# Electronic Supplementary Material (ESI) for CrystEngComm
# This journal is © The Royal Society of Chemistry 2014
#######################################################################
#
# Cambridge Crystallographic Data Centre
# CCDC
#
#######################################################################
#
# This CIF contains data from an original supplementary publication
# deposited with the CCDC, and may include chemical, crystal,
# experimental, refinement, atomic coordinates,
# anisotropic displacement parameters and molecular geometry data,
# as required by the journal to which it was submitted.
#
# This CIF is provided on the understanding that it is used for bona
# fide research purposes only. It may contain copyright material
# of the CCDC or of third parties, and may not be copied or further
# disseminated in any form, whether machine-readable or not,
# except for the purpose of generating routine backup copies
# on your local computer system.
#
# For further information on the CCDC, data deposition and
# data retrieval see:
# www.ccdc.cam.ac.uk
#
# Bona fide researchers may freely download Mercury and enCIFer
# from this site to visualise CIF-encoded structures and
# to carry out CIF format checking respectively.
#
data_L
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety ?
_chemical_formula_sum 'C8 H6 N4 S'
_chemical_formula_weight 190.23
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting Monoclinic
_symmetry_space_group_name_H-M P2(1)/n
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
_cell_length_a 3.90610(10)
_cell_length_b 20.4757(3)
_cell_length_c 10.6097(2)
_cell_angle_alpha 90.00
_cell_angle_beta 98.4360(10)
_cell_angle_gamma 90.00
_cell_volume 839.38(3)
_cell_formula_units_Z 4
_cell_measurement_temperature 296(2)
_cell_measurement_reflns_used ?
_cell_measurement_theta_min ?
_cell_measurement_theta_max ?
_exptl_crystal_description Block
_exptl_crystal_colour colorless
_exptl_crystal_size_max 0.4
_exptl_crystal_size_mid 0.3
_exptl_crystal_size_min 0.2
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.505
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 392
_exptl_absorpt_coefficient_mu 0.337
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.6645
_exptl_absorpt_correction_T_max 0.7456
_exptl_absorpt_process_details 'SADABS (Bruker, 2007)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 296(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 APEXII CCD area detector'
_diffrn_measurement_method \w-scans
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 13505
_diffrn_reflns_av_R_equivalents 0.0387
_diffrn_reflns_av_sigmaI/netI 0.0241
_diffrn_reflns_limit_h_min -5
_diffrn_reflns_limit_h_max 5
_diffrn_reflns_limit_k_min -27
_diffrn_reflns_limit_k_max 27
_diffrn_reflns_limit_l_min -13
_diffrn_reflns_limit_l_max 14
_diffrn_reflns_theta_min 1.99
_diffrn_reflns_theta_max 28.05
_reflns_number_total 2017
_reflns_number_gt 1469
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'APEX2 (Bruker 2007)'
_computing_cell_refinement 'APEX2 and SAINT (Bruker 2007)'
_computing_data_reduction SAINT
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
;
SHELXTL and PLATON (Spek, 2009)
;
_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^)+(0.0603P)^2^+0.0751P] 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 2017
_refine_ls_number_parameters 118
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0589
_refine_ls_R_factor_gt 0.0405
_refine_ls_wR_factor_ref 0.1178
_refine_ls_wR_factor_gt 0.1071
_refine_ls_goodness_of_fit_ref 1.091
_refine_ls_restrained_S_all 1.091
_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
S1 S 0.12788(15) 0.20583(2) 0.40967(4) 0.0593(2) Uani 1 1 d . . .
C2 C 0.2076(5) 0.17153(9) 0.65777(17) 0.0517(4) Uani 1 1 d . . .
H2A H 0.0965 0.2111 0.6667 0.062 Uiso 1 1 calc R . .
C4 C 0.5125(5) 0.05948(9) 0.62212(17) 0.0522(4) Uani 1 1 d . . .
H4A H 0.6201 0.0195 0.6135 0.063 Uiso 1 1 calc R . .
N3 N 0.2105(4) 0.18638(7) 0.17284(15) 0.0520(4) Uani 1 1 d . . .
N4 N -0.0417(4) 0.05877(8) 0.15778(15) 0.0573(4) Uani 1 1 d . . .
C1 C 0.2610(4) 0.15162(8) 0.53676(15) 0.0423(4) Uani 1 1 d . . .
N1 N 0.4148(4) 0.09515(7) 0.51820(14) 0.0495(4) Uani 1 1 d . . .
C3 C 0.4609(5) 0.07915(10) 0.74088(18) 0.0583(5) Uani 1 1 d . . .
H3A H 0.5332 0.0522 0.8102 0.070 Uiso 1 1 calc R . .
N2 N 0.3096(5) 0.13608(8) 0.76033(15) 0.0615(4) Uani 1 1 d . . .
C5 C 0.1059(4) 0.15675(8) 0.27222(15) 0.0428(4) Uani 1 1 d . . .
C6 C -0.0297(5) 0.09371(9) 0.26276(17) 0.0484(4) Uani 1 1 d . . .
H6A H -0.1143 0.0757 0.3326 0.058 Uiso 1 1 calc R . .
C7 C 0.0712(5) 0.08822(10) 0.05933(18) 0.0572(5) Uani 1 1 d . . .
H7A H 0.0725 0.0650 -0.0160 0.069 Uiso 1 1 calc R . .
C8 C 0.1848(6) 0.15141(10) 0.06598(17) 0.0584(5) Uani 1 1 d . . .
H8A H 0.2464 0.1707 -0.0068 0.070 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
S1 0.0916(4) 0.0387(3) 0.0486(3) 0.00160(19) 0.0139(3) 0.0131(2)
C2 0.0643(11) 0.0462(10) 0.0465(10) -0.0094(8) 0.0147(8) -0.0001(8)
C4 0.0643(11) 0.0450(10) 0.0458(10) 0.0004(8) 0.0029(8) 0.0061(8)
N3 0.0685(10) 0.0420(8) 0.0473(8) 0.0087(7) 0.0141(7) -0.0010(7)
N4 0.0688(10) 0.0506(9) 0.0499(9) 0.0015(7) -0.0003(8) -0.0095(8)
C1 0.0501(9) 0.0369(8) 0.0408(9) -0.0041(7) 0.0098(7) -0.0021(7)
N1 0.0633(9) 0.0425(8) 0.0434(8) -0.0038(6) 0.0102(7) 0.0097(7)
C3 0.0740(13) 0.0563(12) 0.0419(10) 0.0035(8) -0.0002(9) -0.0024(10)
N2 0.0803(11) 0.0629(10) 0.0424(9) -0.0061(8) 0.0126(8) -0.0005(9)
C5 0.0486(9) 0.0386(8) 0.0416(9) 0.0072(7) 0.0083(7) 0.0060(7)
C6 0.0532(10) 0.0487(10) 0.0435(9) 0.0074(8) 0.0077(8) -0.0054(8)
C7 0.0735(13) 0.0557(11) 0.0414(10) -0.0006(8) 0.0049(9) -0.0016(9)
C8 0.0775(13) 0.0569(11) 0.0426(10) 0.0077(9) 0.0144(9) -0.0012(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
S1 C5 1.7626(17) . ?
S1 C1 1.7648(17) . ?
C2 N2 1.320(2) . ?
C2 C1 1.392(2) . ?
C2 H2A 0.9300 . ?
C4 N1 1.331(2) . ?
C4 C3 1.366(3) . ?
C4 H4A 0.9300 . ?
N3 C5 1.332(2) . ?
N3 C8 1.332(2) . ?
N4 C6 1.319(2) . ?
N4 C7 1.336(2) . ?
C1 N1 1.331(2) . ?
C3 N2 1.337(3) . ?
C3 H3A 0.9300 . ?
C5 C6 1.393(2) . ?
C6 H6A 0.9300 . ?
C7 C8 1.366(3) . ?
C7 H7A 0.9300 . ?
C8 H8A 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
C5 S1 C1 104.28(8) . . ?
N2 C2 C1 122.11(17) . . ?
N2 C2 H2A 118.9 . . ?
C1 C2 H2A 118.9 . . ?
N1 C4 C3 122.64(17) . . ?
N1 C4 H4A 118.7 . . ?
C3 C4 H4A 118.7 . . ?
C5 N3 C8 115.82(15) . . ?
C6 N4 C7 116.15(16) . . ?
N1 C1 C2 121.53(16) . . ?
N1 C1 S1 121.47(12) . . ?
C2 C1 S1 116.97(13) . . ?
C4 N1 C1 115.78(14) . . ?
N2 C3 C4 121.88(18) . . ?
N2 C3 H3A 119.1 . . ?
C4 C3 H3A 119.1 . . ?
C2 N2 C3 116.05(16) . . ?
N3 C5 C6 121.51(15) . . ?
N3 C5 S1 114.33(13) . . ?
C6 C5 S1 124.03(12) . . ?
N4 C6 C5 121.96(15) . . ?
N4 C6 H6A 119.0 . . ?
C5 C6 H6A 119.0 . . ?
N4 C7 C8 121.94(17) . . ?
N4 C7 H7A 119.0 . . ?
C8 C7 H7A 119.0 . . ?
N3 C8 C7 122.43(17) . . ?
N3 C8 H8A 118.8 . . ?
C7 C8 H8A 118.8 . . ?
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
N2 C2 C1 N1 0.8(3) . . . . ?
N2 C2 C1 S1 -177.24(15) . . . . ?
C5 S1 C1 N1 19.69(17) . . . . ?
C5 S1 C1 C2 -162.27(14) . . . . ?
C3 C4 N1 C1 -0.3(3) . . . . ?
C2 C1 N1 C4 0.1(3) . . . . ?
S1 C1 N1 C4 178.02(13) . . . . ?
N1 C4 C3 N2 -0.3(3) . . . . ?
C1 C2 N2 C3 -1.4(3) . . . . ?
C4 C3 N2 C2 1.2(3) . . . . ?
C8 N3 C5 C6 -1.6(3) . . . . ?
C8 N3 C5 S1 -177.56(14) . . . . ?
C1 S1 C5 N3 -142.40(14) . . . . ?
C1 S1 C5 C6 41.73(17) . . . . ?
C7 N4 C6 C5 -2.5(3) . . . . ?
N3 C5 C6 N4 4.3(3) . . . . ?
S1 C5 C6 N4 179.84(14) . . . . ?
C6 N4 C7 C8 -1.5(3) . . . . ?
C5 N3 C8 C7 -2.5(3) . . . . ?
N4 C7 C8 N3 4.2(3) . . . . ?
_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full 28.05
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max 0.165
_refine_diff_density_min -0.296
_refine_diff_density_rms 0.048
##########################End############################
_database_code_depnum_ccdc_archive 'CCDC 926725'
#######################################################################
#
# Cambridge Crystallographic Data Centre
# CCDC
#
#######################################################################
#
# This CIF contains data from an original supplementary publication
# deposited with the CCDC, and may include chemical, crystal,
# experimental, refinement, atomic coordinates,
# anisotropic displacement parameters and molecular geometry data,
# as required by the journal to which it was submitted.
#
# This CIF is provided on the understanding that it is used for bona
# fide research purposes only. It may contain copyright material
# of the CCDC or of third parties, and may not be copied or further
# disseminated in any form, whether machine-readable or not,
# except for the purpose of generating routine backup copies
# on your local computer system.
#
# For further information on the CCDC, data deposition and
# data retrieval see:
# www.ccdc.cam.ac.uk
#
# Bona fide researchers may freely download Mercury and enCIFer
# from this site to visualise CIF-encoded structures and
# to carry out CIF format checking respectively.
#
data_1
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety ?
_chemical_formula_sum 'C16 H12 Ag3 Cl3 N8 O12 S2'
_chemical_formula_weight 1002.42
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'
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'
S S 0.1246 0.1234 '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'
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_H-M Imma
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y+1/2, z'
'-x, y+1/2, -z'
'x, -y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1, z+1/2'
'-x+1/2, y+1, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x, y-1/2, -z'
'x, -y-1/2, z'
'-x, y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y, -z+1/2'
'x+1/2, -y, z+1/2'
'-x+1/2, y+1/2, z+1/2'
_cell_length_a 19.181(4)
_cell_length_b 11.579(3)
_cell_length_c 12.642(3)
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_volume 2808.0(10)
_cell_formula_units_Z 4
_cell_measurement_temperature 293(2)
_cell_measurement_reflns_used ?
_cell_measurement_theta_min ?
_cell_measurement_theta_max ?
_exptl_crystal_description Block
_exptl_crystal_colour colorless
_exptl_crystal_size_max 0.4
_exptl_crystal_size_mid 0.3
_exptl_crystal_size_min 0.2
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 2.371
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1936
_exptl_absorpt_coefficient_mu 2.581
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.835
_exptl_absorpt_correction_T_max 0.905
_exptl_absorpt_process_details 'SADABS (Bruker, 2007)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 293(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 APEXII CCD area detector'
_diffrn_measurement_method \w-scans
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 9653
_diffrn_reflns_av_R_equivalents 0.0514
_diffrn_reflns_av_sigmaI/netI 0.0392
_diffrn_reflns_limit_h_min -25
_diffrn_reflns_limit_h_max 23
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_l_min -13
_diffrn_reflns_limit_l_max 16
_diffrn_reflns_theta_min 1.93
_diffrn_reflns_theta_max 28.40
_reflns_number_total 1894
_reflns_number_gt 1347
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'APEX2 (Bruker 2007)'
_computing_cell_refinement 'APEX2 and SAINT (Bruker 2007)'
_computing_data_reduction SAINT
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
;
SHELXTL and PLATON (Spek, 2009)
;
_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^)+(0.0372P)^2^+20.4300P] 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 1894
_refine_ls_number_parameters 128
_refine_ls_number_restraints 56
_refine_ls_R_factor_all 0.0676
_refine_ls_R_factor_gt 0.0401
_refine_ls_wR_factor_ref 0.1087
_refine_ls_wR_factor_gt 0.0929
_refine_ls_goodness_of_fit_ref 1.050
_refine_ls_restrained_S_all 1.184
_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 0.7500 0.7500 0.7500 0.0463(3) Uani 1 4 d S . .
Ag2 Ag 0.5000 0.2500 0.65739(7) 0.0350(2) Uani 1 4 d S . .
Ag3 Ag 0.5000 0.2500 0.89404(8) 0.0493(3) Uani 1 4 d S . .
N1 N 0.5833(2) 0.4030(4) 0.6911(4) 0.0427(11) Uani 1 1 d . . .
N2 N 0.6708(2) 0.5917(4) 0.7209(4) 0.0439(12) Uani 1 1 d . . .
S1 S 0.5000 0.46198(19) 0.85374(15) 0.0396(5) Uani 1 2 d S . .
C1 C 0.5720(3) 0.4815(5) 0.7653(4) 0.0336(11) Uani 1 1 d . . .
C2 C 0.6144(3) 0.5749(5) 0.7801(5) 0.0395(13) Uani 1 1 d . . .
H2A H 0.6035 0.6280 0.8328 0.047 Uiso 1 1 calc R . .
C3 C 0.6833(3) 0.5132(6) 0.6472(5) 0.0494(15) Uani 1 1 d . . .
H3A H 0.7231 0.5206 0.6057 0.059 Uiso 1 1 calc R . .
C4 C 0.6395(3) 0.4209(6) 0.6301(5) 0.0519(17) Uani 1 1 d . . .
H4A H 0.6491 0.3699 0.5752 0.062 Uiso 1 1 calc R . .
Cl1 Cl 0.5000 0.2402(17) 0.4062(3) 0.0598(18) Uani 0.50 2 d SPDU . .
O1 O 0.5000 0.2500 0.2967(6) 0.059(2) Uani 1 4 d SDU . .
O2 O 0.5624(5) 0.2500 0.4556(8) 0.124(3) Uani 1 2 d SDU . .
O3 O 0.5000 0.1185(14) 0.4264(12) 0.084(4) Uani 0.50 2 d SPDU . .
Cl2 Cl 0.32597(12) 0.2500 0.95997(18) 0.0591(6) Uani 1 2 d SDU . .
O4 O 0.3220(8) 0.3737(10) 0.9466(13) 0.123(5) Uani 0.50 1 d PDU . .
O5 O 0.2739(5) 0.2500 1.0326(7) 0.123(4) Uani 1 2 d SDU . .
O6 O 0.3935(4) 0.2500 1.0034(7) 0.091(2) Uani 1 2 d SDU . .
O7 O 0.3160(8) 0.2500 0.8553(7) 0.179(6) Uani 1 2 d SDU . .
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 0.0358(5) 0.0261(4) 0.0770(7) 0.000 0.0051(4) 0.000
Ag2 0.0389(5) 0.0300(4) 0.0361(4) 0.000 0.000 0.000
Ag3 0.0569(6) 0.0510(6) 0.0402(5) 0.000 0.000 0.000
N1 0.041(3) 0.039(3) 0.048(3) -0.007(2) 0.004(2) -0.008(2)
N2 0.032(2) 0.040(3) 0.059(3) -0.002(2) -0.003(2) -0.006(2)
S1 0.0385(10) 0.0469(12) 0.0334(10) -0.0042(8) 0.000 0.000
C1 0.030(3) 0.034(3) 0.036(3) -0.003(2) -0.004(2) 0.001(2)
C2 0.034(3) 0.034(3) 0.050(3) -0.009(2) -0.007(2) 0.003(2)
C3 0.038(3) 0.054(4) 0.057(4) -0.009(3) 0.008(3) -0.007(3)
C4 0.047(4) 0.052(4) 0.057(4) -0.016(3) 0.013(3) -0.006(3)
Cl1 0.058(2) 0.089(5) 0.0325(16) 0.003(4) 0.000 0.000
O1 0.066(5) 0.072(6) 0.039(4) 0.000 0.000 0.000
O2 0.107(6) 0.177(9) 0.088(6) 0.000 -0.039(5) 0.000
O3 0.111(9) 0.081(9) 0.061(7) 0.031(7) 0.000 0.000
Cl2 0.0460(13) 0.0855(19) 0.0457(13) 0.000 0.0126(10) 0.000
O4 0.117(10) 0.076(9) 0.176(13) 0.051(9) 0.005(10) 0.015(8)
O5 0.065(5) 0.229(12) 0.076(6) 0.000 0.033(5) 0.000
O6 0.053(4) 0.148(7) 0.072(5) 0.000 0.013(4) 0.000
O7 0.151(10) 0.314(16) 0.071(7) 0.000 0.003(7) 0.000
_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 N2 2.409(5) . ?
Ag1 N2 2.409(5) 11_575 ?
Ag1 N2 2.409(5) 13_666 ?
Ag1 N2 2.409(5) 7_646 ?
Ag2 N1 2.424(5) 2_655 ?
Ag2 N1 2.424(5) . ?
Ag2 N1 2.424(5) 12_655 ?
Ag2 N1 2.424(5) 11_565 ?
Ag2 Ag3 2.9918(14) . ?
Ag3 O6 2.466(7) 2_655 ?
Ag3 O6 2.466(7) . ?
Ag3 S1 2.507(2) 2_655 ?
Ag3 S1 2.507(2) . ?
N1 C1 1.324(7) . ?
N1 C4 1.342(7) . ?
N2 C3 1.324(8) . ?
N2 C2 1.330(7) . ?
S1 C1 1.792(5) 12_655 ?
S1 C1 1.792(5) . ?
C1 C2 1.365(8) . ?
C2 H2A 0.9300 . ?
C3 C4 1.376(9) . ?
C3 H3A 0.9300 . ?
C4 H4A 0.9300 . ?
Cl1 Cl1 0.23(4) 2_655 ?
Cl1 O2 1.355(8) 2_655 ?
Cl1 O2 1.355(8) . ?
Cl1 O1 1.390(8) . ?
Cl1 O3 1.432(15) . ?
Cl1 O3 1.66(3) 2_655 ?
O1 Cl1 1.390(8) 2_655 ?
O2 Cl1 1.355(8) 2_655 ?
O3 Cl1 1.66(3) 2_655 ?
Cl2 O7 1.337(9) . ?
Cl2 O5 1.357(7) . ?
Cl2 O6 1.407(7) . ?
Cl2 O4 1.445(11) . ?
Cl2 O4 1.445(11) 11_565 ?
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
N2 Ag1 N2 99.0(2) . 11_575 ?
N2 Ag1 N2 180.0 . 13_666 ?
N2 Ag1 N2 81.0(2) 11_575 13_666 ?
N2 Ag1 N2 81.0(2) . 7_646 ?
N2 Ag1 N2 180.000(1) 11_575 7_646 ?
N2 Ag1 N2 99.0(2) 13_666 7_646 ?
N1 Ag2 N1 159.7(2) 2_655 . ?
N1 Ag2 N1 93.9(2) 2_655 12_655 ?
N1 Ag2 N1 82.5(2) . 12_655 ?
N1 Ag2 N1 82.5(2) 2_655 11_565 ?
N1 Ag2 N1 93.9(2) . 11_565 ?
N1 Ag2 N1 159.7(2) 12_655 11_565 ?
N1 Ag2 Ag3 79.87(12) 2_655 . ?
N1 Ag2 Ag3 79.87(12) . . ?
N1 Ag2 Ag3 79.87(12) 12_655 . ?
N1 Ag2 Ag3 79.87(12) 11_565 . ?
O6 Ag3 O6 111.8(4) 2_655 . ?
O6 Ag3 S1 96.54(4) 2_655 2_655 ?
O6 Ag3 S1 96.54(4) . 2_655 ?
O6 Ag3 S1 96.54(4) 2_655 . ?
O6 Ag3 S1 96.54(4) . . ?
S1 Ag3 S1 156.55(10) 2_655 . ?
O6 Ag3 Ag2 124.09(19) 2_655 . ?
O6 Ag3 Ag2 124.09(19) . . ?
S1 Ag3 Ag2 78.27(5) 2_655 . ?
S1 Ag3 Ag2 78.27(5) . . ?
C1 N1 C4 115.6(5) . . ?
C1 N1 Ag2 121.2(4) . . ?
C4 N1 Ag2 122.8(4) . . ?
C3 N2 C2 116.3(5) . . ?
C3 N2 Ag1 121.0(4) . . ?
C2 N2 Ag1 122.6(4) . . ?
C1 S1 C1 100.9(3) 12_655 . ?
C1 S1 Ag3 104.51(19) 12_655 . ?
C1 S1 Ag3 104.51(19) . . ?
N1 C1 C2 123.0(5) . . ?
N1 C1 S1 118.8(4) . . ?
C2 C1 S1 118.2(4) . . ?
N2 C2 C1 121.5(5) . . ?
N2 C2 H2A 119.3 . . ?
C1 C2 H2A 119.3 . . ?
N2 C3 C4 122.2(6) . . ?
N2 C3 H3A 118.9 . . ?
C4 C3 H3A 118.9 . . ?
N1 C4 C3 121.4(6) . . ?
N1 C4 H4A 119.3 . . ?
C3 C4 H4A 119.3 . . ?
Cl1 Cl1 O2 85.2(9) 2_655 2_655 ?
Cl1 Cl1 O2 85.2(8) 2_655 . ?
O2 Cl1 O2 124.2(10) 2_655 . ?
Cl1 Cl1 O1 85.3(8) 2_655 . ?
O2 Cl1 O1 116.9(5) 2_655 . ?
O2 Cl1 O1 116.9(5) . . ?
Cl1 Cl1 O3 169.8(6) 2_655 . ?
O2 Cl1 O3 90.1(9) 2_655 . ?
O2 Cl1 O3 90.1(9) . . ?
O1 Cl1 O3 104.9(11) . . ?
Cl1 Cl1 O3 8.8(6) 2_655 2_655 ?
O2 Cl1 O3 81.1(8) 2_655 2_655 ?
O2 Cl1 O3 81.1(8) . 2_655 ?
O1 Cl1 O3 94.1(11) . 2_655 ?
O3 Cl1 O3 160.9(12) . 2_655 ?
Cl1 O1 Cl1 9.4(16) 2_655 . ?
Cl1 O2 Cl1 9.7(17) . 2_655 ?
Cl1 O3 Cl1 1.4(2) . 2_655 ?
O7 Cl2 O5 124.4(8) . . ?
O7 Cl2 O6 121.2(7) . . ?
O5 Cl2 O6 114.5(6) . . ?
O7 Cl2 O4 82.9(7) . . ?
O5 Cl2 O4 92.3(6) . . ?
O6 Cl2 O4 95.4(6) . . ?
