Electronic Supplementary Material for CrystEngComm
This journal is (c) The Royal Society of Chemistry 2006


data_global
_journal_name_full               CrystEngComm
_journal_coden_cambridge         1350
_journal_year                    ?
_journal_volume                  ?
_journal_page_first              ?
_publ_contact_author_name        'Jhy-Der Chen'
_publ_contact_author_email       JDCHEN@CYCU.EDU.TW
loop_
_publ_author_name
'Jhy-Der Chen'
'Zhi-Kai Chan'
'Chih-Yuan Lin'
'Ju-Chun Wang'
;
Chia-Jun Wu
;
'Chun-Wei Yeh'

data_1
_database_code_depnum_ccdc_archive 'CCDC 616573'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H19 Ag4 I4 N17 O12'
_chemical_formula_weight         1604.58

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'
Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Tetragonal
_symmetry_space_group_name_H-M   P4(2)/nmc

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-y+1/2, x, z+1/2'
'y, -x+1/2, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y, -z'
'y+1/2, x+1/2, -z+1/2'
'-y, -x, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'y-1/2, -x, -z-1/2'
'-y, x-1/2, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y, z'
'-y-1/2, -x-1/2, z-1/2'
'y, x, z-1/2'

_cell_length_a                   16.9297(12)
_cell_length_b                   16.9297(12)
_cell_length_c                   6.7285(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1928.5(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    50
_cell_measurement_theta_min      5.10
_cell_measurement_theta_max      12.52

_exptl_crystal_description       column
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.55
_exptl_crystal_size_min          0.40
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.763
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1484
_exptl_absorpt_coefficient_mu    5.279
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.8331
_exptl_absorpt_correction_T_max  0.9757
_exptl_absorpt_process_details   ?

_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  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         3
_diffrn_standards_interval_count 300
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        3.25
_diffrn_reflns_number            1758
_diffrn_reflns_av_R_equivalents  0.0184
_diffrn_reflns_av_sigmaI/netI    0.0244
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         2.41
_diffrn_reflns_theta_max         24.99
_reflns_number_total             907
_reflns_number_gt                749
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_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^)+(0.0201P)^2^+1.0531P] 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     SHELXL
_refine_ls_extinction_coef       0.00123(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         907
_refine_ls_number_parameters     89
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0320
_refine_ls_R_factor_gt           0.0222
_refine_ls_wR_factor_ref         0.0492
_refine_ls_wR_factor_gt          0.0466
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.038
_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
Ag Ag 0.062730(19) 0.562730(19) 0.7500 0.04481(16) Uani 1 2 d S . .
I1A I 0.2500 0.35414(14) 0.2097(3) 0.0629(6) Uani 0.50 2 d SP . .
I1B I 0.2500 0.37384(13) 0.1485(3) 0.0491(4) Uani 0.50 2 d SP . .
N1 N 0.17913(17) 0.50420(18) 0.6791(5) 0.0409(7) Uani 1 1 d . . .
N2 N 0.2500 0.5669(4) 0.9257(10) 0.075(2) Uani 1 2 d S . .
C1 C 0.2500 0.4350(3) 0.4302(8) 0.0378(12) Uani 1 2 d S . .
C2 C 0.1806(2) 0.4593(2) 0.5170(6) 0.0387(8) Uani 1 1 d . . .
C3 C 0.2500 0.5246(3) 0.7591(8) 0.0437(12) Uani 1 2 d S . .
N3 N -0.06893(19) 0.43107(19) 0.7500 0.0455(11) Uani 1 2 d S . .
O1 O -0.01316(18) 0.4276(2) 0.6309(4) 0.0690(9) Uani 1 1 d . . .
O2 O -0.1194(2) 0.3806(2) 0.7500 0.102(2) Uani 1 2 d S . .
H2N H 0.290(3) 0.571(3) 0.984(7) 0.088(19) Uiso 1 1 d . . .
H2 H 0.129(2) 0.446(2) 0.470(5) 0.045(11) Uiso 1 1 d . . .
C6 C -0.2500 0.2500 0.7500 0.196(14) Uiso 1 8 d SD . .
C5 C -0.279(2) 0.2500 0.953(2) 0.14(2) Uiso 0.25 2 d SPD . .
N4 N -0.304(3) 0.2500 1.112(3) 0.31(4) Uiso 0.25 2 d SPD . .

