# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_aa
_database_code_depnum_ccdc_archive 'CCDC 1820806'
_audit_update_record             
;
2018-01-31 deposited with the CCDC.
2018-04-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Ag3 I4, C15 H14 N3'
_chemical_formula_sum            'C15 H14 Ag3 I4 N3'
_chemical_formula_weight         1067.50

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'
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           Monoclinic
_symmetry_space_group_name_H-M   'C2/m  '
_symmetry_space_group_name_Hall  '-C 2y'

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

_cell_length_a                   26.757(7)
_cell_length_b                   6.7094(17)
_cell_length_c                   13.283(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.927(6)
_cell_angle_gamma                90.00
_cell_volume                     2355.8(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    9714
_cell_measurement_theta_min      3.08
_cell_measurement_theta_max      28.26

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.424
_exptl_crystal_size_mid          0.058
_exptl_crystal_size_min          0.047
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.010
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1912
_exptl_absorpt_coefficient_mu    7.716
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      273(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            36335
_diffrn_reflns_av_R_equivalents  0.0240
_diffrn_reflns_av_sigmaI/netI    0.0123
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.35
_diffrn_reflns_theta_max         28.33
_reflns_number_total             3129
_reflns_number_gt                2806
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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 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)+(0.0832P)²+18.0001P] where P=(Fo²+2Fc²)/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       0.00628(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3129
_refine_ls_number_parameters     149
_refine_ls_number_restraints     116
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0488
_refine_ls_wR_factor_ref         0.1512
_refine_ls_wR_factor_gt          0.1377
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_restrained_S_all      1.102
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001

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 0.937983(10) 0.76516(5) 0.18753(2) 0.07600(8) Uani 1 1 d . . .
Ag2 Ag 1.0000 1.25596(6) 0.0000 0.07756(11) Uani 1 2 d S . .
I1 I 1.030406(9) 1.0000 0.172258(18) 0.05729(7) Uani 1 2 d S . .
I2 I 0.965684(10) 0.5000 0.350127(18) 0.05653(7) Uani 1 2 d S . .
I3 I 0.857160(10) 1.0000 0.22447(2) 0.06381(8) Uani 1 2 d S . .
I4 I 0.912638(9) 0.5000 0.008709(18) 0.05555(6) Uani 1 2 d S . .
C1 C 0.8311(2) 0.5000 0.7108(5) 0.1001(18) Uani 1 2 d SDU . .
H1 H 0.8288 0.5000 0.7800 0.120 Uiso 1 2 calc SR . .
C2 C 0.7861(2) 0.5000 0.6373(4) 0.0961(17) Uani 1 2 d SDU . .
H2 H 0.7537 0.5000 0.6542 0.115 Uiso 1 2 calc SR . .
C3 C 0.79630(18) 0.5000 0.5358(3) 0.0788(13) Uani 1 2 d SDU . .
C4 C 0.78562(14) 0.5000 0.3728(3) 0.0636(11) Uani 1 2 d SDU . .
C5 C 0.7641(2) 0.5000 0.2610(3) 0.0762(13) Uani 1 2 d SDU . .
C6 C 0.7122(2) 0.5000 0.2368(4) 0.1047(18) Uani 1 2 d SDU . .
H6 H 0.6925 0.5000 0.2887 0.126 Uiso 1 2 calc SR . .
C7 C 0.6883(3) 0.5000 0.1329(5) 0.117(2) Uani 1 2 d SDU . .
H7 H 0.6532 0.5000 0.1160 0.140 Uiso 1 2 calc SR . .
C8 C 0.7184(3) 0.5000 0.0598(5) 0.1056(19) Uani 1 2 d SU . .
H8 H 0.7040 0.5000 -0.0086 0.127 Uiso 1 2 calc SR . .
C9 C 0.7686(2) 0.5000 0.0855(5) 0.1021(17) Uani 1 2 d SU . .
H9 H 0.7886 0.5000 0.0342 0.122 Uiso 1 2 calc SR . .
C10 C 0.7908(2) 0.5000 0.1813(5) 0.0850(15) Uani 1 2 d SU . .
H10 H 0.8259 0.5000 0.1951 0.102 Uiso 1 2 calc SR . .
C11 C 0.8436(2) 0.5000 0.5130(4) 0.0807(14) Uani 1 2 d SDU . .
C12 C 0.8829(3) 0.5000 0.5792(4) 0.1056(19) Uani 1 2 d SDU . .
H12 H 0.9148 0.5000 0.5596 0.127 Uiso 1 2 calc SR . .
C13 C 0.8781(3) 0.5000 0.6793(4) 0.1055(19) Uani 1 2 d SDU . .
H13 H 0.9071 0.5000 0.7280 0.127 Uiso 1 2 calc SR . .
C14 C 0.94009(15) 1.0000 0.5176(4) 0.0673(12) Uani 1 2 d SU . .
H14A H 0.9515 1.1348 0.5129 0.101 Uiso 0.50 1 calc PR . .
H14B H 0.9449 0.9282 0.4573 0.101 Uiso 0.50 1 calc PR . .
H14C H 0.9591 0.9370 0.5762 0.101 Uiso 0.50 1 calc PR . .
C15 C 0.88611(15) 1.0000 0.5274(3) 0.0590(10) Uani 1 2 d SU . .
N1 N 0.76002(17) 0.5000 0.4456(3) 0.0917(14) Uani 1 2 d SDU . .
H1A H 0.7276 0.5000 0.4413 0.110 Uiso 1 2 calc SR . .
N2 N 0.83511(16) 0.5000 0.4029(3) 0.0836(13) Uani 1 2 d SDU . .
H2A H 0.8580 0.5000 0.3641 0.100 Uiso 1 2 calc SR . .
N3 N 0.84612(16) 1.0000 0.5383(4) 0.0874(13) Uani 1 2 d SU . .