O7 Cl2 O4 82.9(7) . 11_565 ?
O5 Cl2 O4 92.3(6) . 11_565 ?
O6 Cl2 O4 95.4(6) . 11_565 ?
O4 Cl2 O4 165.3(14) . 11_565 ?
Cl2 O6 Ag3 123.0(5) . . ?
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
N1 Ag2 Ag3 O6 132.05(12) 2_655 . . 2_655 ?
N1 Ag2 Ag3 O6 -47.95(12) . . . 2_655 ?
N1 Ag2 Ag3 O6 -132.05(12) 12_655 . . 2_655 ?
N1 Ag2 Ag3 O6 47.95(12) 11_565 . . 2_655 ?
N1 Ag2 Ag3 O6 -47.95(12) 2_655 . . . ?
N1 Ag2 Ag3 O6 132.05(12) . . . . ?
N1 Ag2 Ag3 O6 47.95(12) 12_655 . . . ?
N1 Ag2 Ag3 O6 -132.05(12) 11_565 . . . ?
N1 Ag2 Ag3 S1 42.05(12) 2_655 . . 2_655 ?
N1 Ag2 Ag3 S1 -137.95(12) . . . 2_655 ?
N1 Ag2 Ag3 S1 137.95(12) 12_655 . . 2_655 ?
N1 Ag2 Ag3 S1 -42.05(12) 11_565 . . 2_655 ?
N1 Ag2 Ag3 S1 -137.95(12) 2_655 . . . ?
N1 Ag2 Ag3 S1 42.05(12) . . . . ?
N1 Ag2 Ag3 S1 -42.05(12) 12_655 . . . ?
N1 Ag2 Ag3 S1 137.95(12) 11_565 . . . ?
N1 Ag2 N1 C1 -42.9(4) 2_655 . . . ?
N1 Ag2 N1 C1 38.1(5) 12_655 . . . ?
N1 Ag2 N1 C1 -121.8(4) 11_565 . . . ?
Ag3 Ag2 N1 C1 -42.9(4) . . . . ?
N1 Ag2 N1 C4 144.1(5) 2_655 . . . ?
N1 Ag2 N1 C4 -135.0(5) 12_655 . . . ?
N1 Ag2 N1 C4 65.1(5) 11_565 . . . ?
Ag3 Ag2 N1 C4 144.1(5) . . . . ?
N2 Ag1 N2 C3 122.1(4) 11_575 . . . ?
N2 Ag1 N2 C3 -20(41) 13_666 . . . ?
N2 Ag1 N2 C3 -57.9(4) 7_646 . . . ?
N2 Ag1 N2 C2 -61.2(5) 11_575 . . . ?
N2 Ag1 N2 C2 157(34) 13_666 . . . ?
N2 Ag1 N2 C2 118.8(5) 7_646 . . . ?
O6 Ag3 S1 C1 176.3(3) 2_655 . . 12_655 ?
O6 Ag3 S1 C1 -70.7(3) . . . 12_655 ?
S1 Ag3 S1 C1 52.79(17) 2_655 . . 12_655 ?
Ag2 Ag3 S1 C1 52.79(17) . . . 12_655 ?
O6 Ag3 S1 C1 70.7(3) 2_655 . . . ?
O6 Ag3 S1 C1 -176.3(3) . . . . ?
S1 Ag3 S1 C1 -52.79(17) 2_655 . . . ?
Ag2 Ag3 S1 C1 -52.79(17) . . . . ?
C4 N1 C1 C2 -0.2(8) . . . . ?
Ag2 N1 C1 C2 -173.8(4) . . . . ?
C4 N1 C1 S1 -177.7(5) . . . . ?
Ag2 N1 C1 S1 8.8(6) . . . . ?
C1 S1 C1 N1 -68.2(5) 12_655 . . . ?
Ag3 S1 C1 N1 40.1(5) . . . . ?
C1 S1 C1 C2 114.2(4) 12_655 . . . ?
Ag3 S1 C1 C2 -137.5(4) . . . . ?
C3 N2 C2 C1 0.0(8) . . . . ?
Ag1 N2 C2 C1 -176.9(4) . . . . ?
N1 C1 C2 N2 -0.9(9) . . . . ?
S1 C1 C2 N2 176.6(4) . . . . ?
C2 N2 C3 C4 2.0(9) . . . . ?
Ag1 N2 C3 C4 178.9(5) . . . . ?
C1 N1 C4 C3 2.2(9) . . . . ?
Ag2 N1 C4 C3 175.6(5) . . . . ?
N2 C3 C4 N1 -3.2(11) . . . . ?
O2 Cl1 O1 Cl1 82.2(14) 2_655 . . 2_655 ?
O2 Cl1 O1 Cl1 -82.2(13) . . . 2_655 ?
O3 Cl1 O1 Cl1 180.000(15) . . . 2_655 ?
O3 Cl1 O1 Cl1 0.000(15) 2_655 . . 2_655 ?
O2 Cl1 O2 Cl1 -80.8(16) 2_655 . . 2_655 ?
O1 Cl1 O2 Cl1 82.2(13) . . . 2_655 ?
O3 Cl1 O2 Cl1 -170.9(6) . . . 2_655 ?
O3 Cl1 O2 Cl1 -7.9(5) 2_655 . . 2_655 ?
O2 Cl1 O3 Cl1 -62.1(5) 2_655 . . 2_655 ?
O2 Cl1 O3 Cl1 62.1(5) . . . 2_655 ?
O1 Cl1 O3 Cl1 180.00(9) . . . 2_655 ?
O3 Cl1 O3 Cl1 0.00(8) 2_655 . . 2_655 ?
O7 Cl2 O6 Ag3 0.000(2) . . . . ?
O5 Cl2 O6 Ag3 180.0 . . . . ?
O4 Cl2 O6 Ag3 -85.0(7) . . . . ?
O4 Cl2 O6 Ag3 85.0(7) 11_565 . . . ?
O6 Ag3 O6 Cl2 180.0 2_655 . . . ?
S1 Ag3 O6 Cl2 -80.25(5) 2_655 . . . ?
S1 Ag3 O6 Cl2 80.25(5) . . . . ?
Ag2 Ag3 O6 Cl2 0.000(1) . . . . ?
_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full 28.40
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max 0.836
_refine_diff_density_min -0.947
_refine_diff_density_rms 0.137
_database_code_depnum_ccdc_archive 'CCDC 926718'
#######################################################################
#
# Cambridge Crystallographic Data Centre
# CCDC
#
#######################################################################
#
# This CIF contains data from an original supplementary publication
# deposited with the CCDC, and may include chemical, crystal,
# experimental, refinement, atomic coordinates,
# anisotropic displacement parameters and molecular geometry data,
# as required by the journal to which it was submitted.
#
# This CIF is provided on the understanding that it is used for bona
# fide research purposes only. It may contain copyright material
# of the CCDC or of third parties, and may not be copied or further
# disseminated in any form, whether machine-readable or not,
# except for the purpose of generating routine backup copies
# on your local computer system.
#
# For further information on the CCDC, data deposition and
# data retrieval see:
# www.ccdc.cam.ac.uk
#
# Bona fide researchers may freely download Mercury and enCIFer
# from this site to visualise CIF-encoded structures and
# to carry out CIF format checking respectively.
#
data_complex2
#=====================================
_vrf_PLAT213_2
;
PROBLEM:Atom O5 has ADP max/min Ratio 5.1 prolat
RESPONSE:The poorly disordered atoms of triflate is responsible for the O5
that has ADP max/min ratio 5.1 prolat.
;
_vrf_PLAT241_2
;
PROBLEM:High Ueq as Compared to Neighbors for O5 Check.
RESPONSE:The high U(eq) value of O5 compared to neighbors also can
be ascribed to the large thermal vibration of the disordered triflate.
;
_vrf_PLAT220_I
;
PROBLEM:Large Non-Solvent C Ueq(max)/Ueq(min) 8.1 Ratio.
RESPONSE:The large thermal vibration of the poorly disordered triflate
of S3-containing triflate may lead to the large Non-Solvent C
Ueq(max)/Ueq(min).
;
_vrf_PLAT220_II
;
PROBLEM: Large Non-Solvent O Ueq(max)/Ueq(min) 4.4 Ratio.
RESPONSE:The large thermal vibration of the poorly disordered triflate
of S3-containing triflate also lead to the large Non-Solvent O
Ueq(max)/Ueq(min).
;
_vrf_PLAT242_2
;
PROBLEM:Low Ueq as Compared to Neighbors for Ag2 Check.
RESPONSE: The disordered triflate with large thermal vibration surronds
the heavy Ag2 atom, thus which exhibits low Ueq compared with the triflate.
;
#
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety ?
_chemical_formula_sum 'C19 H12 Ag3 F9 N8 O9 S5'
_chemical_formula_weight 1151.28
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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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 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 22.2549(4)
_cell_length_b 9.4868(2)
_cell_length_c 15.7184(3)
_cell_angle_alpha 90.00
_cell_angle_beta 91.4760(10)
_cell_angle_gamma 90.00
_cell_volume 3317.49(11)
_cell_formula_units_Z 4
_cell_measurement_temperature 296(2)
_cell_measurement_reflns_used ?
_cell_measurement_theta_min ?
_cell_measurement_theta_max ?
_exptl_crystal_description Block
_exptl_crystal_colour colorless
_exptl_crystal_size_max 0.40
_exptl_crystal_size_mid 0.30
_exptl_crystal_size_min 0.20
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 2.305
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 2224
_exptl_absorpt_coefficient_mu 2.180
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.6320
_exptl_absorpt_correction_T_max 0.7456
_exptl_absorpt_process_details 'SADABS (Bruker, 2007)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 296(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 APEXII CCD area detector'
_diffrn_measurement_method \w-scans
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 11014
_diffrn_reflns_av_R_equivalents 0.0211
_diffrn_reflns_av_sigmaI/netI 0.0202
_diffrn_reflns_limit_h_min -25
_diffrn_reflns_limit_h_max 26
_diffrn_reflns_limit_k_min -10
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_theta_min 1.83
_diffrn_reflns_theta_max 25.01
_reflns_number_total 2870
_reflns_number_gt 2562
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'APEX2 (Bruker 2007)'
_computing_cell_refinement 'APEX2 and SAINT (Bruker 2007)'
_computing_data_reduction SAINT
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
;
SHELXTL and PLATON (Spek, 2009)
;
_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^)+(0.0511P)^2^+18.0272P] 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 0.00048(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns 2870
_refine_ls_number_parameters 264
_refine_ls_number_restraints 33
_refine_ls_R_factor_all 0.0396
_refine_ls_R_factor_gt 0.0356
_refine_ls_wR_factor_ref 0.0992
_refine_ls_wR_factor_gt 0.0964
_refine_ls_goodness_of_fit_ref 1.063
_refine_ls_restrained_S_all 1.167
_refine_ls_shift/su_max 0.003
_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 0.5000 0.42475(3) 0.2500 0.04211(7) Uani 1 2 d S . .
Ag2 Ag 0.329651(8) 0.18669(2) 0.608419(11) 0.04462(5) Uani 1 1 d . . .
S1 S 0.28822(2) 0.14533(7) 0.41815(3) 0.03548(15) Uani 1 1 d . . .
S2 S 0.64977(2) 0.38777(6) 0.39572(4) 0.03464(15) Uani 1 1 d . . .
S3 S 0.47820(6) 0.22785(17) 0.74559(9) 0.0556(4) Uani 0.50 1 d PDU . .
F1 F 0.59794(9) 0.2834(2) 0.52816(11) 0.0869(7) Uani 1 1 d . . .
F2 F 0.60332(11) 0.1403(2) 0.42305(16) 0.1095(8) Uani 1 1 d . . .
F3 F 0.68166(10) 0.1858(2) 0.50011(14) 0.0961(7) Uani 1 1 d . . .
F4 F 0.5000 -0.0400(4) 0.7500 0.225(3) Uani 1 2 d SDU . .
F5 F 0.5276(3) 0.0345(5) 0.6431(4) 0.210(3) Uani 0.50 1 d PDU . .
F6 F 0.5319(4) 0.1589(7) 0.7364(5) 0.270(3) Uani 0.50 1 d PDU . .
N1 N 0.38349(8) 0.2378(2) 0.49531(11) 0.0315(5) Uani 1 1 d . . .
N2 N 0.44131(8) 0.3456(2) 0.35557(11) 0.0361(5) Uani 1 1 d . . .
N3 N 0.21553(8) 0.16399(19) 0.28465(11) 0.0318(5) Uani 1 1 d . . .
N4 N 0.28255(8) -0.0088(2) 0.18023(11) 0.0349(5) Uani 1 1 d . . .
O1 O 0.59241(8) 0.4311(2) 0.36201(12) 0.0597(6) Uani 1 1 d . . .
O2 O 0.68889(8) 0.3288(2) 0.33487(11) 0.0518(5) Uani 1 1 d . . .
O3 O 0.67756(8) 0.48725(19) 0.45325(11) 0.0494(5) Uani 1 1 d . . .
O4 O 0.51472(18) 0.3105(4) 0.6855(2) 0.0656(12) Uani 0.50 1 d PD . .
O5 O 0.42506(14) 0.1519(7) 0.7061(3) 0.288(3) Uani 1 1 d D . .
C1 C 0.35895(9) 0.2270(2) 0.41622(12) 0.0262(5) Uani 1 1 d . . .
C2 C 0.38768(9) 0.2830(2) 0.34679(13) 0.0323(6) Uani 1 1 d . . .
H2A H 0.3693 0.2769 0.2931 0.039 Uiso 1 1 calc R . .
C3 C 0.46518(11) 0.3544(3) 0.43402(15) 0.0459(7) Uani 1 1 d . . .
H3A H 0.5023 0.3979 0.4421 0.055 Uiso 1 1 calc R . .
C4 C 0.43648(10) 0.3010(3) 0.50346(15) 0.0455(7) Uani 1 1 d . . .
H4A H 0.4546 0.3093 0.5572 0.055 Uiso 1 1 calc R . .
C5 C 0.26849(9) 0.1107(2) 0.31029(13) 0.0287(5) Uani 1 1 d . . .
C6 C 0.30153(10) 0.0232(2) 0.25929(13) 0.0333(6) Uani 1 1 d . . .
H6A H 0.3376 -0.0142 0.2802 0.040 Uiso 1 1 calc R . .
C7 C 0.23048(11) 0.0458(3) 0.15353(14) 0.0383(6) Uani 1 1 d . . .
H7A H 0.2165 0.0272 0.0984 0.046 Uiso 1 1 calc R . .
C8 C 0.19676(11) 0.1295(3) 0.20592(14) 0.0390(6) Uani 1 1 d . . .
H8A H 0.1598 0.1629 0.1858 0.047 Uiso 1 1 calc R . .
C9 C 0.63243(14) 0.2410(3) 0.4653(2) 0.0623(9) Uani 1 1 d . . .
C10 C 0.4926(4) 0.0638(6) 0.7017(5) 0.211(3) Uani 0.50 1 d PDU . .
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 0.03656(12) 0.05970(15) 0.03064(12) 0.000 0.01230(10) 0.000
Ag2 0.05113(10) 0.05636(11) 0.02704(8) 0.00826(8) 0.01429(8) 0.00252(9)
S1 0.0319(2) 0.0540(3) 0.0206(2) -0.0036(2) 0.0029(2) -0.0124(2)
S2 0.0312(2) 0.0436(3) 0.0291(3) -0.0005(2) -0.0005(2) -0.0041(2)
S3 0.0522(7) 0.0681(8) 0.0460(7) 0.0009(7) -0.0077(7) -0.0099(6)
F1 0.0957(12) 0.1086(14) 0.0581(10) 0.0227(10) 0.0340(9) -0.0037(12)
F2 0.1364(17) 0.0742(11) 0.1181(18) 0.0038(13) 0.0103(15) -0.0535(12)
F3 0.1018(14) 0.0902(12) 0.0961(14) 0.0475(11) -0.0010(12) 0.0233(11)
F4 0.229(5) 0.068(2) 0.374(7) 0.000 -0.076(5) 0.000
F5 0.276(8) 0.075(3) 0.281(7) -0.085(4) 0.061(6) 0.019(4)
F6 0.210(6) 0.218(6) 0.380(7) -0.033(6) -0.015(6) 0.000(5)
N1 0.0294(8) 0.0432(10) 0.0220(8) -0.0006(8) 0.0018(7) -0.0010(8)
N2 0.0300(8) 0.0522(11) 0.0263(9) -0.0019(9) 0.0068(7) -0.0062(9)
N3 0.0345(9) 0.0348(9) 0.0263(9) -0.0014(8) 0.0028(7) -0.0037(8)
N4 0.0436(10) 0.0347(9) 0.0265(9) -0.0032(8) 0.0029(8) -0.0044(8)
O1 0.0349(8) 0.0923(14) 0.0514(10) 0.0115(11) -0.0070(8) 0.0005(10)
O2 0.0534(10) 0.0579(11) 0.0446(10) -0.0037(9) 0.0132(8) 0.0011(9)
O3 0.0546(10) 0.0495(10) 0.0439(9) -0.0071(8) -0.0038(8) -0.0095(8)
O4 0.076(2) 0.082(2) 0.0366(17) 0.0368(17) -0.0254(17) -0.021(2)
O5 0.0891(15) 0.565(9) 0.205(3) 0.152(4) -0.1018(17) -0.131(3)
C1 0.0254(9) 0.0315(10) 0.0216(9) -0.0035(9) -0.0002(8) 0.0005(9)
C2 0.0320(10) 0.0451(12) 0.0198(9) -0.0031(10) -0.0003(8) -0.0023(10)
C3 0.0313(11) 0.0754(16) 0.0310(12) -0.0025(12) 0.0005(9) -0.0148(12)
C4 0.0342(11) 0.0781(17) 0.0241(11) -0.0061(12) -0.0042(9) -0.0125(12)
C5 0.0317(10) 0.0340(11) 0.0204(9) -0.0007(9) 0.0010(8) -0.0073(9)
C6 0.0319(10) 0.0379(11) 0.0303(11) -0.0028(10) 0.0011(9) 0.0008(10)
C7 0.0492(13) 0.0407(12) 0.0248(10) -0.0041(10) -0.0035(10) -0.0052(11)
C8 0.0398(12) 0.0482(13) 0.0286(11) 0.0006(11) -0.0070(10) 0.0000(11)
C9 0.0684(17) 0.0596(17) 0.0595(17) 0.0074(15) 0.0112(15) -0.0106(15)
C10 0.225(6) 0.040(4) 0.367(7) -0.039(5) -0.039(7) -0.006(5)
_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 N2 2.2661(18) 2_655 ?
Ag1 N2 2.2661(18) . ?
Ag2 N1 2.2229(17) . ?
Ag2 N4 2.2981(19) 6_556 ?
Ag2 N3 2.4352(18) 7_556 ?
S1 C1 1.755(2) . ?
S1 C5 1.771(2) . ?
S2 O2 1.4245(19) . ?
S2 O1 1.4299(18) . ?
S2 O3 1.4359(19) . ?
S2 C9 1.818(3) . ?
S3 F6 0.749(8) 2_656 ?
S3 S3 0.977(3) 2_656 ?
S3 O4 1.343(4) 2_656 ?
S3 F6 1.373(8) . ?
S3 O4 1.486(4) . ?
S3 O5 1.505(5) . ?
S3 C10 1.736(7) . ?
S3 C10 1.872(7) 2_656 ?
F1 C9 1.329(4) . ?
F2 C9 1.323(4) . ?
F3 C9 1.320(4) . ?
F4 C10 1.252(7) . ?
F4 C10 1.252(7) 2_656 ?
F5 C10 1.253(10) . ?
F6 S3 0.749(8) 2_656 ?
F6 O5 1.301(9) 2_656 ?
F6 C10 1.361(10) . ?
F6 C10 1.444(11) 2_656 ?
F6 F6 1.492(16) 2_656 ?
F6 O4 1.685(9) . ?
N1 C4 1.326(3) . ?
N1 C1 1.349(3) . ?
N2 C3 1.333(3) . ?
N2 C2 1.337(3) . ?
N3 C5 1.335(3) . ?
N3 C8 1.337(3) . ?
N3 Ag2 2.4352(18) 7_556 ?
N4 C7 1.327(3) . ?
N4 C6 1.337(3) . ?
N4 Ag2 2.2981(19) 6 ?
O4 S3 1.343(4) 2_656 ?
O5 F6 1.301(9) 2_656 ?
O5 C10 1.723(10) . ?
C1 C2 1.385(3) . ?
C2 H2A 0.9300 . ?
C3 C4 1.375(3) . ?
C3 H3A 0.9300 . ?
C4 H4A 0.9300 . ?
C5 C6 1.379(3) . ?
C6 H6A 0.9300 . ?
C7 C8 1.380(3) . ?
C7 H7A 0.9300 . ?
C8 H8A 0.9300 . ?
C10 F6 1.444(11) 2_656 ?
C10 C10 1.547(17) 2_656 ?
C10 S3 1.872(7) 2_656 ?
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
N2 Ag1 N2 141.29(10) 2_655 . ?
N1 Ag2 N4 144.60(7) . 6_556 ?
N1 Ag2 N3 131.74(7) . 7_556 ?
N4 Ag2 N3 83.48(6) 6_556 7_556 ?
C1 S1 C5 105.41(10) . . ?
O2 S2 O1 114.80(11) . . ?
O2 S2 O3 114.85(11) . . ?
O1 S2 O3 114.22(12) . . ?
O2 S2 C9 104.24(13) . . ?
O1 S2 C9 103.99(13) . . ?
O3 S2 C9 102.66(13) . . ?
F6 S3 S3 104.6(6) 2_656 2_656 ?
F6 S3 O4 103.6(7) 2_656 2_656 ?
S3 S3 O4 77.9(2) 2_656 2_656 ?
F6 S3 F6 83.9(9) 2_656 . ?
S3 S3 F6 31.9(3) 2_656 . ?
O4 S3 F6 106.2(4) 2_656 . ?
F6 S3 O4 151.0(7) 2_656 . ?
S3 S3 O4 62.1(2) 2_656 . ?
O4 S3 O4 98.6(3) 2_656 . ?
F6 S3 O4 72.1(4) . . ?
F6 S3 O5 59.8(7) 2_656 . ?
S3 S3 O5 145.7(3) 2_656 . ?
O4 S3 O5 133.4(3) 2_656 . ?
F6 S3 O5 113.9(4) . . ?
O4 S3 O5 115.3(2) . . ?
F6 S3 C10 55.0(7) 2_656 . ?
S3 S3 C10 82.2(3) 2_656 . ?
O4 S3 C10 145.6(3) 2_656 . ?
F6 S3 C10 50.3(4) . . ?
O4 S3 C10 96.4(3) . . ?
O5 S3 C10 63.8(4) . . ?
F6 S3 C10 37.9(7) 2_656 2_656 ?
S3 S3 C10 66.7(3) 2_656 2_656 ?
O4 S3 C10 95.5(3) 2_656 2_656 ?
F6 S3 C10 50.0(4) . 2_656 ?
O4 S3 C10 122.1(3) . 2_656 ?
O5 S3 C10 92.6(4) . 2_656 ?
C10 S3 C10 50.6(5) . 2_656 ?
C10 F4 C10 76.3(7) . 2_656 ?
S3 F6 O5 90.3(8) 2_656 2_656 ?
S3 F6 C10 122.3(9) 2_656 . ?
O5 F6 C10 134.3(7) 2_656 . ?
S3 F6 S3 43.5(5) 2_656 . ?
O5 F6 S3 125.4(7) 2_656 . ?
C10 F6 S3 78.8(5) . . ?
S3 F6 C10 99.8(8) 2_656 2_656 ?
O5 F6 C10 77.6(6) 2_656 2_656 ?
C10 F6 C10 66.9(7) . 2_656 ?
S3 F6 C10 83.3(6) . 2_656 ?
S3 F6 F6 66.2(6) 2_656 2_656 ?
O5 F6 F6 119.4(9) 2_656 2_656 ?
C10 F6 F6 60.6(6) . 2_656 ?
S3 F6 F6 30.0(3) . 2_656 ?
C10 F6 F6 55.2(6) 2_656 2_656 ?
S3 F6 O4 50.8(5) 2_656 . ?
O5 F6 O4 121.8(6) 2_656 . ?
C10 F6 O4 103.8(6) . . ?
S3 F6 O4 57.0(3) . . ?