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
Ag 0.04413(18) 0.04413(18) 0.0462(3) -0.00381(13) 0.00381(13) 0.01223(18)
I1A 0.0447(6) 0.0778(15) 0.0663(14) -0.0416(10) 0.000 0.000
I1B 0.0530(6) 0.0429(8) 0.0513(11) -0.0139(6) 0.000 0.000
N1 0.0325(15) 0.0465(17) 0.0435(17) -0.0051(15) -0.0006(14) 0.0042(14)
N2 0.034(3) 0.130(6) 0.061(4) -0.044(4) 0.000 0.000
C1 0.040(3) 0.030(3) 0.043(3) -0.007(2) 0.000 0.000
C2 0.034(2) 0.0350(19) 0.047(2) -0.0008(17) -0.0014(17) 0.0017(16)
C3 0.043(3) 0.048(3) 0.040(3) -0.006(3) 0.000 0.000
N3 0.0440(15) 0.0440(15) 0.048(2) -0.0001(18) 0.0001(18) 0.000(2)
O1 0.0534(18) 0.106(3) 0.0471(18) 0.0089(17) 0.0109(15) 0.0115(17)
O2 0.071(2) 0.071(2) 0.166(6) -0.017(3) 0.017(3) -0.028(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
Ag N1 2.257(3) 7_456 ?
Ag N1 2.257(3) . ?
I1A I1B 0.530(3) . ?
I1A C1 2.019(6) . ?
I1B C1 2.160(6) . ?
N1 C2 1.330(5) . ?
N1 C3 1.360(4) . ?
N2 C3 1.330(8) . ?
N2 H2N 0.78(5) . ?
C1 C2 1.376(4) 14_655 ?
C1 C2 1.376(4) . ?
C2 H2 0.95(4) . ?
C3 N1 1.360(4) 14_655 ?
N3 O2 1.208(7) . ?
N3 O1 1.240(4) 7_456 ?
N3 O1 1.240(4) . ?
C6 C5 1.4500(18) 12_567 ?
C6 C5 1.4500(18) 11_557 ?
C6 C5 1.4500(18) 2_455 ?
C6 C5 1.4500(19) . ?
C5 C5 0.97(8) 2_455 ?
C5 N4 1.1502(19) . ?
C5 N4 1.76(5) 2_455 ?
N4 C5 1.76(5) 2_455 ?
N4 N4 1.81(11) 2_455 ?

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 Ag N1 144.25(15) 7_456 . ?
I1B I1A C1 98.3(6) . . ?
I1A I1B C1 67.6(5) . . ?
C2 N1 C3 117.0(3) . . ?
C2 N1 Ag 116.1(2) . . ?
C3 N1 Ag 125.1(3) . . ?
C3 N2 H2N 118(4) . . ?
C2 C1 C2 117.4(5) 14_655 . ?
C2 C1 I1A 121.0(2) 14_655 . ?
C2 C1 I1A 121.0(2) . . ?
C2 C1 I1B 121.1(3) 14_655 . ?
C2 C1 I1B 121.1(3) . . ?
I1A C1 I1B 14.05(9) . . ?
N1 C2 C1 122.4(4) . . ?
N1 C2 H2 113(2) . . ?
C1 C2 H2 125(2) . . ?
N2 C3 N1 118.1(2) . . ?
N2 C3 N1 118.1(2) . 14_655 ?
N1 C3 N1 123.9(5) . 14_655 ?
O2 N3 O1 120.4(3) . 7_456 ?
O2 N3 O1 120.4(3) . . ?
O1 N3 O1 119.3(5) 7_456 . ?
C5 C6 C5 39(3) 12_567 11_557 ?
C5 C6 C5 153(2) 12_567 2_455 ?
C5 C6 C5 153(2) 11_557 2_455 ?
C5 C6 C5 153(2) 12_567 . ?
C5 C6 C5 153(2) 11_557 . ?
C5 C6 C5 39(3) 2_455 . ?
C5 C5 N4 112(4) 2_455 . ?
C5 C5 C6 70.5(17) 2_455 . ?
N4 C5 C6 178(5) . . ?
C5 C5 N4 37.5(16) 2_455 2_455 ?
N4 C5 N4 74(5) . 2_455 ?
C6 C5 N4 108(2) . 2_455 ?
C5 N4 C5 31(3) . 2_455 ?
C5 N4 N4 68(4) . 2_455 ?
C5 N4 N4 37.5(16) 2_455 2_455 ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.570
_refine_diff_density_min         -0.544
_refine_diff_density_rms         0.074

