# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2011
# Attachment '- 1-6-crystaldata.CIF'
data_publication_text
#TrackingRef '- 1-6-crystaldata.CIF'
_publ_contact_author_name 'Christoph Janiak'
_publ_contact_author_address
;Institut f\"ur Anorganische Chemie und Strukturchemie
Universit\"at D\"usseldorf
Universit\"atsstr. 1
40225 D\"usseldorf
Germany
;
_publ_contact_author_email janiak@uni-duesseldorf.de
_publ_contact_author_phone +49-211-8112286
loop_
_publ_author_name
_publ_author_address
A.B.Caballero
;Departamento de Qu\'imica Inorg\'anica
Universidad de Granada
Severo Ochoa, s/n
E-18071 Granada
Spain
;
J.K.Vieth
;Institut f\"ur Anorganische und Analytische Chemie
Universit\"at Freiburg
Albertstr. 21
79104 Freiburg
Germany
;
A.Rodriguez-Dieguez
;Departamento de Qu\'imica Inorg\'anica
Universidad de Granada
Severo Ochoa, s/n
E-18071 Granada
Spain
;
I.Vidal
;Departamento de Qu\'imica Org\'anica
Universidad de Granada
Severo Ochoa, s/n
E-18071 Granada
Spain
;
;
J.A.Dobado
;
;Departamento de Qu\'imica Org\'anica
Universidad de Granada
Severo Ochoa, s/n
E-18071 Granada
Spain
;
J.M.Salas
;Departamento de Qu\'imica Inorg\'anica
Universidad de Granada
Severo Ochoa, s/n
E-18071 Granada
Spain
;
C.Janiak
;Institut f\"ur Anorganische Chemie und Strukturchemie
Universit\"at D\"usseldorf
Universit\"atsstr. 1
40225 D\"usseldorf
Germany
;
_publ_requested_journal XXXXX
_publ_section_title
;
Dinuclear silver(I) complexes for the design of metal-ligand networks
based on triazolopyrimidines
;
#==============================================================================
data_AC15
_database_code_depnum_ccdc_archive 'CCDC 819202'
#TrackingRef '- 1-6-crystaldata.CIF'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
[tetrakisacetonitrile-bis(\m-1,2,4-triazolo[1,5-a]pyrimidine)disilver(I)]
bis(tetrafluoroborate)
;
_chemical_name_common
;
(tetrakisacetonitrile-bis(mu-1,2,4-triazolo(1,5-
a)pyrimidine)disilver(i)) bis(tetrafluoroborate)
;
_chemical_melting_point ?
_chemical_formula_moiety 'C18 H20 Ag2 N12, 2(B F4)'
_chemical_formula_sum 'C18 H20 Ag2 B2 F8 N12'
_chemical_formula_weight 793.82
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'
Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 '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'
N N 0.0061 0.0033 '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'
_symmetry_space_group_name_Hall '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 6.2201(2)
_cell_length_b 10.6272(2)
_cell_length_c 11.5588(8)
_cell_angle_alpha 110.016(8)
_cell_angle_beta 99.817(7)
_cell_angle_gamma 91.442(6)
_cell_volume 704.51(6)
_cell_formula_units_Z 1
_cell_measurement_temperature 113(2)
_cell_measurement_reflns_used 61337
_cell_measurement_theta_min 3.4
_cell_measurement_theta_max 45.8
_exptl_crystal_description block
_exptl_crystal_colour colourless
_exptl_crystal_size_max 0.20
_exptl_crystal_size_mid 0.11
_exptl_crystal_size_min 0.10
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.871
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 388
_exptl_absorpt_coefficient_mu 1.476
_exptl_absorpt_correction_type Multi-scan
_exptl_absorpt_correction_T_min 0.7567
_exptl_absorpt_correction_T_max 0.8725
_exptl_absorpt_process_details '(ABSCOR; Higashi, 1995)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 113(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 'Rigaku R-axis Spider Image plate 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 33624
_diffrn_reflns_av_R_equivalents 0.0330
_diffrn_reflns_av_sigmaI/netI 0.0250
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_limit_l_max 17
_diffrn_reflns_theta_min 3.26
_diffrn_reflns_theta_max 33.14
_reflns_number_total 5349
_reflns_number_gt 4679
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'd*trek, CrystalClear (Rigaku, 2007)'
_computing_cell_refinement 'Fsproc, CrystalClear (Rigaku, 2007)'
_computing_data_reduction 'Fsproc, CrystalClear (Rigaku, 2007)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics 'DIAMOND (Crystal Impact, 2009)'
_computing_publication_material ?
_publ_section_references
;
Crystal Impact (2009). DIAMOND. Version3.2. Crystal Impact GbR, Bonn,
Germany.
Higashi, T. (1995). ABSCOR. Rigaku Corporation, Tokyo, Japan.
Rigaku (2007). CrystalClear (Version SM Expert 2.0 r1).
Rigaku Corporation, Tokyo, Japan.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112--122.
;
_publ_section_exptl_refinement
;
Hydrogen atoms for aromatic CH, aliphatic CH, CH~2~ and methyl groups
were positioned geometrically (C---H = 0.94 \%A for
aromatic CH, C---H = 0.99 \%A for aliphatic CH, C---H = 0.98 \%A for CH~2~,
C---H = 0.97 \%A for CH~3~) and refined using a
riding model (AFIX 43 for aromatic CH, AFIX 13 for aliphatic CH,
AFIX 23 for CH~2~, AFIX 33 or rotating group refinement 137 for CH~3~),
with U~iso~(H) = 1.2U~eq~(CH) and U~iso~(H) = 1.5U~eq~(CH~3~).
;
_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^)+(0.0095P)^2^+0.5767P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 5349
_refine_ls_number_parameters 192
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0333
_refine_ls_R_factor_gt 0.0260
_refine_ls_wR_factor_ref 0.0469
_refine_ls_wR_factor_gt 0.0445
_refine_ls_goodness_of_fit_ref 1.145
_refine_ls_restrained_S_all 1.145
_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
Ag Ag 0.830421(19) 0.387818(12) 0.405267(12) 0.01624(3) Uani 1 1 d . . .
N1 N 0.7546(2) 0.91121(13) 0.51574(13) 0.0186(3) Uani 1 1 d . . .
C2 C 0.9360(2) 0.86510(15) 0.55821(15) 0.0180(3) Uani 1 1 d . . .
H21 H 1.0624 0.9231 0.6071 0.022 Uiso 1 1 calc R . .
N3 N 0.9291(2) 0.72889(12) 0.52703(12) 0.0143(2) Uani 1 1 d . . .
C3A C 0.7274(2) 0.68630(14) 0.45974(13) 0.0128(2) Uani 1 1 d . . .
N4 N 0.6326(2) 0.55981(12) 0.40569(12) 0.0139(2) Uani 1 1 d . . .
C5 C 0.4266(2) 0.54631(15) 0.34491(14) 0.0159(3) Uani 1 1 d . . .
H51 H 0.3542 0.4583 0.3056 0.019 Uiso 1 1 calc R . .
C6 C 0.3103(2) 0.65561(15) 0.33570(14) 0.0163(3) Uani 1 1 d . . .
H61 H 0.1626 0.6408 0.2922 0.020 Uiso 1 1 calc R . .
C7 C 0.4116(2) 0.78317(15) 0.38988(14) 0.0162(3) Uani 1 1 d . . .