C10 F6 O4 140.2(7) 2_656 . ?
F6 F6 O4 86.0(4) 2_656 . ?
C4 N1 C1 117.48(18) . . ?
C4 N1 Ag2 121.18(14) . . ?
C1 N1 Ag2 120.45(13) . . ?
C3 N2 C2 117.18(19) . . ?
C3 N2 Ag1 115.67(15) . . ?
C2 N2 Ag1 126.97(14) . . ?
C5 N3 C8 116.04(19) . . ?
C5 N3 Ag2 112.89(13) . 7_556 ?
C8 N3 Ag2 131.06(15) . 7_556 ?
C7 N4 C6 117.23(19) . . ?
C7 N4 Ag2 122.46(15) . 6 ?
C6 N4 Ag2 119.08(15) . 6 ?
S3 O4 S3 40.00(14) 2_656 . ?
S3 O4 F6 25.6(3) 2_656 . ?
S3 O4 F6 50.8(3) . . ?
F6 O5 S3 29.9(3) 2_656 . ?
F6 O5 C10 54.9(5) 2_656 . ?
S3 O5 C10 64.7(3) . . ?
N1 C1 C2 120.87(18) . . ?
N1 C1 S1 111.08(14) . . ?
C2 C1 S1 127.97(16) . . ?
N2 C2 C1 121.19(19) . . ?
N2 C2 H2A 119.4 . . ?
C1 C2 H2A 119.4 . . ?
N2 C3 C4 121.9(2) . . ?
N2 C3 H3A 119.0 . . ?
C4 C3 H3A 119.0 . . ?
N1 C4 C3 121.3(2) . . ?
N1 C4 H4A 119.3 . . ?
C3 C4 H4A 119.3 . . ?
N3 C5 C6 122.15(19) . . ?
N3 C5 S1 114.44(15) . . ?
C6 C5 S1 123.04(16) . . ?
N4 C6 C5 121.1(2) . . ?
N4 C6 H6A 119.5 . . ?
C5 C6 H6A 119.5 . . ?
N4 C7 C8 121.3(2) . . ?
N4 C7 H7A 119.3 . . ?
C8 C7 H7A 119.3 . . ?
N3 C8 C7 122.1(2) . . ?
N3 C8 H8A 118.9 . . ?
C7 C8 H8A 118.9 . . ?
F3 C9 F2 108.2(3) . . ?
F3 C9 F1 107.5(3) . . ?
F2 C9 F1 107.9(3) . . ?
F3 C9 S2 111.5(2) . . ?
F2 C9 S2 111.1(2) . . ?
F1 C9 S2 110.6(2) . . ?
F4 C10 F5 101.3(6) . . ?
F4 C10 F6 101.8(7) . . ?
F5 C10 F6 92.1(7) . . ?
F4 C10 F6 97.4(6) . 2_656 ?
F5 C10 F6 152.4(7) . 2_656 ?
F6 C10 F6 64.2(7) . 2_656 ?
F4 C10 C10 51.8(4) . 2_656 ?
F5 C10 C10 126.9(11) . 2_656 ?
F6 C10 C10 59.1(6) . 2_656 ?
F6 C10 C10 54.0(5) 2_656 2_656 ?
F4 C10 O5 117.3(7) . . ?
F5 C10 O5 134.2(7) . . ?
F6 C10 O5 102.4(5) . . ?
F6 C10 O5 47.5(4) 2_656 . ?
C10 C10 O5 97.1(7) 2_656 . ?
F4 C10 S3 119.1(6) . . ?
F5 C10 S3 128.0(6) . . ?
F6 C10 S3 50.9(4) . . ?
F6 C10 S3 25.2(3) 2_656 . ?
C10 C10 S3 69.3(3) 2_656 . ?
O5 C10 S3 51.6(3) . . ?
F4 C10 S3 110.3(6) . 2_656 ?
F5 C10 S3 107.1(6) . 2_656 ?
F6 C10 S3 19.8(4) . 2_656 ?
F6 C10 S3 46.7(4) 2_656 2_656 ?
C10 C10 S3 60.1(3) 2_656 2_656 ?
O5 C10 S3 82.6(3) . 2_656 ?
S3 C10 S3 31.11(14) . 2_656 ?
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
F6 S3 F6 S3 -130.8(13) 2_656 . . 2_656 ?
O4 S3 F6 S3 -28.4(7) 2_656 . . 2_656 ?
O4 S3 F6 S3 65.7(6) . . . 2_656 ?
O5 S3 F6 S3 176.1(5) . . . 2_656 ?
C10 S3 F6 S3 -179.5(10) . . . 2_656 ?
C10 S3 F6 S3 -111.9(9) 2_656 . . 2_656 ?
F6 S3 F6 O5 -88.5(12) 2_656 . . 2_656 ?
S3 S3 F6 O5 42.4(6) 2_656 . . 2_656 ?
O4 S3 F6 O5 14.0(8) 2_656 . . 2_656 ?
O4 S3 F6 O5 108.1(8) . . . 2_656 ?
O5 S3 F6 O5 -141.6(7) . . . 2_656 ?
C10 S3 F6 O5 -137.2(10) . . . 2_656 ?
C10 S3 F6 O5 -69.5(8) 2_656 . . 2_656 ?
F6 S3 F6 C10 48.7(6) 2_656 . . . ?
S3 S3 F6 C10 179.5(10) 2_656 . . . ?
O4 S3 F6 C10 151.2(5) 2_656 . . . ?
O4 S3 F6 C10 -114.8(5) . . . . ?
O5 S3 F6 C10 -4.4(6) . . . . ?
C10 S3 F6 C10 67.7(7) 2_656 . . . ?
F6 S3 F6 C10 -18.9(6) 2_656 . . 2_656 ?
S3 S3 F6 C10 111.9(9) 2_656 . . 2_656 ?
O4 S3 F6 C10 83.5(5) 2_656 . . 2_656 ?
O4 S3 F6 C10 177.6(5) . . . 2_656 ?
O5 S3 F6 C10 -72.0(6) . . . 2_656 ?
C10 S3 F6 C10 -67.7(7) . . . 2_656 ?
S3 S3 F6 F6 130.8(13) 2_656 . . 2_656 ?
O4 S3 F6 F6 102.5(7) 2_656 . . 2_656 ?
O4 S3 F6 F6 -163.5(8) . . . 2_656 ?
O5 S3 F6 F6 -53.1(9) . . . 2_656 ?
C10 S3 F6 F6 -48.7(6) . . . 2_656 ?
C10 S3 F6 F6 18.9(6) 2_656 . . 2_656 ?
F6 S3 F6 O4 163.5(8) 2_656 . . . ?
S3 S3 F6 O4 -65.7(6) 2_656 . . . ?
O4 S3 F6 O4 -94.1(4) 2_656 . . . ?
O5 S3 F6 O4 110.4(3) . . . . ?
C10 S3 F6 O4 114.8(5) . . . . ?
C10 S3 F6 O4 -177.6(5) 2_656 . . . ?
N4 Ag2 N1 C4 -124.13(19) 6_556 . . . ?
N3 Ag2 N1 C4 62.8(2) 7_556 . . . ?
N4 Ag2 N1 C1 67.0(2) 6_556 . . . ?
N3 Ag2 N1 C1 -106.11(17) 7_556 . . . ?
N2 Ag1 N2 C3 104.03(19) 2_655 . . . ?
N2 Ag1 N2 C2 -71.04(19) 2_655 . . . ?
F6 S3 O4 S3 -68.6(14) 2_656 . . 2_656 ?
O4 S3 O4 S3 71.3(3) 2_656 . . 2_656 ?
F6 S3 O4 S3 -33.0(4) . . . 2_656 ?
O5 S3 O4 S3 -141.6(3) . . . 2_656 ?
C10 S3 O4 S3 -77.6(3) . . . 2_656 ?
C10 S3 O4 S3 -30.8(3) 2_656 . . 2_656 ?
F6 S3 O4 F6 -35.6(16) 2_656 . . . ?
S3 S3 O4 F6 33.0(4) 2_656 . . . ?
O4 S3 O4 F6 104.3(4) 2_656 . . . ?
O5 S3 O4 F6 -108.6(5) . . . . ?
C10 S3 O4 F6 -44.7(4) . . . . ?
C10 S3 O4 F6 2.2(5) 2_656 . . . ?
O5 F6 O4 S3 -60.1(7) 2_656 . . 2_656 ?
C10 F6 O4 S3 120.6(10) . . . 2_656 ?
S3 F6 O4 S3 54.1(5) . . . 2_656 ?
C10 F6 O4 S3 50.3(9) 2_656 . . 2_656 ?
F6 F6 O4 S3 62.3(7) 2_656 . . 2_656 ?
S3 F6 O4 S3 -54.1(5) 2_656 . . . ?
O5 F6 O4 S3 -114.2(8) 2_656 . . . ?
C10 F6 O4 S3 66.6(6) . . . . ?
C10 F6 O4 S3 -3.8(8) 2_656 . . . ?
F6 F6 O4 S3 8.2(4) 2_656 . . . ?
S3 S3 O5 F6 70.5(8) 2_656 . . 2_656 ?
O4 S3 O5 F6 -80.0(8) 2_656 . . 2_656 ?
F6 S3 O5 F6 66.9(11) . . . 2_656 ?
O4 S3 O5 F6 147.6(8) . . . 2_656 ?
C10 S3 O5 F6 63.1(8) . . . 2_656 ?
C10 S3 O5 F6 20.0(8) 2_656 . . 2_656 ?
F6 S3 O5 C10 -63.1(8) 2_656 . . . ?
S3 S3 O5 C10 7.4(6) 2_656 . . . ?
O4 S3 O5 C10 -143.1(4) 2_656 . . . ?
F6 S3 O5 C10 3.8(5) . . . . ?
O4 S3 O5 C10 84.5(4) . . . . ?
C10 S3 O5 C10 -43.1(6) 2_656 . . . ?
C4 N1 C1 C2 -1.5(3) . . . . ?
Ag2 N1 C1 C2 167.80(16) . . . . ?
C4 N1 C1 S1 -178.32(18) . . . . ?
Ag2 N1 C1 S1 -9.0(2) . . . . ?
C5 S1 C1 N1 -169.81(15) . . . . ?
C5 S1 C1 C2 13.6(2) . . . . ?
C3 N2 C2 C1 -1.4(3) . . . . ?
Ag1 N2 C2 C1 173.60(16) . . . . ?
N1 C1 C2 N2 2.0(3) . . . . ?
S1 C1 C2 N2 178.27(17) . . . . ?
C2 N2 C3 C4 0.4(4) . . . . ?
Ag1 N2 C3 C4 -175.2(2) . . . . ?
C1 N1 C4 C3 0.5(4) . . . . ?
Ag2 N1 C4 C3 -168.7(2) . . . . ?
N2 C3 C4 N1 0.1(4) . . . . ?
C8 N3 C5 C6 -1.1(3) . . . . ?
Ag2 N3 C5 C6 179.91(17) 7_556 . . . ?
C8 N3 C5 S1 -174.32(17) . . . . ?
Ag2 N3 C5 S1 6.67(19) 7_556 . . . ?
C1 S1 C5 N3 -124.95(16) . . . . ?
C1 S1 C5 C6 61.9(2) . . . . ?
C7 N4 C6 C5 -0.8(3) . . . . ?
Ag2 N4 C6 C5 -168.38(16) 6 . . . ?
N3 C5 C6 N4 2.1(3) . . . . ?
S1 C5 C6 N4 174.74(17) . . . . ?
C6 N4 C7 C8 -1.4(3) . . . . ?
Ag2 N4 C7 C8 165.78(18) 6 . . . ?
C5 N3 C8 C7 -1.1(3) . . . . ?
Ag2 N3 C8 C7 177.69(17) 7_556 . . . ?
N4 C7 C8 N3 2.4(4) . . . . ?
O2 S2 C9 F3 57.7(2) . . . . ?
O1 S2 C9 F3 178.3(2) . . . . ?
O3 S2 C9 F3 -62.4(2) . . . . ?
O2 S2 C9 F2 -63.1(2) . . . . ?
O1 S2 C9 F2 57.5(3) . . . . ?
O3 S2 C9 F2 176.8(2) . . . . ?
O2 S2 C9 F1 177.2(2) . . . . ?
O1 S2 C9 F1 -62.2(2) . . . . ?
O3 S2 C9 F1 57.1(2) . . . . ?
C10 F4 C10 F5 128.5(10) 2_656 . . . ?
C10 F4 C10 F6 33.8(4) 2_656 . . . ?
C10 F4 C10 F6 -31.2(4) 2_656 . . 2_656 ?
C10 F4 C10 O5 -76.9(6) 2_656 . . . ?
C10 F4 C10 S3 -17.72(16) 2_656 . . . ?
C10 F4 C10 S3 15.24(15) 2_656 . . 2_656 ?
S3 F6 C10 F4 -117.7(10) 2_656 . . . ?
O5 F6 C10 F4 11.1(13) 2_656 . . . ?
S3 F6 C10 F4 -118.1(6) . . . . ?
C10 F6 C10 F4 -30.7(4) 2_656 . . . ?
F6 F6 C10 F4 -92.6(7) 2_656 . . . ?
O4 F6 C10 F4 -169.8(5) . . . . ?
S3 F6 C10 F5 140.2(11) 2_656 . . . ?
O5 F6 C10 F5 -91.0(11) 2_656 . . . ?
S3 F6 C10 F5 139.8(6) . . . . ?
C10 F6 C10 F5 -132.7(8) 2_656 . . . ?
F6 F6 C10 F5 165.4(7) 2_656 . . . ?
O4 F6 C10 F5 88.2(6) . . . . ?
S3 F6 C10 F6 -25.1(8) 2_656 . . 2_656 ?
O5 F6 C10 F6 103.7(12) 2_656 . . 2_656 ?
S3 F6 C10 F6 -25.5(3) . . . 2_656 ?
C10 F6 C10 F6 61.9(7) 2_656 . . 2_656 ?
O4 F6 C10 F6 -77.2(5) . . . 2_656 ?
S3 F6 C10 C10 -87.0(11) 2_656 . . 2_656 ?
O5 F6 C10 C10 41.8(11) 2_656 . . 2_656 ?
S3 F6 C10 C10 -87.4(6) . . . 2_656 ?
F6 F6 C10 C10 -61.9(7) 2_656 . . 2_656 ?
O4 F6 C10 C10 -139.1(7) . . . 2_656 ?
S3 F6 C10 O5 4.0(12) 2_656 . . . ?
O5 F6 C10 O5 132.8(9) 2_656 . . . ?
S3 F6 C10 O5 3.6(5) . . . . ?
C10 F6 C10 O5 91.0(7) 2_656 . . . ?
F6 F6 C10 O5 29.1(6) 2_656 . . . ?
O4 F6 C10 O5 -48.1(7) . . . . ?
S3 F6 C10 S3 0.4(8) 2_656 . . . ?
O5 F6 C10 S3 129.2(12) 2_656 . . . ?
C10 F6 C10 S3 87.4(6) 2_656 . . . ?
F6 F6 C10 S3 25.5(3) 2_656 . . . ?
O4 F6 C10 S3 -51.7(4) . . . . ?
O5 F6 C10 S3 128.8(18) 2_656 . . 2_656 ?
S3 F6 C10 S3 -0.4(8) . . . 2_656 ?
C10 F6 C10 S3 87.0(11) 2_656 . . 2_656 ?
F6 F6 C10 S3 25.1(8) 2_656 . . 2_656 ?
O4 F6 C10 S3 -52.1(8) . . . 2_656 ?
F6 O5 C10 F4 74.0(8) 2_656 . . . ?
S3 O5 C10 F4 106.8(6) . . . . ?
F6 O5 C10 F5 -141.8(10) 2_656 . . . ?
S3 O5 C10 F5 -109.0(8) . . . . ?
F6 O5 C10 F6 -36.4(7) 2_656 . . . ?
S3 O5 C10 F6 -3.5(5) . . . . ?
S3 O5 C10 F6 32.9(4) . . . 2_656 ?
F6 O5 C10 C10 23.5(6) 2_656 . . 2_656 ?
S3 O5 C10 C10 56.3(4) . . . 2_656 ?
F6 O5 C10 S3 -32.9(4) 2_656 . . . ?
F6 O5 C10 S3 -35.1(5) 2_656 . . 2_656 ?
S3 O5 C10 S3 -2.20(17) . . . 2_656 ?
F6 S3 C10 F4 -33.0(9) 2_656 . . . ?
S3 S3 C10 F4 81.0(7) 2_656 . . . ?
O4 S3 C10 F4 26.2(12) 2_656 . . . ?
F6 S3 C10 F4 81.3(8) . . . . ?
O4 S3 C10 F4 141.7(7) . . . . ?
O5 S3 C10 F4 -103.2(8) . . . . ?
C10 S3 C10 F4 14.83(18) 2_656 . . . ?
F6 S3 C10 F5 -169.2(14) 2_656 . . . ?
S3 S3 C10 F5 -55.1(9) 2_656 . . . ?
O4 S3 C10 F5 -110.0(9) 2_656 . . . ?
F6 S3 C10 F5 -54.9(9) . . . . ?
O4 S3 C10 F5 5.5(9) . . . . ?
O5 S3 C10 F5 120.7(10) . . . . ?
C10 S3 C10 F5 -121.3(13) 2_656 . . . ?
F6 S3 C10 F6 -114.3(8) 2_656 . . . ?
S3 S3 C10 F6 -0.2(5) 2_656 . . . ?
O4 S3 C10 F6 -55.1(8) 2_656 . . . ?
O4 S3 C10 F6 60.4(5) . . . . ?
O5 S3 C10 F6 175.5(6) . . . . ?
C10 S3 C10 F6 -66.4(8) 2_656 . . . ?
S3 S3 C10 F6 114.0(8) 2_656 . . 2_656 ?
O4 S3 C10 F6 59.2(11) 2_656 . . 2_656 ?
F6 S3 C10 F6 114.3(8) . . . 2_656 ?
O4 S3 C10 F6 174.7(8) . . . 2_656 ?
O5 S3 C10 F6 -70.2(8) . . . 2_656 ?
C10 S3 C10 F6 47.8(9) 2_656 . . 2_656 ?
F6 S3 C10 C10 -47.8(9) 2_656 . . 2_656 ?
S3 S3 C10 C10 66.2(6) 2_656 . . 2_656 ?
O4 S3 C10 C10 11.4(11) 2_656 . . 2_656 ?
F6 S3 C10 C10 66.4(8) . . . 2_656 ?
O4 S3 C10 C10 126.9(6) . . . 2_656 ?
O5 S3 C10 C10 -118.0(7) . . . 2_656 ?
F6 S3 C10 O5 70.2(8) 2_656 . . . ?
S3 S3 C10 O5 -175.8(3) 2_656 . . . ?
O4 S3 C10 O5 129.4(6) 2_656 . . . ?
F6 S3 C10 O5 -175.5(6) . . . . ?
O4 S3 C10 O5 -115.1(3) . . . . ?
C10 S3 C10 O5 118.0(7) 2_656 . . . ?
F6 S3 C10 S3 -114.0(8) 2_656 . . 2_656 ?
O4 S3 C10 S3 -54.8(6) 2_656 . . 2_656 ?
F6 S3 C10 S3 0.2(5) . . . 2_656 ?
O4 S3 C10 S3 60.7(2) . . . 2_656 ?
O5 S3 C10 S3 175.8(3) . . . 2_656 ?
C10 S3 C10 S3 -66.2(6) 2_656 . . 2_656 ?
_diffrn_measured_fraction_theta_max 0.977
_diffrn_reflns_theta_full 25.01
_diffrn_measured_fraction_theta_full 0.977
_refine_diff_density_max 0.997
_refine_diff_density_min -0.923
_refine_diff_density_rms 0.104
##########################End############################
_database_code_depnum_ccdc_archive 'CCDC 926719'
#######################################################################
#
# Cambridge Crystallographic Data Centre
# CCDC
#
#######################################################################
#
# This CIF contains data from an original supplementary publication
# deposited with the CCDC, and may include chemical, crystal,
# experimental, refinement, atomic coordinates,
# anisotropic displacement parameters and molecular geometry data,
# as required by the journal to which it was submitted.
#
# This CIF is provided on the understanding that it is used for bona
# fide research purposes only. It may contain copyright material
# of the CCDC or of third parties, and may not be copied or further
# disseminated in any form, whether machine-readable or not,
# except for the purpose of generating routine backup copies
# on your local computer system.
#
# For further information on the CCDC, data deposition and
# data retrieval see:
# www.ccdc.cam.ac.uk
#
# Bona fide researchers may freely download Mercury and enCIFer
# from this site to visualise CIF-encoded structures and
# to carry out CIF format checking respectively.
#
data_3
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety ?
_chemical_formula_sum 'C19 H16 Ag3 F9 N8 O12 S5'
_chemical_formula_weight 1203.31
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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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 Triclinic
_symmetry_space_group_name_H-M P-1
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 11.135(5)
_cell_length_b 12.380(6)
_cell_length_c 14.607(7)
_cell_angle_alpha 84.662(12)
_cell_angle_beta 89.537(11)
_cell_angle_gamma 67.261(10)
_cell_volume 1848.3(15)
_cell_formula_units_Z 2
_cell_measurement_temperature 293(2)
_cell_measurement_reflns_used ?
_cell_measurement_theta_min ?
_cell_measurement_theta_max ?
_exptl_crystal_description Block
_exptl_crystal_colour colorless
_exptl_crystal_size_max 0.4
_exptl_crystal_size_mid 0.3
_exptl_crystal_size_min 0.2
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 2.162
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1168
_exptl_absorpt_coefficient_mu 1.967
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.835
_exptl_absorpt_correction_T_max 0.905
_exptl_absorpt_process_details 'SADABS (Bruker, 2007)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 293(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 APEXII CCD area detector'
_diffrn_measurement_method ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 12948
_diffrn_reflns_av_R_equivalents 0.0376
_diffrn_reflns_av_sigmaI/netI 0.0866
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_limit_l_max 17
_diffrn_reflns_theta_min 1.79
_diffrn_reflns_theta_max 28.39
_reflns_number_total 9003
_reflns_number_gt 5120
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'APEX2 (Bruker 2007)'
_computing_cell_refinement 'APEX2 and SAINT (Bruker 2007)'
_computing_data_reduction SAINT
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
;
SHELXTL and PLATON (Spek, 2009)
;
_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^)+(0.0673P)^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 Contr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 9003
_refine_ls_number_parameters 532
_refine_ls_number_restraints 98
_refine_ls_R_factor_all 0.1144
_refine_ls_R_factor_gt 0.0588
_refine_ls_wR_factor_ref 0.1583
_refine_ls_wR_factor_gt 0.1317
_refine_ls_goodness_of_fit_ref 1.019
_refine_ls_restrained_S_all 1.020
_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 1.27092(6) 0.51881(5) 0.73996(4) 0.05698(19) Uani 1 1 d . . .
Ag2 Ag 0.82223(5) 0.90341(5) 0.91585(4) 0.04881(17) Uani 1 1 d . . .
Ag3 Ag 0.24109(6) 1.09228(5) 0.59621(4) 0.04874(17) Uani 1 1 d . . .
N1 N 1.0960(5) 0.6276(4) 0.6337(4) 0.0401(13) Uani 1 1 d . . .
N2 N 0.8955(5) 0.7760(5) 0.5133(4) 0.0417(13) Uani 1 1 d . . .
N3 N 1.1044(5) 1.0334(4) 0.7003(4) 0.0406(13) Uani 1 1 d . . .
N4 N 0.9600(5) 0.9615(4) 0.8291(4) 0.0371(12) Uani 1 1 d . . .
S1 S 1.01157(17) 0.75436(13) 0.77545(11) 0.0393(4) Uani 1 1 d . . .
C1 C 1.0834(7) 0.6032(6) 0.5486(5) 0.0490(18) Uani 1 1 d . . .
H1A H 1.1439 0.5342 0.5289 0.059 Uiso 1 1 calc R . .
C2 C 0.9850(7) 0.6755(6) 0.4884(5) 0.0482(17) Uani 1 1 d . . .
H2A H 0.9805 0.6543 0.4295 0.058 Uiso 1 1 calc R . .
C3 C 0.9043(6) 0.7990(5) 0.5984(4) 0.0385(15) Uani 1 1 d . . .
H3A H 0.8414 0.8664 0.6186 0.046 Uiso 1 1 calc R . .