_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 I3 2.7801(6) . ?
Ag1 I2 2.8076(6) . ?
Ag1 I4 2.9610(6) . ?
Ag1 I1 2.9656(7) . ?
Ag1 Ag1 3.1512(10) 6_575 ?
Ag1 Ag2 3.2034(7) 5_775 ?
Ag2 I4 2.8709(6) 5_775 ?
Ag2 I4 2.8709(6) 1_565 ?
Ag2 I1 2.8756(6) 5_775 ?
Ag2 I1 2.8756(6) . ?
Ag2 Ag1 3.2034(7) 5_775 ?
Ag2 Ag1 3.2034(7) 6_575 ?
Ag2 Ag2 3.2747(12) 5_785 ?
I1 Ag2 2.8756(6) 5_775 ?
I1 Ag1 2.9656(7) 6_575 ?
I2 Ag1 2.8076(6) 6_565 ?
I3 Ag1 2.7801(6) 6_575 ?
I4 Ag2 2.8709(6) 5_775 ?
I4 Ag2 2.8709(6) 1_545 ?
I4 Ag1 2.9610(6) 6_565 ?
C1 C13 1.388(9) . ?
C1 C2 1.427(7) . ?
C1 H1 0.9300 . ?
C2 C3 1.416(7) . ?
C2 H2 0.9300 . ?
C3 C11 1.346(8) . ?
C3 N1 1.420(6) . ?
C4 N1 1.269(6) . ?
C4 N2 1.322(5) . ?
C4 C5 1.508(6) . ?
C5 C10 1.365(8) . ?
C5 C6 1.375(8) . ?
C6 C7 1.429(8) . ?
C6 H6 0.9300 . ?
C7 C8 1.354(11) . ?
C7 H7 0.9300 . ?
C8 C9 1.334(9) . ?
C8 H8 0.9300 . ?
C9 C10 1.317(9) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C11 C12 1.263(8) . ?
C11 N2 1.444(6) . ?
C12 C13 1.355(8) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C14 C15 1.470(6) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 N3 1.102(6) . ?
N1 H1A 0.8600 . ?
N2 H2A 0.8600 . ?

