.4366(6) -0.01912(10) 0.105(3) Uani 1 1 d . . . H12B H 0.1230 0.4276 -0.0267 0.126 Uiso 1 1 calc R . . N13B N 0.2097(3) 0.4232(3) -0.02620(8) 0.0732(15) Uani 1 1 d . . . C14B C 0.2708(4) 0.4557(4) -0.01727(11) 0.090(2) Uani 1 1 d . . . H14B H 0.3081 0.4520 -0.0222 0.108 Uiso 1 1 calc R . . C15B C 0.2815(3) 0.4943(3) -0.00119(9) 0.0720(17) Uani 1 1 d . . . H15B H 0.3263 0.5184 0.0040 0.086 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.1475(6) 0.0973(4) 0.0656(4) -0.0511(3) -0.0200(3) 0.0570(4) Al1 0.0413(7) 0.0413(7) 0.0175(9) 0.000 0.000 0.0206(3) O1 0.0430(17) 0.0414(16) 0.0223(14) -0.0051(10) -0.0005(11) 0.0151(14) C1 0.052(3) 0.069(3) 0.038(2) -0.007(2) 0.0061(19) 0.030(3) O2 0.0495(17) 0.0475(18) 0.0202(13) -0.0018(11) 0.0013(11) 0.0196(15) C2 0.078(4) 0.061(3) 0.028(2) -0.0013(19) 0.019(2) 0.017(3) C3 0.050(3) 0.060(3) 0.034(2) -0.0066(19) -0.0025(18) 0.027(2) C4 0.068(3) 0.057(3) 0.036(2) 0.000(2) 0.013(2) 0.025(3) C5 0.086(5) 0.096(5) 0.076(5) -0.038(4) 0.035(4) -0.003(4) C6 0.124(8) 0.148(8) 0.069(5) -0.007(5) 0.070(6) 0.038(6) N7 0.101(5) 0.124(6) 0.062(4) -0.017(4) 0.050(4) 0.021(4) C8 0.100(6) 0.067(4) 0.117(7) -0.010(4) 0.069(6) 0.001(4) C9 0.068(4) 0.085(4) 0.053(3) -0.005(3) 0.023(3) 0.015(3) C10 0.061(3) 0.053(3) 0.039(2) -0.003(2) 0.004(2) 0.022(2) C11 0.135(7) 0.051(3) 0.054(4) -0.018(3) 0.017(4) 0.009(4) C12 0.086(5) 0.051(3) 0.082(5) -0.022(3) 0.011(4) 0.004(3) N13 0.134(6) 0.097(5) 0.043(3) -0.033(3) 0.001(3) 0.052(5) C14 0.067(3) 0.086(5) 0.026(2) -0.018(2) -0.0044(19) 0.029(3) C15 0.069(3) 0.056(3) 0.031(2) -0.0083(19) -0.0018(19) 0.034(2) Ag1A 0.1306(5) 0.0729(3) 0.0462(3) -0.01556(19) 0.0061(3) 0.0283(3) Al1A 0.0665(9) 0.0665(9) 0.0282(12) 0.000 0.000 0.0333(4) O1A 0.071(2) 0.073(2) 0.0286(17) -0.0106(14) -0.0069(15) 0.039(2) C1A 0.074(4) 0.067(3) 0.027(2) 0.006(2) 0.002(2) 0.022(3) O2A 0.078(3) 0.071(3) 0.0375(19) -0.0042(17) 0.0033(16) 0.040(2) C2A 0.058(3) 0.065(3) 0.055(3) -0.004(2) -0.001(2) 0.020(3) C3A 0.077(4) 0.087(4) 0.052(3) -0.001(3) 0.004(3) 0.048(4) C4A 0.058(3) 0.096(4) 0.034(3) -0.010(3) -0.006(2) 0.020(3) C5A 0.064(3) 0.054(3) 0.041(3) -0.013(2) -0.007(2) 0.026(2) C6A 0.070(4) 0.080(4) 0.049(3) -0.020(3) -0.032(3) 0.018(3) N7A 0.072(4) 0.109(5) 0.037(3) -0.018(2) 0.005(2) 0.019(3) C8A 0.059(4) 0.220(12) 0.048(4) -0.070(6) 0.013(3) -0.007(5) C9A 0.066(4) 0.164(9) 0.050(4) -0.041(5) 0.008(3) 0.025(5) C10A 0.090(4) 0.089(4) 0.032(2) -0.004(2) -0.004(2) 0.049(4) C11A 0.123(6) 0.064(4) 0.034(3) -0.006(2) 0.008(3) 0.033(4) C12A 0.123(6) 0.063(4) 0.047(3) -0.019(3) 0.022(3) 0.024(4) N13A 0.077(3) 0.095(4) 0.046(3) -0.021(3) 0.005(2) 0.029(3) C14A 0.115(6) 0.075(5) 0.064(5) 0.012(4) 0.015(4) 0.016(4) C15A 0.068(4) 0.104(5) 0.050(4) -0.023(3) 0.017(3) 0.020(4) Ag1B 0.1364(5) 0.1011(4) 0.0516(3) -0.0379(3) -0.0056(3) 0.0490(4) Al1B 0.0527(8) 0.0527(8) 0.0209(9) 0.000 0.000 0.0263(4) O1B 0.0513(19) 0.064(2) 0.0262(15) 0.0004(12) 0.0115(13) 0.0276(17) C1B 0.069(3) 0.075(4) 0.034(2) 0.013(2) 0.016(2) 0.038(3) O2B 0.064(2) 0.055(2) 0.0249(15) -0.0042(13) 0.0029(12) 0.0335(17) C2B 0.050(3) 0.053(3) 0.062(3) -0.004(2) 0.019(2) 0.013(2) C3B 0.056(3) 0.072(3) 0.0246(19) -0.0014(19) 0.0001(18) 0.029(3) C4B 0.072(4) 0.067(3) 0.033(2) 0.001(2) 0.021(2) 0.021(3) C5B 0.104(5) 0.066(4) 0.054(4) -0.025(3) 0.029(4) 0.010(4) C6B 0.078(4) 0.103(5) 0.051(4) -0.017(3) 0.025(3) 0.018(4) N7B 0.078(4) 0.063(3) 0.063(3) -0.005(2) 0.034(3) 0.024(3) C8B 0.105(6) 0.114(6) 0.044(4) 0.005(4) 0.025(4) 0.039(5) C9B 0.095(5) 0.123(6) 0.057(4) -0.035(4) 0.013(4) 0.043(5) C10B 0.076(4) 0.057(3) 0.054(3) -0.011(2) -0.006(3) 0.026(3) C11B 0.075(4) 0.112(6) 0.048(3) -0.015(3) 0.006(3) 0.031(4) C12B 0.077(4) 0.158(8) 0.055(4) -0.056(5) -0.007(3) 0.041(5) N13B 0.089(4) 0.061(3) 0.045(3) -0.015(2) 0.008(2) 0.019(3) C14B 0.076(4) 0.101(5) 0.083(5) -0.054(4) -0.014(3) 0.035(4) C15B 0.070(4) 0.060(3) 0.063(3) -0.007(3) 0.030(3) 0.015(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N13 2.135(6) . ? Ag1 N7 2.182(6) 12_554 ? Al1 O1 1.861(3) . ? Al1 O1 1.861(3) 3_565 ? Al1 O1 1.861(3) 2_665 ? Al1 O2 1.885(3) 3_565 ? Al1 O2 1.885(3) . ? Al1 O2 1.885(3) 2_665 ? O1 C1 1.256(7) . ? C1 C2 1.379(8) . ? C1 C4 1.529(7) . ? O2 C3 1.286(7) . ? C2 C3 1.409(7) . ? C3 C10 1.487(7) . ? C4 C5 1.351(9) . ? C4 C9 1.362(9) . ? C5 C6 1.407(10) . ? C6 N7 1.355(14) . ? N7 C8 1.242(12) . ? N7 Ag1 2.182(6) 18_554 ? C8 C9 1.395(9) . ? C10 C15 1.359(7) . ? C10 C11 1.408(9) . ? C11 C12 1.368(10) . ? C12 N13 1.341(12) . ? N13 C14 1.300(11) . ? C14 C15 1.396(8) . ? Ag1A N13A 2.110(6) . ? Ag1A N7A 2.196(6) 12_554 ? Al1A O1A 1.864(4) 2_665 ? Al1A O1A 1.864(4) . ? Al1A O1A 1.866(4) 3_565 ? Al1A O2A 1.875(4) . ? Al1A O2A 1.876(4) 2_665 ? Al1A O2A 1.877(4) 3_565 ? O1A C1A 1.288(7) . ? C1A C2A 1.409(8) . ? C1A C4A 1.489(9) . ? O2A C3A 1.299(9) . ? C2A C3A 1.372(9) . ? C3A C10A 1.476(9) . ? C4A C5A 1.373(8) . ? C4A C9A 1.429(10) . ? C5A C6A 1.383(10) . ? C6A N7A 1.299(10) . ? N7A C8A 1.350(9) . ? N7A Ag1A 2.196(6) 18_554 ? C8A C9A 1.322(10) . ? C10A C11A 1.378(11) . ? C10A C15A 1.425(9) . ? C11A C12A 1.399(8) . ? C12A N13A 1.352(9) . ? N13A C14A 1.276(11) . ? C14A C15A 1.452(12) . ? Ag1B N13B 2.113(5) . ? Ag1B N7B 2.203(5) 12_554 ? Al1B O1B 1.875(3) . ? Al1B O1B 1.876(3) 2_665 ? Al1B O1B 1.877(3) 3_565 ? Al1B O2B 1.893(4) . ? Al1B O2B 1.895(4) 3_565 ? Al1B O2B 1.895(4) 2_665 ? O1B C1B 1.285(7) . ? C1B C2B 1.411(8) . ? C1B C4B 1.498(7) . ? O2B C3B 1.265(7) . ? C2B C3B 1.441(7) . ? C3B C10B 1.451(8) . ? C4B C9B 1.326(11) . ? C4B C5B 1.421(8) . ? C5B C6B 1.318(10) . ? C6B N7B 1.383(10) . ? N7B C8B 1.299(11) . ? N7B Ag1B 2.203(5) 18_554 ? C8B C9B 1.390(11) . ? C10B C15B 1.337(10) . ? C10B C11B 1.433(10) . ? C11B C12B 1.329(9) . ? C12B N13B 1.362(10) . ? N13B C14B 1.352(10) . ? C14B C15B 1.395(9) . ? 