C4 C 1.0027(6) 0.7274(4) 0.6582(4) 0.0309(13) Uani 1 1 d . . .
C5 C 1.0237(6) 0.8937(5) 0.7646(4) 0.0314(13) Uani 1 1 d . . .
C6 C 1.0964(6) 0.9280(5) 0.7016(4) 0.0380(15) Uani 1 1 d . . .
H6A H 1.1414 0.8772 0.6587 0.046 Uiso 1 1 calc R . .
C7 C 1.0416(7) 1.1009(5) 0.7655(5) 0.0441(16) Uani 1 1 d . . .
H7A H 1.0461 1.1741 0.7673 0.053 Uiso 1 1 calc R . .
C8 C 0.9706(7) 1.0657(5) 0.8300(5) 0.0454(17) Uani 1 1 d . . .
H8A H 0.9293 1.1147 0.8750 0.055 Uiso 1 1 calc R . .
N5 N 0.6342(5) 0.9510(5) 0.8165(4) 0.0477(14) Uani 1 1 d . . .
N6 N 0.4227(5) 1.0227(5) 0.6930(4) 0.0378(12) Uani 1 1 d . . .
N7 N 0.2472(5) 1.3900(4) 0.8511(4) 0.0386(13) Uani 1 1 d . . .
N8 N 0.1976(5) 1.2311(5) 0.9780(4) 0.0415(13) Uani 1 1 d . . .
S2 S 0.33227(18) 1.24516(14) 0.72383(12) 0.0475(5) Uani 1 1 d . . .
C9 C 0.6127(7) 0.8760(6) 0.7656(5) 0.0485(18) Uani 1 1 d . . .
H9A H 0.6702 0.7975 0.7721 0.058 Uiso 1 1 calc R . .
C10 C 0.5087(7) 0.9098(6) 0.7034(5) 0.0485(18) Uani 1 1 d . . .
H10A H 0.4980 0.8546 0.6688 0.058 Uiso 1 1 calc R . .
C11 C 0.4425(6) 1.0963(5) 0.7450(4) 0.0376(15) Uani 1 1 d . . .
C12 C 0.5470(7) 1.0626(6) 0.8056(5) 0.0489(18) Uani 1 1 d . . .
H12A H 0.5576 1.1182 0.8398 0.059 Uiso 1 1 calc R . .
C13 C 0.2498(6) 1.2002(5) 0.8965(4) 0.0414(16) Uani 1 1 d . . .
H13A H 0.2695 1.1238 0.8819 0.050 Uiso 1 1 calc R . .
C14 C 0.2747(6) 1.2787(5) 0.8343(4) 0.0348(14) Uani 1 1 d . . .
C15 C 0.1935(7) 1.4212(6) 0.9319(5) 0.0495(18) Uani 1 1 d . . .
H15A H 0.1709 1.4983 0.9456 0.059 Uiso 1 1 calc R . .
C16 C 0.1713(7) 1.3431(6) 0.9940(5) 0.0524(19) Uani 1 1 d . . .
H16A H 0.1365 1.3680 1.0501 0.063 Uiso 1 1 calc R . .
S3 S 0.10055(19) 0.51319(15) 0.25467(14) 0.0495(5) Uani 1 1 d . . .
O3 O -0.0104(5) 0.6157(5) 0.2709(4) 0.0716(16) Uani 1 1 d . . .
O2 O 0.0748(7) 0.4368(5) 0.1979(5) 0.092(2) Uani 1 1 d . . .
O1 O 0.1755(7) 0.4580(7) 0.3374(5) 0.112(3) Uani 1 1 d . . .
F13 F 0.3064(7) 0.4818(6) 0.1612(6) 0.137(3) Uani 1 1 d . . .
F12 F 0.1386(8) 0.6247(7) 0.1095(5) 0.132(3) Uani 1 1 d . . .
F11 F 0.2392(7) 0.6392(7) 0.2263(5) 0.135(3) Uani 1 1 d . . .
C17 C 0.2045(10) 0.5664(8) 0.1858(6) 0.068(2) Uani 1 1 d . . .
S4 S 0.36512(19) 0.85953(16) 0.46357(16) 0.0575(5) Uani 1 1 d . . .
O4 O 0.3412(8) 0.9703(6) 0.4196(9) 0.176(5) Uani 1 1 d . . .
O5 O 0.3310(7) 0.8597(9) 0.5570(5) 0.142(4) Uani 1 1 d . . .
O6 O 0.4906(5) 0.7746(4) 0.4468(4) 0.0704(17) Uani 1 1 d . . .
C18 C 0.2499(14) 0.8104(14) 0.4193(11) 0.117(4) Uani 1 1 d U . .
F21 F 0.1305(7) 0.8743(8) 0.4378(7) 0.173(4) Uani 1 1 d U . .
F22 F 0.2711(9) 0.7066(7) 0.4351(9) 0.197(5) Uani 1 1 d U . .
F23 F 0.2703(14) 0.8266(14) 0.3231(7) 0.252(7) Uani 1 1 d U . .
S5 S 0.6560(7) 1.1431(5) 1.0478(4) 0.0629(18) Uani 0.50 1 d PD . .
S5' S 0.7116(5) 1.1561(5) 1.0489(4) 0.0505(14) Uani 0.50 1 d PD . .
O7 O 0.6838(8) 1.1460(6) 1.1428(4) 0.103(2) Uani 1 1 d DU . .
O8 O 0.7694(16) 1.0981(18) 0.9928(16) 0.107(7) Uani 0.50 1 d PDU . .
O8' O 0.8198(17) 1.182(2) 1.0262(14) 0.156(8) Uani 0.50 1 d PU . .
O9' O 0.703(3) 1.0683(16) 0.9992(15) 0.141(9) Uani 0.50 1 d PU . .
O9 O 0.5373(14) 1.1308(19) 1.0226(11) 0.151(9) Uani 0.50 1 d PDU . .
C19 C 0.5908(9) 1.2863(6) 1.0016(5) 0.111(4) Uani 1 1 d DU . .
F32 F 0.4774(8) 1.3213(13) 1.0383(9) 0.269(8) Uani 1 1 d DU . .
F31 F 0.6318(16) 1.3636(8) 1.0276(7) 0.258(8) Uani 1 1 d DU . .
F33 F 0.5786(9) 1.3051(7) 0.9125(5) 0.146(3) Uani 1 1 d DU . .
O1W O 1.3555(7) 0.6657(6) 0.7427(5) 0.095(2) Uani 1 1 d . . .
H1C H 1.4421 0.6491 0.7190 0.142 Uiso 1 1 d R . .
H1B H 1.3862 0.6690 0.8046 0.142 Uiso 1 1 d R . .
H2WB H 1.4656 0.5226 0.5989 0.142 Uiso 1 1 d R . .
H2WC H 1.5219 0.3968 0.6400 0.142 Uiso 1 1 d R . .
O2W O 1.4126(7) 0.4675(5) 0.6106(5) 0.092(2) Uani 1 1 d . . .
O3W O 1.5619(7) 0.6146(7) 0.6156(6) 0.110(2) 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 0.0676(4) 0.0396(3) 0.0527(4) 0.0054(3) 0.0072(3) -0.0109(3)
Ag2 0.0510(3) 0.0527(3) 0.0410(3) -0.0017(2) 0.0131(2) -0.0191(3)
Ag3 0.0538(3) 0.0503(3) 0.0423(3) 0.0005(2) -0.0054(2) -0.0215(3)
N1 0.042(3) 0.036(3) 0.037(3) -0.007(2) 0.002(2) -0.008(2)
N2 0.043(3) 0.042(3) 0.037(3) -0.006(3) 0.000(3) -0.014(3)
N3 0.043(3) 0.037(3) 0.045(3) -0.007(2) 0.009(3) -0.019(2)
N4 0.042(3) 0.038(3) 0.038(3) -0.014(2) 0.013(2) -0.020(2)
S1 0.0601(11) 0.0292(7) 0.0305(8) -0.0060(6) 0.0084(8) -0.0189(7)
C1 0.056(4) 0.035(3) 0.048(4) -0.019(3) 0.012(4) -0.006(3)
C2 0.063(5) 0.048(4) 0.035(4) -0.009(3) -0.003(3) -0.021(4)
C3 0.041(4) 0.031(3) 0.038(4) -0.009(3) 0.005(3) -0.007(3)
C4 0.044(4) 0.019(2) 0.033(3) -0.009(2) 0.006(3) -0.014(3)
C5 0.038(3) 0.026(3) 0.029(3) -0.004(2) -0.001(3) -0.011(3)
C6 0.042(4) 0.035(3) 0.036(4) -0.006(3) 0.011(3) -0.013(3)
C7 0.051(4) 0.033(3) 0.051(4) -0.006(3) 0.003(3) -0.020(3)
C8 0.055(4) 0.038(3) 0.052(4) -0.022(3) 0.017(4) -0.025(3)
N5 0.040(3) 0.044(3) 0.048(4) -0.004(3) -0.004(3) -0.005(3)
N6 0.038(3) 0.045(3) 0.036(3) -0.009(2) 0.004(2) -0.021(3)
N7 0.043(3) 0.031(3) 0.034(3) 0.000(2) 0.003(2) -0.007(2)
N8 0.051(3) 0.041(3) 0.031(3) -0.004(2) 0.005(3) -0.015(3)
S2 0.0613(11) 0.0375(8) 0.0291(9) -0.0037(7) 0.0089(8) -0.0033(8)
C9 0.051(4) 0.035(3) 0.052(5) -0.005(3) 0.003(4) -0.008(3)
C10 0.054(4) 0.036(3) 0.056(5) -0.011(3) 0.000(4) -0.015(3)
C11 0.035(3) 0.041(3) 0.034(4) -0.007(3) 0.006(3) -0.011(3)
C12 0.049(4) 0.044(4) 0.050(4) -0.012(3) -0.001(3) -0.012(3)
C13 0.049(4) 0.036(3) 0.036(4) -0.008(3) 0.006(3) -0.013(3)
C14 0.036(3) 0.032(3) 0.030(3) -0.006(3) 0.002(3) -0.006(3)
C15 0.066(5) 0.039(3) 0.039(4) -0.017(3) 0.012(4) -0.013(3)
C16 0.065(5) 0.047(4) 0.036(4) -0.010(3) 0.023(4) -0.011(4)
S3 0.0548(11) 0.0384(9) 0.0547(12) -0.0114(8) 0.0097(9) -0.0162(8)
O3 0.063(4) 0.058(3) 0.084(4) -0.022(3) 0.012(3) -0.010(3)
O2 0.149(6) 0.076(4) 0.092(5) -0.054(4) 0.063(5) -0.080(4)
O1 0.072(5) 0.138(6) 0.092(5) 0.048(5) -0.006(4) -0.017(4)
F13 0.111(5) 0.117(5) 0.187(8) -0.046(5) 0.096(5) -0.045(4)
F12 0.187(7) 0.155(6) 0.074(4) 0.037(4) -0.002(5) -0.099(6)
F11 0.165(7) 0.166(6) 0.148(6) -0.076(5) 0.048(5) -0.135(6)
C17 0.089(7) 0.067(5) 0.060(6) -0.008(5) 0.020(5) -0.041(5)
S4 0.0508(11) 0.0437(9) 0.0777(15) -0.0220(10) 0.0256(10) -0.0149(9)
O4 0.099(6) 0.050(4) 0.335(15) 0.035(6) 0.087(8) 0.004(4)
O5 0.084(5) 0.261(11) 0.091(6) -0.106(7) 0.035(4) -0.060(6)
O6 0.061(4) 0.053(3) 0.081(4) -0.012(3) 0.033(3) -0.004(3)
C18 0.101(10) 0.131(12) 0.128(13) -0.017(10) -0.026(8) -0.053(9)
F21 0.055(4) 0.196(8) 0.253(11) 0.010(8) -0.045(5) -0.040(5)
F22 0.156(7) 0.108(6) 0.384(17) -0.075(8) 0.062(8) -0.103(6)
F23 0.315(15) 0.395(19) 0.119(8) 0.001(10) -0.078(9) -0.223(15)
S5 0.091(5) 0.057(3) 0.046(3) -0.016(2) 0.015(3) -0.031(3)
S5' 0.052(3) 0.045(3) 0.041(2) -0.0096(19) 0.001(2) -0.003(2)
O7 0.124(6) 0.108(5) 0.057(4) 0.006(4) -0.005(4) -0.026(5)
O8 0.094(12) 0.095(13) 0.129(13) -0.051(10) 0.060(11) -0.024(9)
O8' 0.095(12) 0.24(2) 0.151(17) 0.062(15) -0.031(11) -0.097(13)
O9' 0.24(2) 0.061(9) 0.094(13) -0.054(10) -0.039(15) -0.012(13)
O9 0.193(19) 0.26(2) 0.117(14) -0.102(15) 0.085(13) -0.197(19)
C19 0.159(13) 0.081(7) 0.069(8) -0.021(6) 0.005(8) -0.016(8)
F32 0.091(6) 0.332(17) 0.236(13) 0.067(11) 0.025(7) 0.058(8)
F31 0.56(3) 0.121(7) 0.148(9) -0.009(6) -0.042(12) -0.187(12)
F33 0.200(8) 0.133(6) 0.085(5) 0.040(4) -0.048(5) -0.054(6)
O1W 0.116(6) 0.110(5) 0.092(5) -0.049(4) 0.041(4) -0.073(5)
O2W 0.096(5) 0.063(4) 0.110(6) -0.019(4) 0.046(4) -0.023(3)
O3W 0.089(5) 0.127(6) 0.105(6) 0.005(5) 0.000(4) -0.038(5)
_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 N7 2.255(5) 1_645 ?
Ag1 O1W 2.352(6) . ?
Ag1 N1 2.376(6) . ?
Ag1 O2W 2.421(6) . ?
Ag2 N8 2.242(5) 2_677 ?
Ag2 N4 2.265(5) . ?
Ag2 O9' 2.399(17) . ?
Ag2 N5 2.403(6) . ?
Ag3 N2 2.273(6) 2_676 ?
Ag3 N6 2.302(6) . ?
Ag3 N3 2.403(5) 1_455 ?
N1 C1 1.327(9) . ?
N1 C4 1.348(7) . ?
N2 C3 1.313(8) . ?
N2 C2 1.339(8) . ?
N2 Ag3 2.273(6) 2_676 ?
N3 C7 1.335(8) . ?
N3 C6 1.340(7) . ?
N3 Ag3 2.403(5) 1_655 ?
N4 C5 1.332(7) . ?
N4 C8 1.340(7) . ?
S1 C5 1.774(6) . ?
S1 C4 1.786(6) . ?
C1 C2 1.374(10) . ?
C1 H1A 0.9300 . ?
C2 H2A 0.9300 . ?
C3 C4 1.368(9) . ?
C3 H3A 0.9300 . ?
C5 C6 1.365(8) . ?
C6 H6A 0.9300 . ?
C7 C8 1.371(9) . ?
C7 H7A 0.9300 . ?
C8 H8A 0.9300 . ?
N5 C9 1.333(9) . ?
N5 C12 1.343(8) . ?
N6 C11 1.321(8) . ?
N6 C10 1.350(8) . ?
N7 C14 1.337(7) . ?
N7 C15 1.340(8) . ?
N7 Ag1 2.255(5) 1_465 ?
N8 C13 1.342(8) . ?
N8 C16 1.345(8) . ?
N8 Ag2 2.242(5) 2_677 ?
S2 C14 1.758(6) . ?
S2 C11 1.775(6) . ?
C9 C10 1.383(10) . ?
C9 H9A 0.9300 . ?
C10 H10A 0.9300 . ?
C11 C12 1.372(10) . ?
C12 H12A 0.9300 . ?
C13 C14 1.374(9) . ?
C13 H13A 0.9300 . ?
C15 C16 1.356(10) . ?
C15 H15A 0.9300 . ?
C16 H16A 0.9300 . ?
S3 O2 1.422(6) . ?
S3 O3 1.426(5) . ?
S3 O1 1.431(7) . ?
S3 C17 1.798(8) . ?
F13 C17 1.288(10) . ?
F12 C17 1.325(11) . ?
F11 C17 1.299(10) . ?
S4 O4 1.386(7) . ?
S4 O5 1.414(8) . ?
S4 O6 1.423(5) . ?
S4 C18 1.768(13) . ?
C18 F22 1.213(15) . ?
C18 F21 1.299(14) . ?
C18 F23 1.430(17) . ?
S5 S5' 0.698(6) . ?
S5 O9' 1.173(18) . ?
S5 O7 1.431(7) . ?
S5 O8 1.440(8) . ?
S5 O9 1.442(8) . ?
S5 C19 1.707(8) . ?
S5 O8' 2.074(17) . ?
S5' O8 1.160(16) . ?
S5' O8' 1.392(17) . ?
S5' O9' 1.394(17) . ?
S5' O7 1.409(9) . ?
S5' C19 1.737(8) . ?
S5' O9 2.125(10) . ?
O8 O9' 0.94(3) . ?
O8 O8' 1.48(3) . ?
O9' O9 1.75(3) . ?
C19 F32 1.296(7) . ?
C19 F31 1.296(7) . ?
C19 F33 1.299(7) . ?
O1W H1C 0.9731 . ?
O1W H1B 0.9793 . ?
O2W H2WB 1.0625 . ?
O2W H2WC 1.2437 . ?
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
N7 Ag1 O1W 132.3(2) 1_645 . ?
N7 Ag1 N1 120.0(2) 1_645 . ?
O1W Ag1 N1 96.1(2) . . ?
N7 Ag1 O2W 125.48(19) 1_645 . ?
O1W Ag1 O2W 82.0(2) . . ?
N1 Ag1 O2W 88.3(2) . . ?
N8 Ag2 N4 146.4(2) 2_677 . ?
N8 Ag2 O9' 94.8(6) 2_677 . ?
N4 Ag2 O9' 104.9(7) . . ?
N8 Ag2 N5 102.7(2) 2_677 . ?
N4 Ag2 N5 104.3(2) . . ?
O9' Ag2 N5 89.6(6) . . ?
N2 Ag3 N6 152.94(19) 2_676 . ?
N2 Ag3 N3 105.9(2) 2_676 1_455 ?
N6 Ag3 N3 95.95(19) . 1_455 ?
C1 N1 C4 115.1(6) . . ?
C1 N1 Ag1 126.1(4) . . ?
C4 N1 Ag1 118.6(4) . . ?
C3 N2 C2 116.7(6) . . ?
C3 N2 Ag3 123.5(4) . 2_676 ?
C2 N2 Ag3 119.1(5) . 2_676 ?
C7 N3 C6 116.6(5) . . ?
C7 N3 Ag3 120.8(4) . 1_655 ?
C6 N3 Ag3 122.3(4) . 1_655 ?
C5 N4 C8 117.0(5) . . ?
C5 N4 Ag2 117.5(4) . . ?
C8 N4 Ag2 124.9(4) . . ?
C5 S1 C4 102.3(3) . . ?
N1 C1 C2 122.9(6) . . ?
N1 C1 H1A 118.5 . . ?
C2 C1 H1A 118.5 . . ?
N2 C2 C1 120.9(6) . . ?
N2 C2 H2A 119.5 . . ?
C1 C2 H2A 119.5 . . ?
N2 C3 C4 122.3(5) . . ?
N2 C3 H3A 118.8 . . ?
C4 C3 H3A 118.8 . . ?
N1 C4 C3 121.9(6) . . ?
N1 C4 S1 115.3(5) . . ?
C3 C4 S1 122.7(4) . . ?
N4 C5 C6 121.9(5) . . ?
N4 C5 S1 112.8(4) . . ?
C6 C5 S1 125.2(4) . . ?
N3 C6 C5 121.4(5) . . ?
N3 C6 H6A 119.3 . . ?
C5 C6 H6A 119.3 . . ?
N3 C7 C8 122.1(6) . . ?
N3 C7 H7A 119.0 . . ?
C8 C7 H7A 119.0 . . ?
N4 C8 C7 120.9(6) . . ?
N4 C8 H8A 119.6 . . ?
C7 C8 H8A 119.6 . . ?
C9 N5 C12 116.2(6) . . ?
C9 N5 Ag2 124.9(4) . . ?
C12 N5 Ag2 118.8(5) . . ?
C11 N6 C10 116.9(6) . . ?
C11 N6 Ag3 118.5(4) . . ?
C10 N6 Ag3 124.6(5) . . ?
C14 N7 C15 116.4(5) . . ?
C14 N7 Ag1 120.0(4) . 1_465 ?
C15 N7 Ag1 123.3(4) . 1_465 ?
C13 N8 C16 115.7(6) . . ?
C13 N8 Ag2 120.8(4) . 2_677 ?
C16 N8 Ag2 123.2(4) . 2_677 ?
C14 S2 C11 102.0(3) . . ?
N5 C9 C10 122.8(6) . . ?
N5 C9 H9A 118.6 . . ?
C10 C9 H9A 118.6 . . ?
N6 C10 C9 120.1(6) . . ?
N6 C10 H10A 119.9 . . ?
C9 C10 H10A 119.9 . . ?
N6 C11 C12 122.7(6) . . ?
N6 C11 S2 115.1(5) . . ?
C12 C11 S2 122.0(5) . . ?
N5 C12 C11 121.3(7) . . ?
N5 C12 H12A 119.4 . . ?
C11 C12 H12A 119.4 . . ?
N8 C13 C14 121.6(6) . . ?
N8 C13 H13A 119.2 . . ?
C14 C13 H13A 119.2 . . ?
N7 C14 C13 122.0(5) . . ?
N7 C14 S2 114.7(5) . . ?
C13 C14 S2 123.1(5) . . ?
N7 C15 C16 121.6(6) . . ?
N7 C15 H15A 119.2 . . ?
C16 C15 H15A 119.2 . . ?
N8 C16 C15 122.7(6) . . ?
N8 C16 H16A 118.6 . . ?
C15 C16 H16A 118.6 . . ?
O2 S3 O3 114.6(4) . . ?
O2 S3 O1 115.8(5) . . ?
O3 S3 O1 111.8(4) . . ?
O2 S3 C17 103.2(4) . . ?
O3 S3 C17 105.2(4) . . ?
O1 S3 C17 104.7(5) . . ?
F13 C17 F11 109.7(9) . . ?
F13 C17 F12 107.0(8) . . ?
F11 C17 F12 106.9(8) . . ?
F13 C17 S3 112.1(6) . . ?
F11 C17 S3 112.7(6) . . ?
F12 C17 S3 108.2(7) . . ?
O4 S4 O5 114.1(6) . . ?
O4 S4 O6 113.4(4) . . ?
O5 S4 O6 114.4(5) . . ?
O4 S4 C18 107.4(7) . . ?
O5 S4 C18 99.2(6) . . ?
O6 S4 C18 106.8(6) . . ?
F22 C18 F21 110.6(14) . . ?
F22 C18 F23 105.1(14) . . ?
F21 C18 F23 110.2(13) . . ?
F22 C18 S4 116.9(11) . . ?
F21 C18 S4 113.3(10) . . ?
F23 C18 S4 99.6(10) . . ?
S5' S5 O9' 92.8(18) . . ?
S5' S5 O7 74.0(9) . . ?
O9' S5 O7 129.9(13) . . ?
S5' S5 O8 52.8(12) . . ?
O9' S5 O8 40.8(13) . . ?
O7 S5 O8 114.5(12) . . ?
S5' S5 O9 165.7(12) . . ?
O9' S5 O9 83.3(15) . . ?
O7 S5 O9 118.9(8) . . ?
O8 S5 O9 120.2(12) . . ?
S5' S5 C19 80.7(8) . . ?
O9' S5 C19 119.4(13) . . ?
O7 S5 C19 106.1(5) . . ?
O8 S5 C19 100.3(10) . . ?
O9 S5 C19 89.2(10) . . ?
S5' S5 O8' 10.0(9) . . ?
O9' S5 O8' 86.2(16) . . ?
O7 S5 O8' 84.0(7) . . ?
O8 S5 O8' 45.4(11) . . ?
O9 S5 O8' 156.2(9) . . ?
C19 S5 O8' 77.5(7) . . ?
S5 S5' O8 98.6(14) . . ?
S5 S5' O8' 165.0(14) . . ?
O8 S5' O8' 70.1(13) . . ?
S5 S5' O9' 57.2(15) . . ?
O8 S5' O9' 42.2(11) . . ?
O8' S5' O9' 112.3(16) . . ?