#===END

data_2
_database_code_depnum_ccdc_archive 'CCDC 616574'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C4 H4 Ag F6 I N3 P'
_chemical_formula_weight         473.84

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Tetragonal
_symmetry_space_group_name_H-M   I4(1)/a

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   18.711(3)
_cell_length_b                   18.711(3)
_cell_length_c                   22.584(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     7906.3(19)
_cell_formula_units_Z            16
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    32
_cell_measurement_theta_min      4.85
_cell_measurement_theta_max      12.47

_exptl_crystal_description       block
_exptl_crystal_colour            pale_yellow
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.45
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.592
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3488
_exptl_absorpt_coefficient_mu    2.695
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.7857
_exptl_absorpt_correction_T_max  0.9560
_exptl_absorpt_process_details   ?

_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  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         3
_diffrn_standards_interval_count 297
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        7.05
_diffrn_reflns_number            3456
_diffrn_reflns_av_R_equivalents  0.0342
_diffrn_reflns_av_sigmaI/netI    0.0944
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.18
_diffrn_reflns_theta_max         24.50
_reflns_number_total             3240
_reflns_number_gt                1167
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_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^)+(0.0142P)^2^+15.2270P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3240
_refine_ls_number_parameters     145
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0995
_refine_ls_R_factor_gt           0.0481
_refine_ls_wR_factor_ref         0.1133
_refine_ls_wR_factor_gt          0.1030
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.034
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
1 -0.015 -0.003 -0.003 3787.7 2589.5
_platon_squeeze_details          
;
A. L. Spek, J Appl. Cryst., 2003, 36, 7-13.
;

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
I I 0.55839(4) 0.65434(4) 0.01630(3) 0.1115(3) Uani 1 1 d . . .
Ag Ag 0.34322(5) 0.47084(5) -0.11159(4) 0.1245(4) Uani 1 1 d . . .
N1 N 0.3709(5) 0.5352(5) -0.0346(3) 0.090(3) Uani 1 1 d . . .
N2 N 0.2662(5) 0.5030(6) 0.0147(5) 0.167(6) Uani 1 1 d . . .
H2B H 0.2388 0.5072 0.0452 0.200 Uiso 1 1 calc R . .
H2C H 0.2530 0.4771 -0.0147 0.200 Uiso 1 1 calc R . .
N3 N 0.3466(5) 0.5764(5) 0.0603(4) 0.095(3) Uani 1 1 d . . .
C1 C 0.3259(7) 0.5352(7) 0.0133(5) 0.104(4) Uani 1 1 d . . .
C2 C 0.4335(6) 0.5702(6) -0.0332(4) 0.094(4) Uani 1 1 d . . .
H2A H 0.4621 0.5686 -0.0668 0.113 Uiso 1 1 calc R . .
C3 C 0.4578(5) 0.6080(5) 0.0142(4) 0.086(3) Uani 1 1 d . . .
C4 C 0.4109(8) 0.6106(6) 0.0612(4) 0.103(4) Uani 1 1 d . . .
H4A H 0.4235 0.6367 0.0947 0.124 Uiso 1 1 calc R . .
P P 0.5178(3) 0.5137(3) -0.2077(2) 0.1553(17) Uani 1 1 d . . .
F1 F 0.6001(5) 0.4823(5) -0.2076(4) 0.203(4) Uani 1 1 d . . .
F2 F 0.5386(6) 0.5718(7) -0.1606(5) 0.288(6) Uani 1 1 d . . .
F3 F 0.4962(5) 0.4575(6) -0.1578(4) 0.232(5) Uani 1 1 d . . .
F4 F 0.5384(7) 0.5716(6) -0.2537(5) 0.293(7) Uani 1 1 d . . .
F5 F 0.4943(9) 0.4563(7) -0.2538(5) 0.353(9) Uani 1 1 d . . .
F6 F 0.4333(7) 0.5412(6) -0.2074(5) 0.276(6) 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
I 0.1110(6) 0.1364(7) 0.0872(5) -0.0118(5) -0.0073(5) -0.0038(5)
Ag 0.1425(9) 0.1611(9) 0.0699(5) -0.0433(6) -0.0099(6) -0.0069(7)
N1 0.111(7) 0.101(7) 0.058(5) -0.024(5) 0.003(5) 0.002(6)
N2 0.111(9) 0.231(14) 0.158(11) -0.052(9) 0.056(8) -0.066(9)
N3 0.104(8) 0.107(8) 0.073(6) -0.013(6) 0.020(6) 0.016(6)
C1 0.149(12) 0.120(10) 0.042(6) -0.025(7) 0.024(8) 0.014(9)
C2 0.103(9) 0.132(11) 0.048(6) -0.041(6) -0.001(6) 0.027(8)
C3 0.097(8) 0.100(8) 0.060(6) -0.012(6) -0.002(6) 0.017(7)
C4 0.160(13) 0.115(10) 0.035(6) -0.005(6) -0.008(8) 0.043(9)
P 0.204(6) 0.158(4) 0.104(3) 0.003(3) 0.028(3) 0.048(4)
F1 0.169(8) 0.234(10) 0.207(9) -0.008(8) 0.037(7) 0.054(7)
F2 0.285(13) 0.318(14) 0.259(12) -0.154(12) 0.085(10) -0.063(11)
F3 0.200(9) 0.294(13) 0.202(9) 0.075(10) 0.028(7) 0.048(8)
F4 0.466(19) 0.221(11) 0.193(9) 0.091(9) 0.151(11) 0.029(11)
F5 0.58(3) 0.332(16) 0.147(8) -0.106(11) -0.052(12) 0.132(16)
F6 0.305(14) 0.189(10) 0.334(14) 0.053(10) -0.004(12) 0.084(10)