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 N13 Ag1 N7 168.5(3) . 12_554 ? O1 Al1 O1 87.41(14) . 3_565 ? O1 Al1 O1 87.41(14) . 2_665 ? O1 Al1 O1 87.41(14) 3_565 2_665 ? O1 Al1 O2 92.67(14) . 3_565 ? O1 Al1 O2 89.93(12) 3_565 3_565 ? O1 Al1 O2 177.33(15) 2_665 3_565 ? O1 Al1 O2 89.93(13) . . ? O1 Al1 O2 177.33(15) 3_565 . ? O1 Al1 O2 92.66(14) 2_665 . ? O2 Al1 O2 90.00(14) 3_565 . ? O1 Al1 O2 177.32(15) . 2_665 ? O1 Al1 O2 92.67(14) 3_565 2_665 ? O1 Al1 O2 89.92(13) 2_665 2_665 ? O2 Al1 O2 90.00(14) 3_565 2_665 ? O2 Al1 O2 90.00(14) . 2_665 ? C1 O1 Al1 128.2(3) . . ? O1 C1 C2 126.1(4) . . ? O1 C1 C4 116.8(4) . . ? C2 C1 C4 117.0(5) . . ? C3 O2 Al1 127.1(3) . . ? C1 C2 C3 119.3(5) . . ? O2 C3 C2 125.2(5) . . ? O2 C3 C10 113.0(4) . . ? C2 C3 C10 121.8(5) . . ? C5 C4 C9 118.4(6) . . ? C5 C4 C1 117.7(6) . . ? C9 C4 C1 123.6(5) . . ? C4 C5 C6 118.4(8) . . ? N7 C6 C5 120.3(9) . . ? C8 N7 C6 117.0(6) . . ? C8 N7 Ag1 123.8(6) . 18_554 ? C6 N7 Ag1 117.9(5) . 18_554 ? N7 C8 C9 124.5(7) . . ? C4 C9 C8 118.2(7) . . ? C15 C10 C11 115.9(5) . . ? C15 C10 C3 122.3(5) . . ? C11 C10 C3 121.2(5) . . ? C12 C11 C10 117.7(7) . . ? N13 C12 C11 125.6(7) . . ? C14 N13 C12 116.3(6) . . ? C14 N13 Ag1 119.0(5) . . ? C12 N13 Ag1 124.7(6) . . ? N13 C14 C15 122.2(5) . . ? C10 C15 C14 121.7(6) . . ? N13A Ag1A N7A 166.6(3) . 12_554 ? O1A Al1A O1A 87.86(18) 2_665 . ? O1A Al1A O1A 87.82(18) 2_665 3_565 ? O1A Al1A O1A 87.82(18) . 3_565 ? O1A Al1A O2A 93.37(18) 2_665 . ? O1A Al1A O2A 91.63(18) . . ? O1A Al1A O2A 178.7(2) 3_565 . ? O1A Al1A O2A 91.58(18) 2_665 2_665 ? O1A Al1A O2A 178.8(2) . 2_665 ? O1A Al1A O2A 93.27(18) 3_565 2_665 ? O2A Al1A O2A 87.3(2) . 2_665 ? O1A Al1A O2A 178.6(2) 2_665 3_565 ? O1A Al1A O2A 93.32(18) . 3_565 ? O1A Al1A O2A 91.53(17) 3_565 3_565 ? O2A Al1A O2A 87.3(2) . 3_565 ? O2A Al1A O2A 87.2(2) 2_665 3_565 ? C1A O1A Al1A 129.9(3) . . ? O1A C1A C2A 123.6(5) . . ? O1A C1A C4A 116.1(5) . . ? C2A C1A C4A 120.0(5) . . ? C3A O2A Al1A 126.4(4) . . ? C3A C2A C1A 120.5(6) . . ? O2A C3A C2A 127.5(6) . . ? O2A C3A C10A 111.7(5) . . ? C2A C3A C10A 120.3(6) . . ? C5A C4A C9A 118.0(6) . . ? C5A C4A C1A 118.6(6) . . ? C9A C4A C1A 123.3(6) . . ? C4A C5A C6A 118.7(6) . . ? N7A C6A C5A 122.9(5) . . ? C6A N7A C8A 118.0(7) . . ? C6A N7A Ag1A 117.8(5) . 18_554 ? C8A N7A Ag1A 124.1(5) . 18_554 ? C9A C8A N7A 124.5(7) . . ? C8A C9A C4A 117.3(7) . . ? C11A C10A C15A 116.6(6) . . ? C11A C10A C3A 123.9(6) . . ? C15A C10A C3A 119.3(7) . . ? C10A C11A C12A 121.2(6) . . ? N13A C12A C11A 120.8(7) . . ? C14A N13A C12A 119.1(7) . . ? C14A N13A Ag1A 120.6(6) . . ? C12A N13A Ag1A 118.4(5) . . ? N13A C14A C15A 123.7(7) . . ? C10A C15A C14A 117.2(7) . . ? N13B Ag1B N7B 168.9(2) . 12_554 ? O1B Al1B O1B 90.79(17) . 2_665 ? O1B Al1B O1B 90.74(17) . 3_565 ? O1B Al1B O1B 90.74(17) 2_665 3_565 ? O1B Al1B O2B 90.43(15) . . ? O1B Al1B O2B 92.69(15) 2_665 . ? O1B Al1B O2B 176.37(17) 3_565 . ? O1B Al1B O2B 92.65(15) . 3_565 ? O1B Al1B O2B 176.39(17) 2_665 3_565 ? O1B Al1B O2B 90.34(15) 3_565 3_565 ? O2B Al1B O2B 86.17(17) . 3_565 ? O1B Al1B O2B 176.46(18) . 2_665 ? O1B Al1B O2B 90.38(15) 2_665 2_665 ? O1B Al1B O2B 92.59(15) 3_565 2_665 ? O2B Al1B O2B 86.17(17) . 2_665 ? O2B Al1B O2B 86.13(17) 3_565 2_665 ? C1B O1B Al1B 128.2(3) . . ? O1B C1B C2B 124.7(5) . . ? O1B C1B C4B 116.5(5) . . ? C2B C1B C4B 118.7(5) . . ? C3B O2B Al1B 128.2(3) . . ? C1B C2B C3B 120.0(5) . . ? O2B C3B C2B 123.8(5) . . ? O2B C3B C10B 115.4(5) . . ? C2B C3B C10B 120.7(5) . . ? C9B C4B C5B 116.0(6) . . ? C9B C4B C1B 126.2(5) . . ? C5B C4B C1B 117.6(6) . . ? C6B C5B C4B 119.4(7) . . ? C5B C6B N7B 122.6(7) . . ? C8B N7B C6B 118.7(6) . . ? C8B N7B Ag1B 121.5(5) . 18_554 ? C6B N7B Ag1B 118.2(4) . 18_554 ? N7B C8B C9B 119.6(9) . . ? C4B C9B C8B 123.4(7) . . ? C15B C10B C11B 115.1(6) . . ? C15B C10B C3B 122.5(6) . . ? C11B C10B C3B 122.1(6) . . ? C12B C11B C10B 119.9(7) . . ? C11B C12B N13B 123.3(8) . . ? C14B N13B C12B 114.1(6) . . ? C14B N13B Ag1B 121.1(5) . . ? C12B N13B Ag1B 124.6(5) . . ? N13B C14B C15B 123.0(7) . . ? C10B C15B C14B 121.4(7) . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 72.39 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 2.332 _refine_diff_density_min -0.432 _refine_diff_density_rms 0.114 #===end data_compound_4_h08clr1 _database_code_depnum_ccdc_archive 'CCDC 771701' #TrackingRef '- dppd-strucs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H45 O18 N9 Ga1 Ag3 S3' _chemical_formula_weight 1489.42 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' O O 0.0106 0.0060 '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' Ga Ga 0.2307 1.6083 '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 Rhombohedral _symmetry_space_group_name_H-M R3c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x+y, y, z+1/2' 'x, x-y, z+1/2' '-y, -x, z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' '-x+y+2/3, y+1/3, z+5/6' 'x+2/3, x-y+1/3, z+5/6' '-y+2/3, -x+1/3, z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x+y+1/3, y+2/3, z+7/6' 'x+1/3, x-y+2/3, z+7/6' '-y+1/3, -x+2/3, z+7/6' _cell_length_a 22.9930(6) _cell_length_b 22.9930(6) _cell_length_c 71.297(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 32643.2(16) _cell_formula_units_Z 18 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 239993 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 25.028 _exptl_crystal_description block _exptl_crystal_colour pale-straw _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.363 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 13356 _exptl_absorpt_coefficient_mu 1.310 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5929 _exptl_absorpt_correction_T_max 0.8407 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device_type '95mm CCD camera on \k-goniostat' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 90151 _diffrn_reflns_av_R_equivalents 0.1249 _diffrn_reflns_av_sigmaI/netI 0.0587 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -78 _diffrn_reflns_limit_l_max 78 _diffrn_reflns_theta_min 3.51 _diffrn_reflns_theta_max 23.25 _reflns_number_total 10267 _reflns_number_gt 6998 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97/2 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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. This structure suffered from the same issues as the isostructural aluminium analogue. It was notable in this case that suitably sized samples for crystallography all contained an internal flaw, which has impacted on the Rint of the data collected. Diffraction fall-off resulted in the using data to a maximum resolution of 0.9\%A in the final least squares. To minimize the esds on that data, a 3-day data collection was undertaken. The asymmetric unit then, as presented, consists of three Ga1/3(L-Ag) fragments, three nitrates and some disordered solvent of recrystallisation. The nitrates were hopelessly disordered, which suggests that they do not bind in any periodic way to the silvers. Thus, the anions and the disordered solvent were treated with the PLATON SQUEEZE routine and given the diffuse nature of the solvent and the available volume, three molecules of DMSO have been included in the asymmetric unit. A correction for racemic twinning was also included in the refinement. 6-membered rings were treated as rigid hexagons, and the ADPs in each were refined subject to similarity restraints. ; _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^)+(0.1979P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.39(3) _refine_ls_number_reflns 10267 _refine_ls_number_parameters 425 _refine_ls_number_restraints 217 _refine_ls_R_factor_all 0.1102 _refine_ls_R_factor_gt 0.0883 _refine_ls_wR_factor_ref 0.2856 _refine_ls_wR_factor_gt 0.2698 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.086 _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 0.81852(8) 1.17805(8) 0.667658(19) 0.1256(6) Uani 1 1 d . . . Ga1 Ga 1.0000 1.0000 0.74302(2) 0.0379(5) Uani 1 3 d S . . O1 O 0.9222(3) 0.9564(3) 0.75984(8) 0.0454(18) Uani 1 1 d . . . C1 C 0.8743(5) 0.9703(6) 0.76103(14) 0.058(3) Uani 1 1 d . . . Ag2 Ag 0.79655(8) 1.12833(9) 0.57079(2) 0.1289(6) Uani 1 1 d . . . Ga2 Ga 1.0000 1.0000 0.65469(2) 0.0430(4) Uani 1 3 d S . . O2 O 0.9535(3) 1.0343(4) 0.72738(9) 0.0489(18) Uani 1 1 d . . . C2 C 0.8653(6) 1.0076(6) 0.74807(18) 0.073(3) Uani 1 1 d . . . H2 H 0.8318 1.0187 0.7510 0.088 Uiso 1 1 calc R . . Ag3 Ag 0.84949(9) 1.15397(10) 0.46845(2) 0.1350(7) Uani 1 1 d . . . Ga3 Ga 1.0000 1.0000 0.56014(3) 0.0536(6) Uani 1 3 d S . . O3 O 0.9224(4) 0.9560(3) 0.67105(9) 0.0523(19) Uani 1 1 d . . . C3 C 0.8981(7) 1.0327(6) 0.73076(18) 0.080(4) Uani 1 1 d . . . O4 O 0.9521(4) 1.0302(4) 0.63815(9) 0.0518(19) Uani 1 1 d . . . C4 C 0.8631(6) 0.9495(8) 0.66784(17) 0.091(4) Uani 1 1 d . . . O5 O 0.9245(4) 0.9666(4) 0.57658(10) 0.065(2) Uani 1 1 d . . . C5 C 0.8441(6) 0.9764(6) 0.65380(14) 0.069(3) Uani 1 1 d . . . H5 H 0.7998 0.9694 0.6533 0.083 Uiso 1 1 calc R . . O6 O 0.9638(4) 1.0410(3) 0.54340(11) 0.058(2) Uani 1 1 d . . . C6 C 0.8910(6) 1.0144(5) 0.64007(15) 0.060(3) Uani 1 1 d . . . C7 C 0.8609(6) 0.9598(6) 0.56989(16) 0.071(3) Uani 1 1 d . . . C8 C 0.8529(7) 0.9841(9) 0.55392(17) 0.109(5) Uani 1 1 d . . . H8 H 0.8078 0.9701 0.5505 0.130 Uiso 1 1 calc R . . C9 C 0.9010(5) 1.0266(6) 0.54174(15) 0.068(3) Uani 1 1 d . . . N100 N 0.7556(4) 0.8899(5) 0.80974(11) 0.130(3) Uani 1 1 d GU . . C101 C 0.8240(4) 0.9122(5) 0.81009(11) 0.111(3) Uani 1 1 d GU . . H101 H 0.8444 0.9087 0.8213 0.134 Uiso 1 1 calc R . . C102 C 0.8626(3) 0.9398(5) 0.79406(13) 0.097(3) Uani 1 1 d GU . . H102 H 0.9094 0.9551 0.7943 0.117 Uiso 1 1 calc R . . C103 C 0.8327(4) 0.9450(5) 0.77768(11) 0.090(3) Uani 1 1 d GU . . C104 C 0.7643(4) 0.9226(6) 0.77732(11) 0.106(3) Uani 1 1 d GU . . H104 H 0.7439 0.9261 0.7661 0.127 Uiso 1 1 calc R . . C105 C 0.7257(3) 0.8951(6) 0.79335(13) 0.111(3) Uani 1 1 d GU . . H105 H 0.6789 0.8798 0.7931 0.134 Uiso 1 1 calc R . . N200 N 0.8436(4) 1.1305(4) 0.68947(9) 0.076(2) Uani 1 1 d GU . . C201 C 0.8886(4) 1.1085(4) 0.68548(7) 0.073(2) Uani 1 1 d GU . . H201 H 0.9077 1.1149 0.6733 0.088 Uiso 1 1 calc R . . C202 C 0.9058(4) 1.0772(4) 0.69931(9) 0.072(2) Uani 1 1 d GU . . H202 H 0.9366 1.0621 0.6966 0.086 Uiso 1 1 calc R . . C203 C 0.8779(4) 1.0678(5) 0.71712(8) 0.075(2) Uani 1 1 d GU . . C204 C 0.8329(4) 1.0898(5) 0.72111(8) 0.086(2) Uani 1 1 d GU . . H204 H 0.8138 1.0834 0.7333 0.103 Uiso 1 1 calc R . . C205 C 0.8157(4) 1.1211(5) 0.70729(10) 0.084(2) Uani 1 1 d GU . . H205 H 0.7849 1.1362 0.7100 0.100 Uiso 1 1 calc R . . N300 N 0.7295(3) 0.8493(5) 0.71425(9) 0.098(3) Uani 1 1 d GU . . C301 C 0.7031(3) 0.8528(5) 0.69702(10) 0.105(3) Uani 1 1 d GU . . H301 H 0.6560 0.8342 0.6956 0.126 Uiso 1 1 calc R . . C302 C 0.7456(4) 0.8835(5) 0.68186(8) 0.098(3) Uani 1 1 d GU . . H302 H 0.7275 0.8859 0.6701 0.118 Uiso 1 1 calc R . . C303 C 0.8145(3) 0.9108(5) 0.68393(8) 0.081(3) Uani 1 1 d GU . . C304 C 0.8409(3) 0.9073(5) 0.70116(10) 0.078(2) Uani 1 1 d GU . . H304 H 0.8880 0.9259 