H71 H 0.3395 0.8592 0.3841 0.019 Uiso 1 1 calc R . .
N8 N 0.6207(2) 0.79507(12) 0.45228(12) 0.0140(2) Uani 1 1 d . . .
N11 N 0.9394(3) 0.35868(19) 0.19869(16) 0.0375(4) Uani 1 1 d . . .
C11 C 0.8559(3) 0.36883(19) 0.10715(17) 0.0262(3) Uani 1 1 d . . .
C12 C 0.7492(3) 0.3822(2) -0.00966(18) 0.0331(4) Uani 1 1 d . . .
H121 H 0.5915 0.3577 -0.0236 0.050 Uiso 1 1 calc R . .
H122 H 0.8100 0.3224 -0.0793 0.050 Uiso 1 1 calc R . .
H123 H 0.7742 0.4754 -0.0048 0.050 Uiso 1 1 calc R . .
N21 N 0.5149(2) 0.22252(15) 0.30291(15) 0.0279(3) Uani 1 1 d . . .
C21 C 0.4065(3) 0.14194(18) 0.22132(17) 0.0253(3) Uani 1 1 d . . .
C22 C 0.2670(4) 0.0393(2) 0.1154(2) 0.0446(6) Uani 1 1 d . . .
H221 H 0.3514 -0.0366 0.0806 0.067 Uiso 1 1 calc R . .
H222 H 0.2130 0.0773 0.0508 0.067 Uiso 1 1 calc R . .
H223 H 0.1425 0.0083 0.1435 0.067 Uiso 1 1 calc R . .
F1 F 0.23263(18) 0.32109(10) 0.79326(10) 0.0282(2) Uani 1 1 d . . .
F2 F -0.01278(18) 0.14924(11) 0.77067(12) 0.0349(3) Uani 1 1 d . . .
F3 F 0.3482(2) 0.11608(12) 0.78015(13) 0.0380(3) Uani 1 1 d . . .
F4 F 0.2283(2) 0.24631(14) 0.95427(11) 0.0395(3) Uani 1 1 d . . .
B B 0.2006(3) 0.20728(19) 0.82458(18) 0.0201(3) 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
Ag 0.01438(5) 0.01284(5) 0.02100(6) 0.00688(4) -0.00031(4) 0.00375(4)
N1 0.0165(6) 0.0118(6) 0.0261(7) 0.0064(5) 0.0003(5) 0.0019(5)
C2 0.0165(6) 0.0135(7) 0.0232(7) 0.0066(6) 0.0015(5) 0.0022(5)
N3 0.0138(5) 0.0121(5) 0.0172(6) 0.0059(5) 0.0015(4) 0.0030(4)
C3A 0.0140(6) 0.0124(6) 0.0140(6) 0.0062(5) 0.0038(5) 0.0052(5)
N4 0.0137(5) 0.0121(5) 0.0161(6) 0.0054(5) 0.0023(4) 0.0020(4)
C5 0.0153(6) 0.0141(6) 0.0179(7) 0.0061(5) 0.0015(5) 0.0018(5)
C6 0.0137(6) 0.0174(7) 0.0184(7) 0.0078(6) 0.0013(5) 0.0032(5)
C7 0.0142(6) 0.0168(7) 0.0192(7) 0.0085(6) 0.0026(5) 0.0056(5)
N8 0.0142(5) 0.0106(5) 0.0171(6) 0.0054(5) 0.0020(4) 0.0033(4)
N11 0.0425(10) 0.0476(11) 0.0246(8) 0.0128(8) 0.0121(7) 0.0037(8)
C11 0.0237(8) 0.0274(9) 0.0237(8) 0.0025(7) 0.0084(6) -0.0004(7)
C12 0.0294(9) 0.0343(10) 0.0264(9) 0.0032(8) -0.0036(7) 0.0063(8)
N21 0.0244(7) 0.0230(7) 0.0332(8) 0.0082(6) 0.0014(6) -0.0037(6)
C21 0.0245(8) 0.0218(8) 0.0311(9) 0.0140(7) 0.0002(7) -0.0022(6)
C22 0.0531(13) 0.0349(11) 0.0355(11) 0.0140(9) -0.0187(10) -0.0203(10)
F1 0.0365(6) 0.0218(5) 0.0303(5) 0.0126(4) 0.0102(5) 0.0032(4)
F2 0.0224(5) 0.0281(6) 0.0468(7) 0.0089(5) -0.0032(5) -0.0025(4)
F3 0.0336(6) 0.0331(6) 0.0527(8) 0.0184(6) 0.0138(5) 0.0186(5)
F4 0.0432(7) 0.0564(8) 0.0229(5) 0.0200(6) 0.0045(5) 0.0017(6)
B 0.0198(8) 0.0202(8) 0.0215(8) 0.0092(7) 0.0025(6) 0.0034(6)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ag N3 2.1786(12) 2_766 ?
Ag N4 2.2281(12) . ?
Ag N21 2.4393(15) . ?
Ag N11 2.5127(16) . ?
Ag Ag 3.0868(4) 2_766 ?
N1 C2 1.3260(19) . ?
N1 N8 1.3692(18) . ?
C2 N3 1.3644(19) . ?
C2 H21 0.9500 . ?
N3 C3A 1.3351(18) . ?
N3 Ag 2.1786(12) 2_766 ?
C3A N4 1.3433(19) . ?
C3A N8 1.3679(17) . ?
N4 C5 1.3305(18) . ?
C5 C6 1.409(2) . ?
C5 H51 0.9500 . ?
C6 C7 1.367(2) . ?
C6 H61 0.9500 . ?
C7 N8 1.3556(18) . ?
C7 H71 0.9500 . ?
N11 C11 1.138(2) . ?
C11 C12 1.454(3) . ?
C12 H121 0.9800 . ?
C12 H122 0.9800 . ?
C12 H123 0.9800 . ?
N21 C21 1.131(2) . ?
C21 C22 1.455(3) . ?
C22 H221 0.9800 . ?
C22 H222 0.9800 . ?
C22 H223 0.9800 . ?
F1 B 1.395(2) . ?
F2 B 1.394(2) . ?
F3 B 1.382(2) . ?
F4 B 1.390(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
N3 Ag N4 159.12(5) 2_766 . ?
N3 Ag N21 102.45(5) 2_766 . ?
N4 Ag N21 92.84(5) . . ?
N3 Ag N11 98.93(6) 2_766 . ?
N4 Ag N11 94.71(6) . . ?
N21 Ag N11 91.59(6) . . ?
N3 Ag Ag 78.52(3) 2_766 2_766 ?
N4 Ag Ag 83.04(3) . 2_766 ?
N21 Ag Ag 164.87(4) . 2_766 ?
N11 Ag Ag 103.23(4) . 2_766 ?
C2 N1 N8 101.92(12) . . ?
N1 C2 N3 115.55(14) . . ?
N1 C2 H21 122.2 . . ?
N3 C2 H21 122.2 . . ?
C3A N3 C2 103.30(12) . . ?
C3A N3 Ag 127.97(10) . 2_766 ?
C2 N3 Ag 128.12(10) . 2_766 ?
N3 C3A N4 128.59(13) . . ?
N3 C3A N8 108.96(12) . . ?
N4 C3A N8 122.45(13) . . ?
C5 N4 C3A 115.90(12) . . ?
C5 N4 Ag 124.02(10) . . ?
C3A N4 Ag 119.78(9) . . ?