_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
I C3 2.073(10) . ?
Ag N1 2.178(8) . ?
Ag N3 2.192(8) 4_454 ?
N1 C2 1.342(11) . ?
N1 C1 1.371(12) . ?
N2 C1 1.269(13) . ?
N3 C4 1.362(12) . ?
N3 C1 1.368(13) . ?
N3 Ag 2.192(8) 3 ?
C2 C3 1.361(12) . ?
C3 C4 1.379(12) . ?
P F4 1.550(10) . ?
P F5 1.557(12) . ?
P F2 1.572(10) . ?
P F3 1.594(10) . ?
P F1 1.648(9) . ?
P F6 1.662(12) . ?

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 Ag N3 174.4(4) . 4_454 ?
C2 N1 C1 121.2(9) . . ?
C2 N1 Ag 119.7(7) . . ?
C1 N1 Ag 118.9(8) . . ?
C4 N3 C1 121.9(10) . . ?
C4 N3 Ag 115.4(8) . 3 ?
C1 N3 Ag 122.8(9) . 3 ?
N2 C1 N3 119.8(11) . . ?
N2 C1 N1 124.1(12) . . ?
N3 C1 N1 115.9(12) . . ?
N1 C2 C3 124.3(10) . . ?
C2 C3 C4 114.3(10) . . ?
C2 C3 I 122.6(9) . . ?
C4 C3 I 123.1(9) . . ?
N3 C4 C3 122.2(10) . . ?
F4 P F5 96.0(7) . . ?
F4 P F2 84.8(7) . . ?
F5 P F2 178.0(8) . . ?
F4 P F3 176.8(7) . . ?
F5 P F3 87.0(7) . . ?
F2 P F3 92.2(6) . . ?
F4 P F1 91.0(6) . . ?
F5 P F1 91.1(7) . . ?
F2 P F1 90.8(7) . . ?
F3 P F1 90.0(5) . . ?
F4 P F6 91.4(7) . . ?
F5 P F6 87.0(8) . . ?
F2 P F6 91.1(6) . . ?
F3 P F6 87.7(6) . . ?
F1 P F6 177.1(7) . . ?