0.7026 0.094 Uiso 1 1 calc R . . C305 C 0.7984(4) 0.8766(5) 0.71632(8) 0.085(3) Uani 1 1 d GU . . H305 H 0.8164 0.8742 0.7281 0.102 Uiso 1 1 calc R . . N400 N 0.8320(4) 1.1015(5) 0.59536(10) 0.097(2) Uani 1 1 d GU . . C401 C 0.7925(4) 1.0774(6) 0.61138(11) 0.102(3) Uani 1 1 d GU . . H401 H 0.7529 1.0805 0.6125 0.123 Uiso 1 1 calc R . . C402 C 0.8109(4) 1.0489(5) 0.62571(10) 0.095(3) Uani 1 1 d GU . . H402 H 0.7839 1.0324 0.6367 0.114 Uiso 1 1 calc R . . C403 C 0.8687(4) 1.0444(5) 0.62404(10) 0.089(2) Uani 1 1 d GU . . C404 C 0.9082(4) 1.0684(5) 0.60802(12) 0.091(3) Uani 1 1 d GU . . H404 H 0.9477 1.0654 0.6069 0.109 Uiso 1 1 calc R . . C405 C 0.8898(4) 1.0970(5) 0.59368(9) 0.087(3) Uani 1 1 d GU . . H405 H 0.9168 1.1134 0.5827 0.104 Uiso 1 1 calc R . . N500 N 0.7070(5) 0.8598(7) 0.61152(16) 0.144(4) Uani 1 1 d GU . . C501 C 0.6958(5) 0.8901(8) 0.59614(17) 0.149(4) Uani 1 1 d GU . . H501 H 0.6535 0.8873 0.5945 0.179 Uiso 1 1 calc R . . C502 C 0.7467(5) 0.9245(8) 0.58310(15) 0.127(4) Uani 1 1 d GU . . H502 H 0.7391 0.9453 0.5726 0.153 Uiso 1 1 calc R . . C503 C 0.8087(5) 0.9286(7) 0.58545(14) 0.121(3) Uani 1 1 d GU . . C504 C 0.8198(5) 0.8983(7) 0.60083(16) 0.124(4) Uani 1 1 d GU . . H504 H 0.8621 0.9011 0.6024 0.149 Uiso 1 1 calc R . . C505 C 0.7689(6) 0.8639(7) 0.61386(14) 0.125(3) Uani 1 1 d GU . . H505 H 0.7765 0.8431 0.6244 0.150 Uiso 1 1 calc R . . N600 N 0.8626(5) 1.1065(6) 0.49300(12) 0.121(3) Uani 1 1 d GU . . C601 C 0.8111(4) 1.0493(6) 0.50140(14) 0.134(3) Uani 1 1 d GU . . H601 H 0.7670 1.0288 0.4964 0.160 Uiso 1 1 calc R . . C602 C 0.8242(5) 1.0222(5) 0.51718(15) 0.136(3) Uani 1 1 d GU . . H602 H 0.7891 0.9831 0.5229 0.163 Uiso 1 1 calc R . . C603 C 0.8888(5) 1.0523(6) 0.52455(13) 0.109(3) Uani 1 1 d GU . . C604 C 0.9403(4) 1.1095(6) 0.51614(15) 0.123(3) Uani 1 1 d GU . . H604 H 0.9844 1.1300 0.5212 0.147 Uiso 1 1 calc R . . C605 C 0.9272(4) 1.1366(5) 0.50037(15) 0.127(3) Uani 1 1 d GU . . H605 H 0.9624 1.1756 0.4946 0.152 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.1715(14) 0.1481(13) 0.0870(10) 0.0366(8) -0.0279(8) 0.1023(12) Ga1 0.0442(7) 0.0442(7) 0.0254(9) 0.000 0.000 0.0221(3) O1 0.025(4) 0.066(5) 0.027(3) 0.009(3) 0.009(3) 0.009(3) C1 0.043(6) 0.073(7) 0.050(6) 0.008(5) 0.012(4) 0.022(5) Ag2 0.1913(15) 0.1972(16) 0.0717(7) 0.0427(9) 0.0130(9) 0.1522(13) Ga2 0.0509(6) 0.0509(6) 0.0271(10) 0.000 0.000 0.0255(3) O2 0.049(4) 0.077(5) 0.035(4) 0.010(3) -0.004(3) 0.042(4) C2 0.063(7) 0.081(8) 0.085(9) -0.016(7) 0.008(6) 0.043(6) Ag3 0.1745(15) 0.1955(17) 0.0828(10) 0.0658(9) 0.0185(8) 0.1282(15) Ga3 0.0622(9) 0.0622(9) 0.0363(11) 0.000 0.000 0.0311(4) O3 0.038(4) 0.075(5) 0.031(4) 0.020(3) 0.012(3) 0.019(4) C3 0.087(9) 0.087(9) 0.080(9) 0.053(7) 0.032(7) 0.055(8) O4 0.054(5) 0.063(4) 0.034(4) 0.009(3) -0.003(3) 0.025(4) C4 0.055(8) 0.137(11) 0.044(7) 0.010(7) 0.035(6) 0.020(8) O5 0.075(6) 0.066(5) 0.039(4) 0.002(3) 0.016(4) 0.025(4) C5 0.083(8) 0.101(9) 0.042(6) 0.020(6) 0.006(5) 0.060(7) O6 0.057(5) 0.044(4) 0.061(5) 0.005(3) 0.016(3) 0.016(4) C6 0.064(8) 0.063(6) 0.068(7) 0.020(5) 0.015(5) 0.043(6) C7 0.082(8) 0.093(9) 0.066(8) -0.010(7) -0.016(6) 0.066(7) C8 0.080(9) 0.170(15) 0.052(8) 0.025(8) 0.020(7) 0.044(10) C9 0.037(6) 0.084(8) 0.064(7) 0.026(6) 0.019(5) 0.016(6) N100 0.102(5) 0.155(6) 0.110(6) 0.041(5) 0.050(5) 0.048(5) C101 0.092(5) 0.147(6) 0.101(6) 0.043(5) 0.046(5) 0.064(5) C102 0.086(5) 0.132(6) 0.090(5) 0.037(5) 0.049(4) 0.067(5) C103 0.086(5) 0.124(6) 0.083(5) 0.033(5) 0.040(4) 0.070(5) C104 0.092(5) 0.140(6) 0.094(5) 0.034(5) 0.044(4) 0.065(5) C105 0.092(5) 0.145(6) 0.102(6) 0.040(5) 0.046(5) 0.063(5) N200 0.100(4) 0.099(4) 0.057(4) 0.041(3) -0.003(3) 0.071(4) C201 0.094(5) 0.097(5) 0.048(4) 0.032(3) 0.003(3) 0.063(4) C202 0.092(5) 0.097(5) 0.050(4) 0.024(4) 0.015(3) 0.065(4) C203 0.094(5) 0.107(5) 0.057(4) 0.020(4) 0.015(4) 0.074(4) C204 0.103(5) 0.113(5) 0.066(4) 0.024(4) 0.012(4) 0.072(4) C205 0.102(5) 0.110(5) 0.068(4) 0.030(4) 0.007(4) 0.075(4) N300 0.076(4) 0.138(5) 0.053(4) 0.024(4) 0.008(4) 0.032(4) C301 0.079(4) 0.139(6) 0.057(4) 0.030(4) -0.001(4) 0.024(4) C302 0.072(4) 0.138(6) 0.053(4) 0.029(4) 0.003(4) 0.029(4) C303 0.065(4) 0.124(6) 0.044(4) 0.032(4) 0.009(4) 0.040(4) C304 0.068(4) 0.117(5) 0.042(4) 0.028(4) 0.008(3) 0.041(4) C305 0.070(4) 0.128(5) 0.046(4) 0.028(4) 0.007(4) 0.042(4) N400 0.123(5) 0.118(5) 0.068(4) 0.034(4) 0.011(4) 0.073(5) C401 0.117(5) 0.132(6) 0.074(4) 0.038(4) 0.012(4) 0.073(5) C402 0.105(5) 0.135(6) 0.067(4) 0.042(4) 0.015(4) 0.076(5) C403 0.097(5) 0.130(5) 0.060(4) 0.033(4) 0.011(4) 0.071(5) C404 0.099(5) 0.126(5) 0.065(4) 0.038(4) 0.009(4) 0.069(5) C405 0.109(5) 0.116(5) 0.062(4) 0.035(4) 0.008(4) 0.076(5) N500 0.124(6) 0.192(8) 0.110(6) 0.080(6) 0.026(5) 0.074(6) C501 0.123(6) 0.199(8) 0.108(6) 0.072(6) 0.035(5) 0.068(6) C502 0.108(6) 0.189(8) 0.096(6) 0.072(6) 0.042(5) 0.082(6) C503 0.108(6) 0.182(8) 0.094(6) 0.069(6) 0.040(5) 0.089(6) C504 0.114(6) 0.181(8) 0.097(6) 0.076(6) 0.032(5) 0.089(6) C505 0.113(6) 0.183(8) 0.104(6) 0.077(6) 0.028(5) 0.092(6) N600 0.132(6) 0.182(7) 0.093(6) 0.060(5) 0.019(5) 0.112(6) C601 0.143(6) 0.186(8) 0.096(6) 0.063(5) 0.011(5) 0.101(6) C602 0.148(6) 0.181(8) 0.099(6) 0.065(5) 0.015(5) 0.097(6) C603 0.127(6) 0.168(7) 0.090(6) 0.062(5) 0.022(5) 0.118(6) C604 0.131(6) 0.179(8) 0.099(6) 0.059(5) 0.024(5) 0.108(6) C605 0.131(6) 0.187(8) 0.098(6) 0.061(5) 0.020(5) 0.107(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N200 2.139(4) . ? Ag1 N100 2.175(6) 10_554 ? Ga1 O1 1.962(6) . ? Ga1 O1 1.962(6) 2_765 ? Ga1 O1 1.962(6) 3_675 ? Ga1 O2 1.963(7) 2_765 ? Ga1 O2 