N4 C5 C6 123.48(14) . . ?
N4 C5 H51 118.3 . . ?
C6 C5 H51 118.3 . . ?
C7 C6 C5 119.48(13) . . ?
C7 C6 H61 120.3 . . ?
C5 C6 H61 120.3 . . ?
N8 C7 C6 116.20(13) . . ?
N8 C7 H71 121.9 . . ?
C6 C7 H71 121.9 . . ?
C7 N8 C3A 122.48(13) . . ?
C7 N8 N1 127.26(12) . . ?
C3A N8 N1 110.27(12) . . ?
C11 N11 Ag 135.01(16) . . ?
N11 C11 C12 179.8(2) . . ?
C11 C12 H121 109.5 . . ?
C11 C12 H122 109.5 . . ?
H121 C12 H122 109.5 . . ?
C11 C12 H123 109.5 . . ?
H121 C12 H123 109.5 . . ?
H122 C12 H123 109.5 . . ?
C21 N21 Ag 155.29(15) . . ?
N21 C21 C22 179.3(2) . . ?
C21 C22 H221 109.5 . . ?
C21 C22 H222 109.5 . . ?
H221 C22 H222 109.5 . . ?
C21 C22 H223 109.5 . . ?
H221 C22 H223 109.5 . . ?
H222 C22 H223 109.5 . . ?
F3 B F4 110.37(14) . . ?
F3 B F2 109.80(15) . . ?
F4 B F2 109.25(15) . . ?
F3 B F1 110.02(14) . . ?
F4 B F1 108.76(15) . . ?
F2 B F1 108.60(14) . . ?
_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full 33.14
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max 1.392
_refine_diff_density_min -0.972
_refine_diff_density_rms 0.116
#===END
data_AC84
_database_code_depnum_ccdc_archive 'CCDC 819203'
#TrackingRef '- 1-6-crystaldata.CIF'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
[tetrakisacetonitrile-bis(\m-1,2,4-triazolo[1,5-a]pyrimidine)disilver(I)]
bis(perchlorate)
;
_chemical_name_common
;
(tetrakisacetonitrile-bis(mu-1,2,4-triazolo(1,5-
a)pyrimidine)disilver(i)) bis(perchlorate)
;
_chemical_melting_point ?
_chemical_formula_moiety 'C18 H20 Ag2 N12, 2(Cl O4)'
_chemical_formula_sum 'C18 H20 Ag2 Cl2 N12 O8'
_chemical_formula_weight 819.10
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'
Ag Ag -0.8971 1.1015 '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'
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'
_symmetry_cell_setting triclinic
_symmetry_space_group_name_H-M 'P -1'
_symmetry_space_group_name_Hall '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 6.32530(10)
_cell_length_b 10.7545(2)
_cell_length_c 11.5478(8)
_cell_angle_alpha 110.093(8)
_cell_angle_beta 100.489(7)
_cell_angle_gamma 90.426(6)
_cell_volume 723.32(5)
_cell_formula_units_Z 1
_cell_measurement_temperature 123(2)
_cell_measurement_reflns_used 58005
_cell_measurement_theta_min 3.2
_cell_measurement_theta_max 41.1
_exptl_crystal_description Prism
_exptl_crystal_colour Colorless
_exptl_crystal_size_max 0.21
_exptl_crystal_size_mid 0.11
_exptl_crystal_size_min 0.09
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.880
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 404
_exptl_absorpt_coefficient_mu 1.602
_exptl_absorpt_correction_type Multi-Scan
_exptl_absorpt_correction_T_min 0.7296
_exptl_absorpt_correction_T_max 0.8692
_exptl_absorpt_process_details '(ABSCOR; Higashi, 1995)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 123(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 'Rigaku R-axis Spider Image plate 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 73832
_diffrn_reflns_av_R_equivalents 0.0362
_diffrn_reflns_av_sigmaI/netI 0.0365
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_k_min -18
_diffrn_reflns_limit_k_max 19
_diffrn_reflns_limit_l_min -21
_diffrn_reflns_limit_l_max 21
_diffrn_reflns_theta_min 3.24
_diffrn_reflns_theta_max 41.13
_reflns_number_total 9586
_reflns_number_gt 7488
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'd*trek, CrystalClear (Rigaku, 2007)'
_computing_cell_refinement 'Fsproc, CrystalClear (Rigaku, 2007)'
_computing_data_reduction 'Fsproc, CrystalClear (Rigaku, 2007)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics 'DIAMOND (Crystal Impact, 2009)'
_computing_publication_material ?
_publ_section_references
;
Crystal Impact (2009). DIAMOND. Version3.2. Crystal Impact GbR, Bonn,
Germany.
Higashi, T. (1995). ABSCOR. Rigaku Corporation, Tokyo, Japan.
Rigaku (2007). CrystalClear (Version SM Expert 2.0 r1).
Rigaku Corporation, Tokyo, Japan.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112--122.
;
_publ_section_exptl_refinement
;
Hydrogen atoms for aromatic CH, aliphatic CH, CH~2~ and methyl groups
were positioned geometrically (C---H = 0.94 \%A for
aromatic CH, C---H = 0.99 \%A for aliphatic CH, C---H = 0.98 \%A for CH~2~,
C---H = 0.97 \%A for CH~3~) and refined using a
riding model (AFIX 43 for aromatic CH, AFIX 13 for aliphatic CH,
AFIX 23 for CH~2~, AFIX 33 or rotating group refinement 137 for CH~3~),
with U~iso~(H) = 1.2U~eq~(CH) and U~iso~(H) = 1.5U~eq~(CH~3~).
;
_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^)+(0.0299P)^2^+1.5795P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 9586
_refine_ls_number_parameters 192
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0720
_refine_ls_R_factor_gt 0.0485
_refine_ls_wR_factor_ref 0.1016
_refine_ls_wR_factor_gt 0.0876
_refine_ls_goodness_of_fit_ref 1.079
_refine_ls_restrained_S_all 1.079
_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
Ag Ag 0.83137(2) 0.390209(15) 0.405003(16) 0.01971(4) Uani 1 1 d . . .
N11 N 0.9528(5) 0.3690(3) 0.2034(2) 0.0412(6) Uani 1 1 d . . .
C11 C 0.8647(4) 0.3754(3) 0.1107(3) 0.0324(5) Uani 1 1 d . . .
C12 C 0.7517(6) 0.3857(4) -0.0072(3) 0.0467(8) Uani 1 1 d . . .
H12A H 0.8003 0.4694 -0.0136 0.070 Uiso 1 1 calc R . .
H12B H 0.5961 0.3836 -0.0092 0.070 Uiso 1 1 calc R . .
H12C H 0.7828 0.3110 -0.0779 0.070 Uiso 1 1 calc R . .
N21 N 0.5230(4) 0.2291(2) 0.2980(2) 0.0323(4) Uani 1 1 d . . .
C21 C 0.4086(4) 0.1499(2) 0.2202(2) 0.0280(4) Uani 1 1 d . . .
C22 C 0.2606(6) 0.0500(3) 0.1206(3) 0.0433(7) Uani 1 1 d . . .
H22A H 0.1658 0.0927 0.0709 0.052 Uiso 1 1 calc R . .
H22B H 0.1734 0.0035 0.1574 0.052 Uiso 1 1 calc R . .
H22C H 0.3423 -0.0138 0.0662 0.052 Uiso 1 1 calc R . .