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
I3 Ag1 I2 110.064(17) . . ?
I3 Ag1 I4 113.236(16) . . ?
I2 Ag1 I4 103.69(2) . . ?
I3 Ag1 I1 113.00(2) . . ?
I2 Ag1 I1 105.420(16) . . ?
I4 Ag1 I1 110.729(15) . . ?
I3 Ag1 Ag1 55.477(11) . 6_575 ?
I2 Ag1 Ag1 129.321(12) . 6_575 ?
I4 Ag1 Ag1 126.930(12) . 6_575 ?
I1 Ag1 Ag1 57.907(12) . 6_575 ?
I3 Ag1 Ag2 132.321(15) . 5_775 ?
I2 Ag1 Ag2 117.608(18) . 5_775 ?
I4 Ag1 Ag2 55.346(15) . 5_775 ?
I1 Ag1 Ag2 55.406(12) . 5_775 ?
Ag1 Ag1 Ag2 92.536(10) 6_575 5_775 ?
I4 Ag2 I4 110.45(2) 5_775 1_565 ?
I4 Ag2 I1 116.112(12) 5_775 5_775 ?
I4 Ag2 I1 103.950(13) 1_565 5_775 ?
I4 Ag2 I1 103.950(13) 5_775 . ?
I4 Ag2 I1 116.112(12) 1_565 . ?
I1 Ag2 I1 106.66(2) 5_775 . ?
I4 Ag2 Ag1 58.039(12) 5_775 5_775 ?
I4 Ag2 Ag1 125.437(14) 1_565 5_775 ?
I1 Ag2 Ag1 58.098(15) 5_775 5_775 ?
I1 Ag2 Ag1 118.400(18) . 5_775 ?
I4 Ag2 Ag1 125.437(14) 5_775 6_575 ?
I4 Ag2 Ag1 58.039(12) 1_565 6_575 ?
I1 Ag2 Ag1 118.400(18) 5_775 6_575 ?
I1 Ag2 Ag1 58.098(15) . 6_575 ?
Ag1 Ag2 Ag1 174.929(19) 5_775 6_575 ?
I4 Ag2 Ag2 55.227(12) 5_775 5_785 ?
I4 Ag2 Ag2 55.227(12) 1_565 5_785 ?
I1 Ag2 Ag2 126.670(12) 5_775 5_785 ?
I1 Ag2 Ag2 126.670(12) . 5_785 ?
Ag1 Ag2 Ag2 92.536(10) 5_775 5_785 ?
Ag1 Ag2 Ag2 92.536(10) 6_575 5_785 ?
Ag2 I1 Ag2 73.34(2) 5_775 . ?
Ag2 I1 Ag1 66.496(12) 5_775 . ?
Ag2 I1 Ag1 103.637(15) . . ?
Ag2 I1 Ag1 103.637(15) 5_775 6_575 ?
Ag2 I1 Ag1 66.496(13) . 6_575 ?
Ag1 I1 Ag1 64.19(2) . 6_575 ?
Ag1 I2 Ag1 78.64(2) 6_565 . ?
Ag1 I3 Ag1 69.05(2) 6_575 . ?
Ag2 I4 Ag2 69.55(2) 5_775 1_545 ?
Ag2 I4 Ag1 66.616(12) 5_775 . ?
Ag2 I4 Ag1 106.765(15) 1_545 . ?
Ag2 I4 Ag1 106.765(15) 5_775 6_565 ?
Ag2 I4 Ag1 66.616(12) 1_545 6_565 ?
Ag1 I4 Ag1 73.86(2) . 6_565 ?
C13 C1 C2 120.1(5) . . ?
C13 C1 H1 120.0 . . ?
C2 C1 H1 120.0 . . ?
C3 C2 C1 112.7(5) . . ?
C3 C2 H2 123.7 . . ?
C1 C2 H2 123.7 . . ?
C11 C3 C2 122.8(4) . . ?
C11 C3 N1 110.7(4) . . ?
C2 C3 N1 126.6(5) . . ?
N1 C4 N2 113.8(4) . . ?
N1 C4 C5 125.6(4) . . ?
N2 C4 C5 120.6(4) . . ?
C10 C5 C6 116.7(5) . . ?
C10 C5 C4 126.8(5) . . ?
C6 C5 C4 116.6(5) . . ?
C5 C6 C7 120.8(6) . . ?
C5 C6 H6 119.6 . . ?
C7 C6 H6 119.6 . . ?
C8 C7 C6 117.7(6) . . ?
C8 C7 H7 121.2 . . ?
C6 C7 H7 121.2 . . ?
C9 C8 C7 120.3(6) . . ?
C9 C8 H8 119.9 . . ?
C7 C8 H8 119.9 . . ?
C10 C9 C8 122.2(7) . . ?
C10 C9 H9 118.9 . . ?
C8 C9 H9 118.9 . . ?
C9 C10 C5 122.5(5) . . ?
C9 C10 H10 118.7 . . ?
C5 C10 H10 118.7 . . ?
C12 C11 C3 123.6(5) . . ?
C12 C11 N2 133.5(6) . . ?
C3 C11 N2 102.9(4) . . ?
C11 C12 C13 119.2(7) . . ?
C11 C12 H12 120.4 . . ?
C13 C12 H12 120.4 . . ?
C12 C13 C1 121.7(6) . . ?
C12 C13 H13 119.2 . . ?
C1 C13 H13 119.2 . . ?
C15 C14 H14A 109.5 . . ?
C15 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C15 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N3 C15 C14 177.5(5) . . ?
C4 N1 C3 105.3(4) . . ?
C4 N1 H1A 127.4 . . ?
C3 N1 H1A 127.4 . . ?
C4 N2 C11 107.4(4) . . ?
C4 N2 H2A 126.3 . . ?
C11 N2 H2A 126.3 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1A N3 0.86 2.03 2.881(6) 168.6 7_666
N2 H2A I2 0.86 2.92 3.669(4) 147.3 .