_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_theta_full        24.50
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         0.557
_refine_diff_density_min         -0.381
_refine_diff_density_rms         0.088

#===END

data_3
_database_code_depnum_ccdc_archive 'CCDC 616575'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C4 H4 Ag Cl I N3 O4'
_chemical_formula_weight         428.32

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pnna

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z'
'-x+1/2, y+1/2, -z+1/2'
'x, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z'
'x-1/2, -y-1/2, z-1/2'
'-x, y-1/2, z-1/2'

_cell_length_a                   19.1267(17)
_cell_length_b                   11.4655(9)
_cell_length_c                   9.0154(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1977.1(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    34
_cell_measurement_theta_min      3.55
_cell_measurement_theta_max      18.38

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.878
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1584
_exptl_absorpt_coefficient_mu    5.424
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5224
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   ?

_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  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         3
_diffrn_standards_interval_count 100
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            2320
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_av_sigmaI/netI    0.0408
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.13
_diffrn_reflns_theta_max         25.00
_reflns_number_total             1741
_reflns_number_gt                1227
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_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^)+(0.0185P)^2^+28.8658P] 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       0.00025(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         1741
_refine_ls_number_parameters     130
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0791
_refine_ls_R_factor_gt           0.0501
_refine_ls_wR_factor_ref         0.1091
_refine_ls_wR_factor_gt          0.0983
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.052
_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
I I 0.43992(4) -0.06851(7) -0.27658(10) 0.0610(3) Uani 1 1 d . . .
Ag1 Ag 0.60047(7) -0.2500 0.2500 0.0735(5) Uani 1 2 d S . .
Ag2 Ag 0.7500 0.0000 -0.26202(15) 0.0575(4) Uani 1 2 d S . .
N1 N 0.6016(4) -0.1924(8) 0.0192(9) 0.043(2) Uani 1 1 d . . .
N2 N 0.7207(4) -0.2019(8) -0.0073(10) 0.053(2) Uani 1 1 d . . .
H2A H 0.7245 -0.2454 0.0768 0.063 Uiso 1 1 d R . .
H2B H 0.7527 -0.2115 -0.0831 0.063 Uiso 1 1 d R . .
N3 N 0.6597(4) -0.1059(7) -0.1878(9) 0.0376(19) Uani 1 1 d . . .
C1 C 0.6599(5) -0.1674(8) -0.0608(10) 0.035(2) Uani 1 1 d . . .
C2 C 0.5982(5) -0.0796(9) -0.2464(12) 0.043(2) Uani 1 1 d . . .
H2C H 0.5970 -0.0402 -0.3365 0.052 Uiso 1 1 calc R . .
C3 C 0.5358(5) -0.1084(8) -0.1789(10) 0.036(2) Uani 1 1 d . . .
C4 C 0.5399(5) -0.1624(9) -0.0425(12) 0.048(3) Uani 1 1 d . . .
H4A H 0.4988 -0.1787 0.0086 0.058 Uiso 1 1 calc R . .
Cl1 Cl 0.7500 0.0000 -0.6256(4) 0.0562(10) Uani 1 2 d S . .
Cl2 Cl 0.60958(19) 0.2500 0.7500 0.0544(10) Uani 1 2 d S . .
O1 O 0.8085(5) -0.0083(12) -0.5314(11) 0.111(4) Uani 1 1 d . . .
O2 O 0.7439(9) -0.0969(10) -0.7132(11) 0.132(5) Uani 1 1 d . . .
O3 O 0.5638(11) 0.3113(13) 0.821(2) 0.267(14) Uani 1 1 d . . .
O4 O 0.6450(7) 0.1701(10) 0.826(3) 0.224(11) 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
I 0.0409(4) 0.0682(5) 0.0739(6) 0.0020(5) -0.0175(4) 0.0025(4)
Ag1 0.0587(8) 0.1240(13) 0.0379(7) 0.0238(8) 0.000 0.000
Ag2 0.0416(6) 0.0701(8) 0.0607(8) 0.000 0.000 -0.0181(6)
N1 0.042(5) 0.053(5) 0.034(4) 0.005(4) 0.004(4) 0.005(4)
N2 0.043(5) 0.078(6) 0.037(5) 0.004(5) 0.004(4) 0.018(5)
N3 0.038(4) 0.039(4) 0.036(4) 0.004(4) 0.001(4) 0.001(4)
C1 0.033(5) 0.044(6) 0.029(5) -0.009(5) 0.001(4) -0.003(5)
C2 0.045(5) 0.042(5) 0.043(5) 0.003(6) -0.001(5) 0.003(5)
C3 0.030(5) 0.044(6) 0.034(5) -0.004(5) -0.004(4) 0.000(4)
C4 0.035(5) 0.060(7) 0.048(6) -0.005(6) 0.004(5) 0.002(5)
Cl1 0.049(2) 0.075(3) 0.045(2) 0.000 0.000 -0.004(2)
Cl2 0.0386(19) 0.062(2) 0.062(2) -0.006(2) 0.000 0.000
O1 0.051(5) 0.207(12) 0.076(6) -0.038(8) -0.015(5) 0.023(7)
O2 0.223(14) 0.104(8) 0.069(7) -0.034(6) -0.011(9) -0.035(9)
O3 0.39(3) 0.128(12) 0.28(2) 0.095(14) 0.27(2) 0.101(15)
O4 0.159(12) 0.082(8) 0.43(3) 0.004(13) -0.199(17) 0.024(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
I C3 2.085(9) . ?
Ag1 N1 2.184(8) 4_545 ?
Ag1 N1 2.184(8) . ?
Ag2 N3 2.215(8) 2_655 ?
Ag2 N3 2.215(8) . ?
N1 C4 1.348(12) . ?
N1 C1 1.358(12) . ?
N2 C1 1.320(12) . ?
N2 H2A 0.9105 . ?
N2 H2B 0.9240 . ?
N3 C2 1.325(12) . ?
N3 C1 1.345(12) . ?
C2 C3 1.380(13) . ?
C2 H2C 0.9300 . ?
C3 C4 1.379(14) . ?
C4 H4A 0.9300 . ?
Cl1 O2 1.368(10) . ?
Cl1 O2 1.368(10) 2_655 ?
Cl1 O1 1.408(9) 2_655 ?
Cl1 O1 1.408(9) . ?
Cl2 O3 1.294(14) 4_556 ?
Cl2 O3 1.294(14) . ?
Cl2 O4 1.329(13) . ?
Cl2 O4 1.329(13) 4_556 ?