N1 N 0.7522(3) 0.90890(18) 0.5216(2) 0.0232(3) Uani 1 1 d . . .
C2 C 0.9330(3) 0.8617(2) 0.5612(2) 0.0222(4) Uani 1 1 d . . .
H21 H 1.0583 0.9178 0.6091 0.027 Uiso 1 1 calc R . .
N3 N 0.9273(3) 0.72709(17) 0.52883(16) 0.0176(3) Uani 1 1 d . . .
C3A C 0.7278(3) 0.68667(18) 0.46390(18) 0.0153(3) Uani 1 1 d . . .
N4 N 0.6344(3) 0.56270(16) 0.40913(16) 0.0157(3) Uani 1 1 d . . .
C5 C 0.4303(3) 0.55088(19) 0.34967(19) 0.0182(3) Uani 1 1 d . . .
H51 H 0.3598 0.4643 0.3098 0.022 Uiso 1 1 calc R . .
C6 C 0.3129(3) 0.6595(2) 0.3426(2) 0.0192(3) Uani 1 1 d . . .
H61 H 0.1667 0.6459 0.2999 0.023 Uiso 1 1 calc R . .
C7 C 0.4125(3) 0.7855(2) 0.3983(2) 0.0195(3) Uani 1 1 d . . .
H71 H 0.3401 0.8615 0.3944 0.023 Uiso 1 1 calc R . .
N8 N 0.6197(3) 0.79520(16) 0.45902(17) 0.0174(3) Uani 1 1 d . . .
Cl Cl 0.20575(8) 0.20693(5) 0.82528(5) 0.02404(9) Uani 1 1 d . . .
O1 O -0.0112(3) 0.1475(2) 0.7700(3) 0.0439(5) Uani 1 1 d . . .
O2 O 0.2367(5) 0.2517(3) 0.9599(2) 0.0511(6) Uani 1 1 d . . .
O3 O 0.2341(4) 0.32122(19) 0.78922(19) 0.0332(4) Uani 1 1 d . . .
O4 O 0.3596(4) 0.1136(2) 0.7795(3) 0.0486(6) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ag 0.01607(6) 0.01597(6) 0.02628(7) 0.00851(5) -0.00013(4) 0.00485(4)
N11 0.0482(14) 0.0502(15) 0.0295(11) 0.0152(11) 0.0157(10) 0.0046(12)
C11 0.0269(10) 0.0339(12) 0.0314(11) 0.0041(10) 0.0082(9) 0.0005(9)
C12 0.0403(15) 0.0455(17) 0.0377(15) 0.0022(13) -0.0091(12) 0.0089(13)
N21 0.0270(9) 0.0250(9) 0.0392(11) 0.0084(8) -0.0014(8) -0.0044(7)
C21 0.0263(10) 0.0247(10) 0.0333(11) 0.0137(9) 0.0000(8) -0.0020(8)
C22 0.0482(16) 0.0355(14) 0.0397(14) 0.0170(12) -0.0141(12) -0.0167(12)
N1 0.0183(7) 0.0145(7) 0.0333(9) 0.0067(6) -0.0005(6) 0.0028(5)
C2 0.0190(8) 0.0155(8) 0.0297(10) 0.0067(7) 0.0008(7) 0.0019(6)
N3 0.0151(6) 0.0155(6) 0.0213(7) 0.0066(5) 0.0011(5) 0.0025(5)
C3A 0.0144(6) 0.0144(7) 0.0188(7) 0.0075(6) 0.0043(5) 0.0057(5)
N4 0.0153(6) 0.0138(6) 0.0191(6) 0.0073(5) 0.0026(5) 0.0032(5)
C5 0.0163(7) 0.0150(7) 0.0239(8) 0.0087(6) 0.0018(6) 0.0029(6)
C6 0.0138(7) 0.0195(8) 0.0242(8) 0.0090(7) 0.0010(6) 0.0035(6)
C7 0.0162(7) 0.0162(7) 0.0265(9) 0.0089(7) 0.0021(6) 0.0050(6)
N8 0.0152(6) 0.0140(6) 0.0229(7) 0.0074(5) 0.0020(5) 0.0043(5)
Cl 0.0227(2) 0.0247(2) 0.0263(2) 0.01161(18) 0.00361(17) 0.00152(17)
O1 0.0281(9) 0.0311(10) 0.0638(15) 0.0114(10) -0.0021(9) -0.0041(7)
O2 0.0642(16) 0.0659(16) 0.0286(10) 0.0253(11) 0.0053(10) 0.0010(13)
O3 0.0446(11) 0.0244(8) 0.0367(10) 0.0151(7) 0.0140(8) 0.0026(7)
O4 0.0438(12) 0.0410(12) 0.0660(16) 0.0235(12) 0.0128(11) 0.0243(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
Ag N3 2.1845(16) 2_766 ?
Ag N4 2.2339(15) . ?
Ag N21 2.436(2) . ?
Ag N11 2.520(2) . ?
Ag Ag 3.0987(5) 2_766 ?
N11 C11 1.138(4) . ?
C11 C12 1.459(4) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
N21 C21 1.134(3) . ?
C21 C22 1.448(4) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
N1 C2 1.324(3) . ?
N1 N8 1.370(2) . ?
C2 N3 1.363(3) . ?
C2 H21 0.9500 . ?
N3 C3A 1.329(2) . ?
N3 Ag 2.1845(16) 2_766 ?
C3A N4 1.341(2) . ?
C3A N8 1.369(2) . ?
N4 C5 1.330(2) . ?
C5 C6 1.407(3) . ?
C5 H51 0.9500 . ?
C6 C7 1.374(3) . ?
C6 H61 0.9500 . ?
C7 N8 1.354(2) . ?
C7 H71 0.9500 . ?
Cl O2 1.435(2) . ?
Cl O4 1.439(2) . ?
Cl O1 1.445(2) . ?
Cl O3 1.4464(19) . ?
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 Ag N4 158.63(6) 2_766 . ?
N3 Ag N21 103.05(7) 2_766 . ?
N4 Ag N21 92.94(7) . . ?
N3 Ag N11 97.48(8) 2_766 . ?
N4 Ag N11 95.62(8) . . ?
N21 Ag N11 93.32(9) . . ?
N3 Ag Ag 78.31(4) 2_766 2_766 ?
N4 Ag Ag 82.84(4) . 2_766 ?
N21 Ag Ag 166.32(6) . 2_766 ?
N11 Ag Ag 100.02(7) . 2_766 ?
C11 N11 Ag 132.3(2) . . ?
N11 C11 C12 179.1(3) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C21 N21 Ag 160.2(2) . . ?
N21 C21 C22 179.2(3) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C2 N1 N8 101.91(16) . . ?
N1 C2 N3 115.52(18) . . ?
N1 C2 H21 122.2 . . ?
N3 C2 H21 122.2 . . ?
C3A N3 C2 103.47(16) . . ?
C3A N3 Ag 127.93(13) . 2_766 ?
C2 N3 Ag 127.85(13) . 2_766 ?
N3 C3A N4 128.93(16) . . ?
N3 C3A N8 108.98(16) . . ?
N4 C3A N8 122.09(16) . . ?
C5 N4 C3A 116.21(16) . . ?
C5 N4 Ag 123.76(13) . . ?
C3A N4 Ag 119.73(12) . . ?
N4 C5 C6 123.64(18) . . ?
N4 C5 H51 118.2 . . ?
C6 C5 H51 118.2 . . ?