_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_theta_full        28.33
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         1.818
_refine_diff_density_min         -1.822
_refine_diff_density_rms         0.464
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_aa_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1820807'
_audit_update_record             
;
2018-01-31 deposited with the CCDC.
2018-04-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Ag3 I4?? C15 H15 N2'
_chemical_formula_sum            'C15 H15 Ag3 I4 N2'
_chemical_formula_weight         1054.50

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'
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 '
_symmetry_space_group_name_Hall  '-P 2a 2bc '


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                   7.5462(4)
_cell_length_b                   22.2417(12)
_cell_length_c                   13.1833(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2212.7(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    9991
_cell_measurement_theta_min      2.40
_cell_measurement_theta_max      28.29

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.423
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.032
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.165
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1888
_exptl_absorpt_coefficient_mu    8.211
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2788
_exptl_absorpt_correction_T_max  0.7681
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      273(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            37421
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_av_sigmaI/netI    0.0147
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.11
_diffrn_reflns_theta_max         28.33
_reflns_number_total             2715
_reflns_number_gt                2516
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0412P)²+11.4075P] where P=(Fo²+2Fc²)/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         2715
_refine_ls_number_parameters     112
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0364
_refine_ls_wR_factor_ref         0.0944
_refine_ls_wR_factor_gt          0.0929
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_restrained_S_all      1.093
_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
Ag2 Ag -0.06362(7) 0.74708(2) 0.88300(4) 0.05547(16) Uani 1 1 d . . .
Ag1 Ag 0.33467(9) 0.7500 0.7500 0.05139(19) Uani 1 2 d S . .
I2 I 0.06782(5) 0.74061(2) 1.08320(3) 0.04434(13) Uani 1 1 d . . .
I1 I 0.06908(4) 0.656623(14) 0.74244(2) 0.03405(11) Uani 1 1 d . . .
N1 N 0.6815(5) 0.54341(16) 0.7063(3) 0.0289(7) Uani 1 1 d . . .
C9 C 0.5820(7) 0.5968(2) 0.7369(4) 0.0384(11) Uani 1 1 d . . .
H9A H 0.5470 0.5929 0.8066 0.058 Uiso 1 1 calc R . .
H9B H 0.4785 0.6007 0.6952 0.058 Uiso 1 1 calc R . .
H10C H 0.6552 0.6318 0.7291 0.058 Uiso 1 1 calc R . .
C8 C 0.7500 0.5000 1.0861(6) 0.056(2) Uani 1 2 d S . .
H8 H 0.7500 0.5000 1.1567 0.067 Uiso 1 2 calc SR . .
C7 C 0.7903(8) 0.5523(3) 1.0345(4) 0.0499(13) Uani 1 1 d . . .
H7 H 0.8153 0.5873 1.0702 0.060 Uiso 1 1 calc R . .
C6 C 0.7935(7) 0.5525(2) 0.9302(4) 0.0393(11) Uani 1 1 d . . .
H6 H 0.8245 0.5873 0.8952 0.047 Uiso 1 1 calc R . .
C5 C 0.7500 0.5000 0.8767(5) 0.0312(12) Uani 1 2 d S . .
C4 C 0.7500 0.5000 0.7660(5) 0.0282(12) Uani 1 2 d S . .
C3 C 0.7081(6) 0.52781(18) 0.6055(3) 0.0285(8) Uani 1 1 d . . .
C2 C 0.6663(6) 0.5578(2) 0.5163(4) 0.0356(10) Uani 1 1 d . . .
H2 H 0.6129 0.5955 0.5163 0.043 Uiso 1 1 calc R . .
C1 C 0.7088(8) 0.5282(2) 0.4279(4) 0.0414(11) Uani 1 1 d . . .
H1 H 0.6819 0.5463 0.3661 0.050 Uiso 1 1 calc R . .


