# 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 F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² 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/[σ²(Fo²)+(0.0493P)²+4.6781P] where P=(Fo²+2Fc²)/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 . . .


_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