C7 C6 C5 119.13(17) . . ?
C7 C6 H61 120.4 . . ?
C5 C6 H61 120.4 . . ?
N8 C7 C6 116.19(17) . . ?
N8 C7 H71 121.9 . . ?
C6 C7 H71 121.9 . . ?
C7 N8 C3A 122.73(17) . . ?
C7 N8 N1 127.15(16) . . ?
C3A N8 N1 110.11(15) . . ?
O2 Cl O4 111.26(16) . . ?
O2 Cl O1 109.84(16) . . ?
O4 Cl O1 110.18(15) . . ?
O2 Cl O3 108.16(14) . . ?
O4 Cl O3 108.96(14) . . ?
O1 Cl O3 108.37(14) . . ?
_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full 41.13
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max 1.585
_refine_diff_density_min -1.580
_refine_diff_density_rms 0.189
#===END
data_an93
_database_code_depnum_ccdc_archive 'CCDC 819204'
#TrackingRef '- 1-6-crystaldata.CIF'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
[bis(\m-7-amine-1,2,4-triazolo[1,5-a]pyrimidine)disilver(I)]
bis(perchlorate)
;
_chemical_name_common
;(bis(mu-7-amine-1,2,4-triazolo(1,5-a)pyrimidine)disilver(i))
bis(perchlorate)
;
_chemical_melting_point ?
_chemical_formula_moiety 'C10 H10 Ag2 N10, 2(Cl O4) '
_chemical_formula_sum 'C10 H10 Ag2 Cl2 N10 O8'
_chemical_formula_weight 684.92
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'
Cl Cl 0.1484 0.1585 '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
_symmetry_space_group_name_Hall '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 5.7889(15)
_cell_length_b 8.389(2)
_cell_length_c 10.138(3)
_cell_angle_alpha 109.414(3)
_cell_angle_beta 91.774(3)
_cell_angle_gamma 102.566(3)
_cell_volume 450.4(2)
_cell_formula_units_Z 1
_cell_measurement_temperature 113(2)
_cell_measurement_reflns_used 2206
_cell_measurement_theta_min 2.653
_cell_measurement_theta_max 26.855
_exptl_crystal_description prismatic
_exptl_crystal_colour colourless
_exptl_crystal_size_max 0.32
_exptl_crystal_size_mid 0.18
_exptl_crystal_size_min 0.16
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 2.525
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 332
_exptl_absorpt_coefficient_mu 2.543
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.4966
_exptl_absorpt_correction_T_max 0.6864
_exptl_absorpt_process_details '(ABSCOR; Higashi, 1995)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 113(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 'Rigaku R-axis Spider Image plate 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 4319
_diffrn_reflns_av_R_equivalents 0.0306
_diffrn_reflns_av_sigmaI/netI 0.0373
_diffrn_reflns_limit_h_min -6
_diffrn_reflns_limit_h_max 6
_diffrn_reflns_limit_k_min -9
_diffrn_reflns_limit_k_max 9
_diffrn_reflns_limit_l_min -12
_diffrn_reflns_limit_l_max 12
_diffrn_reflns_theta_min 2.14
_diffrn_reflns_theta_max 25.00
_reflns_number_total 1575
_reflns_number_gt 1450
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'd*trek, CrystalClear (Rigaku, 2007)'
_computing_cell_refinement 'Fsproc, CrystalClear (Rigaku, 2007)'
_computing_data_reduction 'Fsproc, CrystalClear (Rigaku, 2007)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics 'DIAMOND (Crystal Impact, 2009)'
_computing_publication_material ?
_publ_section_references
;
Crystal Impact (2009). DIAMOND. Version3.2. Crystal Impact GbR, Bonn,
Germany.
Higashi, T. (1995). ABSCOR. Rigaku Corporation, Tokyo, Japan.
Rigaku (2007). CrystalClear (Version SM Expert 2.0 r1).
Rigaku Corporation, Tokyo, Japan.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112--122.
;
_publ_section_exptl_refinement
;
Hydrogen atoms for aromatic CH, aliphatic CH, CH~2~ and methyl groups
were positioned geometrically (C---H = 0.94 \%A for
aromatic CH, C---H = 0.99 \%A for aliphatic CH, C---H = 0.98 \%A for CH~2~,
C---H = 0.97 \%A for CH~3~) and refined using a
riding model (AFIX 43 for aromatic CH, AFIX 13 for aliphatic CH,
AFIX 23 for CH~2~, AFIX 33 or rotating group refinement 137 for CH~3~),
with U~iso~(H) = 1.2U~eq~(CH) and U~iso~(H) = 1.5U~eq~(CH~3~).
;
_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^)+(0.0637P)^2^+0.7405P] 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 1575
_refine_ls_number_parameters 153
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0434
_refine_ls_R_factor_gt 0.0396
_refine_ls_wR_factor_ref 0.1034
_refine_ls_wR_factor_gt 0.1014
_refine_ls_goodness_of_fit_ref 1.102
_refine_ls_restrained_S_all 1.102
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ag Ag 0.49054(7) 0.56828(5) 0.38359(4) 0.0292(2) Uani 1 1 d . . .
Cl Cl 0.5676(2) 0.80527(17) 0.17999(13) 0.0262(3) Uani 1 1 d . . .
C2 C 0.0975(9) 0.7806(7) 0.4737(6) 0.0269(12) Uani 1 1 d . . .
H2 H 0.1030 0.8062 0.3912 0.032 Uiso 1 1 calc R . .
C3A C 0.1864(9) 0.6727(7) 0.6262(6) 0.0266(12) Uani 1 1 d . . .
C5 C 0.1753(10) 0.6090(7) 0.8237(6) 0.0268(12) Uani 1 1 d . . .
H5 H 0.2264 0.5548 0.8816 0.032 Uiso 1 1 calc R . .
C6 C 0.0128(10) 0.7035(7) 0.8675(6) 0.0275(12) Uani 1 1 d . . .
H6 H -0.0453 0.7087 0.9529 0.033 Uiso 1 1 calc R . .
C7 C -0.0712(11) 0.7926(8) 0.7919(6) 0.0355(14) Uani 1 1 d . . .
N1 N -0.0449(8) 0.8384(6) 0.5670(5) 0.0286(10) Uani 1 1 d . . .
N3 N 0.2347(8) 0.6831(6) 0.5018(5) 0.0264(10) Uani 1 1 d . . .
N4 N 0.2672(8) 0.5894(6) 0.6998(5) 0.0274(10) Uani 1 1 d . . .
N8 N 0.0198(9) 0.7701(7) 0.6686(5) 0.0369(13) Uani 1 1 d . . .
N71 N -0.2300(9) 0.8892(7) 0.8175(7) 0.0361(13) Uani 1 1 d . . .
O1 O 0.4043(8) 0.6405(6) 0.1479(5) 0.0432(11) Uani 1 1 d . . .
O2 O 0.5154(7) 0.9276(6) 0.3068(4) 0.0378(10) Uani 1 1 d . . .
O3 O 0.5481(8) 0.8699(6) 0.0675(4) 0.0357(10) Uani 1 1 d . . .
O4 O 0.8043(7) 0.7868(6) 0.2000(4) 0.0378(10) Uani 1 1 d . . .
H72 H -0.281(16) 0.923(13) 0.753(9) 0.08(3) Uiso 1 1 d . . .
