# Electronic Supplementary Material for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Gopal Das' _publ_contact_author_email GDAS@IITG.ERNET.IN _publ_section_title ; Precursory Ag-bipyridine metallo-organic framework (MOF): A new and efficient route for the synthesis of Ag nanoparticles ; loop_ _publ_author_name 'Gopal Das' 'Avijit Pramanik' data_Agcluster _database_code_depnum_ccdc_archive 'CCDC 687882' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H16 Ag5 N9 O15' _chemical_formula_weight 1161.77 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C2/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.6476(12) _cell_length_b 8.0624(4) _cell_length_c 17.5990(9) _cell_angle_alpha 90.00 _cell_angle_beta 103.582(3) _cell_angle_gamma 90.00 _cell_volume 2985.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 7210 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 28.23 _exptl_crystal_description reactangular _exptl_crystal_colour yellow _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.590 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2216 _exptl_absorpt_coefficient_mu 3.318 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.275 _exptl_absorpt_correction_T_max 0.440 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22489 _diffrn_reflns_av_R_equivalents 0.0199 _diffrn_reflns_av_sigmaI/netI 0.0135 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 28.30 _reflns_number_total 3667 _reflns_number_gt 3380 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0493P)^2^+4.6781P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3667 _refine_ls_number_parameters 223 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0390 _refine_ls_R_factor_gt 0.0364 _refine_ls_wR_factor_ref 0.0915 _refine_ls_wR_factor_gt 0.0900 _refine_ls_goodness_of_fit_ref 1.214 _refine_ls_restrained_S_all 1.214 _refine_ls_shift/su_max 0.016 _refine_ls_shift/su_mean 0.072 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 0.192797(13) 0.18061(4) 0.163944(15) 0.04608(10) Uani 1 1 d . . . Ag3 Ag 0.0000 0.94463(6) 0.2500 0.05406(13) Uani 1 2 d S . . Ag2 Ag 0.120686(15) 0.49209(4) 0.176654(17) 0.05085(11) Uani 1 1 d . . . N2 N 0.06842(13) 0.3521(3) 0.07193(14) 0.0336(5) Uani 1 1 d . . . N1 N 0.20199(12) 0.3620(3) 0.07215(14) 0.0321(5) Uani 1 1 d . . . C5 C 0.09060(14) 0.3302(4) 0.00702(16) 0.0308(6) Uani 1 1 d . . . C6 C 0.15503(14) 0.3956(4) 0.00873(16) 0.0308(6) Uani 1 1 d . . . O5 O 0.04619(14) 0.6609(4) 0.2392(2) 0.0623(8) Uani 1 1 d . . . C4 C 0.05470(16) 0.2533(5) -0.05885(18) 0.0421(7) Uani 1 1 d . . . H4 H 0.0711 0.2386 -0.1028 0.050 Uiso 1 1 calc R . . C1 C 0.00983(16) 0.2970(5) 0.0712(2) 0.0410(7) Uani 1 1 d . . . H1 H -0.0055 0.3108 0.1159 0.049 Uiso 1 1 calc R . . C2 C -0.02864(16) 0.2210(5) 0.0073(2) 