S5 S5' O7 77.6(9) . . ?
O8 S5' O7 140.0(13) . . ?
O8' S5' O7 117.5(10) . . ?
O9' S5' O7 114.8(12) . . ?
S5 S5' C19 75.9(8) . . ?
O8 S5' C19 112.0(14) . . ?
O8' S5' C19 98.7(10) . . ?
O9' S5' C19 105.5(11) . . ?
O7 S5' C19 105.6(5) . . ?
S5 S5' O9 9.6(8) . . ?
O8 S5' O9 94.4(12) . . ?
O8' S5' O9 155.9(10) . . ?
O9' S5' O9 55.0(12) . . ?
O7 S5' O9 86.4(6) . . ?
C19 S5' O9 69.3(7) . . ?
S5' O7 S5 28.4(3) . . ?
O9' O8 S5' 82.2(13) . . ?
O9' O8 S5 54.2(12) . . ?
S5' O8 S5 28.6(4) . . ?
O9' O8 O8' 145(2) . . ?
S5' O8 O8' 62.4(13) . . ?
S5 O8 O8' 90.6(12) . . ?
S5' O8' O8 47.6(8) . . ?
S5' O8' S5 5.0(5) . . ?
O8 O8' S5 44.0(5) . . ?
O8 O9' S5 85.0(15) . . ?
O8 O9' S5' 55.6(13) . . ?
S5 O9' S5' 30.0(5) . . ?
O8 O9' O9 134(2) . . ?
S5 O9' O9 55.0(12) . . ?
S5' O9' O9 84.3(11) . . ?
O8 O9' Ag2 92(2) . . ?
S5 O9' Ag2 172.2(18) . . ?
S5' O9' Ag2 145.3(19) . . ?
O9 O9' Ag2 130.4(13) . . ?
S5 O9 O9' 41.8(7) . . ?
S5 O9 S5' 4.7(4) . . ?
O9' O9 S5' 40.7(6) . . ?
F32 C19 F31 99.9(10) . . ?
F32 C19 F33 110.5(10) . . ?
F31 C19 F33 105.7(9) . . ?
F32 C19 S5 100.5(8) . . ?
F31 C19 S5 121.4(7) . . ?
F33 C19 S5 117.1(6) . . ?
F32 C19 S5' 118.4(7) . . ?
F31 C19 S5' 101.3(8) . . ?
F33 C19 S5' 117.9(6) . . ?
S5 C19 S5' 23.4(2) . . ?
Ag1 O1W H1C 117.7 . . ?
Ag1 O1W H1B 111.6 . . ?
H1C O1W H1B 90.9 . . ?
Ag1 O2W H2WB 112.2 . . ?
Ag1 O2W H2WC 108.4 . . ?
H2WB O2W H2WC 80.8 . . ?
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
N7 Ag1 N1 C1 -99.9(6) 1_645 . . . ?
O1W Ag1 N1 C1 112.6(6) . . . . ?
O2W Ag1 N1 C1 30.9(6) . . . . ?
N7 Ag1 N1 C4 83.9(5) 1_645 . . . ?
O1W Ag1 N1 C4 -63.6(5) . . . . ?
O2W Ag1 N1 C4 -145.3(5) . . . . ?
N8 Ag2 N4 C5 66.7(6) 2_677 . . . ?
O9' Ag2 N4 C5 -169.4(7) . . . . ?
N5 Ag2 N4 C5 -76.0(5) . . . . ?
N8 Ag2 N4 C8 -121.9(6) 2_677 . . . ?
O9' Ag2 N4 C8 2.0(8) . . . . ?
N5 Ag2 N4 C8 95.4(6) . . . . ?
C4 N1 C1 C2 1.8(10) . . . . ?
Ag1 N1 C1 C2 -174.5(5) . . . . ?
C3 N2 C2 C1 -2.4(10) . . . . ?
Ag3 N2 C2 C1 168.6(5) 2_676 . . . ?
N1 C1 C2 N2 0.1(11) . . . . ?
C2 N2 C3 C4 2.7(9) . . . . ?
Ag3 N2 C3 C4 -167.8(5) 2_676 . . . ?
C1 N1 C4 C3 -1.4(9) . . . . ?
Ag1 N1 C4 C3 175.1(4) . . . . ?
C1 N1 C4 S1 175.1(5) . . . . ?
Ag1 N1 C4 S1 -8.3(6) . . . . ?
N2 C3 C4 N1 -0.9(10) . . . . ?
N2 C3 C4 S1 -177.1(5) . . . . ?
C5 S1 C4 N1 122.3(5) . . . . ?
C5 S1 C4 C3 -61.2(6) . . . . ?
C8 N4 C5 C6 -0.2(10) . . . . ?
Ag2 N4 C5 C6 171.9(5) . . . . ?
C8 N4 C5 S1 175.8(5) . . . . ?
Ag2 N4 C5 S1 -12.1(6) . . . . ?
C4 S1 C5 N4 143.6(5) . . . . ?
C4 S1 C5 C6 -40.5(6) . . . . ?
C7 N3 C6 C5 2.3(10) . . . . ?
Ag3 N3 C6 C5 176.4(5) 1_655 . . . ?
N4 C5 C6 N3 -1.8(10) . . . . ?
S1 C5 C6 N3 -177.3(5) . . . . ?
C6 N3 C7 C8 -1.0(10) . . . . ?
Ag3 N3 C7 C8 -175.2(6) 1_655 . . . ?
C5 N4 C8 C7 1.5(10) . . . . ?
Ag2 N4 C8 C7 -169.9(5) . . . . ?
N3 C7 C8 N4 -1.0(12) . . . . ?
N8 Ag2 N5 C9 -64.4(6) 2_677 . . . ?
N4 Ag2 N5 C9 95.5(6) . . . . ?
O9' Ag2 N5 C9 -159.3(8) . . . . ?
N8 Ag2 N5 C12 120.3(5) 2_677 . . . ?
N4 Ag2 N5 C12 -79.9(5) . . . . ?
O9' Ag2 N5 C12 25.4(8) . . . . ?
N2 Ag3 N6 C11 49.6(7) 2_676 . . . ?
N3 Ag3 N6 C11 -94.5(4) 1_455 . . . ?
N2 Ag3 N6 C10 -133.3(5) 2_676 . . . ?
N3 Ag3 N6 C10 82.7(5) 1_455 . . . ?
C12 N5 C9 C10 1.2(10) . . . . ?
Ag2 N5 C9 C10 -174.3(5) . . . . ?
C11 N6 C10 C9 -0.8(10) . . . . ?
Ag3 N6 C10 C9 -178.0(5) . . . . ?
N5 C9 C10 N6 -0.7(11) . . . . ?
C10 N6 C11 C12 1.7(9) . . . . ?
Ag3 N6 C11 C12 179.1(5) . . . . ?
C10 N6 C11 S2 176.5(5) . . . . ?
Ag3 N6 C11 S2 -6.1(6) . . . . ?
C14 S2 C11 N6 126.8(5) . . . . ?
C14 S2 C11 C12 -58.4(6) . . . . ?
C9 N5 C12 C11 -0.2(10) . . . . ?
Ag2 N5 C12 C11 175.5(5) . . . . ?
N6 C11 C12 N5 -1.3(11) . . . . ?
S2 C11 C12 N5 -175.7(5) . . . . ?
C16 N8 C13 C14 0.2(10) . . . . ?
Ag2 N8 C13 C14 -173.4(5) 2_677 . . . ?
C15 N7 C14 C13 -0.2(10) . . . . ?
Ag1 N7 C14 C13 -173.5(5) 1_465 . . . ?
C15 N7 C14 S2 175.0(5) . . . . ?
Ag1 N7 C14 S2 1.6(7) 1_465 . . . ?
N8 C13 C14 N7 -0.7(11) . . . . ?
N8 C13 C14 S2 -175.5(5) . . . . ?
C11 S2 C14 N7 146.7(5) . . . . ?
C11 S2 C14 C13 -38.2(7) . . . . ?
C14 N7 C15 C16 1.5(11) . . . . ?
Ag1 N7 C15 C16 174.6(6) 1_465 . . . ?
C13 N8 C16 C15 1.1(11) . . . . ?
Ag2 N8 C16 C15 174.6(6) 2_677 . . . ?
N7 C15 C16 N8 -2.1(13) . . . . ?
O2 S3 C17 F13 -55.9(9) . . . . ?
O3 S3 C17 F13 -176.3(8) . . . . ?
O1 S3 C17 F13 65.7(9) . . . . ?
O2 S3 C17 F11 179.8(8) . . . . ?
O3 S3 C17 F11 59.4(9) . . . . ?
O1 S3 C17 F11 -58.6(9) . . . . ?
O2 S3 C17 F12 61.8(7) . . . . ?
O3 S3 C17 F12 -58.6(7) . . . . ?
O1 S3 C17 F12 -176.6(7) . . . . ?
O4 S4 C18 F22 165.4(13) . . . . ?
O5 S4 C18 F22 -75.6(14) . . . . ?
O6 S4 C18 F22 43.4(15) . . . . ?
O4 S4 C18 F21 -64.2(13) . . . . ?
O5 S4 C18 F21 54.8(13) . . . . ?
O6 S4 C18 F21 173.8(11) . . . . ?
O4 S4 C18 F23 52.9(12) . . . . ?
O5 S4 C18 F23 171.8(11) . . . . ?
O6 S4 C18 F23 -69.2(11) . . . . ?
O9' S5 S5' O8 9(2) . . . . ?
O7 S5 S5' O8 139.5(14) . . . . ?
O9 S5 S5' O8 -65(5) . . . . ?
C19 S5 S5' O8 -110.6(13) . . . . ?
O8' S5 S5' O8 -40(5) . . . . ?
O9' S5 S5' O8' 49(6) . . . . ?
O7 S5 S5' O8' 179(100) . . . . ?
O8 S5 S5' O8' 40(5) . . . . ?
O9 S5 S5' O8' -25(9) . . . . ?
C19 S5 S5' O8' -71(5) . . . . ?
O7 S5 S5' O9' 130.8(12) . . . . ?
O8 S5 S5' O9' -9(2) . . . . ?
O9 S5 S5' O9' -74(5) . . . . ?
C19 S5 S5' O9' -119.3(12) . . . . ?
O8' S5 S5' O9' -49(6) . . . . ?
O9' S5 S5' O7 -130.8(12) . . . . ?
O8 S5 S5' O7 -139.5(14) . . . . ?
O9 S5 S5' O7 156(5) . . . . ?
C19 S5 S5' O7 109.9(4) . . . . ?
O8' S5 S5' O7 -179(100) . . . . ?
O9' S5 S5' C19 119.3(12) . . . . ?
O7 S5 S5' C19 -109.9(4) . . . . ?
O8 S5 S5' C19 110.6(13) . . . . ?
O9 S5 S5' C19 46(5) . . . . ?
O8' S5 S5' C19 71(5) . . . . ?
O9' S5 S5' O9 74(5) . . . . ?
O7 S5 S5' O9 -156(5) . . . . ?
O8 S5 S5' O9 65(5) . . . . ?
C19 S5 S5' O9 -46(5) . . . . ?
O8' S5 S5' O9 25(9) . . . . ?
O8 S5' O7 S5 -89(2) . . . . ?
O8' S5' O7 S5 -179.8(16) . . . . ?
O9' S5' O7 S5 -44.5(14) . . . . ?
C19 S5' O7 S5 71.3(8) . . . . ?
O9 S5' O7 S5 4.0(9) . . . . ?
O9' S5 O7 S5' 80(2) . . . . ?
O8 S5 O7 S5' 34.7(11) . . . . ?
O9 S5 O7 S5' -173.3(15) . . . . ?
C19 S5 O7 S5' -75.0(8) . . . . ?
O8' S5 O7 S5' 0.1(9) . . . . ?
S5 S5' O8 O9' -11(3) . . . . ?
O8' S5' O8 O9' 179(3) . . . . ?
O7 S5' O8 O9' 70(3) . . . . ?
C19 S5' O8 O9' -89(3) . . . . ?
O9 S5' O8 O9' -20(3) . . . . ?
O8' S5' O8 S5 -169.8(13) . . . . ?
O9' S5' O8 S5 11(3) . . . . ?
O7 S5' O8 S5 80.9(17) . . . . ?
C19 S5' O8 S5 -78.2(10) . . . . ?
O9 S5' O8 S5 -8.8(9) . . . . ?
S5 S5' O8 O8' 169.8(13) . . . . ?
O9' S5' O8 O8' -179(3) . . . . ?
O7 S5' O8 O8' -109.4(17) . . . . ?
C19 S5' O8 O8' 91.5(12) . . . . ?
O9 S5' O8 O8' 161.0(11) . . . . ?
S5' S5 O8 O9' 167(3) . . . . ?
O7 S5 O8 O9' 123(2) . . . . ?
O9 S5 O8 O9' -28(3) . . . . ?
C19 S5 O8 O9' -123(3) . . . . ?
O8' S5 O8 O9' 176(4) . . . . ?
O9' S5 O8 S5' -167(3) . . . . ?
O7 S5 O8 S5' -43.4(13) . . . . ?
O9 S5 O8 S5' 165.0(15) . . . . ?
C19 S5 O8 S5' 69.8(12) . . . . ?
O8' S5 O8 S5' 9.0(11) . . . . ?
S5' S5 O8 O8' -9.0(11) . . . . ?
O9' S5 O8 O8' -176(4) . . . . ?
O7 S5 O8 O8' -52.4(15) . . . . ?
O9 S5 O8 O8' 156.0(14) . . . . ?
C19 S5 O8 O8' 60.8(14) . . . . ?
S5 S5' O8' O8 -42(5) . . . . ?
O9' S5' O8' O8 0(2) . . . . ?
O7 S5' O8' O8 136.9(15) . . . . ?
C19 S5' O8' O8 -110.3(15) . . . . ?
O9 S5' O8' O8 -52(3) . . . . ?
O8 S5' O8' S5 42(5) . . . . ?
O9' S5' O8' S5 43(5) . . . . ?
O7 S5' O8' S5 179(100) . . . . ?
C19 S5' O8' S5 -68(5) . . . . ?
O9 S5' O8' S5 -10(4) . . . . ?
O9' O8 O8' S5' -1(5) . . . . ?
S5 O8 O8' S5' 4.9(6) . . . . ?
O9' O8 O8' S5 -6(5) . . . . ?
S5' O8 O8' S5 -4.9(6) . . . . ?
O9' S5 O8' S5' -131(6) . . . . ?
O7 S5 O8' S5' -1(5) . . . . ?
O8 S5 O8' S5' -134(6) . . . . ?
O9 S5 O8' S5' 165(5) . . . . ?
C19 S5 O8' S5' 107(5) . . . . ?
S5' S5 O8' O8 134(6) . . . . ?
O9' S5 O8' O8 3(2) . . . . ?
O7 S5 O8' O8 133.6(16) . . . . ?
O9 S5 O8' O8 -61(3) . . . . ?
C19 S5 O8' O8 -118.4(16) . . . . ?
S5' O8 O9' S5 6.4(16) . . . . ?
O8' O8 O9' S5 7(6) . . . . ?
S5 O8 O9' S5' -6.4(16) . . . . ?
O8' O8 O9' S5' 1(5) . . . . ?
S5' O8 O9' O9 34(4) . . . . ?
S5 O8 O9' O9 28(3) . . . . ?
O8' O8 O9' O9 35(8) . . . . ?
S5' O8 O9' Ag2 -166.4(9) . . . . ?
S5 O8 O9' Ag2 -172.8(16) . . . . ?
O8' O8 O9' Ag2 -165(5) . . . . ?
S5' S5 O9' O8 -11(3) . . . . ?
O7 S5 O9' O8 -82(3) . . . . ?
O9 S5 O9' O8 156(3) . . . . ?
C19 S5 O9' O8 70(3) . . . . ?
O8' S5 O9' O8 -3(3) . . . . ?
O7 S5 O9' S5' -71.4(16) . . . . ?
O8 S5 O9' S5' 11(3) . . . . ?
O9 S5 O9' S5' 166.2(13) . . . . ?
C19 S5 O9' S5' 80.9(12) . . . . ?
O8' S5 O9' S5' 7.5(9) . . . . ?
S5' S5 O9' O9 -166.2(13) . . . . ?
O7 S5 O9' O9 122.4(16) . . . . ?
O8 S5 O9' O9 -156(3) . . . . ?
C19 S5 O9' O9 -85.3(13) . . . . ?
O8' S5 O9' O9 -158.7(10) . . . . ?
S5' S5 O9' Ag2 58(16) . . . . ?
O7 S5 O9' Ag2 -14(17) . . . . ?
O8 S5 O9' Ag2 68(15) . . . . ?
O9 S5 O9' Ag2 -136(16) . . . . ?
C19 S5 O9' Ag2 139(15) . . . . ?
O8' S5 O9' Ag2 65(16) . . . . ?
S5 S5' O9' O8 167(3) . . . . ?
O8' S5' O9' O8 -1(3) . . . . ?
O7 S5' O9' O8 -138(2) . . . . ?
C19 S5' O9' O8 106(3) . . . . ?
O9 S5' O9' O8 156(3) . . . . ?
O8 S5' O9' S5 -167(3) . . . . ?
O8' S5' O9' S5 -167.9(14) . . . . ?
O7 S5' O9' S5 54.5(12) . . . . ?
C19 S5' O9' S5 -61.4(12) . . . . ?
O9 S5' O9' S5 -11.3(10) . . . . ?
S5 S5' O9' O9 11.3(10) . . . . ?
O8 S5' O9' O9 -156(3) . . . . ?
O8' S5' O9' O9 -156.5(12) . . . . ?
O7 S5' O9' O9 65.8(12) . . . . ?
C19 S5' O9' O9 -50.1(12) . . . . ?
S5 S5' O9' Ag2 -168(3) . . . . ?
O8 S5' O9' Ag2 24(2) . . . . ?
O8' S5' O9' Ag2 24(3) . . . . ?
O7 S5' O9' Ag2 -114(2) . . . . ?
C19 S5' O9' Ag2 130(2) . . . . ?
O9 S5' O9' Ag2 -180(3) . . . . ?
N8 Ag2 O9' O8 130(3) 2_677 . . . ?
N4 Ag2 O9' O8 -23(3) . . . . ?
N5 Ag2 O9' O8 -128(3) . . . . ?
N8 Ag2 O9' S5 62(16) 2_677 . . . ?
N4 Ag2 O9' S5 -91(16) . . . . ?
N5 Ag2 O9' S5 165(16) . . . . ?
N8 Ag2 O9' S5' 110(3) 2_677 . . . ?
N4 Ag2 O9' S5' -43(3) . . . . ?
N5 Ag2 O9' S5' -148(3) . . . . ?
N8 Ag2 O9' O9 -69.9(18) 2_677 . . . ?
N4 Ag2 O9' O9 137.5(17) . . . . ?
N5 Ag2 O9' O9 32.8(18) . . . . ?
S5' S5 O9 O9' 75(5) . . . . ?
O7 S5 O9 O9' -132.2(14) . . . . ?
O8 S5 O9 O9' 18(2) . . . . ?
C19 S5 O9 O9' 119.7(13) . . . . ?
O8' S5 O9 O9' 64(3) . . . . ?
O9' S5 O9 S5' -75(5) . . . . ?
O7 S5 O9 S5' 153(6) . . . . ?
O8 S5 O9 S5' -56(5) . . . . ?
C19 S5 O9 S5' 45(5) . . . . ?
O8' S5 O9 S5' -10(4) . . . . ?
O8 O9' O9 S5 -35(4) . . . . ?
S5' O9' O9 S5 -6.9(6) . . . . ?
Ag2 O9' O9 S5 173(2) . . . . ?
O8 O9' O9 S5' -28(3) . . . . ?
S5 O9' O9 S5' 6.9(6) . . . . ?
Ag2 O9' O9 S5' 180(2) . . . . ?
O8 S5' O9 S5 116(5) . . . . ?
O8' S5' O9 S5 164(6) . . . . ?
O9' S5' O9 S5 100(6) . . . . ?
O7 S5' O9 S5 -24(5) . . . . ?
C19 S5' O9 S5 -132(5) . . . . ?
S5 S5' O9 O9' -100(6) . . . . ?
O8 S5' O9 O9' 16(2) . . . . ?
O8' S5' O9 O9' 64(3) . . . . ?
O7 S5' O9 O9' -123.9(13) . . . . ?
C19 S5' O9 O9' 127.8(13) . . . . ?
S5' S5 C19 F32 -142.2(12) . . . . ?
O9' S5 C19 F32 129.8(19) . . . . ?
O7 S5 C19 F32 -72.0(10) . . . . ?
O8 S5 C19 F32 168.6(14) . . . . ?
O9 S5 C19 F32 48.0(11) . . . . ?
O8' S5 C19 F32 -151.9(12) . . . . ?
S5' S5 C19 F31 -33.7(13) . . . . ?
O9' S5 C19 F31 -121.7(19) . . . . ?
O7 S5 C19 F31 36.5(12) . . . . ?
O8 S5 C19 F31 -83.0(14) . . . . ?
O9 S5 C19 F31 156.5(11) . . . . ?
O8' S5 C19 F31 -43.4(12) . . . . ?
S5' S5 C19 F33 98.1(12) . . . . ?
O9' S5 C19 F33 10(2) . . . . ?
O7 S5 C19 F33 168.4(9) . . . . ?
O8 S5 C19 F33 48.9(14) . . . . ?
O9 S5 C19 F33 -71.7(11) . . . . ?
O8' S5 C19 F33 88.4(11) . . . . ?
O9' S5 C19 S5' -88.0(19) . . . . ?
O7 S5 C19 S5' 70.2(9) . . . . ?
O8 S5 C19 S5' -49.2(13) . . . . ?
O9 S5 C19 S5' -169.8(12) . . . . ?
O8' S5 C19 S5' -9.7(10) . . . . ?
S5 S5' C19 F32 43.2(14) . . . . ?
O8 S5' C19 F32 137.0(15) . . . . ?
O8' S5' C19 F32 -151.1(15) . . . . ?
O9' S5' C19 F32 92.8(17) . . . . ?
O7 S5' C19 F32 -29.3(13) . . . . ?
O9 S5' C19 F32 50.6(12) . . . . ?
S5 S5' C19 F31 151.1(11) . . . . ?
O8 S5' C19 F31 -115.2(13) . . . . ?
O8' S5' C19 F31 -43.3(13) . . . . ?
O9' S5' C19 F31 -159.4(14) . . . . ?
O7 S5' C19 F31 78.6(9) . . . . ?
O9 S5' C19 F31 158.4(9) . . . . ?
S5 S5' C19 F33 -94.2(12) . . . . ?
O8 S5' C19 F33 -0.5(15) . . . . ?
O8' S5' C19 F33 71.4(14) . . . . ?
O9' S5' C19 F33 -44.7(16) . . . . ?
O7 S5' C19 F33 -166.7(9) . . . . ?
O9 S5' C19 F33 -86.9(10) . . . . ?
O8 S5' C19 S5 93.7(14) . . . . ?
O8' S5' C19 S5 165.6(15) . . . . ?
O9' S5' C19 S5 49.5(15) . . . . ?
O7 S5' C19 S5 -72.5(9) . . . . ?
O9 S5' C19 S5 7.4(9) . . . . ?
_diffrn_measured_fraction_theta_max 0.971
_diffrn_reflns_theta_full 28.39
_diffrn_measured_fraction_theta_full 0.971
_refine_diff_density_max 0.967
_refine_diff_density_min -0.699
_refine_diff_density_rms 0.134
_database_code_depnum_ccdc_archive 'CCDC 743076'
#######################################################################
#
# Cambridge Crystallographic Data Centre
# CCDC
#
#######################################################################
#
# This CIF contains data from an original supplementary publication
# deposited with the CCDC, and may include chemical, crystal,
# experimental, refinement, atomic coordinates,
# anisotropic displacement parameters and molecular geometry data,
# as required by the journal to which it was submitted.
#
# This CIF is provided on the understanding that it is used for bona
# fide research purposes only. It may contain copyright material
# of the CCDC or of third parties, and may not be copied or further
# disseminated in any form, whether machine-readable or not,
# except for the purpose of generating routine backup copies
# on your local computer system.
#
# For further information on the CCDC, data deposition and
# data retrieval see:
# www.ccdc.cam.ac.uk
#
# Bona fide researchers may freely download Mercury and enCIFer
# from this site to visualise CIF-encoded structures and
# to carry out CIF format checking respectively.
#
data_4
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety ?