H71 H -0.310(16) 0.884(12) 0.884(10) 0.08(3) Uiso 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
Ag 0.0304(3) 0.0329(3) 0.0229(3) 0.00412(19) 0.01018(18) 0.0127(2)
Cl 0.0296(7) 0.0273(7) 0.0206(7) 0.0058(5) 0.0062(5) 0.0080(5)
C2 0.026(3) 0.034(3) 0.020(3) 0.007(2) 0.006(2) 0.009(2)
C3A 0.021(3) 0.026(3) 0.026(3) -0.002(2) 0.005(2) 0.008(2)
C5 0.032(3) 0.026(3) 0.016(3) 0.002(2) 0.008(2) 0.004(2)
C6 0.030(3) 0.029(3) 0.022(3) 0.007(2) 0.010(2) 0.004(2)
C7 0.034(3) 0.037(3) 0.029(3) 0.005(3) 0.010(2) 0.004(3)
N1 0.033(3) 0.032(3) 0.023(2) 0.011(2) 0.0064(19) 0.009(2)
N3 0.023(2) 0.030(3) 0.022(2) 0.0030(19) 0.0035(18) 0.007(2)
N4 0.028(2) 0.029(3) 0.020(2) 0.0009(19) 0.0077(19) 0.009(2)
N8 0.028(3) 0.035(3) 0.035(3) -0.004(2) 0.010(2) 0.005(2)
N71 0.031(3) 0.031(3) 0.048(4) 0.009(3) 0.022(3) 0.014(2)
O1 0.050(3) 0.034(2) 0.034(2) 0.0079(19) -0.001(2) -0.004(2)
O2 0.035(2) 0.045(3) 0.024(2) -0.0007(18) 0.0115(17) 0.0105(19)
O3 0.042(2) 0.043(2) 0.030(2) 0.0175(19) 0.0109(18) 0.019(2)
O4 0.036(2) 0.040(2) 0.033(2) 0.0035(19) 0.0043(18) 0.0166(19)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ag N3 2.126(4) . ?
Ag N4 2.137(4) 2_666 ?
Ag Ag 2.9549(10) 2_666 ?
Cl O1 1.423(5) . ?
Cl O3 1.427(4) . ?
Cl O4 1.428(4) . ?
Cl O2 1.442(4) . ?
C2 N1 1.314(7) . ?
C2 N3 1.344(7) . ?
C3A N4 1.316(7) . ?
C3A N3 1.327(7) . ?
C3A N8 1.385(7) . ?
C5 C6 1.351(8) . ?
C5 N4 1.353(7) . ?
C6 C7 1.378(9) . ?
C7 N71 1.330(8) . ?
C7 N8 1.342(8) . ?
N1 N8 1.411(7) . ?
N4 Ag 2.137(4) 2_666 ?
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 Ag N4 164.43(18) . 2_666 ?
N3 Ag Ag 81.07(13) . 2_666 ?
N4 Ag Ag 83.90(13) 2_666 2_666 ?
O1 Cl O3 110.0(3) . . ?
O1 Cl O4 109.3(3) . . ?
O3 Cl O4 109.5(3) . . ?
O1 Cl O2 109.8(3) . . ?
O3 Cl O2 108.8(3) . . ?
O4 Cl O2 109.4(2) . . ?
N1 C2 N3 117.6(5) . . ?
N4 C3A N3 130.8(5) . . ?
N4 C3A N8 124.0(5) . . ?
N3 C3A N8 105.2(5) . . ?
C6 C5 N4 123.3(5) . . ?
C5 C6 C7 123.3(5) . . ?
N71 C7 N8 115.9(6) . . ?
N71 C7 C6 131.5(6) . . ?
N8 C7 C6 112.6(5) . . ?
C2 N1 N8 98.6(4) . . ?
C3A N3 C2 106.2(4) . . ?
C3A N3 Ag 123.8(4) . . ?
C2 N3 Ag 130.0(4) . . ?
C3A N4 C5 113.9(5) . . ?
C3A N4 Ag 120.1(3) . 2_666 ?
C5 N4 Ag 126.0(4) . 2_666 ?
C7 N8 C3A 122.9(6) . . ?
C7 N8 N1 124.7(5) . . ?
C3A N8 N1 112.4(5) . . ?
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full 25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max 1.403
_refine_diff_density_min -1.012
_refine_diff_density_rms 0.178
#===END
data_an86
_database_code_depnum_ccdc_archive 'CCDC 819205'
#TrackingRef '- 1-6-crystaldata.CIF'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
[acetonitrile-bis(\m-5,7-dimethyl-1,2,4-
triazolo[1,5-a]pyrimidine)disilver(I)] tetrafluoroborate perchlorate
;
_chemical_name_common
;
(acetonitrile-bis(mu-5,7-dimethyl-1,2,4-triazolo(1,5-
a)pyrimidine)disilver(i)) tetrafluoroborate perchlorate
;
_chemical_melting_point ?
_chemical_formula_moiety 'C16 H19 Ag2 N9, F6 P, Cl O4'
_chemical_formula_sum 'C16 H19 Ag2 Cl F6 N9 O4 P'
_chemical_formula_weight 797.56
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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'
_symmetry_cell_setting triclinic
_symmetry_space_group_name_H-M P-1
_symmetry_space_group_name_Hall '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 11.228(5)
_cell_length_b 11.471(5)
_cell_length_c 12.191(5)
_cell_angle_alpha 110.932(5)
_cell_angle_beta 112.874(5)
_cell_angle_gamma 97.284(5)
_cell_volume 1285.2(10)
_cell_formula_units_Z 2
_cell_measurement_temperature 293(2)
_cell_measurement_reflns_used 4452
_cell_measurement_theta_min 2.39
_cell_measurement_theta_max 23.57
_exptl_crystal_description prismatic
_exptl_crystal_colour colourless
_exptl_crystal_size_max 0.45
_exptl_crystal_size_mid 0.32
_exptl_crystal_size_min 0.20
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 2.061
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 780
_exptl_absorpt_coefficient_mu 1.777
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.5019
_exptl_absorpt_correction_T_max 0.7176
_exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 293(2)
_diffrn_radiation_wavelength 0.71069
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker SMART APEX CCD system'
_diffrn_measurement_method '\f and \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 13078
_diffrn_reflns_av_R_equivalents 0.0190
_diffrn_reflns_av_sigmaI/netI 0.0233
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_l_min -14
_diffrn_reflns_limit_l_max 14
_diffrn_reflns_theta_min 2.00
_diffrn_reflns_theta_max 25.30
_reflns_number_total 4676
_reflns_number_gt 3802
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'Bruker APEXII'
_computing_cell_refinement 'Bruker APEXII'
_computing_data_reduction 'Bruker APEXII'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'DIAMOND (Crystal Impact, 2009)'
_computing_publication_material ?
_publ_section_references
;
Crystal Impact (2009). DIAMOND. Version3.2. Crystal Impact GbR, Bonn,
Germany.
Sheldrick, G. M. (1996). SADABS. University of G\"ottingen, Germany.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112--122.
;
_publ_section_exptl_refinement
;
Hydrogen atoms for aromatic CH, aliphatic CH, CH~2~ and methyl groups
were positioned geometrically (C---H = 0.94 \%A for
aromatic CH, C---H = 0.99 \%A for aliphatic CH, C---H = 0.98 \%A for CH~2~,
C---H = 0.97 \%A for CH~3~) and refined using a
riding model (AFIX 43 for aromatic CH, AFIX 13 for aliphatic CH,
AFIX 23 for CH~2~, AFIX 33 or rotating group refinement 137 for CH~3~),
with U~iso~(H) = 1.2U~eq~(CH) and U~iso~(H) = 1.5U~eq~(CH~3~).