0.0450(8) Uani 1 1 d . . . H2 H -0.0693 0.1857 0.0087 0.054 Uiso 1 1 calc R . . C3 C -0.00591(17) 0.1983(5) -0.0588(2) 0.0491(9) Uani 1 1 d . . . H3 H -0.0309 0.1468 -0.1027 0.059 Uiso 1 1 calc R . . C7 C 0.16615(17) 0.4877(5) -0.05357(19) 0.0406(7) Uani 1 1 d . . . H7 H 0.1335 0.5068 -0.0975 0.049 Uiso 1 1 calc R . . C10 C 0.26004(15) 0.4239(5) 0.0755(2) 0.0412(7) Uani 1 1 d . . . H10 H 0.2923 0.4029 0.1196 0.049 Uiso 1 1 calc R . . C8 C 0.22618(18) 0.5506(5) -0.0496(2) 0.0471(8) Uani 1 1 d . . . H8 H 0.2343 0.6139 -0.0903 0.057 Uiso 1 1 calc R . . C9 C 0.27373(18) 0.5178(5) 0.0158(2) 0.0466(8) Uani 1 1 d . . . H9 H 0.3146 0.5584 0.0197 0.056 Uiso 1 1 calc R . . O3 O 0.22006(12) -0.0644(3) 0.23126(15) 0.0482(6) Uani 1 1 d . . . N3 N 0.18727(12) -0.1869(3) 0.20305(16) 0.0343(5) Uani 1 1 d . . . O1 O 0.15581(13) -0.1871(4) 0.13494(15) 0.0558(7) Uani 1 1 d . . . O2 O 0.18783(12) -0.3113(3) 0.24620(16) 0.0459(6) Uani 1 1 d . . . O4 O 0.0000 0.4294(6) 0.2500 0.0760(14) Uani 1 2 d S . . N4 N 0.0000 0.5803(5) 0.2500 0.0395(8) Uani 1 2 d S . . O8 O 0.15454(14) 1.2592(4) 0.29317(17) 0.0580(7) Uani 1 1 d . . . O6 O 0.08869(13) 1.0944(4) 0.21892(15) 0.0520(6) Uani 1 1 d . . . N5 N 0.11111(14) 1.1552(4) 0.28551(16) 0.0396(6) Uani 1 1 d . . . O7 O 0.08961(14) 1.1101(5) 0.34143(16) 0.0599(8) 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 0.04720(16) 0.04596(18) 0.04216(15) 0.01731(11) 0.00461(11) -0.00314(11) Ag3 0.0492(2) 0.0463(2) 0.0674(3) 0.000 0.01531(19) 0.000 Ag2 0.0614(2) 0.04564(19) 0.04902(17) -0.01979(11) 0.02001(13) -0.01661(13) N2 0.0367(12) 0.0346(14) 0.0301(11) -0.0020(10) 0.0092(9) -0.0047(10) N1 0.0339(12) 0.0334(13) 0.0284(11) 0.0034(9) 0.0058(9) -0.0044(10) C5 0.0332(13) 0.0308(15) 0.0278(12) 0.0032(10) 0.0062(10) 0.0033(11) C6 0.0337(13) 0.0315(15) 0.0275(12) 0.0017(10) 0.0077(10) 0.0011(11) O5 0.0521(16) 0.066(2) 0.077(2) -0.0078(16) 0.0327(15) -0.0117(14) C4 0.0402(16) 0.055(2) 0.0295(14) -0.0035(13) 0.0049(11) -0.0009(15) C1 0.0385(16) 0.0459(19) 0.0413(16) 0.0007(13) 0.0147(13) -0.0043(14) C2 0.0339(15) 0.052(2) 0.0474(18) 0.0009(15) 0.0063(13) -0.0075(15) C3 0.0410(17) 0.060(2) 0.0411(17) -0.0062(16) -0.0011(13) -0.0068(16) C7 0.0425(17) 0.047(2) 0.0338(15) 0.0113(13) 0.0126(12) 0.0057(14) C10 0.0345(15) 0.048(2) 0.0406(16) 0.0018(14) 0.0073(12) -0.0070(14) C8 0.0497(19) 0.050(2) 0.0480(18) 0.0138(16) 0.0251(15) 0.0017(16) C9 0.0409(17) 0.048(2) 0.055(2) 0.0026(16) 0.0193(15) -0.0088(15) O3 0.0474(13) 0.0363(13) 0.0526(14) 0.0063(11) -0.0046(10) -0.0139(11) N3 0.0273(11) 0.0348(14) 0.0399(13) 0.0012(10) 0.0060(9) -0.0004(10) O1 0.0472(14) 0.077(2) 0.0368(12) 0.0042(12) -0.0032(10) -0.0124(13) O2 0.0434(13) 0.0316(12) 0.0559(14) 0.0091(10) -0.0021(11) -0.0037(10) O4 0.119(4) 0.041(3) 0.077(3) 0.000 0.040(3) 