1.964(7) . ? Ga1 O2 1.964(7) 3_675 ? O1 C1 1.293(13) . ? C1 C2 1.345(16) . ? C1 C103 1.451(11) . ? Ag2 N400 2.148(5) . ? Ag2 N300 2.154(5) 10_554 ? Ga2 O3 1.940(7) 3_675 ? Ga2 O3 1.940(7) 2_765 ? Ga2 O3 1.940(7) . ? Ga2 O4 1.962(7) . ? Ga2 O4 1.962(7) 2_765 ? Ga2 O4 1.962(7) 3_675 ? O2 C3 1.279(13) . ? C2 C3 1.410(16) . ? C2 H2 0.9500 . ? Ag3 N600 2.162(6) . ? Ag3 N500 2.177(7) 10_554 ? Ga3 O5 1.909(8) 3_675 ? Ga3 O5 1.909(8) 2_765 ? Ga3 O5 1.909(8) . ? Ga3 O6 1.947(9) . ? Ga3 O6 1.947(9) 2_765 ? Ga3 O6 1.947(9) 3_675 ? O3 C4 1.315(16) . ? C3 C203 1.478(12) . ? O4 C6 1.271(12) . ? C4 C5 1.358(18) . ? C4 C303 1.537(12) . ? O5 C7 1.469(14) . ? C5 C6 1.393(15) . ? C5 H5 0.9500 . ? O6 C9 1.314(13) . ? C6 C403 1.548(11) . ? C7 C8 1.322(17) . ? C7 C503 1.525(14) . ? C8 C9 1.361(16) . ? C8 H8 0.9500 . ? C9 C603 1.448(12) . ? N100 C101 1.3900 . ? N100 C105 1.3900 . ? N100 Ag1 2.175(6) 16_544 ? C101 C102 1.3900 . ? C101 H101 0.9500 . ? C102 C103 1.3900 . ? C102 H102 0.9500 . ? C103 C104 1.3900 . ? C104 C105 1.3900 . ? C104 H104 0.9500 . ? C105 H105 0.9500 . ? N200 C201 1.3900 . ? N200 C205 1.3900 . ? C201 C202 1.3900 . ? C201 H201 0.9500 . ? C202 C203 1.3900 . ? C202 H202 0.9500 . ? C203 C204 1.3900 . ? C204 C205 1.3900 . ? C204 H204 0.9500 . ? C205 H205 0.9500 . ? N300 C301 1.3900 . ? N300 C305 1.3900 . ? N300 Ag2 2.154(5) 16_544 ? C301 C302 1.3900 . ? C301 H301 0.9500 . ? C302 C303 1.3900 . ? C302 H302 0.9500 . ? C303 C304 1.3900 . ? C304 C305 1.3900 . ? C304 H304 0.9500 . ? C305 H305 0.9500 . ? N400 C401 1.3900 . ? N400 C405 1.3900 . ? C401 C402 1.3900 . ? C401 H401 0.9500 . ? C402 C403 1.3900 . ? C402 H402 0.9500 . ? C403 C404 1.3900 . ? C404 C405 1.3900 . ? C404 H404 0.9500 . ? C405 H405 0.9500 . ? N500 C501 1.3900 . ? N500 C505 1.3900 . ? N500 Ag3 2.177(7) 16_544 ? C501 C502 1.3900 . ? C501 H501 0.9500 . ? C502 C503 1.3900 . ? C502 H502 0.9500 . ? C503 C504 1.3900 . ? C504 C505 1.3900 . ? C504 H504 0.9500 . ? C505 H505 0.9500 . ? N600 C601 1.3900 . ? N600 C605 1.3900 . ? C601 C602 1.3900 . ? C601 H601 0.9500 . ? C602 C603 1.3900 . ? C602 H602 0.9500 . ? C603 C604 1.3900 . ? C604 C605 1.3900 . ? C604 H604 0.9500 . ? C605 H605 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N200 Ag1 N100 172.5(3) . 10_554 ? O1 Ga1 O1 86.5(3) . 2_765 ? O1 Ga1 O1 86.5(3) . 3_675 ? O1 Ga1 O1 86.5(3) 2_765 3_675 ? O1 Ga1 O2 91.8(3) . 2_765 ? O1 Ga1 O2 90.7(3) 2_765 2_765 ? O1 Ga1 O2 176.8(3) 3_675 2_765 ? O1 Ga1 O2 90.7(3) . . ? O1 Ga1 O2 176.8(3) 2_765 . ? O1 Ga1 O2 91.8(3) 3_675 . ? O2 Ga1 O2 90.9(3) 2_765 . ? O1 Ga1 O2 176.8(3) . 3_675 ? O1 Ga1 O2 91.8(3) 2_765 3_675 ? O1 Ga1 O2 90.6(3) 3_675 3_675 ? O2 Ga1 O2 90.9(3) 2_765 3_675 ? O2 Ga1 O2 90.9(3) . 3_675 ? C1 O1 Ga1 125.8(6) . . ? O1 C1 C2 122.2(9) . . ? O1 C1 C103 115.2(9) . . ? C2 C1 C103 122.5(10) . . ? N400 Ag2 N300 163.5(4) . 10_554 ? O3 Ga2 O3 87.6(3) 3_675 2_765 ? O3 Ga2 O3 87.6(3) 3_675 . ? O3 Ga2 O3 87.6(3) 2_765 . ? O3 Ga2 O4 94.1(3) 3_675 . ? O3 Ga2 O4 177.6(3) 2_765 . ? O3 Ga2 O4 90.7(3) . . ? O3 Ga2 O4 177.6(3) 3_675 2_765 ? O3 Ga2 O4 90.7(3) 2_765 2_765 ? O3 Ga2 O4 94.1(3) . 2_765 ? O4 Ga2 O4 87.6(3) . 2_765 ? O3 Ga2 O4 90.7(3) 3_675 3_675 ? O3 Ga2 O4 94.1(3) 2_765 3_675 ? O3 Ga2 O4 177.6(3) . 3_675 ? O4 Ga2 O4 87.6(3) . 3_675 ? O4 Ga2 O4 87.6(3) 2_765 3_675 ? C3 O2 Ga1 128.0(6) . . ? C1 C2 C3 129.9(10) . . ? C1 C2 H2 115.0 . . ? C3 C2 H2 115.0 . . ? N600 Ag3 N500 170.9(4) . 10_554 ? O5 Ga3 O5 86.3(4) 3_675 2_765 ? O5 Ga3 O5 86.3(4) 3_675 . ? O5 Ga3 O5 86.3(4) 2_765 . ? O5 Ga3 O6 94.7(3) 3_675 . ? O5 Ga3 O6 178.6(3) 2_765 . ? O5 Ga3 O6 92.7(3) . . ? O5 Ga3 O6 178.6(3) 3_675 2_765 ? O5 Ga3 O6 92.7(3) 2_765 2_765 ? O5 Ga3 O6 94.7(3) . 2_765 ? O6 Ga3 O6 86.3(3) . 2_765 ? O5 Ga3 O6 92.7(3) 3_675 3_675 ? O5 Ga3 O6 94.7(3) 2_765 3_675 ? O5 Ga3 O6 178.6(3) . 3_675 ? O6 Ga3 O6 86.3(3) . 3_675 ? O6 Ga3 O6 86.3(3) 2_765 3_675 ? C4 O3 Ga2 125.9(7) . . ? O2 C3 C2 119.8(10) . . ? O2 C3 C203 116.1(9) . . ? C2 C3 C203 123.4(10) . . ? C6 O4 Ga2 124.8(6) . . ? O3 C4 C5 128.8(10) . . ? O3 C4 C303 110.4(11) . . ? C5 C4 C303 120.5(11) . . ? C7 O5 Ga3 120.0(7) . . ? C4 C5 C6 118.7(11) . . ? C4 C5 H5 120.6 . . ? C6 C5 H5 120.6 . . ? C9 O6 Ga3 128.0(6) . . ? O4 C6 C5 130.7(10) . . ? O4 C6 C403 111.0(8) . . ? C5 C6 C403 118.3(9) . . ? C8 C7 O5 125.2(12) . . ? C8 C7 C503 125.5(11) . . ? O5 C7 C503 108.8(8) . . ? C7 C8 C9 128.2(14) . . ? C7 C8 H8 115.9 . . ? C9 C8 H8 115.9 . . ? O6 C9 C8 121.3(11) . . ? O6 C9 C603 112.7(8) . . ? C8 C9 C603 125.4(11) . . ? C101 N100 C105 120.0 . . ? C101 N100 Ag1 121.3(5) . 16_544 ? C105 N100 Ag1 118.7(5) . 16_544 ? N100 C101 C102 120.0 . . ? N100 C101 H101 120.0 . . ? C102 C101 H101 120.0 . . ? C103 C102 C101 120.0 . . ? C103 C102 H102 120.0 . . ? C101 C102 H102 120.0 . . ? C102 C103 C104 120.0 . . ? C102 C103 C1 117.8(7) . . ? C104 C103 C1 122.1(7) . . ? C103 C104 C105 120.0 . . ? C103 C104 H104 120.0 . . ? C105 C104 H104 120.0 . . ? C104 C105 N100 120.0 . . ? C104 C105 H105 120.0 . . ? N100 C105 H105 120.0 . . ? C201 N200 C205 120.0 . . ? C201 N200 Ag1 118.5(3) . . ? C205 N200 Ag1 121.5(3) . . ? C202 C201 N200 120.0 . . ? C202 C201 H201 120.0 . . ? N200 C201 H201 120.0 . . ? C201 C202 C203 120.0 . . ? C201 C202 H202 120.0 . . ? C203 C202 H202 120.0 . . ? C204 C203 C202 120.0 . . ? C204 C203 C3 123.9(6) . . ? C202 C203 C3 116.1(6) . . ? C205 C204 C203 120.0 . . ? C205 C204 H204 120.0 . . ? C203 C204 H204 120.0 . . ? C204 C205 N200 120.0 . . ? C204 C205 H205 120.0 . . ? N200 C205 H205 120.0 . . ? C301 N300 C305 120.0 . . ? C301 N300 Ag2 121.3(4) . 16_544 ? C305 N300 Ag2 118.5(4) . 