;
_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^)+(0.0646P)^2^+1.1555P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 4676
_refine_ls_number_parameters 357
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0521
_refine_ls_R_factor_gt 0.0420
_refine_ls_wR_factor_ref 0.1190
_refine_ls_wR_factor_gt 0.1123
_refine_ls_goodness_of_fit_ref 1.048
_refine_ls_restrained_S_all 1.048
_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 0.41587(4) 0.07347(4) 0.40362(4) 0.05776(15) Uani 1 1 d . . .
Ag2 Ag 0.66352(4) 0.27337(4) 0.64737(4) 0.06584(16) Uani 1 1 d . . .
N1 N 0.6114(4) 0.0810(4) 0.1593(4) 0.0626(11) Uani 1 1 d . . .
C2 C 0.5103(5) 0.0496(5) 0.1816(5) 0.0613(13) Uani 1 1 d . . .
H2 H 0.4234 -0.0009 0.1129 0.074 Uiso 1 1 calc R . .
N3 N 0.5401(4) 0.0954(4) 0.3118(4) 0.0545(10) Uani 1 1 d . . .
C3A C 0.6727(5) 0.1642(4) 0.3769(5) 0.0492(10) Uani 1 1 d . . .
N4 N 0.7534(4) 0.2312(4) 0.5077(4) 0.0533(9) Uani 1 1 d . . .
C5 C 0.8833(5) 0.2891(5) 0.5451(5) 0.0613(13) Uani 1 1 d . . .
C51 C 0.9796(6) 0.3648(7) 0.6907(6) 0.090(2) Uani 1 1 d . . .
H51A H 0.9558 0.4418 0.7274 0.135 Uiso 1 1 calc R . .
H51B H 1.0706 0.3903 0.7034 0.135 Uiso 1 1 calc R . .
H51C H 0.9741 0.3110 0.7344 0.135 Uiso 1 1 calc R . .
C6 C 0.9292(6) 0.2816(6) 0.4521(6) 0.0693(14) Uani 1 1 d . . .
H6 H 1.0201 0.3236 0.4826 0.083 Uiso 1 1 calc R . .
C7 C 0.8466(5) 0.2157(5) 0.3197(6) 0.0644(13) Uani 1 1 d . . .
C71 C 0.8812(6) 0.2051(7) 0.2118(7) 0.0857(18) Uani 1 1 d . . .
H71A H 0.9706 0.2637 0.2491 0.129 Uiso 1 1 calc R . .
H71B H 0.8165 0.2281 0.1507 0.129 Uiso 1 1 calc R . .
H71C H 0.8791 0.1167 0.1657 0.129 Uiso 1 1 calc R . .
N8 N 0.7153(4) 0.1553(4) 0.2847(4) 0.0551(10) Uani 1 1 d . . .
N11 N 0.1913(5) 0.0881(5) 0.6259(5) 0.0694(12) Uani 1 1 d . . .
C12 C 0.2076(6) 0.0557(5) 0.5201(6) 0.0656(13) Uani 1 1 d . . .
H12 H 0.1353 0.0040 0.4354 0.079 Uiso 1 1 calc R . .
N13 N 0.3355(4) 0.1011(4) 0.5394(4) 0.0536(9) Uani 1 1 d . . .
C13A C 0.4065(5) 0.1735(4) 0.6720(5) 0.0509(11) Uani 1 1 d . . .
N14 N 0.5384(4) 0.2437(4) 0.7446(4) 0.0533(9) Uani 1 1 d . . .
C15 C 0.5825(5) 0.3069(5) 0.8757(5) 0.0601(12) Uani 1 1 d . . .
C151 C 0.7276(6) 0.3901(6) 0.9611(6) 0.0815(17) Uani 1 1 d . . .
H51D H 0.7839 0.3446 0.9320 0.122 Uiso 1 1 calc R . .
H51E H 0.7539 0.4079 1.0518 0.122 Uiso 1 1 calc R . .
H51F H 0.7384 0.4712 0.9543 0.122 Uiso 1 1 calc R . .
C16 C 0.4970(7) 0.2985(6) 0.9328(6) 0.0732(15) Uani 1 1 d . . .
H16 H 0.5326 0.3430 1.0245 0.088 Uiso 1 1 calc R . .
C17 C 0.3635(6) 0.2272(5) 0.8575(5) 0.0659(13) Uani 1 1 d . . .
C171 C 0.2638(7) 0.2123(7) 0.9072(6) 0.092(2) Uani 1 1 d . . .
H71D H 0.2262 0.1211 0.8815 0.138 Uiso 1 1 calc R . .
H71E H 0.1922 0.2459 0.8699 0.138 Uiso 1 1 calc R . .
H71F H 0.3085 0.2601 1.0024 0.138 Uiso 1 1 calc R . .
N18 N 0.3225(4) 0.1655(4) 0.7248(4) 0.0577(10) Uani 1 1 d . . .
N9 N 0.7491(6) 0.5051(5) 0.7411(6) 0.0919(16) Uani 1 1 d . . .
C8 C 0.7452(6) 0.6023(6) 0.7434(6) 0.0736(15) Uani 1 1 d . . .
C9 C 0.7406(7) 0.7300(6) 0.7494(7) 0.0887(18) Uani 1 1 d . . .
H9A H 0.6498 0.7343 0.7266 0.133 Uiso 1 1 calc R . .
H9B H 0.7674 0.7433 0.6879 0.133 Uiso 1 1 calc R . .
H9C H 0.8017 0.7969 0.8379 0.133 Uiso 1 1 calc R . .
Cl Cl 0.89216(12) 0.11221(13) 0.86396(12) 0.0635(3) Uani 1 1 d . . .
O1 O 0.9825(6) 0.2214(6) 0.9780(5) 0.144(2) Uani 1 1 d . . .
O2 O 0.8313(8) 0.1505(7) 0.7637(6) 0.162(3) Uani 1 1 d . . .
O3 O 0.9488(6) 0.0162(5) 0.8133(7) 0.130(2) Uani 1 1 d . . .
O4 O 0.7848(7) 0.0531(6) 0.8783(7) 0.162(3) Uani 1 1 d . . .
P P 0.34735(14) 0.49710(14) 0.65543(15) 0.0618(4) Uani 1 1 d . . .
F1 F 0.2784(7) 0.5728(7) 0.7312(6) 0.171(2) Uani 1 1 d . . .
F2 F 0.2746(7) 0.3763(7) 0.6471(10) 0.225(4) Uani 1 1 d . . .
F3 F 0.4664(7) 0.5093(7) 0.7801(5) 0.179(3) Uani 1 1 d . . .
F4 F 0.4249(7) 0.6196(6) 0.6725(11) 0.246(5) Uani 1 1 d . . .
F5 F 0.2269(6) 0.4813(7) 0.5287(6) 0.163(2) Uani 1 1 d . . .