_chemical_formula_sum 'C8 H8 Ag2 N6 O7 S'
_chemical_formula_weight 548.00
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting Monoclinic
_symmetry_space_group_name_H-M Cc
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'
_cell_length_a 8.9469(2)
_cell_length_b 23.6973(6)
_cell_length_c 7.3859(2)
_cell_angle_alpha 90.00
_cell_angle_beta 108.400(2)
_cell_angle_gamma 90.00
_cell_volume 1485.88(6)
_cell_formula_units_Z 4
_cell_measurement_temperature 296(2)
_cell_measurement_reflns_used ?
_cell_measurement_theta_min ?
_cell_measurement_theta_max ?
_exptl_crystal_description Block
_exptl_crystal_colour colorless
_exptl_crystal_size_max 0.40
_exptl_crystal_size_mid 0.30
_exptl_crystal_size_min 0.20
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 2.450
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1056
_exptl_absorpt_coefficient_mu 2.825
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.5846
_exptl_absorpt_correction_T_max 0.7456
_exptl_absorpt_process_details 'SADABS (Bruker, 2007)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 296(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 APEXII CCD area detector'
_diffrn_measurement_method \w-scans
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 6427
_diffrn_reflns_av_R_equivalents 0.0244
_diffrn_reflns_av_sigmaI/netI 0.0338
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_k_min -31
_diffrn_reflns_limit_k_max 26
_diffrn_reflns_limit_l_min -9
_diffrn_reflns_limit_l_max 9
_diffrn_reflns_theta_min 2.55
_diffrn_reflns_theta_max 27.98
_reflns_number_total 2920
_reflns_number_gt 2651
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'APEX2 (Bruker 2007)'
_computing_cell_refinement 'APEX2 and SAINT (Bruker 2007)'
_computing_data_reduction SAINT
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
;
SHELXTL and PLATON (Spek, 2009)
;
_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^)+(0.0317P)^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 SHELXL
_refine_ls_extinction_coef 0.00099(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack 0.00(3)
_refine_ls_number_reflns 2920
_refine_ls_number_parameters 218
_refine_ls_number_restraints 2
_refine_ls_R_factor_all 0.0325
_refine_ls_R_factor_gt 0.0280
_refine_ls_wR_factor_ref 0.0640
_refine_ls_wR_factor_gt 0.0610
_refine_ls_goodness_of_fit_ref 1.030
_refine_ls_restrained_S_all 1.029
_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 1.04772(4) 0.321142(15) 1.39524(4) 0.04750(12) Uani 1 1 d . . .
Ag2 Ag 0.49372(6) 0.506994(17) 0.71678(7) 0.06248(15) Uani 1 1 d . . .
S1 S 0.76689(16) 0.29120(5) 1.02657(16) 0.0422(3) Uani 1 1 d . . .
N1 N 0.9119(4) 0.38699(15) 1.1618(5) 0.0367(8) Uani 1 1 d . . .
N2 N 0.6939(5) 0.45479(16) 0.8995(6) 0.0437(9) Uani 1 1 d . . .
N3 N 0.7210(4) 0.22076(14) 0.7444(5) 0.0348(8) Uani 1 1 d . . .
N4 N 0.9090(5) 0.27536(15) 0.5619(6) 0.0379(8) Uani 1 1 d . . .
N5 N 0.2094(5) 0.54640(17) 0.4426(6) 0.0431(9) Uani 1 1 d . . .
N6 N 0.5576(6) 0.62228(19) 0.9048(8) 0.0530(10) Uani 1 1 d . . .
O1 O 0.0892(5) 0.57091(15) 0.3376(6) 0.0596(9) Uani 1 1 d . . .
O2 O 0.3438(5) 0.56322(17) 0.4452(6) 0.0615(10) Uani 1 1 d . . .
O3 O 0.2000(5) 0.50591(16) 0.5419(6) 0.0641(11) Uani 1 1 d . . .
O4 O 0.4583(6) 0.58740(18) 0.9266(7) 0.0699(12) Uani 1 1 d . . .
O5 O 0.6567(7) 0.6053(2) 0.8328(10) 0.1003(19) Uani 1 1 d . . .
O6 O 0.5549(6) 0.67156(18) 0.9597(8) 0.0785(15) Uani 1 1 d . . .
O1W O 1.2740(6) 0.35956(18) 1.6215(6) 0.0677(11) Uani 1 1 d . . .
C1 C 0.7918(5) 0.36502(18) 1.0219(6) 0.0347(9) Uani 1 1 d . . .
C2 C 0.6847(6) 0.3991(2) 0.8922(7) 0.0423(10) Uani 1 1 d . . .
H2A H 0.6033 0.3823 0.7963 0.051 Uiso 1 1 calc R . .
C3 C 0.8152(6) 0.47719(19) 1.0382(7) 0.0442(11) Uani 1 1 d . . .
H3A H 0.8276 0.5162 1.0462 0.053 Uiso 1 1 calc R . .
C4 C 0.9224(6) 0.44309(19) 1.1696(7) 0.0434(11) Uani 1 1 d . . .
H4A H 1.0037 0.4599 1.2656 0.052 Uiso 1 1 calc R . .
C5 C 0.7939(5) 0.26931(17) 0.8096(6) 0.0331(9) Uani 1 1 d . . .
C6 C 0.8870(5) 0.29670(18) 0.7188(7) 0.0352(9) Uani 1 1 d . . .
H6A H 0.9351 0.3306 0.7681 0.042 Uiso 1 1 calc R . .
C7 C 0.8390(6) 0.22584(18) 0.4999(7) 0.0407(10) Uani 1 1 d . . .
H7A H 0.8528 0.2094 0.3920 0.049 Uiso 1 1 calc R . .
C8 C 0.7487(6) 0.19909(19) 0.5902(7) 0.0402(10) Uani 1 1 d . . .
H8A H 0.7044 0.1644 0.5436 0.048 Uiso 1 1 calc R . .
H1WA H 1.3067 0.3893 1.5719 0.060 Uiso 1 1 d R . .
H1WB H 1.2341 0.3803 1.6969 0.060 Uiso 1 1 d 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 0.04154(18) 0.0558(2) 0.0488(2) 0.00640(18) 0.01932(15) 0.00303(16)
Ag2 0.0529(2) 0.0572(2) 0.0702(3) 0.0078(2) 0.0093(2) 0.01447(19)
S1 0.0589(7) 0.0367(5) 0.0358(5) -0.0044(4) 0.0216(5) -0.0100(5)
N1 0.0334(19) 0.0409(19) 0.0352(19) -0.0037(15) 0.0097(16) -0.0039(14)
N2 0.039(2) 0.044(2) 0.048(2) 0.0019(18) 0.0143(18) 0.0050(17)
N3 0.0348(18) 0.0310(16) 0.0375(19) -0.0001(15) 0.0097(15) -0.0033(14)
N4 0.038(2) 0.0410(19) 0.039(2) -0.0022(16) 0.0180(17) -0.0016(15)
N5 0.040(2) 0.045(2) 0.046(2) -0.0015(18) 0.0160(18) 0.0026(17)
N6 0.044(2) 0.064(3) 0.049(2) 0.007(2) 0.0105(18) 0.004(2)
O1 0.056(2) 0.056(2) 0.059(2) 0.0060(18) 0.0062(18) 0.0116(17)
O2 0.047(2) 0.067(2) 0.072(3) 0.000(2) 0.021(2) -0.0103(18)
O3 0.062(3) 0.060(2) 0.068(3) 0.021(2) 0.018(2) -0.0001(18)
O4 0.074(3) 0.068(3) 0.079(3) -0.017(2) 0.040(3) -0.017(2)
O5 0.090(4) 0.107(4) 0.135(5) -0.015(4) 0.081(4) -0.001(3)
O6 0.062(2) 0.059(2) 0.100(4) -0.012(2) 0.004(3) -0.0010(19)
O1W 0.075(3) 0.076(3) 0.055(2) -0.014(2) 0.025(2) -0.024(2)
C1 0.036(2) 0.039(2) 0.031(2) -0.0036(17) 0.0123(18) -0.0004(16)
C2 0.040(2) 0.045(2) 0.039(2) -0.0024(19) 0.008(2) 0.0015(18)
C3 0.052(3) 0.035(2) 0.048(3) -0.004(2) 0.019(2) -0.001(2)
C4 0.041(2) 0.041(2) 0.048(3) -0.006(2) 0.012(2) -0.0076(18)
C5 0.030(2) 0.034(2) 0.033(2) 0.0033(16) 0.0072(17) 0.0023(15)
C6 0.035(2) 0.032(2) 0.040(2) -0.0007(17) 0.0124(18) -0.0009(16)
C7 0.047(3) 0.039(2) 0.039(2) -0.0041(18) 0.018(2) 0.0004(19)
C8 0.044(3) 0.035(2) 0.043(2) -0.009(2) 0.017(2) -0.0032(18)
_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 N4 2.280(4) 1_556 ?
Ag1 N1 2.358(4) . ?
Ag1 O1W 2.363(4) . ?
Ag1 N3 2.392(4) 4 ?
Ag2 N2 2.244(4) . ?
Ag2 O2 2.429(4) . ?
Ag2 O3 2.536(4) . ?
Ag2 O4 2.538(4) . ?
S1 C1 1.765(4) . ?
S1 C5 1.772(5) . ?
N1 C4 1.333(6) . ?
N1 C1 1.339(5) . ?
N2 C2 1.321(6) . ?
N2 C3 1.344(7) . ?
N3 C5 1.335(5) . ?
N3 C8 1.342(6) . ?
N3 Ag1 2.392(4) 4_454 ?
N4 C6 1.335(6) . ?
N4 C7 1.341(6) . ?
N4 Ag1 2.280(4) 1_554 ?
N5 O3 1.227(6) . ?
N5 O1 1.252(5) . ?
N5 O2 1.262(6) . ?
N6 O5 1.236(7) . ?
N6 O6 1.239(6) . ?
N6 O4 1.261(7) . ?
O1W H1WA 0.8857 . ?
O1W H1WB 0.8969 . ?
C1 C2 1.382(6) . ?
C2 H2A 0.9300 . ?
C3 C4 1.388(7) . ?
C3 H3A 0.9300 . ?
C4 H4A 0.9300 . ?
C5 C6 1.384(6) . ?
C6 H6A 0.9300 . ?
C7 C8 1.357(7) . ?
C7 H7A 0.9300 . ?
C8 H8A 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
N4 Ag1 N1 117.83(14) 1_556 . ?
N4 Ag1 O1W 107.01(15) 1_556 . ?
N1 Ag1 O1W 113.00(14) . . ?
N4 Ag1 N3 126.68(12) 1_556 4 ?
N1 Ag1 N3 101.21(13) . 4 ?
O1W Ag1 N3 87.29(15) . 4 ?
N2 Ag2 O2 157.99(14) . . ?
N2 Ag2 O3 143.41(14) . . ?
O2 Ag2 O3 51.08(13) . . ?
N2 Ag2 O4 106.05(16) . . ?
O2 Ag2 O4 87.11(15) . . ?
O3 Ag2 O4 90.55(15) . . ?
C1 S1 C5 102.6(2) . . ?
C4 N1 C1 116.7(4) . . ?
C4 N1 Ag1 128.0(3) . . ?
C1 N1 Ag1 114.2(3) . . ?
C2 N2 C3 116.8(4) . . ?
C2 N2 Ag2 119.9(3) . . ?
C3 N2 Ag2 122.7(3) . . ?
C5 N3 C8 115.8(4) . . ?
C5 N3 Ag1 120.3(3) . 4_454 ?
C8 N3 Ag1 123.9(3) . 4_454 ?
C6 N4 C7 116.6(4) . . ?
C6 N4 Ag1 122.9(3) . 1_554 ?
C7 N4 Ag1 120.5(3) . 1_554 ?
O3 N5 O1 121.7(4) . . ?
O3 N5 O2 118.9(4) . . ?
O1 N5 O2 119.4(4) . . ?
O5 N6 O6 122.5(6) . . ?
O5 N6 O4 118.2(5) . . ?
O6 N6 O4 119.3(6) . . ?
N5 O2 Ag2 96.6(3) . . ?
N5 O3 Ag2 92.4(3) . . ?
N6 O4 Ag2 100.7(4) . . ?
Ag1 O1W H1WA 109.6 . . ?
Ag1 O1W H1WB 103.3 . . ?
H1WA O1W H1WB 93.9 . . ?
N1 C1 C2 121.3(4) . . ?
N1 C1 S1 116.5(3) . . ?
C2 C1 S1 121.9(3) . . ?
N2 C2 C1 122.3(4) . . ?
N2 C2 H2A 118.8 . . ?
C1 C2 H2A 118.8 . . ?
N2 C3 C4 121.1(4) . . ?
N2 C3 H3A 119.5 . . ?
C4 C3 H3A 119.5 . . ?
N1 C4 C3 121.8(4) . . ?
N1 C4 H4A 119.1 . . ?
C3 C4 H4A 119.1 . . ?
N3 C5 C6 122.0(4) . . ?
N3 C5 S1 112.8(3) . . ?
C6 C5 S1 125.1(3) . . ?
N4 C6 C5 121.3(4) . . ?
N4 C6 H6A 119.4 . . ?
C5 C6 H6A 119.4 . . ?
N4 C7 C8 121.8(5) . . ?
N4 C7 H7A 119.1 . . ?
C8 C7 H7A 119.1 . . ?
N3 C8 C7 122.5(4) . . ?
N3 C8 H8A 118.8 . . ?
C7 C8 H8A 118.8 . . ?
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
N4 Ag1 N1 C4 107.3(4) 1_556 . . . ?
O1W Ag1 N1 C4 -18.4(4) . . . . ?
N3 Ag1 N1 C4 -110.2(4) 4 . . . ?
N4 Ag1 N1 C1 -60.2(3) 1_556 . . . ?
O1W Ag1 N1 C1 174.1(3) . . . . ?
N3 Ag1 N1 C1 82.3(3) 4 . . . ?
O2 Ag2 N2 C2 -97.2(5) . . . . ?
O3 Ag2 N2 C2 24.1(5) . . . . ?
O4 Ag2 N2 C2 137.9(4) . . . . ?
O2 Ag2 N2 C3 92.6(5) . . . . ?
O3 Ag2 N2 C3 -146.0(4) . . . . ?
O4 Ag2 N2 C3 -32.2(4) . . . . ?
O3 N5 O2 Ag2 -10.9(5) . . . . ?
O1 N5 O2 Ag2 169.8(4) . . . . ?
N2 Ag2 O2 N5 145.0(4) . . . . ?
O3 Ag2 O2 N5 5.9(3) . . . . ?
O4 Ag2 O2 N5 -87.1(3) . . . . ?
O1 N5 O3 Ag2 -170.4(4) . . . . ?
O2 N5 O3 Ag2 10.4(5) . . . . ?
N2 Ag2 O3 N5 -161.7(3) . . . . ?
O2 Ag2 O3 N5 -6.0(3) . . . . ?
O4 Ag2 O3 N5 79.8(3) . . . . ?
O5 N6 O4 Ag2 -14.5(7) . . . . ?
O6 N6 O4 Ag2 167.2(4) . . . . ?
N2 Ag2 O4 N6 85.5(4) . . . . ?
O2 Ag2 O4 N6 -76.5(4) . . . . ?
O3 Ag2 O4 N6 -127.5(4) . . . . ?
C4 N1 C1 C2 0.1(7) . . . . ?
Ag1 N1 C1 C2 169.1(4) . . . . ?
C4 N1 C1 S1 -173.8(4) . . . . ?
Ag1 N1 C1 S1 -4.8(4) . . . . ?
C5 S1 C1 N1 -118.0(4) . . . . ?
C5 S1 C1 C2 68.1(4) . . . . ?
C3 N2 C2 C1 1.2(7) . . . . ?
Ag2 N2 C2 C1 -169.4(4) . . . . ?
N1 C1 C2 N2 -0.5(8) . . . . ?
S1 C1 C2 N2 173.1(4) . . . . ?
C2 N2 C3 C4 -1.7(7) . . . . ?
Ag2 N2 C3 C4 168.7(4) . . . . ?
C1 N1 C4 C3 -0.6(7) . . . . ?
Ag1 N1 C4 C3 -167.9(4) . . . . ?
N2 C3 C4 N1 1.5(8) . . . . ?
C8 N3 C5 C6 2.6(6) . . . . ?
Ag1 N3 C5 C6 -175.7(3) 4_454 . . . ?
C8 N3 C5 S1 -174.0(3) . . . . ?
Ag1 N3 C5 S1 7.7(4) 4_454 . . . ?
C1 S1 C5 N3 -154.6(3) . . . . ?
C1 S1 C5 C6 28.9(4) . . . . ?
C7 N4 C6 C5 -1.2(6) . . . . ?
Ag1 N4 C6 C5 176.0(3) 1_554 . . . ?
N3 C5 C6 N4 -0.5(7) . . . . ?
S1 C5 C6 N4 175.6(3) . . . . ?
C6 N4 C7 C8 0.9(7) . . . . ?
Ag1 N4 C7 C8 -176.4(4) 1_554 . . . ?
C5 N3 C8 C7 -3.0(7) . . . . ?
Ag1 N3 C8 C7 175.3(4) 4_454 . . . ?
N4 C7 C8 N3 1.3(8) . . . . ?
_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full 27.98
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max 0.459
_refine_diff_density_min -0.537
_refine_diff_density_rms 0.076
_database_code_depnum_ccdc_archive 'CCDC 926720'
#######################################################################
#
# Cambridge Crystallographic Data Centre
# CCDC
#
#######################################################################
#
# This CIF contains data from an original supplementary publication
# deposited with the CCDC, and may include chemical, crystal,
# experimental, refinement, atomic coordinates,
# anisotropic displacement parameters and molecular geometry data,
# as required by the journal to which it was submitted.
#
# This CIF is provided on the understanding that it is used for bona
# fide research purposes only. It may contain copyright material
# of the CCDC or of third parties, and may not be copied or further
# disseminated in any form, whether machine-readable or not,
# except for the purpose of generating routine backup copies
# on your local computer system.
#
# For further information on the CCDC, data deposition and
# data retrieval see:
# www.ccdc.cam.ac.uk
#
# Bona fide researchers may freely download Mercury and enCIFer
# from this site to visualise CIF-encoded structures and
# to carry out CIF format checking respectively.
#
data_complex5
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety ?
_chemical_formula_sum 'C8 H6 Ag N5 O2 S'
_chemical_formula_weight 344.11
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'
S S 0.1246 0.1234 '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 Orthorhombic
_symmetry_space_group_name_H-M Pnma
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'
_cell_length_a 8.5705(7)
_cell_length_b 15.3195(13)
_cell_length_c 8.4310(6)
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_volume 1106.95(15)
_cell_formula_units_Z 4
_cell_measurement_temperature 296(2)
_cell_measurement_reflns_used ?
_cell_measurement_theta_min ?
_cell_measurement_theta_max ?
_exptl_crystal_description Block
_exptl_crystal_colour colorless
_exptl_crystal_size_max 0.40
_exptl_crystal_size_mid 0.30
_exptl_crystal_size_min 0.20
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 2.065
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 672
_exptl_absorpt_coefficient_mu 2.006
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.6121
_exptl_absorpt_correction_T_max 0.7456
_exptl_absorpt_process_details 'SADABS (Bruker, 2007)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 296(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 APEXII CCD area detector'
_diffrn_measurement_method \w-scans
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 4983
_diffrn_reflns_av_R_equivalents 0.0189
_diffrn_reflns_av_sigmaI/netI 0.0162
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_k_max 20
_diffrn_reflns_limit_l_min -11
_diffrn_reflns_limit_l_max 11
_diffrn_reflns_theta_min 2.66
_diffrn_reflns_theta_max 28.00
_reflns_number_total 1381
_reflns_number_gt 1243
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'APEX2 (Bruker 2007)'
_computing_cell_refinement 'APEX2 and SAINT (Bruker 2007)'
_computing_data_reduction SAINT
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
;
SHELXTL and PLATON (Spek, 2009)
;
_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^)+(0.0256P)^2^+0.8331P] 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 0.0054(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns 1381
_refine_ls_number_parameters 89
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0263
_refine_ls_R_factor_gt 0.0231
_refine_ls_wR_factor_ref 0.0591
_refine_ls_wR_factor_gt 0.0564
_refine_ls_goodness_of_fit_ref 1.051
_refine_ls_restrained_S_all 1.051
_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 0.55784(3) 0.2500 0.57112(3) 0.04850(12) Uani 1 2 d S . .
S1 S 0.62689(10) 0.2500 0.16127(11) 0.0481(2) Uani 1 2 d S . .
O1 O 0.8313(3) 0.31839(14) 0.7554(3) 0.0785(6) Uani 1 1 d . . .
N1 N 0.4806(2) 0.35369(12) 0.3728(2) 0.0383(4) Uani 1 1 d . . .
N2 N 0.3630(3) 0.46450(15) 0.1398(3) 0.0597(6) Uani 1 1 d . . .
N3 N 0.7755(5) 0.2500 0.7126(4) 0.0449(10) Uani 0.80 2 d SP . .
N3' N 0.842(2) 0.2500 0.7657(19) 0.040(3) Uani 0.20 2 d SP . .
C1 C 0.5070(2) 0.33958(13) 0.2192(2) 0.0362(4) Uani 1 1 d . . .
C2 C 0.4478(3) 0.39414(18) 0.1035(3) 0.0506(6) Uani 1 1 d . . .
H2A H 0.4675 0.3815 -0.0026 0.061 Uiso 1 1 calc R . .
C3 C 0.3354(3) 0.47775(16) 0.2929(3) 0.0534(6) Uani 1 1 d . . .
H3A H 0.2764 0.5259 0.3231 0.064 Uiso 1 1 calc R . .
C4 C 0.3912(3) 0.42251(15) 0.4083(3) 0.0452(5) Uani 1 1 d . . .
H4A H 0.3660 0.4333 0.5139 0.054 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 0.04608(17) 0.0623(2) 0.03716(15) 0.000 -0.00613(10) 0.000
S1 0.0427(4) 0.0461(4) 0.0555(5) 0.000 0.0182(4) 0.000
O1 0.1106(19) 0.0529(13) 0.0718(13) -0.0029(10) -0.0054(14) -0.0076(12)
N1 0.0411(9) 0.0365(9) 0.0372(9) 0.0016(7) 0.0005(7) -0.0037(8)
N2 0.0758(15) 0.0487(12) 0.0546(12) 0.0113(10) -0.0061(12) 0.0087(11)
N3 0.045(2) 0.058(3) 0.0315(18) 0.000 -0.0072(15) 0.000
N3' 0.046(9) 0.029(8) 0.045(9) 0.000 0.007(7) 0.000
C1 0.0364(10) 0.0342(9) 0.0380(10) 0.0016(8) 0.0018(8) -0.0070(8)
C2 0.0669(16) 0.0470(13) 0.0378(11) 0.0057(10) -0.0011(10) -0.0015(12)
C3 0.0607(15) 0.0392(11) 0.0604(14) 0.0021(11) 0.0008(12) 0.0073(11)
C4 0.0538(13) 0.0388(11) 0.0431(11) -0.0044(9) 0.0029(10) -0.0009(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
Ag1 N3 2.214(4) . ?
Ag1 N3' 2.306(18) 6_557 ?
Ag1 N1 2.3996(18) 7_565 ?
Ag1 N1 2.3996(18) . ?
S1 C1 1.783(2) 7_565 ?
S1 C1 1.783(2) . ?
O1 N3' 1.055(3) . ?
O1 N3 1.207(3) . ?
N1 C1 1.332(3) . ?
N1 C4 1.338(3) . ?
N2 C3 1.329(3) . ?
N2 C2 1.336(4) . ?
N3 N3' 0.724(17) . ?
N3 O1 1.207(3) 7_565 ?
N3' O1 1.055(3) 7_565 ?
N3' Ag1 2.306(18) 6_657 ?
C1 C2 1.382(3) . ?
C2 H2A 0.9300 . ?
C3 C4 1.375(3) . ?
C3 H3A 0.9300 . ?
C4 H4A 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
N3 Ag1 N3' 110.8(4) . 6_557 ?
N3 Ag1 N1 127.43(7) . 7_565 ?
N3' Ag1 N1 101.2(3) 6_557 7_565 ?