_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
Ag2 I2 2.8204(7) 6_557 ?
Ag2 I2 2.8233(7) . ?
Ag2 I1 2.8853(6) 4_566 ?
Ag2 I1 2.9128(6) . ?
Ag1 I2 2.8239(5) 6_657 ?
Ag1 I2 2.8239(6) 7_675 ?
Ag1 I1 2.8879(6) . ?
Ag1 I1 2.8879(6) 4_566 ?
I2 Ag2 2.8204(7) 6_657 ?
I2 Ag1 2.8239(5) 6_557 ?
I1 Ag2 2.8853(6) 4_566 ?
N1 C4 1.349(5) . ?
N1 C3 1.388(5) . ?
N1 C9 1.462(6) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H10C 0.9600 . ?
C8 C7 1.381(8) 2_665 ?
C8 C7 1.381(8) . ?
C8 H8 0.9300 . ?
C7 C6 1.376(7) . ?
C7 H7 0.9300 . ?
C6 C5 1.402(6) . ?
C6 H6 0.9300 . ?
C5 C6 1.402(6) 2_665 ?
C5 C4 1.460(9) . ?
C4 N1 1.349(5) 2_665 ?
C3 C2 1.388(6) . ?
C3 C3 1.389(8) 2_665 ?
C2 C1 1.376(7) . ?
C2 H2 0.9300 . ?
C1 C1 1.401(11) 2_665 ?
C1 H1 0.9300 . ?

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
I2 Ag2 I2 101.312(17) 6_557 . ?
I2 Ag2 I1 118.08(2) 6_557 4_566 ?
I2 Ag2 I1 116.86(2) . 4_566 ?
I2 Ag2 I1 113.85(2) 6_557 . ?
I2 Ag2 I1 116.02(2) . . ?
I1 Ag2 I1 91.650(18) 4_566 . ?
I2 Ag1 I2 102.92(3) 6_657 7_675 ?
I2 Ag1 I1 113.957(11) 6_657 . ?
I2 Ag1 I1 117.304(10) 7_675 . ?
I2 Ag1 I1 117.304(10) 6_657 4_566 ?
I2 Ag1 I1 113.957(11) 7_675 4_566 ?
I1 Ag1 I1 92.11(2) . 4_566 ?
Ag2 I2 Ag2 119.442(19) 6_657 . ?
Ag2 I2 Ag1 119.183(19) 6_657 6_557 ?
Ag2 I2 Ag1 120.35(2) . 6_557 ?
Ag2 I1 Ag1 74.145(15) 4_566 . ?
Ag2 I1 Ag2 74.49(2) 4_566 . ?
Ag1 I1 Ag2 73.734(15) . . ?
C4 N1 C3 108.9(4) . . ?
C4 N1 C9 128.1(4) . . ?
C3 N1 C9 122.8(4) . . ?
N1 C9 H9A 109.5 . . ?
N1 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N1 C9 H10C 109.5 . . ?
H9A C9 H10C 109.5 . . ?
H9B C9 H10C 109.5 . . ?
C7 C8 C7 121.0(7) 2_665 . ?
C7 C8 H8 119.5 2_665 . ?
C7 C8 H8 119.5 . . ?
C6 C7 C8 120.0(6) . . ?
C6 C7 H7 120.0 . . ?
C8 C7 H7 120.0 . . ?
C7 C6 C5 119.7(5) . . ?
C7 C6 H6 120.1 . . ?
C5 C6 H6 120.1 . . ?
C6 C5 C6 119.7(6) . 2_665 ?
C6 C5 C4 120.2(3) . . ?
C6 C5 C4 120.2(3) 2_665 . ?
N1 C4 N1 108.6(5) 2_665 . ?
N1 C4 C5 125.7(3) 2_665 . ?
N1 C4 C5 125.7(3) . . ?
C2 C3 N1 131.1(4) . . ?
C2 C3 C3 122.1(3) . 2_665 ?
N1 C3 C3 106.8(2) . 2_665 ?
C1 C2 C3 115.8(4) . . ?
C1 C2 H2 122.1 . . ?
C3 C2 H2 122.1 . . ?
C2 C1 C1 122.1(3) . 2_665 ?
C2 C1 H1 118.9 . . ?
C1 C1 H1 118.9 2_665 . ?