0.000 N4 0.049(2) 0.041(2) 0.0318(17) 0.000 0.0162(15) 0.000 O8 0.0564(16) 0.0637(19) 0.0533(15) -0.0052(13) 0.0119(12) -0.0186(14) O6 0.0569(15) 0.0590(17) 0.0395(12) -0.0040(11) 0.0101(11) -0.0092(13) N5 0.0394(14) 0.0435(16) 0.0370(13) 0.0028(11) 0.0116(10) 0.0033(12) O7 0.0613(17) 0.082(2) 0.0428(13) 0.0098(14) 0.0246(12) -0.0004(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.223(2) . ? Ag1 O3 2.308(3) . ? Ag1 Ag2 2.9929(5) . ? Ag3 O6 2.436(3) . ? Ag3 O6 2.437(3) 2 ? Ag3 O5 2.522(3) . ? Ag3 O5 2.522(3) 2 ? Ag3 O7 2.582(3) . ? Ag3 O7 2.582(3) 2 ? Ag2 N2 2.230(3) . ? Ag2 O2 2.300(2) 1_565 ? Ag2 O5 2.549(3) . ? N2 C1 1.341(4) . ? N2 C5 1.351(4) . ? N1 C10 1.340(4) . ? N1 C6 1.349(4) . ? C5 C4 1.382(4) . ? C5 C6 1.485(4) . ? C6 C7 1.391(4) . ? O5 N4 1.244(4) . ? C4 C3 1.385(5) . ? C1 C2 1.377(5) . ? C2 C3 1.377(5) . ? C7 C8 1.381(5) . ? C10 C9 1.383(5) . ? C8 C9 1.377(5) . ? O3 N3 1.250(4) . ? N3 O1 1.232(4) . ? N3 O2 1.256(4) . ? O2 Ag2 2.300(2) 1_545 ? O4 N4 1.216(7) . ? N4 O5 1.244(4) 2 ? O8 N5 1.243(4) . ? O6 N5 1.258(4) . ? N5 O7 1.238(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 O3 151.73(11) . . ? N1 Ag1 Ag2 68.86(7) . . ? O3 Ag1 Ag2 139.01(8) . . ? O6 Ag3 O6 120.60(15) . 2 ? O6 Ag3 O5 94.90(10) . . ? O6 Ag3 O5 144.46(10) 2 . ? O6 Ag3 O5 144.46(10) . 2 ? O6 Ag3 O5 94.90(10) 2 2 ? O5 Ag3 O5 49.74(13) . 2 ? O6 Ag3 O7 50.76(8) . . ? O6 Ag3 O7 96.91(10) 2 . ? O5 Ag3 O7 105.22(11) . . ? O5 Ag3 O7 132.46(10) 2 . ? O6 Ag3 O7 96.92(10) . 2 ? O6 Ag3 O7 50.76(8) 2 2 ? O5 Ag3 O7 132.46(10) . 2 ? O5 Ag3 O7 105.22(11) 2 2 ? O7 Ag3 O7 117.77(15) . 2 ? N2 Ag2 O2 157.44(10) . 1_565 ? N2 Ag2 O5 112.18(10) . . ? O2 Ag2 O5 77.70(10) 1_565 . ? N2 Ag2 Ag1 71.69(7) . . ? O2 Ag2 Ag1 110.04(7) 1_565 . ? O5 Ag2 Ag1 150.94(8) . . ? C1 N2 C5 118.2(3) . . ? C1 N2 Ag2 118.1(2) . . ? C5 N2 Ag2 123.6(2) . . ? C10 N1 C6 118.6(3) . . ? C10 N1 Ag1 117.1(2) . . ? C6 N1 Ag1 123.7(2) . . ? N2 C5 C4 121.8(3) . . ? N2 C5 C6 117.1(2) . . ? C4 C5 C6 121.1(3) . . ? N1 C6 C7 121.5(3) . . ? N1 C6 C5 117.9(2) . . ? C7 C6 C5 120.6(3) . . ? N4 O5 Ag3 96.6(2) . . ? N4 O5 Ag2 113.6(2) . . ? Ag3 O5 Ag2 144.98(14) . . ? C5 C4 C3 119.3(3) . . ? N2 C1 C2 123.0(3) . . ? C1 C2 C3 118.8(3) . . ? C2 C3 C4 119.0(3) . . ? C8 C7 C6 119.4(3) . . ? N1 C10 C9 122.4(3) . . ? C9 C8 C7 118.8(3) . . ? C8 C9 C10 119.2(3) . . ? N3 O3 Ag1 114.83(19) . . ? O1 N3 O3 121.4(3) . . ? O1 N3 O2 120.8(3) . . ? O3 N3 O2 117.8(3) . . ? N3 O2 Ag2 108.26(19) . 1_545 ? O4 N4 O5 121.5(2) . 2 ? O4 N4 O5 121.5(2) . . ? O5 N4 O5 117.0(5) 2 . ? N5 O6 Ag3 97.83(19) . . ? O7 N5 O8 121.9(3) . . ? O7 N5 O6 119.4(3) . . ? O8 N5 O6 118.7(3) . . ? N5 O7 Ag3 91.4(2) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.728 _refine_diff_density_min -2.264 _refine_diff_density_rms 0.346