N3 Ag1 N1 127.43(7) . . ?
N3' Ag1 N1 101.2(3) 6_557 . ?
N1 Ag1 N1 82.90(9) 7_565 . ?
C1 S1 C1 100.67(13) 7_565 . ?
N3' O1 N3 36.5(9) . . ?
C1 N1 C4 116.31(19) . . ?
C1 N1 Ag1 121.55(14) . . ?
C4 N1 Ag1 121.57(15) . . ?
C3 N2 C2 116.3(2) . . ?
N3' N3 O1 60.2(2) . . ?
N3' N3 O1 60.2(2) . 7_565 ?
O1 N3 O1 120.5(5) . 7_565 ?
N3' N3 Ag1 174.4(13) . . ?
O1 N3 Ag1 119.7(2) . . ?
O1 N3 Ag1 119.7(2) 7_565 . ?
N3 N3' O1 83.2(10) . 7_565 ?
N3 N3' O1 83.2(10) . . ?
O1 N3' O1 166(2) 7_565 . ?
N3 N3' Ag1 178.4(16) . 6_657 ?
O1 N3' Ag1 96.8(10) 7_565 6_657 ?
O1 N3' Ag1 96.8(10) . 6_657 ?
N1 C1 C2 121.8(2) . . ?
N1 C1 S1 119.29(16) . . ?
C2 C1 S1 118.92(18) . . ?
N2 C2 C1 121.7(2) . . ?
N2 C2 H2A 119.1 . . ?
C1 C2 H2A 119.1 . . ?
N2 C3 C4 122.1(2) . . ?
N2 C3 H3A 118.9 . . ?
C4 C3 H3A 118.9 . . ?
N1 C4 C3 121.7(2) . . ?
N1 C4 H4A 119.1 . . ?
C3 C4 H4A 119.1 . . ?
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
N3 Ag1 N1 C1 95.32(19) . . . . ?
N3' Ag1 N1 C1 -137.3(3) 6_557 . . . ?
N1 Ag1 N1 C1 -37.22(19) 7_565 . . . ?
N3 Ag1 N1 C4 -93.7(2) . . . . ?
N3' Ag1 N1 C4 33.7(3) 6_557 . . . ?
N1 Ag1 N1 C4 133.75(16) 7_565 . . . ?
N3' O1 N3 O1 -1.4(13) . . . 7_565 ?
N3' O1 N3 Ag1 173.5(15) . . . . ?
N3' Ag1 N3 N3' 0.00(4) 6_557 . . . ?
N1 Ag1 N3 N3' -123.53(9) 7_565 . . . ?
N1 Ag1 N3 N3' 123.53(11) . . . . ?
N3' Ag1 N3 O1 -87.5(3) 6_557 . . . ?
N1 Ag1 N3 O1 149.0(3) 7_565 . . . ?
N1 Ag1 N3 O1 36.1(4) . . . . ?
N3' Ag1 N3 O1 87.5(3) 6_557 . . 7_565 ?
N1 Ag1 N3 O1 -36.1(4) 7_565 . . 7_565 ?
N1 Ag1 N3 O1 -149.0(3) . . . 7_565 ?
O1 N3 N3' O1 -178.7(13) . . . 7_565 ?
Ag1 N3 N3' O1 90.7(7) . . . 7_565 ?
O1 N3 N3' O1 178.7(13) 7_565 . . . ?
Ag1 N3 N3' O1 -90.7(7) . . . . ?
O1 N3 N3' Ag1 -89.3(8) . . . 6_657 ?
O1 N3 N3' Ag1 89.3(8) 7_565 . . 6_657 ?
Ag1 N3 N3' Ag1 180.00(12) . . . 6_657 ?
N3 O1 N3' O1 6(6) . . . 7_565 ?
N3 O1 N3' Ag1 178.4(16) . . . 6_657 ?
C4 N1 C1 C2 1.3(3) . . . . ?
Ag1 N1 C1 C2 172.73(17) . . . . ?
C4 N1 C1 S1 179.27(17) . . . . ?
Ag1 N1 C1 S1 -9.3(2) . . . . ?
C1 S1 C1 N1 67.4(2) 7_565 . . . ?
C1 S1 C1 C2 -114.61(17) 7_565 . . . ?
C3 N2 C2 C1 -1.7(4) . . . . ?
N1 C1 C2 N2 1.0(4) . . . . ?
S1 C1 C2 N2 -177.0(2) . . . . ?
C2 N2 C3 C4 0.3(4) . . . . ?
C1 N1 C4 C3 -2.8(3) . . . . ?
Ag1 N1 C4 C3 -174.19(19) . . . . ?
N2 C3 C4 N1 2.1(4) . . . . ?
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full 28.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max 0.557
_refine_diff_density_min -0.590
_refine_diff_density_rms 0.062
##########################End############################
_database_code_depnum_ccdc_archive 'CCDC 926721'
#######################################################################
#
# Cambridge Crystallographic Data Centre
# CCDC
#
#######################################################################
#
# This CIF contains data from an original supplementary publication
# deposited with the CCDC, and may include chemical, crystal,
# experimental, refinement, atomic coordinates,
# anisotropic displacement parameters and molecular geometry data,
# as required by the journal to which it was submitted.
#
# This CIF is provided on the understanding that it is used for bona
# fide research purposes only. It may contain copyright material
# of the CCDC or of third parties, and may not be copied or further
# disseminated in any form, whether machine-readable or not,
# except for the purpose of generating routine backup copies
# on your local computer system.
#
# For further information on the CCDC, data deposition and
# data retrieval see:
# www.ccdc.cam.ac.uk
#
# Bona fide researchers may freely download Mercury and enCIFer
# from this site to visualise CIF-encoded structures and
# to carry out CIF format checking respectively.
#
data_complex6
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety ?
_chemical_formula_sum 'C8 H6 Ag2 N6 O4 S'
_chemical_formula_weight 497.99
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'
S S 0.1246 0.1234 '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 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 18.4365(17)
_cell_length_b 10.2983(9)
_cell_length_c 15.905(3)
_cell_angle_alpha 90.00
_cell_angle_beta 118.923(3)
_cell_angle_gamma 90.00
_cell_volume 2643.1(5)
_cell_formula_units_Z 8
_cell_measurement_temperature 296(2)
_cell_measurement_reflns_used ?
_cell_measurement_theta_min ?
_cell_measurement_theta_max ?
_exptl_crystal_description Block
_exptl_crystal_colour colorless
_exptl_crystal_size_max 0.40
_exptl_crystal_size_mid 0.30
_exptl_crystal_size_min 0.20
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 2.503
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1904
_exptl_absorpt_coefficient_mu 3.146
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.656325
_exptl_absorpt_correction_T_max 1.000000
_exptl_absorpt_process_details 'SADABS (Bruker, 2007)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 296(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 APEXII CCD area detector'
_diffrn_measurement_method \w-scans
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 9335
_diffrn_reflns_av_R_equivalents 0.0205
_diffrn_reflns_av_sigmaI/netI 0.0166
_diffrn_reflns_limit_h_min -21
_diffrn_reflns_limit_h_max 21
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_theta_min 2.35
_diffrn_reflns_theta_max 25.01
_reflns_number_total 2310
_reflns_number_gt 2133
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'APEX2 (Bruker 2007)'
_computing_cell_refinement 'APEX2 and SAINT (Bruker 2007)'
_computing_data_reduction SAINT
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
;
SHELXTL and PLATON (Spek, 2009)
;
_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^)+(0.0260P)^2^+16.7249P] 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 2310
_refine_ls_number_parameters 199
_refine_ls_number_restraints 33
_refine_ls_R_factor_all 0.0332
_refine_ls_R_factor_gt 0.0306
_refine_ls_wR_factor_ref 0.0711
_refine_ls_wR_factor_gt 0.0695
_refine_ls_goodness_of_fit_ref 1.036
_refine_ls_restrained_S_all 1.057
_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 0.59940(2) 0.89995(3) 0.35884(3) 0.04955(13) Uani 1 1 d . . .
Ag2 Ag 0.62175(2) 0.27192(4) 0.16931(3) 0.05640(14) Uani 1 1 d . . .
S1 S 0.58867(7) 0.32800(10) 0.37327(10) 0.0458(3) Uani 1 1 d . . .
N1 N 0.4722(2) 0.4713(4) 0.3737(3) 0.0410(8) Uani 1 1 d . . .
N2 N 0.5419(2) 0.7096(3) 0.3695(3) 0.0372(8) Uani 1 1 d . . .
N3 N 0.7098(2) 0.3634(4) 0.3302(3) 0.0457(9) Uani 1 1 d . . .
N4 N 0.8203(2) 0.4658(4) 0.5089(3) 0.0409(8) Uani 1 1 d . . .
N5 N 0.4693(3) 1.0245(4) 0.3453(4) 0.0381(10) Uani 0.80 1 d PDU . .
N5' N 0.4251(16) 1.089(2) 0.3123(19) 0.046(4) Uani 0.20 1 d PU . .
N6 N 0.7399(3) 0.8053(5) 0.3766(4) 0.0618(12) Uani 1 1 d . . .
O1 O 0.4046(3) 1.0465(5) 0.2590(4) 0.0817(13) Uani 1 1 d DU . .
O2 O 0.4778(3) 1.1065(5) 0.4013(4) 0.0872(14) Uani 1 1 d DU . .
O3 O 0.7356(3) 0.7061(4) 0.3327(4) 0.0784(12) Uani 1 1 d . . .
O4 O 0.8017(3) 0.8742(4) 0.3967(3) 0.0732(12) Uani 1 1 d . . .
C1 C 0.5447(2) 0.4796(4) 0.3736(3) 0.0327(9) Uani 1 1 d . . .
C2 C 0.5784(3) 0.5987(4) 0.3697(3) 0.0362(9) Uani 1 1 d . . .
H2A H 0.6277 0.6006 0.3672 0.043 Uiso 1 1 calc R . .
C3 C 0.4707(3) 0.7014(5) 0.3724(4) 0.0494(12) Uani 1 1 d . . .
H3A H 0.4439 0.7772 0.3738 0.059 Uiso 1 1 calc R . .
C4 C 0.4365(3) 0.5844(5) 0.3731(4) 0.0506(12) Uani 1 1 d . . .
H4A H 0.3861 0.5833 0.3732 0.061 Uiso 1 1 calc R . .
C5 C 0.6896(2) 0.3774(4) 0.3994(3) 0.0355(9) Uani 1 1 d . . .
C6 C 0.7450(3) 0.4263(4) 0.4884(3) 0.0385(9) Uani 1 1 d . . .
H6A H 0.7291 0.4316 0.5356 0.046 Uiso 1 1 calc R . .
C7 C 0.8405(3) 0.4523(5) 0.4401(3) 0.0473(11) Uani 1 1 d . . .
H7A H 0.8928 0.4784 0.4519 0.057 Uiso 1 1 calc R . .
C8 C 0.7866(3) 0.4009(5) 0.3519(4) 0.0534(13) Uani 1 1 d . . .
H8A H 0.8037 0.3920 0.3060 0.064 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 0.0511(2) 0.0349(2) 0.0658(3) -0.00252(16) 0.03075(19) -0.00496(15)
Ag2 0.0532(2) 0.0532(2) 0.0718(3) -0.01132(19) 0.0374(2) -0.01824(18)
S1 0.0352(6) 0.0271(5) 0.0803(8) -0.0026(5) 0.0320(6) -0.0021(4)
N1 0.0351(19) 0.0380(19) 0.058(2) -0.0001(17) 0.0292(18) -0.0003(15)
N2 0.0341(18) 0.0303(17) 0.048(2) 0.0022(15) 0.0206(16) 0.0011(14)
N3 0.034(2) 0.055(2) 0.048(2) -0.0049(19) 0.0201(17) -0.0039(17)
N4 0.0323(19) 0.041(2) 0.048(2) -0.0038(17) 0.0183(17) -0.0001(16)
N5 0.028(2) 0.028(2) 0.057(3) -0.009(2) 0.019(2) 0.0073(19)
N5' 0.067(9) 0.036(8) 0.063(9) -0.027(7) 0.055(7) -0.031(8)
N6 0.055(3) 0.071(3) 0.074(3) 0.008(3) 0.043(2) 0.012(2)
O1 0.087(3) 0.066(3) 0.118(4) -0.032(3) 0.070(3) -0.016(2)
O2 0.061(3) 0.094(4) 0.100(3) 0.017(3) 0.034(3) 0.007(2)
O3 0.077(3) 0.059(2) 0.119(4) -0.005(3) 0.063(3) -0.004(2)
O4 0.064(2) 0.079(3) 0.092(3) -0.027(2) 0.050(2) -0.009(2)
C1 0.029(2) 0.031(2) 0.040(2) 0.0011(17) 0.0186(18) 0.0020(16)
C2 0.028(2) 0.034(2) 0.049(2) 0.0023(18) 0.0208(19) 0.0006(16)
C3 0.046(3) 0.036(2) 0.078(3) -0.001(2) 0.039(3) 0.006(2)
C4 0.040(3) 0.045(3) 0.082(4) 0.001(2) 0.041(3) 0.003(2)
C5 0.029(2) 0.0257(19) 0.053(2) 0.0025(18) 0.0216(19) 0.0048(16)
C6 0.037(2) 0.037(2) 0.048(2) 0.0009(19) 0.026(2) 0.0028(18)
C7 0.030(2) 0.060(3) 0.055(3) -0.003(2) 0.023(2) -0.002(2)
C8 0.039(3) 0.079(4) 0.050(3) -0.010(3) 0.027(2) -0.007(2)
_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 N2 2.274(3) . ?
Ag1 N4 2.349(4) 7_666 ?
Ag1 O1 2.380(5) 2_655 ?
Ag1 N5 2.635(4) . ?
Ag2 N5' 2.15(2) 2_645 ?
Ag2 O2 2.353(5) 2_645 ?
Ag2 O4 2.374(4) 4_645 ?
Ag2 N3 2.461(4) . ?
Ag2 N1 2.557(4) 2_655 ?
S1 C1 1.760(4) . ?
S1 C5 1.773(4) . ?
N1 C4 1.337(6) . ?
N1 C1 1.340(5) . ?
N1 Ag2 2.557(4) 2_655 ?
N2 C2 1.324(5) . ?
N2 C3 1.338(6) . ?
N3 C5 1.330(6) . ?
N3 C8 1.341(6) . ?
N4 C7 1.322(6) . ?
N4 C6 1.328(5) . ?
N4 Ag1 2.349(4) 7_666 ?
N5 N5' 0.99(3) . ?
N5 O2 1.182(6) . ?
N5 O1 1.332(7) . ?
N5' O1 0.86(2) . ?
N5' O2 1.28(3) . ?
N5' Ag2 2.15(2) 2_665 ?
N6 O3 1.218(6) . ?
N6 O4 1.245(6) . ?
O1 Ag1 2.380(5) 2_655 ?
O2 Ag2 2.353(5) 2_665 ?
O4 Ag2 2.374(4) 4_655 ?
C1 C2 1.389(6) . ?
C2 H2A 0.9300 . ?
C3 C4 1.363(7) . ?
C3 H3A 0.9300 . ?
C4 H4A 0.9300 . ?
C5 C6 1.379(6) . ?
C6 H6A 0.9300 . ?
C7 C8 1.374(7) . ?
C7 H7A 0.9300 . ?
C8 H8A 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
N2 Ag1 N4 123.72(13) . 7_666 ?
N2 Ag1 O1 140.15(16) . 2_655 ?
N4 Ag1 O1 95.64(16) 7_666 2_655 ?
N2 Ag1 N5 89.27(13) . . ?
N4 Ag1 N5 86.65(13) 7_666 . ?
O1 Ag1 N5 86.92(15) 2_655 . ?
N5' Ag2 O2 32.7(7) 2_645 2_645 ?
N5' Ag2 O4 144.4(5) 2_645 4_645 ?
O2 Ag2 O4 127.07(18) 2_645 4_645 ?
N5' Ag2 N3 107.5(7) 2_645 . ?
O2 Ag2 N3 138.05(16) 2_645 . ?
O4 Ag2 N3 93.21(15) 4_645 . ?
N5' Ag2 N1 118.3(5) 2_645 2_655 ?
O2 Ag2 N1 100.51(14) 2_645 2_655 ?
O4 Ag2 N1 89.78(13) 4_645 2_655 ?
N3 Ag2 N1 89.55(13) . 2_655 ?
C1 S1 C5 100.19(18) . . ?
C4 N1 C1 115.7(4) . . ?
C4 N1 Ag2 115.4(3) . 2_655 ?
C1 N1 Ag2 126.7(3) . 2_655 ?
C2 N2 C3 116.8(4) . . ?
C2 N2 Ag1 119.3(3) . . ?
C3 N2 Ag1 123.9(3) . . ?
C5 N3 C8 116.1(4) . . ?
C5 N3 Ag2 126.4(3) . . ?
C8 N3 Ag2 117.5(3) . . ?
C7 N4 C6 116.4(4) . . ?
C7 N4 Ag1 119.7(3) . 7_666 ?
C6 N4 Ag1 122.1(3) . 7_666 ?
N5' N5 O2 72.0(14) . . ?
N5' N5 O1 40.4(13) . . ?
O2 N5 O1 112.4(5) . . ?
N5' N5 Ag1 149.2(12) . . ?
O2 N5 Ag1 120.2(4) . . ?
O1 N5 Ag1 119.6(3) . . ?
O1 N5' N5 92(2) . . ?
O1 N5' O2 153(3) . . ?
N5 N5' O2 61.1(16) . . ?
O1 N5' Ag2 125(3) . 2_665 ?
N5 N5' Ag2 144(2) . 2_665 ?
O2 N5' Ag2 82.5(11) . 2_665 ?
O3 N6 O4 115.0(4) . . ?
N5' O1 N5 47.7(19) . . ?
N5' O1 Ag1 158.3(19) . 2_655 ?
N5 O1 Ag1 112.0(3) . 2_655 ?
N5 O2 N5' 46.9(11) . . ?
N5 O2 Ag2 111.6(4) . 2_665 ?
N5' O2 Ag2 64.8(11) . 2_665 ?
N6 O4 Ag2 107.4(3) . 4_655 ?
N1 C1 C2 121.5(4) . . ?
N1 C1 S1 113.8(3) . . ?
C2 C1 S1 124.6(3) . . ?
N2 C2 C1 121.7(4) . . ?
N2 C2 H2A 119.2 . . ?
C1 C2 H2A 119.2 . . ?
N2 C3 C4 121.5(4) . . ?
N2 C3 H3A 119.3 . . ?
C4 C3 H3A 119.3 . . ?
N1 C4 C3 122.8(4) . . ?
N1 C4 H4A 118.6 . . ?
C3 C4 H4A 118.6 . . ?
N3 C5 C6 121.6(4) . . ?
N3 C5 S1 117.2(3) . . ?
C6 C5 S1 121.2(3) . . ?
N4 C6 C5 122.1(4) . . ?
N4 C6 H6A 119.0 . . ?
C5 C6 H6A 119.0 . . ?
N4 C7 C8 122.1(4) . . ?
N4 C7 H7A 118.9 . . ?
C8 C7 H7A 118.9 . . ?
N3 C8 C7 121.7(4) . . ?
N3 C8 H8A 119.1 . . ?
C7 C8 H8A 119.2 . . ?
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
N4 Ag1 N2 C2 -100.7(3) 7_666 . . . ?
O1 Ag1 N2 C2 89.5(4) 2_655 . . . ?
N5 Ag1 N2 C2 173.9(3) . . . . ?
N4 Ag1 N2 C3 81.8(4) 7_666 . . . ?
O1 Ag1 N2 C3 -88.0(4) 2_655 . . . ?
N5 Ag1 N2 C3 -3.7(4) . . . . ?
N5' Ag2 N3 C5 -50.5(6) 2_645 . . . ?
O2 Ag2 N3 C5 -36.2(5) 2_645 . . . ?
O4 Ag2 N3 C5 158.9(4) 4_645 . . . ?
N1 Ag2 N3 C5 69.2(4) 2_655 . . . ?
N5' Ag2 N3 C8 128.2(6) 2_645 . . . ?
O2 Ag2 N3 C8 142.5(4) 2_645 . . . ?
O4 Ag2 N3 C8 -22.4(4) 4_645 . . . ?
N1 Ag2 N3 C8 -112.2(4) 2_655 . . . ?
N2 Ag1 N5 N5' -132(3) . . . . ?
N4 Ag1 N5 N5' 105(3) 7_666 . . . ?
O1 Ag1 N5 N5' 9(3) 2_655 . . . ?
N2 Ag1 N5 O2 122.3(5) . . . . ?
N4 Ag1 N5 O2 -1.5(5) 7_666 . . . ?
O1 Ag1 N5 O2 -97.4(5) 2_655 . . . ?
N2 Ag1 N5 O1 -90.8(4) . . . . ?
N4 Ag1 N5 O1 145.4(4) 7_666 . . . ?
O1 Ag1 N5 O1 49.5(4) 2_655 . . . ?
O2 N5 N5' O1 -179.7(16) . . . . ?
Ag1 N5 N5' O1 61(3) . . . . ?
O1 N5 N5' O2 179.7(16) . . . . ?
Ag1 N5 N5' O2 -119(2) . . . . ?
O2 N5 N5' Ag2 3(2) . . . 2_665 ?
O1 N5 N5' Ag2 -177(3) . . . 2_665 ?
Ag1 N5 N5' Ag2 -116(3) . . . 2_665 ?
O2 N5' O1 N5 -1(3) . . . . ?
Ag2 N5' O1 N5 178(2) 2_665 . . . ?
N5 N5' O1 Ag1 -24(4) . . . 2_655 ?
O2 N5' O1 Ag1 -25(7) . . . 2_655 ?
Ag2 N5' O1 Ag1 154(3) 2_665 . . 2_655 ?
O2 N5 O1 N5' 0.3(17) . . . . ?
Ag1 N5 O1 N5' -148.9(17) . . . . ?
N5' N5 O1 Ag1 170.7(17) . . . 2_655 ?
O2 N5 O1 Ag1 171.1(4) . . . 2_655 ?
Ag1 N5 O1 Ag1 21.8(4) . . . 2_655 ?
O1 N5 O2 N5' -0.2(11) . . . . ?
Ag1 N5 O2 N5' 148.8(12) . . . . ?
N5' N5 O2 Ag2 -1.7(11) . . . 2_665 ?
O1 N5 O2 Ag2 -1.9(6) . . . 2_665 ?
Ag1 N5 O2 Ag2 147.1(2) . . . 2_665 ?
O1 N5' O2 N5 1(4) . . . . ?
Ag2 N5' O2 N5 -178.2(12) 2_665 . . . ?
O1 N5' O2 Ag2 179(5) . . . 2_665 ?
N5 N5' O2 Ag2 178.2(12) . . . 2_665 ?
O3 N6 O4 Ag2 1.8(6) . . . 4_655 ?
C4 N1 C1 C2 -2.1(6) . . . . ?
Ag2 N1 C1 C2 160.4(3) 2_655 . . . ?
C4 N1 C1 S1 -179.4(4) . . . . ?
Ag2 N1 C1 S1 -16.9(5) 2_655 . . . ?
C5 S1 C1 N1 -167.9(3) . . . . ?
C5 S1 C1 C2 14.9(4) . . . . ?
C3 N2 C2 C1 -0.6(6) . . . . ?
Ag1 N2 C2 C1 -178.3(3) . . . . ?
N1 C1 C2 N2 2.5(7) . . . . ?
S1 C1 C2 N2 179.5(3) . . . . ?
C2 N2 C3 C4 -1.5(7) . . . . ?
Ag1 N2 C3 C4 176.1(4) . . . . ?
C1 N1 C4 C3 0.0(7) . . . . ?
Ag2 N1 C4 C3 -164.5(4) 2_655 . . . ?
N2 C3 C4 N1 1.9(9) . . . . ?
C8 N3 C5 C6 -0.8(7) . . . . ?
Ag2 N3 C5 C6 177.9(3) . . . . ?
C8 N3 C5 S1 -179.7(4) . . . . ?
Ag2 N3 C5 S1 -1.1(5) . . . . ?
C1 S1 C5 N3 -112.3(3) . . . . ?
C1 S1 C5 C6 68.8(4) . . . . ?
C7 N4 C6 C5 -2.0(6) . . . . ?
Ag1 N4 C6 C5 162.6(3) 7_666 . . . ?