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 N1 178.9(4) 4_545 . ?
N3 Ag2 N3 144.8(4) 2_655 . ?
C4 N1 C1 116.5(8) . . ?
C4 N1 Ag1 117.5(7) . . ?
C1 N1 Ag1 125.3(6) . . ?
C1 N2 H2A 122.6 . . ?
C1 N2 H2B 110.5 . . ?
H2A N2 H2B 119.8 . . ?
C2 N3 C1 117.5(9) . . ?
C2 N3 Ag2 116.6(6) . . ?
C1 N3 Ag2 122.9(6) . . ?
N2 C1 N3 118.0(9) . . ?
N2 C1 N1 117.8(9) . . ?
N3 C1 N1 124.1(9) . . ?
N3 C2 C3 122.6(9) . . ?
N3 C2 H2C 118.7 . . ?
C3 C2 H2C 118.7 . . ?
C2 C3 C4 116.8(9) . . ?
C2 C3 I 121.5(7) . . ?
C4 C3 I 121.7(7) . . ?
N1 C4 C3 122.1(9) . . ?
N1 C4 H4A 118.9 . . ?
C3 C4 H4A 118.9 . . ?
O2 Cl1 O2 109.4(10) . 2_655 ?
O2 Cl1 O1 109.6(8) . 2_655 ?
O2 Cl1 O1 111.2(8) 2_655 2_655 ?
O2 Cl1 O1 111.2(8) . . ?
O2 Cl1 O1 109.6(8) 2_655 . ?
O1 Cl1 O1 105.8(8) 2_655 . ?
O3 Cl2 O3 95(2) 4_556 . ?
O3 Cl2 O4 103.0(8) 4_556 . ?
O3 Cl2 O4 117.7(13) . . ?
O3 Cl2 O4 117.7(13) 4_556 4_556 ?
O3 Cl2 O4 103.0(8) . 4_556 ?
O4 Cl2 O4 118.7(16) . 4_556 ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.933
_refine_diff_density_min         -0.979
_refine_diff_density_rms         0.162

#===END