16_544 ? N300 C301 C302 120.0 . . ? N300 C301 H301 120.0 . . ? C302 C301 H301 120.0 . . ? C303 C302 C301 120.0 . . ? C303 C302 H302 120.0 . . ? C301 C302 H302 120.0 . . ? C304 C303 C302 120.0 . . ? C304 C303 C4 118.7(7) . . ? C302 C303 C4 121.1(7) . . ? C303 C304 C305 120.0 . . ? C303 C304 H304 120.0 . . ? C305 C304 H304 120.0 . . ? C304 C305 N300 120.0 . . ? C304 C305 H305 120.0 . . ? N300 C305 H305 120.0 . . ? C401 N400 C405 120.0 . . ? C401 N400 Ag2 121.2(4) . . ? C405 N400 Ag2 117.7(4) . . ? C402 C401 N400 120.0 . . ? C402 C401 H401 120.0 . . ? N400 C401 H401 120.0 . . ? C403 C402 C401 120.0 . . ? C403 C402 H402 120.0 . . ? C401 C402 H402 120.0 . . ? C402 C403 C404 120.0 . . ? C402 C403 C6 120.8(6) . . ? C404 C403 C6 119.2(6) . . ? C403 C404 C405 120.0 . . ? C403 C404 H404 120.0 . . ? C405 C404 H404 120.0 . . ? C404 C405 N400 120.0 . . ? C404 C405 H405 120.0 . . ? N400 C405 H405 120.0 . . ? C501 N500 C505 120.0 . . ? C501 N500 Ag3 122.5(5) . 16_544 ? C505 N500 Ag3 116.6(5) . 16_544 ? C502 C501 N500 120.0 . . ? C502 C501 H501 120.0 . . ? N500 C501 H501 120.0 . . ? C501 C502 C503 120.0 . . ? C501 C502 H502 120.0 . . ? C503 C502 H502 120.0 . . ? C502 C503 C504 120.0 . . ? C502 C503 C7 119.0(7) . . ? C504 C503 C7 120.6(7) . . ? C505 C504 C503 120.0 . . ? C505 C504 H504 120.0 . . ? C503 C504 H504 120.0 . . ? C504 C505 N500 120.0 . . ? C504 C505 H505 120.0 . . ? N500 C505 H505 120.0 . . ? C601 N600 C605 120.0 . . ? C601 N600 Ag3 124.0(5) . . ? C605 N600 Ag3 116.0(5) . . ? N600 C601 C602 120.0 . . ? N600 C601 H601 120.0 . . ? C602 C601 H601 120.0 . . ? C603 C602 C601 120.0 . . ? C603 C602 H602 120.0 . . ? C601 C602 H602 120.0 . . ? C602 C603 C604 120.0 . . ? C602 C603 C9 119.6(8) . . ? C604 C603 C9 120.2(8) . . ? C603 C604 C605 120.0 . . ? C603 C604 H604 120.0 . . ? C605 C604 H604 120.0 . . ? C604 C605 N600 120.0 . . ? C604 C605 H605 120.0 . . ? N600 C605 H605 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Ga1 O1 C1 160.5(8) 2_765 . . . ? O1 Ga1 O1 C1 73.7(9) 3_675 . . . ? O2 Ga1 O1 C1 -109.0(8) 2_765 . . . ? O2 Ga1 O1 C1 -18.0(8) . . . . ? O2 Ga1 O1 C1 102(5) 3_675 . . . ? Ga1 O1 C1 C2 13.7(15) . . . . ? Ga1 O1 C1 C103 -164.1(7) . . . . ? O1 Ga1 O2 C3 8.9(10) . . . . ? O1 Ga1 O2 C3 -19(6) 2_765 . . . ? O1 Ga1 O2 C3 -77.7(10) 3_675 . . . ? O2 Ga1 O2 C3 100.7(12) 2_765 . . . ? O2 Ga1 O2 C3 -168.3(10) 3_675 . . . ? O1 C1 C2 C3 6(2) . . . . ? C103 C1 C2 C3 -175.8(13) . . . . ? O3 Ga2 O3 C4 100.6(11) 3_675 . . . ? O3 Ga2 O3 C4 -171.7(10) 2_765 . . . ? O4 Ga2 O3 C4 6.5(10) . . . . ? O4 Ga2 O3 C4 -81.1(10) 2_765 . . . ? O4 Ga2 O3 C4 54(8) 3_675 . . . ? Ga1 O2 C3 C2 4.3(18) . . . . ? Ga1 O2 C3 C203 174.9(7) . . . . ? C1 C2 C3 O2 -16(2) . . . . ? C1 C2 C3 C203 173.9(12) . . . . ? O3 Ga2 O4 C6 -92.3(8) 3_675 . . . ? O3 Ga2 O4 C6 42(8) 2_765 . . . ? O3 Ga2 O4 C6 -4.7(9) . . . . ? O4 Ga2 O4 C6 89.4(10) 2_765 . . . ? O4 Ga2 O4 C6 177.1(9) 3_675 . . . ? Ga2 O3 C4 C5 -7(2) . . . . ? Ga2 O3 C4 C303 179.1(7) . . . . ? O5 Ga3 O5 C7 114.2(9) 3_675 . . . ? O5 Ga3 O5 C7 -159.3(8) 2_765 . . . ? O6 Ga3 O5 C7 19.7(7) . . . . ? O6 Ga3 O5 C7 -66.9(7) 2_765 . . . ? O6 Ga3 O5 C7 69(15) 3_675 . . . ? O3 C4 C5 C6 3(2) . . . . ? C303 C4 C5 C6 176.3(11) . . . . ? O5 Ga3 O6 C9 -106.8(9) 3_675 . . . ? O5 Ga3 O6 C9 25(16) 2_765 . . . ? O5 Ga3 O6 C9 -20.3(10) . . . . ? O6 Ga3 O6 C9 74.2(11) 2_765 . . . ? O6 Ga3 O6 C9 160.7(9) 3_675 . . . ? Ga2 O4 C6 C5 2.9(17) . . . . ? Ga2 O4 C6 C403 -177.3(6) . . . . ? C4 C5 C6 O4 -1(2) . . . . ? C4 C5 C6 C403 179.5(12) . . . . ? Ga3 O5 C7 C8 -10.6(16) . . . . ? Ga3 O5 C7 C503 177.0(8) . . . . ? O5 C7 C8 C9 -9(3) . . . . ? C503 C7 C8 C9 162.0(15) . . . . ? Ga3 O6 C9 C8 8.3(18) . . . . ? Ga3 O6 C9 C603 -163.1(8) . . . . ? C7 C8 C9 O6 11(3) . . . . ? C7 C8 C9 C603 -179.0(15) . . . . ? C105 N100 C101 C102 0.0 . . . . ? Ag1 N100 C101 C102 178.8(8) 16_544 . . . ? N100 C101 C102 C103 0.0 . . . . ? C101 C102 C103 C104 0.0 . . . . ? C101 C102 C103 C1 -176.4(10) . . . . ? O1 C1 C103 C102 31.4(12) . . . . ? C2 C1 C103 C102 -146.4(10) . . . . ? O1 C1 C103 C104 -144.9(8) . . . . ? C2 C1 C103 C104 37.3(14) . . . . ? C102 C103 C104 C105 0.0 . . . . ? C1 C103 C104 C105 176.2(10) . . . . ? C103 C104 C105 N100 0.0 . . . . ? C101 N100 C105 C104 0.0 . . . . ? Ag1 N100 C105 C104 -178.9(7) 16_544 . . . ? N100 Ag1 N200 C201 5(3) 10_554 . . . ? N100 Ag1 N200 C205 -175(3) 10_554 . . . ? C205 N200 C201 C202 0.0 . . . . ? Ag1 N200 C201 C202 -179.7(6) . . . . ? N200 C201 C202 C203 0.0 . . . . ? C201 C202 C203 C204 0.0 . . . . ? C201 C202 C203 C3 178.8(10) . . . . ? O2 C3 C203 C204 -158.8(9) . . . . ? C2 C3 C203 C204 11.4(17) . . . . ? O2 C3 C203 C202 22.4(15) . . . . ? C2 C3 C203 C202 -167.3(11) . . . . ? C202 C203 C204 C205 0.0 . . . . ? C3 C203 C204 C205 -178.7(10) . . . . ? C203 C204 C205 N200 0.0 . . . . ? C201 N200 C205 C204 0.0 . . . . ? Ag1 N200 C205 C204 179.7(6) . . . . ? C305 N300 C301 C302 0.0 . . . . ? Ag2 N300 C301 C302 -174.7(7) 16_544 . . . ? N300 C301 C302 C303 0.0 . . . . ? C301 C302 C303 C304 0.0 . . . . ? C301 C302 C303 C4 -175.5(11) . . . . ? O3 C4 C303 C304 20.0(15) . . . . ? C5 C4 C303 C304 -154.6(11) . . . . ? O3 C4 C303 C302 -164.5(8) . . . . ? C5 C4 C303 C302 21.0(17) . . . . ? C302 C303 C304 C305 0.0 . . . . ? C4 C303 C304 C305 175.6(11) . . . . ? C303 C304 C305 N300 0.0 . . . . ? C301 N300 C305 C304 0.0 . . . . ? Ag2 N300 C305 C304 174.9(7) 16_544 . . . ? N300 Ag2 N400 C401 121.6(11) 10_554 . . . ? N300 Ag2 N400 C405 -70.1(13) 10_554 . . . ? C405 N400 C401 C402 0.0 . . . . ? Ag2 N400 C401 C402 168.1(7) . . . . ? N400 C401 C402 C403 0.0 . . . . ? C401 C402 C403 C404 0.0 . . . . ? C401 C402 C403 C6 