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
I2 Ag2 I2 Ag2 -178.554(7) 6_557 . . 6_657 ?
I1 Ag2 I2 Ag2 -48.81(4) 4_566 . . 6_657 ?
I1 Ag2 I2 Ag2 57.64(4) . . . 6_657 ?
I2 Ag2 I2 Ag1 -10.22(3) 6_557 . . 6_557 ?
I1 Ag2 I2 Ag1 119.52(2) 4_566 . . 6_557 ?
I1 Ag2 I2 Ag1 -134.03(2) . . . 6_557 ?
I2 Ag1 I1 Ag2 160.45(2) 6_657 . . 4_566 ?
I2 Ag1 I1 Ag2 -79.24(2) 7_675 . . 4_566 ?
I1 Ag1 I1 Ag2 39.206(12) 4_566 . . 4_566 ?
I2 Ag1 I1 Ag2 82.380(19) 6_657 . . . ?
I2 Ag1 I1 Ag2 -157.30(2) 7_675 . . . ?
I1 Ag1 I1 Ag2 -38.862(12) 4_566 . . . ?
I2 Ag2 I1 Ag2 83.112(17) 6_557 . . 4_566 ?
I2 Ag2 I1 Ag2 -159.860(19) . . . 4_566 ?
I1 Ag2 I1 Ag2 -38.73(2) 4_566 . . 4_566 ?
I2 Ag2 I1 Ag1 160.73(2) 6_557 . . . ?
I2 Ag2 I1 Ag1 -82.24(2) . . . . ?
I1 Ag2 I1 Ag1 38.891(14) 4_566 . . . ?
C7 C8 C7 C6 -1.1(4) 2_665 . . . ?
C8 C7 C6 C5 2.1(8) . . . . ?
C7 C6 C5 C6 -1.1(4) . . . 2_665 ?
C7 C6 C5 C4 178.9(4) . . . . ?
C3 N1 C4 N1 -0.6(2) . . . 2_665 ?
C9 N1 C4 N1 174.9(5) . . . 2_665 ?
C3 N1 C4 C5 179.4(2) . . . . ?
C9 N1 C4 C5 -5.1(5) . . . . ?
C6 C5 C4 N1 136.1(3) . . . 2_665 ?
C6 C5 C4 N1 -43.9(3) 2_665 . . 2_665 ?
C6 C5 C4 N1 -43.9(3) . . . . ?
C6 C5 C4 N1 136.1(3) 2_665 . . . ?
C4 N1 C3 C2 -178.3(4) . . . . ?
C9 N1 C3 C2 5.9(8) . . . . ?
C4 N1 C3 C3 1.5(6) . . . 2_665 ?
C9 N1 C3 C3 -174.3(5) . . . 2_665 ?
N1 C3 C2 C1 -178.6(5) . . . . ?
C3 C3 C2 C1 1.7(8) 2_665 . . . ?
C3 C2 C1 C1 -0.8(10) . . . 2_665 ?

_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_theta_full        28.33
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         1.499
_refine_diff_density_min         -1.923
_refine_diff_density_rms         0.208