N3 C5 C6 N4 2.3(7) . . . . ?
S1 C5 C6 N4 -178.8(3) . . . . ?
C6 N4 C7 C8 0.4(7) . . . . ?
Ag1 N4 C7 C8 -164.6(4) 7_666 . . . ?
C5 N3 C8 C7 -0.8(8) . . . . ?
Ag2 N3 C8 C7 -179.6(4) . . . . ?
N4 C7 C8 N3 1.0(8) . . . . ?
_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full 25.01
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max 1.104
_refine_diff_density_min -1.120
_refine_diff_density_rms 0.086
##########################End############################
_database_code_depnum_ccdc_archive 'CCDC 926722'
#######################################################################
#
# Cambridge Crystallographic Data Centre
# CCDC
#
#######################################################################
#
# This CIF contains data from an original supplementary publication
# deposited with the CCDC, and may include chemical, crystal,
# experimental, refinement, atomic coordinates,
# anisotropic displacement parameters and molecular geometry data,
# as required by the journal to which it was submitted.
#
# This CIF is provided on the understanding that it is used for bona
# fide research purposes only. It may contain copyright material
# of the CCDC or of third parties, and may not be copied or further
# disseminated in any form, whether machine-readable or not,
# except for the purpose of generating routine backup copies
# on your local computer system.
#
# For further information on the CCDC, data deposition and
# data retrieval see:
# www.ccdc.cam.ac.uk
#
# Bona fide researchers may freely download Mercury and enCIFer
# from this site to visualise CIF-encoded structures and
# to carry out CIF format checking respectively.
#
data_complex7
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety ?
_chemical_formula_sum 'C14 H6 Ag2 F10 N4 O4 S'
_chemical_formula_weight 732.03
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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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 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 18.7675(4)
_cell_length_b 22.3080(4)
_cell_length_c 13.9336(5)
_cell_angle_alpha 90.00
_cell_angle_beta 128.1470(10)
_cell_angle_gamma 90.00
_cell_volume 4587.6(2)
_cell_formula_units_Z 8
_cell_measurement_temperature 296(2)
_cell_measurement_reflns_used ?
_cell_measurement_theta_min ?
_cell_measurement_theta_max ?
_exptl_crystal_description Block
_exptl_crystal_colour colorless
_exptl_crystal_size_max 0.40
_exptl_crystal_size_mid 0.30
_exptl_crystal_size_min 0.20
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 2.120
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 2800
_exptl_absorpt_coefficient_mu 1.908
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.6164
_exptl_absorpt_correction_T_max 0.7456
_exptl_absorpt_process_details 'SADABS (Bruker, 2007)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 296(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 APEXII CCD area detector'
_diffrn_measurement_method \w-scans
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 20228
_diffrn_reflns_av_R_equivalents 0.0372
_diffrn_reflns_av_sigmaI/netI 0.0420
_diffrn_reflns_limit_h_min -24
_diffrn_reflns_limit_h_max 24
_diffrn_reflns_limit_k_min -29
_diffrn_reflns_limit_k_max 29
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_theta_min 1.65
_diffrn_reflns_theta_max 27.98
_reflns_number_total 5473
_reflns_number_gt 2692
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'APEX2 (Bruker 2007)'
_computing_cell_refinement 'APEX2 and SAINT (Bruker 2007)'
_computing_data_reduction SAINT
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
;
SHELXTL and PLATON (Spek, 2009)
;
_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^)+(0.0815P)^2^+8.4853P] 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 5473
_refine_ls_number_parameters 316
_refine_ls_number_restraints 66
_refine_ls_R_factor_all 0.1198
_refine_ls_R_factor_gt 0.0574
_refine_ls_wR_factor_ref 0.1868
_refine_ls_wR_factor_gt 0.1534
_refine_ls_goodness_of_fit_ref 1.042
_refine_ls_restrained_S_all 1.062
_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 0.51953(4) 0.57169(3) 0.64919(6) 0.0847(3) Uani 1 1 d . . .
Ag2 Ag 0.64420(6) 0.25986(3) 0.82663(7) 0.1181(4) Uani 1 1 d . . .
S1 S 0.39101(11) 0.44653(8) 0.50477(16) 0.0704(5) Uani 1 1 d . . .
F1 F 0.7812(5) 0.6582(5) 1.1385(8) 0.249(5) Uani 1 1 d DU . .
F2 F 0.7962(7) 0.6473(8) 0.9999(11) 0.303(7) Uani 1 1 d DU . .
F3 F 0.9094(5) 0.5861(7) 1.1937(12) 0.325(8) Uani 1 1 d DU . .
F4 F 0.8048(8) 0.5464(7) 1.1808(12) 0.293(7) Uani 1 1 d DU . .
F5 F 0.8143(7) 0.5271(8) 1.0489(11) 0.329(9) Uani 1 1 d DU . .
F6 F 0.4591(6) 0.1977(6) 0.9494(9) 0.226(5) Uani 1 1 d . . .
F7 F 0.5835(6) 0.1593(5) 1.1022(6) 0.237(5) Uani 1 1 d . . .
F8 F 0.4458(6) 0.1146(5) 0.8056(9) 0.222(4) Uani 1 1 d . . .
F9 F 0.5589(9) 0.0701(4) 0.9545(15) 0.278(8) Uani 1 1 d . . .
F10 F 0.4498(9) 0.0816(7) 0.9556(14) 0.292(7) Uani 1 1 d . . .
O1 O 0.6401(5) 0.5874(4) 0.8680(6) 0.141(3) Uani 1 1 d U . .
O2 O 0.6213(5) 0.6070(4) 1.0025(7) 0.133(2) Uani 1 1 d U . .
O3 O 0.5495(5) 0.2420(3) 0.8852(6) 0.133(2) Uani 1 1 d . . .
O4 O 0.6591(4) 0.1772(3) 0.9859(6) 0.118(2) Uani 1 1 d . . .
N1 N 0.5621(4) 0.4718(2) 0.6767(4) 0.0644(13) Uani 1 1 d . . .
N2 N 0.6179(4) 0.3548(3) 0.7479(5) 0.0763(15) Uani 1 1 d . . .
N3 N 0.3854(4) 0.3625(3) 0.3630(5) 0.0783(15) Uani 1 1 d . . .
N4 N 0.2441(4) 0.3001(3) 0.3302(5) 0.0782(16) Uani 1 1 d . . .
C1 C 0.5042(4) 0.4265(3) 0.6197(5) 0.0571(14) Uani 1 1 d . . .
C2 C 0.5326(5) 0.3676(3) 0.6574(6) 0.0712(18) Uani 1 1 d . . .
H2A H 0.4906 0.3366 0.6180 0.085 Uiso 1 1 calc R . .
C3 C 0.6761(5) 0.3997(4) 0.7991(6) 0.085(2) Uani 1 1 d . . .
H3A H 0.7372 0.3916 0.8597 0.102 Uiso 1 1 calc R . .
C4 C 0.6488(5) 0.4580(4) 0.7654(7) 0.083(2) Uani 1 1 d . . .
H4A H 0.6915 0.4886 0.8050 0.100 Uiso 1 1 calc R . .
C5 C 0.3482(4) 0.3796(3) 0.4161(5) 0.0617(15) Uani 1 1 d . . .
C6 C 0.2793(4) 0.3490(3) 0.3999(6) 0.0687(16) Uani 1 1 d . . .
H6A H 0.2558 0.3625 0.4384 0.082 Uiso 1 1 calc R . .
C7 C 0.2809(6) 0.2828(4) 0.2793(7) 0.092(2) Uani 1 1 d . . .
H7A H 0.2587 0.2485 0.2310 0.111 Uiso 1 1 calc R . .
C8 C 0.3515(6) 0.3137(4) 0.2952(7) 0.091(2) Uani 1 1 d . . .
H8A H 0.3754 0.2998 0.2574 0.110 Uiso 1 1 calc R . .
C9 C 0.6654(6) 0.6032(5) 0.9668(8) 0.100(2) Uani 1 1 d U . .
C10 C 0.7632(8) 0.6215(8) 1.0533(10) 0.154(4) Uani 1 1 d DU . .
C11 C 0.8223(10) 0.5717(10) 1.1081(16) 0.221(7) Uani 1 1 d DU . .
C12 C 0.5866(6) 0.1970(4) 0.9482(7) 0.091(2) Uani 1 1 d . . .
C13 C 0.5334(8) 0.1656(6) 0.9831(11) 0.132(4) Uani 1 1 d U . .
C14 C 0.5014(12) 0.1078(10) 0.9333(17) 0.171(5) Uani 1 1 d U . .
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 0.0770(4) 0.0830(4) 0.0985(5) -0.0024(3) 0.0564(4) -0.0032(3)
Ag2 0.1497(7) 0.1024(6) 0.1166(6) 0.0449(4) 0.0895(6) 0.0638(5)
S1 0.0604(9) 0.0600(9) 0.0765(11) 0.0005(8) 0.0351(9) -0.0006(8)
F1 0.145(6) 0.299(11) 0.173(7) -0.153(8) 0.033(5) -0.021(7)
F2 0.176(8) 0.460(19) 0.219(10) 0.038(12) 0.096(8) -0.125(10)
F3 0.067(4) 0.50(2) 0.277(11) -0.144(12) 0.042(6) -0.019(7)
F4 0.151(8) 0.371(17) 0.212(12) 0.034(11) 0.040(8) 0.021(9)
F5 0.153(8) 0.425(18) 0.215(11) -0.142(12) 0.016(7) 0.091(10)
F6 0.162(7) 0.328(14) 0.217(9) 0.021(9) 0.132(7) 0.071(8)
F7 0.229(9) 0.342(13) 0.096(5) 0.047(6) 0.078(6) -0.058(9)
F8 0.158(7) 0.269(11) 0.173(8) -0.048(8) 0.070(6) -0.051(7)
F9 0.241(12) 0.139(7) 0.44(2) 0.042(9) 0.206(15) 0.035(7)
F10 0.251(13) 0.344(16) 0.350(17) 0.004(12) 0.220(13) -0.096(11)
O1 0.125(5) 0.180(7) 0.075(4) -0.029(4) 0.040(4) -0.033(5)
O2 0.110(5) 0.164(6) 0.132(5) -0.026(5) 0.078(4) -0.011(4)
O3 0.145(6) 0.120(5) 0.110(5) 0.038(4) 0.067(5) 0.061(5)
O4 0.091(4) 0.128(5) 0.126(5) 0.007(4) 0.064(4) 0.023(4)
N1 0.064(3) 0.068(3) 0.058(3) -0.004(3) 0.036(3) -0.006(3)
N2 0.071(4) 0.082(4) 0.059(3) 0.004(3) 0.032(3) 0.008(3)
N3 0.081(4) 0.077(4) 0.076(4) -0.003(3) 0.048(3) -0.003(3)
N4 0.077(4) 0.077(4) 0.066(3) -0.013(3) 0.037(3) -0.017(3)
C1 0.061(3) 0.063(4) 0.050(3) 0.003(3) 0.036(3) -0.004(3)
C2 0.068(4) 0.071(4) 0.063(4) 0.008(3) 0.035(4) 0.003(3)
C3 0.065(4) 0.109(6) 0.059(4) 0.003(4) 0.028(4) 0.011(5)
C4 0.062(4) 0.095(6) 0.073(5) -0.009(4) 0.032(4) -0.011(4)
C5 0.058(3) 0.062(4) 0.054(3) 0.004(3) 0.029(3) 0.001(3)
C6 0.062(4) 0.068(4) 0.064(4) 0.001(3) 0.033(3) -0.002(3)
C7 0.110(6) 0.082(5) 0.080(5) -0.023(4) 0.056(5) -0.015(5)
C8 0.096(6) 0.099(6) 0.085(5) -0.021(5) 0.058(5) -0.015(5)
C9 0.080(5) 0.131(6) 0.075(5) -0.024(4) 0.041(4) -0.031(5)
C10 0.085(6) 0.269(12) 0.095(6) -0.046(8) 0.049(6) -0.025(7)
C11 0.087(8) 0.355(16) 0.151(12) -0.087(12) 0.038(9) -0.002(10)
C12 0.088(6) 0.096(6) 0.065(5) 0.002(4) 0.035(5) 0.013(5)
C13 0.116(8) 0.145(10) 0.105(8) 0.024(7) 0.053(7) 0.015(8)
C14 0.145(11) 0.191(14) 0.167(12) 0.032(11) 0.091(10) -0.005(11)
_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 O2 2.275(7) 2_656 ?
Ag1 N1 2.318(5) . ?
Ag1 N3 2.397(6) 5_666 ?
Ag1 O1 2.453(6) . ?
Ag1 Ag1 3.3126(12) 2_656 ?
Ag2 N4 2.278(6) 8_556 ?
Ag2 N2 2.294(6) . ?
Ag2 O3 2.403(9) . ?
S1 C1 1.753(6) . ?
S1 C5 1.782(7) . ?
F1 C10 1.304(12) . ?
F2 C10 1.354(12) . ?
F3 C11 1.338(14) . ?
F4 C11 1.364(16) . ?
F5 C11 1.241(15) . ?
F6 C13 1.368(13) . ?
F7 C13 1.315(12) . ?
F8 C14 1.409(18) . ?
F9 C14 1.251(19) . ?
F10 C14 1.324(17) . ?
O1 C9 1.198(10) . ?
O2 C9 1.203(11) . ?
O2 Ag1 2.275(7) 2_656 ?
O3 C12 1.228(10) . ?
O4 C12 1.200(10) . ?
N1 C1 1.328(8) . ?
N1 C4 1.337(9) . ?
N2 C2 1.319(8) . ?
N2 C3 1.320(10) . ?
N3 C8 1.320(9) . ?
N3 C5 1.348(8) . ?
N3 Ag1 2.397(6) 5_666 ?
N4 C7 1.318(10) . ?
N4 C6 1.333(8) . ?
N4 Ag2 2.278(6) 8_455 ?
C1 C2 1.395(9) . ?
C2 H2A 0.9300 . ?
C3 C4 1.370(11) . ?
C3 H3A 0.9300 . ?
C4 H4A 0.9300 . ?
C5 C6 1.352(9) . ?
C6 H6A 0.9300 . ?
C7 C8 1.384(11) . ?
C7 H7A 0.9300 . ?
C8 H8A 0.9300 . ?
C9 C10 1.502(13) . ?
C10 C11 1.41(2) . ?
C12 C13 1.525(15) . ?
C13 C14 1.41(2) . ?
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 Ag1 N1 124.8(3) 2_656 . ?
O2 Ag1 N3 102.2(2) 2_656 5_666 ?
N1 Ag1 N3 113.9(2) . 5_666 ?
O2 Ag1 O1 139.1(3) 2_656 . ?
N1 Ag1 O1 88.4(2) . . ?
N3 Ag1 O1 81.1(2) 5_666 . ?
O2 Ag1 Ag1 92.8(2) 2_656 2_656 ?
N1 Ag1 Ag1 95.37(12) . 2_656 ?
N3 Ag1 Ag1 128.65(15) 5_666 2_656 ?
O1 Ag1 Ag1 57.5(2) . 2_656 ?
N4 Ag2 N2 118.9(2) 8_556 . ?
N4 Ag2 O3 131.8(2) 8_556 . ?
N2 Ag2 O3 109.2(2) . . ?
C1 S1 C5 101.1(3) . . ?
C9 O1 Ag1 151.2(8) . . ?
C9 O2 Ag1 107.0(6) . 2_656 ?
C12 O3 Ag2 99.6(6) . . ?
C1 N1 C4 117.2(6) . . ?
C1 N1 Ag1 124.1(4) . . ?
C4 N1 Ag1 118.2(5) . . ?
C2 N2 C3 117.6(6) . . ?
C2 N2 Ag2 115.6(5) . . ?
C3 N2 Ag2 125.5(5) . . ?
C8 N3 C5 116.2(7) . . ?
C8 N3 Ag1 120.4(5) . 5_666 ?
C5 N3 Ag1 121.8(5) . 5_666 ?
C7 N4 C6 116.3(7) . . ?
C7 N4 Ag2 120.9(5) . 8_455 ?
C6 N4 Ag2 121.8(5) . 8_455 ?
N1 C1 C2 120.7(6) . . ?
N1 C1 S1 115.8(5) . . ?
C2 C1 S1 123.3(5) . . ?
N2 C2 C1 121.3(6) . . ?
N2 C2 H2A 119.4 . . ?
C1 C2 H2A 119.4 . . ?
N2 C3 C4 121.8(7) . . ?
N2 C3 H3A 119.1 . . ?
C4 C3 H3A 119.1 . . ?
N1 C4 C3 121.2(7) . . ?
N1 C4 H4A 119.4 . . ?
C3 C4 H4A 119.4 . . ?
N3 C5 C6 122.2(6) . . ?
N3 C5 S1 116.9(5) . . ?
C6 C5 S1 120.9(5) . . ?
N4 C6 C5 121.8(7) . . ?
N4 C6 H6A 119.1 . . ?
C5 C6 H6A 119.1 . . ?
N4 C7 C8 122.4(7) . . ?
N4 C7 H7A 118.8 . . ?
C8 C7 H7A 118.8 . . ?
N3 C8 C7 121.1(8) . . ?
N3 C8 H8A 119.5 . . ?
C7 C8 H8A 119.5 . . ?
O1 C9 O2 127.6(9) . . ?
O1 C9 C10 115.0(9) . . ?
O2 C9 C10 117.5(9) . . ?
F1 C10 F2 106.6(15) . . ?
F1 C10 C11 109.0(12) . . ?
F2 C10 C11 99.2(14) . . ?
F1 C10 C9 113.6(10) . . ?
F2 C10 C9 114.9(10) . . ?
C11 C10 C9 112.5(13) . . ?
F5 C11 F3 111.3(16) . . ?
F5 C11 F4 100.2(19) . . ?
F3 C11 F4 99.2(16) . . ?
F5 C11 C10 122.5(16) . . ?
F3 C11 C10 114.3(17) . . ?
F4 C11 C10 105.0(15) . . ?
O4 C12 O3 127.1(10) . . ?
O4 C12 C13 118.7(9) . . ?
O3 C12 C13 114.2(9) . . ?
F7 C13 F6 105.8(12) . . ?
F7 C13 C14 106.2(13) . . ?
F6 C13 C14 106.0(14) . . ?
F7 C13 C12 110.7(10) . . ?
F6 C13 C12 112.3(11) . . ?
C14 C13 C12 115.3(13) . . ?
F9 C14 F10 107.3(18) . . ?
F9 C14 F8 103.2(19) . . ?
F10 C14 F8 105.5(15) . . ?
F9 C14 C13 117.1(17) . . ?
F10 C14 C13 116.0(19) . . ?
F8 C14 C13 106.3(14) . . ?
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
O2 Ag1 O1 C9 23.8(18) 2_656 . . . ?
N1 Ag1 O1 C9 -123.4(16) . . . . ?
N3 Ag1 O1 C9 122.1(16) 5_666 . . . ?
Ag1 Ag1 O1 C9 -26.1(15) 2_656 . . . ?
N4 Ag2 O3 C12 17.2(7) 8_556 . . . ?
N2 Ag2 O3 C12 -165.4(5) . . . . ?
O2 Ag1 N1 C1 -12.2(6) 2_656 . . . ?
N3 Ag1 N1 C1 -138.3(4) 5_666 . . . ?
O1 Ag1 N1 C1 142.2(5) . . . . ?
Ag1 Ag1 N1 C1 85.0(4) 2_656 . . . ?
O2 Ag1 N1 C4 175.9(5) 2_656 . . . ?
N3 Ag1 N1 C4 49.8(5) 5_666 . . . ?
O1 Ag1 N1 C4 -29.7(5) . . . . ?
Ag1 Ag1 N1 C4 -86.9(5) 2_656 . . . ?
N4 Ag2 N2 C2 123.4(5) 8_556 . . . ?
O3 Ag2 N2 C2 -54.3(5) . . . . ?
N4 Ag2 N2 C3 -70.2(6) 8_556 . . . ?
O3 Ag2 N2 C3 112.1(6) . . . . ?
C4 N1 C1 C2 4.4(9) . . . . ?
Ag1 N1 C1 C2 -167.6(4) . . . . ?
C4 N1 C1 S1 179.5(5) . . . . ?
Ag1 N1 C1 S1 7.5(6) . . . . ?
C5 S1 C1 N1 158.1(4) . . . . ?
C5 S1 C1 C2 -26.8(6) . . . . ?
C3 N2 C2 C1 -2.0(9) . . . . ?
Ag2 N2 C2 C1 165.5(5) . . . . ?
N1 C1 C2 N2 -2.2(9) . . . . ?
S1 C1 C2 N2 -177.0(5) . . . . ?
C2 N2 C3 C4 3.9(11) . . . . ?
Ag2 N2 C3 C4 -162.2(6) . . . . ?
C1 N1 C4 C3 -2.5(10) . . . . ?
Ag1 N1 C4 C3 169.9(6) . . . . ?
N2 C3 C4 N1 -1.7(12) . . . . ?
C8 N3 C5 C6 -0.9(10) . . . . ?
Ag1 N3 C5 C6 164.7(5) 5_666 . . . ?
C8 N3 C5 S1 -178.4(6) . . . . ?
Ag1 N3 C5 S1 -12.8(7) 5_666 . . . ?
C1 S1 C5 N3 -62.5(5) . . . . ?
C1 S1 C5 C6 119.9(5) . . . . ?
C7 N4 C6 C5 0.8(10) . . . . ?
Ag2 N4 C6 C5 170.0(5) 8_455 . . . ?
N3 C5 C6 N4 0.0(10) . . . . ?
S1 C5 C6 N4 177.4(5) . . . . ?
C6 N4 C7 C8 -0.9(12) . . . . ?
Ag2 N4 C7 C8 -170.2(6) 8_455 . . . ?
C5 N3 C8 C7 0.8(11) . . . . ?
Ag1 N3 C8 C7 -165.0(6) 5_666 . . . ?
N4 C7 C8 N3 0.0(13) . . . . ?
Ag1 O1 C9 O2 23(2) . . . . ?
Ag1 O1 C9 C10 -155.8(13) . . . . ?
Ag1 O2 C9 O1 4.1(15) 2_656 . . . ?
Ag1 O2 C9 C10 -177.4(10) 2_656 . . . ?
O1 C9 C10 F1 155.9(13) . . . . ?
O2 C9 C10 F1 -22.9(19) . . . . ?
O1 C9 C10 F2 33(2) . . . . ?
O2 C9 C10 F2 -146.0(14) . . . . ?
O1 C9 C10 C11 -79.7(15) . . . . ?
O2 C9 C10 C11 101.6(15) . . . . ?
F1 C10 C11 F5 172.9(19) . . . . ?
F2 C10 C11 F5 -76(2) . . . . ?
C9 C10 C11 F5 46(3) . . . . ?
F1 C10 C11 F3 -48(2) . . . . ?
F2 C10 C11 F3 63.6(18) . . . . ?
C9 C10 C11 F3 -174.5(13) . . . . ?
F1 C10 C11 F4 60.1(16) . . . . ?
F2 C10 C11 F4 171.2(11) . . . . ?
C9 C10 C11 F4 -66.9(14) . . . . ?
Ag2 O3 C12 O4 12.7(10) . . . . ?
Ag2 O3 C12 C13 -169.3(7) . . . . ?
O4 C12 C13 F7 53.0(15) . . . . ?
O3 C12 C13 F7 -125.2(11) . . . . ?
O4 C12 C13 F6 170.9(9) . . . . ?
O3 C12 C13 F6 -7.3(14) . . . . ?
O4 C12 C13 C14 -67.5(14) . . . . ?
O3 C12 C13 C14 114.3(13) . . . . ?
F7 C13 C14 F9 -67(2) . . . . ?
F6 C13 C14 F9 -179.0(16) . . . . ?
C12 C13 C14 F9 56(2) . . . . ?
F7 C13 C14 F10 61.6(19) . . . . ?
F6 C13 C14 F10 -50.6(18) . . . . ?
C12 C13 C14 F10 -175.4(13) . . . . ?
F7 C13 C14 F8 178.5(12) . . . . ?
F6 C13 C14 F8 66.3(16) . . . . ?
C12 C13 C14 F8 -58.5(17) . . . . ?
_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full 27.98
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max 1.027
_refine_diff_density_min -1.507
_refine_diff_density_rms 0.090
##########################End############################
_database_code_depnum_ccdc_archive 'CCDC 926723'