178.4(10) . . . . ? O4 C6 C403 C402 -163.0(8) . . . . ? C5 C6 C403 C402 16.7(13) . . . . ? O4 C6 C403 C404 15.4(12) . . . . ? C5 C6 C403 C404 -164.8(9) . . . . ? C402 C403 C404 C405 0.0 . . . . ? C6 C403 C404 C405 -178.4(10) . . . . ? C403 C404 C405 N400 0.0 . . . . ? C401 N400 C405 C404 0.0 . . . . ? Ag2 N400 C405 C404 -168.5(7) . . . . ? C505 N500 C501 C502 0.0 . . . . ? Ag3 N500 C501 C502 168.7(11) 16_544 . . . ? N500 C501 C502 C503 0.0 . . . . ? C501 C502 C503 C504 0.0 . . . . ? C501 C502 C503 C7 173.2(13) . . . . ? C8 C7 C503 C502 0.2(19) . . . . ? O5 C7 C503 C502 172.6(9) . . . . ? C8 C7 C503 C504 173.3(13) . . . . ? O5 C7 C503 C504 -14.3(14) . . . . ? C502 C503 C504 C505 0.0 . . . . ? C7 C503 C504 C505 -173.1(13) . . . . ? C503 C504 C505 N500 0.0 . . . . ? C501 N500 C505 C504 0.0 . . . . ? Ag3 N500 C505 C504 -169.3(10) 16_544 . . . ? N500 Ag3 N600 C601 19(4) 10_554 . . . ? N500 Ag3 N600 C605 -161(3) 10_554 . . . ? C605 N600 C601 C602 0.0 . . . . ? Ag3 N600 C601 C602 180.0(8) . . . . ? N600 C601 C602 C603 0.0 . . . . ? C601 C602 C603 C604 0.0 . . . . ? C601 C602 C603 C9 175.6(11) . . . . ? O6 C9 C603 C602 156.1(9) . . . . ? C8 C9 C603 C602 -14.9(18) . . . . ? O6 C9 C603 C604 -28.3(14) . . . . ? C8 C9 C603 C604 160.7(13) . . . . ? C602 C603 C604 C605 0.0 . . . . ? C9 C603 C604 C605 -175.6(11) . . . . ? C603 C604 C605 N600 0.0 . . . . ? C601 N600 C605 C604 0.0 . . . . ? Ag3 N600 C605 C604 180.0(8) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 23.25 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.916 _refine_diff_density_min -0.919 _refine_diff_density_rms 0.136 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.020 -0.012 -0.024 17416 4511 ' ' _platon_squeeze_details ; ; #===end data_compound_5_k08adb26 _database_code_depnum_ccdc_archive 'CCDC 771702' #TrackingRef '- dppd-strucs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H47 Cl4 Eu N8 O9' _chemical_formula_weight 1245.76 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' O O 0.0106 0.0060 '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' Eu Eu -0.1578 3.6682 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Fddd loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/4, -y+1/4, z' 'x, -y+1/4, -z+1/4' '-x+1/4, y, -z+1/4' 'x, y+1/2, z+1/2' '-x+1/4, -y+3/4, z+1/2' 'x, -y+3/4, -z+3/4' '-x+1/4, y+1/2, -z+3/4' 'x+1/2, y, z+1/2' '-x+3/4, -y+1/4, z+1/2' 'x+1/2, -y+1/4, -z+3/4' '-x+3/4, y, -z+3/4' 'x+1/2, y+1/2, z' '-x+3/4, -y+3/4, z' 'x+1/2, -y+3/4, -z+1/4' '-x+3/4, y+1/2, -z+1/4' '-x, -y, -z' 'x-1/4, y-1/4, -z' '-x, y-1/4, z-1/4' 'x-1/4, -y, z-1/4' '-x, -y+1/2, -z+1/2' 'x-1/4, y+1/4, -z+1/2' '-x, y+1/4, z+1/4' 'x-1/4, -y+1/2, z+1/4' '-x+1/2, -y, -z+1/2' 'x+1/4, y-1/4, -z+1/2' '-x+1/2, y-1/4, z+1/4' 'x+1/4, -y, z+1/4' '-x+1/2, -y+1/2, -z' 'x+1/4, y+1/4, -z' '-x+1/2, y+1/4, z-1/4' 'x+1/4, -y+1/2, z-1/4' _cell_length_a 15.1070(4) _cell_length_b 27.3860(7) _cell_length_c 29.0380(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 12013.6(5) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 69792 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 25.028 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.378 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5040 _exptl_absorpt_coefficient_mu 1.279 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.80 _exptl_absorpt_correction_T_max 0.89 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 '95mm CCD camera on \k-goniostat' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 47751 _diffrn_reflns_av_R_equivalents 0.1149 _diffrn_reflns_av_sigmaI/netI 0.0360 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 4.02 _diffrn_reflns_theta_max 25.02 _reflns_number_total 2638 _reflns_number_gt 2424 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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. The asymmetric unit in this structure consists of one chloride anion, 1/4 of a europium (located at a special position in the space group), a diffuse region of solvent and one partially protonated acac ligand. The latter is neutral for 75% of the time (i.e only one of the ligand nitrogens is protonated), and positively charged for the remaining 25% of the time (i.e. both nitrogens protonated). Said nitrogen-bound ligand hydrogens are disordered such that one proton is located on N1 on 65% of the structure, and another on N2 in 60% of the structure. These partial atoms (H1 and H2) were located and refined at a distance of 0.9 from the parent atoms. The solvent is proximate to crystallographic symmetry and could not be successfully resolved. Hence, PLATON SQUEEZE was utilized, which gave an estimate of 1 molecule of ethanol per europium, which has been included in the formulation. This structure is best represented by the following formula where L1 = [C13H9N2O2]-: [Eu(L1-H2)1(L1-H)3]Cl4?EtOH ; _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^)+(0.0506P)^2^+63.3648P] 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 2638 _refine_ls_number_parameters 174 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0602 _refine_ls_R_factor_gt 0.0502 _refine_ls_wR_factor_ref 0.1123 _refine_ls_wR_factor_gt 0.1079 _refine_ls_goodness_of_fit_ref 1.192 _refine_ls_restrained_S_all 1.192 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Eu1 Eu 0.1250 0.1250 0.1250 0.03297(18) Uani 1 4 d S . . Cl1 Cl 0.73697(9) 0.05883(6) 0.04676(6) 0.0646(4) Uani 1 1 d . . . O1 O 0.0724(2) 0.07920(12) 0.05923(10) 0.0364(7) Uani 1 1 d . . . O2 O 0.2388(2) 0.07625(13) 0.09556(11) 0.0427(8) Uani 1 1 d . . . N1 N -0.0670(3) 0.03809(15) -0.08896(14) 0.0407(10) Uani 1 1 d D . . N2 N 0.5396(3) 0.06250(19) 0.03893(18) 0.0562(12) Uani 1 1 d D . . C1 C 0.1104(3) 0.06481(17) 0.02335(14) 0.0330(10) Uani 1 1 d . . . C2 C 0.2027(3) 0.05941(18) 0.01798(16) 0.0382(11) Uani 1 1 d . . . H2A H 0.2262 0.0509 -0.0113 0.046 Uiso 1 1 calc R . . C3 C 0.2598(3) 0.06639(18) 0.05492(16) 0.0375(11) Uani 1 1 d . . . C4 C 0.3599(3) 0.06338(18) 0.04751(16) 0.0408(11) Uani 1 1 d . . . C5 C 0.3995(4) 0.0606(3) 0.0045(2) 0.0662(18) Uani 1 1 d . . . H5 H 0.3648 0.0587 -0.0227 0.079 Uiso 1 1 calc R . . C6 C 0.4905(4) 0.0605(3) 0.0024(2) 0.0714(19) Uani 1 1 d . . . H6 H 0.5183 0.0590 -0.0270 0.086 Uiso 1 1 calc R . . C7 C 0.5035(4) 0.0657(2) 0.0808(2) 0.0573(15) Uani 1 1 d . . . H7 H 0.5405 0.0674 0.1072 0.069 Uiso 1 1 calc R . . C8 C 0.4140(3) 0.0664(2) 0.08587(18) 0.0476(13) Uani 1 1 d . . . H8 H 0.3886 0.0690 0.1157 0.057 Uiso 1 1 calc R . . C9 C 0.0500(3) 0.05426(17) -0.01731(14) 0.0338(10) Uani 1 1 d . . . C10 C -0.0384(3) 0.06728(18) -0.01348(16) 0.0408(12) Uani 1 1 d . . . H10 H -0.0598 0.0821 0.0139 0.049 Uiso 1 1 calc R . . C11 C -0.0949(4) 0.0585(2) -0.04987(18) 0.0469(12) Uani 1 1 d . . . H11 H -0.1555 0.0673 -0.0470 0.056 Uiso 1 1 calc R . . C12 C 0.0169(4) 0.0245(2) -0.09245(18) 0.0503(13) Uani 1 1 d . . . H12 H 0.0361 0.0094 -0.1202 0.060 Uiso 1 1 calc R . . C13 C 0.0780(3) 0.0315(2) -0.05716(16) 0.0454(12) Uani 1 1 d . . . H13 H 0.1375 0.0208 -0.0604 0.054 Uiso 1 1 calc R . . H2 H 0.5986(10) 0.065(3) 0.035(2) 0.024(19) Uiso 0.60 1 d PD . . H1 H -0.106(5) 0.035(3) -0.112(2) 0.05(3) Uiso 0.65 1 d PD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.0231(3) 0.0538(3) 0.0220(2) 0.000 0.000 0.000 Cl1 0.0346(7) 0.0792(10) 0.0801(10) -0.0142(8) 0.0022(7) 0.0049(7) O1 0.0314(18) 0.054(2) 0.0242(15) -0.0003(14) 0.0004(13) -0.0002(15) O2 0.0307(18) 0.069(2) 0.0286(17) 0.0009(16) -0.0029(13) 0.0095(16) N1 0.039(3) 0.047(2) 0.036(2) 0.0026(19) -0.0097(18) -0.0016(19) N2 0.028(2) 0.077(3) 0.064(3) -0.004(3) 0.006(2) 0.006(2) C1 0.030(3) 0.040(2) 0.029(2) 0.0035(19) -0.0017(19) -0.001(2) C2 0.036(3) 0.050(3) 0.029(2) -0.003(2) -0.001(2) 0.005(2) C3 0.034(3) 0.046(3) 0.033(3) 0.002(2) 0.000(2) 0.013(2) C4 0.035(3) 0.048(3) 0.039(3) -0.003(2) 0.001(2) 0.009(2) C5 0.035(3) 0.114(5) 0.049(3) -0.009(3) 0.000(2) 0.016(3) C6 0.045(4) 0.118(6) 0.051(3) -0.009(4) 0.006(3) 0.013(4) C7 0.039(3) 0.080(4) 0.053(3) 0.000(3) -0.006(3) -0.001(3) C8 0.031(3) 0.069(4) 0.043(3) -0.005(3) -0.001(2) 0.001(3) C9 0.038(3) 0.038(3) 0.026(2) 0.0015(19) -0.0041(19) -0.002(2) C10 0.040(3) 0.048(3) 0.034(3) -0.007(2) -0.008(2) 0.001(2) C11 0.044(3) 0.052(3) 0.045(3) 0.001(2) -0.011(2) 0.003(2) C12 0.050(3) 0.066(4) 0.035(3) -0.014(2) -0.003(2) -0.005(3) C13 0.036(3) 0.067(3) 0.033(3) -0.005(2) -0.002(2) 0.000(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu1 O2 2.338(3) 3 ? Eu1 O2 2.338(3) 2 ? Eu1 O2 2.338(3) . ? Eu1 O2 2.338(3) 4 ? Eu1 O1 2.419(3) 3 ? Eu1 O1 2.419(3) 4 ? Eu1 O1 2.419(3) 2 ? Eu1 O1 2.419(3) . ? O1 C1 1.253(5) . ? O2 C3 1.251(5) . ? N1 C12 1.324(7) . ? N1 C11 1.334(7) . ? N1 H1 0.898(10) . ? N2 C6 1.297(8) . ? N2 C7 1.336(7) . ? N2 H2 0.900(10) . ? C1 C2 1.411(6) . ? C1 C9 1.520(6) . ? C2 C3 1.389(6) . ? C2 H2A 0.9500 . ? C3 C4 1.531(7) . ? C4 C8 1.384(7) . ? C4 C5 1.386(7) . ? C5 C6 1.375(8) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.360(7) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 C13 1.381(7) . ? C9 C10 1.386(7) . ? C10 C11 1.379(7) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C13 1.392(7) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Eu1 O2 110.37(18) 3 2 ? O2 Eu1 O2 85.37(17) 3 . ? O2 Eu1 O2 137.11(15) 2 . ? O2 Eu1 O2 137.11(15) 3 4 ? O2 Eu1 O2 85.37(17) 2 4 ? O2 Eu1 O2 110.37(18) . 4 ? O2 Eu1 O1 69.92(11) 3 3 ? O2 Eu1 O1 75.60(11) 2 3 ? O2 Eu1 O1 145.70(10) . 3 ? O2 Eu1 O1 76.47(11) 4 3 ? O2 Eu1 O1 76.47(11) 3 4 ? O2 Eu1 O1 145.70(10) 2 4 ? O2 Eu1 O1 75.60(11) . 4 ? O2 Eu1 O1 69.92(11) 4 4 ? O1 Eu1 O1 75.72(15) 3 4 ? O2 Eu1 O1 75.60(11) 3 2 ? O2 Eu1 O1 69.92(11) 2 2 ? O2 Eu1 O1 76.46(11) . 2 ? O2 Eu1 O1 145.70(10) 4 2 ? O1 Eu1 O1 117.54(15) 3 2 ? O1 Eu1 O1 141.66(14) 4 2 ? O2 Eu1 O1 145.70(10) 3 . ? O2 Eu1 O1 76.46(11) 2 . ? O2 Eu1 O1 69.92(11) . . ? O2 Eu1 O1 75.60(11) 4 . ? O1 Eu1 O1 141.66(14) 3 . ? O1 Eu1 O1 117.54(15) 4 . ? O1 Eu1 O1 75.72(15) 2 . ? C1 O1 Eu1 132.0(3) . . ? C3 O2 Eu1 130.9(3) . . ? C12 N1 C11 119.1(4) . . ? C12 N1 H1 123(6) . . ? C11 N1 H1 118(6) . . ? C6 N2 C7 120.9(5) . . ? C6 N2 H2 118(5) . . ? C7 N2 H2 120(5) . . ? O1 C1 C2 125.3(4) . . ? O1 C1 C9 115.5(4) . . ? C2 C1 C9 119.2(4) . . ? C3 C2 C1 120.9(4) . . ? C3 C2 H2A 119.6 . . ? C1 C2 H2A 119.6 . . ? O2 C3 C2 126.9(4) . . ? O2 C3 C4 113.2(4) . . ? C2 C3 C4 119.8(4) . . ? C8 C4 C5 118.3(5) . . ? C8 C4 C3 117.8(4) . . ? C5 C4 C3 123.8(4) . . ? C6 C5 C4 118.2(5) . . ? C6 C5 H5 120.9 . . ? C4 C5 H5 120.9 . . ? N2 C6 C5 122.3(6) . . ? N2 C6 H6 118.9 . . ? C5 C6 H6 118.9 . . ? N2 C7 C8 120.4(5) . . ? N2 C7 H7 119.8 . . ? C8 C7 H7 119.8 . . ? C7 C8 C4 119.9(5) . . ? C7 C8 H8 120.0 . . ? C4 C8 H8 120.0 . . ? C13 C9 C10 118.6(4) . . ? C13 C9 C1 123.6(4) . . ? C10 C9 C1 117.8(4) . . ? C11 C10 C9 119.3(5) . . ? C11 C10 H10 120.3 . . ? C9 C10 H10 120.3 . . ? N1 C11 C10 122.0(5) . . ? N1 C11 H11 119.0 . . ? C10 C11 H11 119.0 . . ? N1 C12 C13 122.6(5) . . ? N1 C12 H12 118.7 . . ? C13 C12 H12 118.7 . . ? C9 C13 C12 118.4(5) . . ? C9 C13 H13 120.8 . . ? C12 C13 H13 120.8 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.513 _refine_diff_density_min -0.353 _refine_diff_density_rms 0.086 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material #===end