F6 F 0.4141(6) 0.4124(6) 0.5772(5) 0.1445(18) 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 0.0487(2) 0.0663(3) 0.0485(2) 0.02208(19) 0.01953(18) 0.00905(18)
Ag2 0.0576(3) 0.0697(3) 0.0522(2) 0.0200(2) 0.02076(19) 0.00222(19)
N1 0.055(2) 0.075(3) 0.050(2) 0.023(2) 0.023(2) 0.016(2)
C2 0.055(3) 0.068(3) 0.047(3) 0.020(2) 0.017(2) 0.014(2)
N3 0.045(2) 0.061(2) 0.048(2) 0.0231(19) 0.0163(18) 0.0086(18)
C3A 0.044(2) 0.049(2) 0.051(3) 0.025(2) 0.018(2) 0.012(2)
N4 0.044(2) 0.059(2) 0.050(2) 0.0255(19) 0.0157(18) 0.0093(18)
C5 0.042(3) 0.065(3) 0.063(3) 0.028(3) 0.015(2) 0.008(2)
C51 0.055(3) 0.107(5) 0.069(4) 0.026(4) 0.010(3) 0.004(3)
C6 0.047(3) 0.077(4) 0.079(4) 0.036(3) 0.026(3) 0.015(3)
C7 0.050(3) 0.071(3) 0.077(4) 0.035(3) 0.031(3) 0.020(3)
C71 0.075(4) 0.103(5) 0.098(5) 0.047(4) 0.056(4) 0.026(4)
N8 0.049(2) 0.060(2) 0.055(2) 0.026(2) 0.023(2) 0.0159(19)
N11 0.061(3) 0.071(3) 0.064(3) 0.020(2) 0.030(2) 0.009(2)
C12 0.059(3) 0.066(3) 0.060(3) 0.021(3) 0.026(3) 0.010(3)
N13 0.055(2) 0.055(2) 0.048(2) 0.0211(19) 0.0239(19) 0.0129(19)
C13A 0.058(3) 0.044(2) 0.048(3) 0.019(2) 0.023(2) 0.016(2)
N14 0.057(2) 0.049(2) 0.044(2) 0.0171(18) 0.0199(19) 0.0108(18)
C15 0.063(3) 0.058(3) 0.050(3) 0.023(2) 0.020(2) 0.017(2)
C151 0.074(4) 0.086(4) 0.051(3) 0.017(3) 0.016(3) 0.008(3)
C16 0.090(4) 0.075(4) 0.054(3) 0.024(3) 0.037(3) 0.025(3)
C17 0.073(4) 0.063(3) 0.058(3) 0.022(3) 0.035(3) 0.016(3)
C171 0.107(5) 0.105(5) 0.072(4) 0.031(4) 0.061(4) 0.021(4)
N18 0.061(3) 0.055(2) 0.053(2) 0.020(2) 0.029(2) 0.0117(19)
N9 0.093(4) 0.063(3) 0.102(4) 0.034(3) 0.037(3) 0.010(3)
C8 0.053(3) 0.070(4) 0.069(4) 0.018(3) 0.020(3) 0.000(3)
C9 0.090(5) 0.077(4) 0.106(5) 0.048(4) 0.044(4) 0.027(3)
Cl 0.0497(7) 0.0702(8) 0.0546(7) 0.0237(6) 0.0164(6) 0.0078(6)
O1 0.086(4) 0.143(5) 0.086(4) -0.013(3) 0.004(3) -0.017(3)
O2 0.248(8) 0.160(5) 0.088(4) 0.069(4) 0.056(5) 0.123(6)
O3 0.122(4) 0.119(4) 0.200(6) 0.081(4) 0.105(4) 0.069(4)
O4 0.133(5) 0.150(5) 0.181(6) 0.024(5) 0.117(5) -0.014(4)
P 0.0527(7) 0.0625(8) 0.0659(8) 0.0315(7) 0.0223(7) 0.0139(6)
F1 0.187(6) 0.203(6) 0.156(5) 0.076(4) 0.097(5) 0.124(5)
F2 0.160(6) 0.191(6) 0.451(13) 0.220(8) 0.176(8) 0.107(5)
F3 0.170(6) 0.228(7) 0.102(4) 0.051(4) 0.037(4) 0.111(5)
F4 0.132(5) 0.137(5) 0.503(15) 0.175(7) 0.148(7) 0.051(4)
F5 0.112(4) 0.231(6) 0.140(5) 0.106(5) 0.030(3) 0.059(4)
F6 0.150(5) 0.171(5) 0.121(4) 0.055(3) 0.073(3) 0.074(4)
_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 N13 2.124(4) . ?
Ag1 N3 2.141(4) . ?
Ag1 Ag2 2.9852(10) . ?
Ag2 N14 2.227(4) . ?
Ag2 N4 2.241(4) . ?
Ag2 N9 2.371(6) . ?
N1 C2 1.303(7) . ?
N1 N8 1.362(6) . ?
C2 N3 1.362(6) . ?
C2 H2 0.9300 . ?
N3 C3A 1.344(6) . ?
C3A N4 1.334(6) . ?
C3A N8 1.360(6) . ?
N4 C5 1.340(6) . ?
C5 C6 1.398(8) . ?
C5 C51 1.497(8) . ?
C51 H51A 0.9600 . ?
C51 H51B 0.9600 . ?
C51 H51C 0.9600 . ?
C6 C7 1.350(7) . ?
C6 H6 0.9300 . ?
C7 N8 1.369(6) . ?
C7 C71 1.481(8) . ?
C71 H71A 0.9600 . ?
C71 H71B 0.9600 . ?
C71 H71C 0.9600 . ?
N11 C12 1.302(7) . ?
N11 N18 1.391(6) . ?
C12 N13 1.361(7) . ?
C12 H12 0.9300 . ?
N13 C13A 1.346(6) . ?
C13A N14 1.339(6) . ?
C13A N18 1.343(6) . ?
N14 C15 1.338(6) . ?
C15 C16 1.400(8) . ?
C15 C151 1.491(8) . ?
C151 H51D 0.9600 . ?
C151 H51E 0.9600 . ?
C151 H51F 0.9600 . ?
C16 C17 1.357(8) . ?
C16 H16 0.9300 . ?
C17 N18 1.360(6) . ?
C17 C171 1.484(8) . ?
C171 H71D 0.9600 . ?
C171 H71E 0.9600 . ?
C171 H71F 0.9600 . ?
N9 C8 1.112(7) . ?
C8 C9 1.448(9) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
Cl O1 1.367(5) . ?
Cl O2 1.402(5) . ?
Cl O4 1.408(5) . ?
Cl O3 1.413(5) . ?
P F4 1.454(6) . ?
P F2 1.465(6) . ?
P F3 1.530(5) . ?
P F1 1.536(5) . ?
P F5 1.537(5) . ?
P F6 1.579(5) . ?
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
N13 Ag1 N3 163.84(15) . . ?
N13 Ag1 Ag2 82.31(12) . . ?
N3 Ag1 Ag2 82.05(11) . . ?
N14 Ag2 N4 160.78(14) . . ?
N14 Ag2 N9 103.04(18) . . ?
N4 Ag2 N9 95.83(18) . . ?
N14 Ag2 Ag1 82.18(11) . . ?
N4 Ag2 Ag1 82.24(11) . . ?
N9 Ag2 Ag1 133.17(15) . . ?
C2 N1 N8 102.2(4) . . ?
N1 C2 N3 115.8(5) . . ?
N1 C2 H2 122.1 . . ?
N3 C2 H2 122.1 . . ?
C3A N3 C2 103.3(4) . . ?
C3A N3 Ag1 125.3(3) . . ?
C2 N3 Ag1 131.4(3) . . ?
N4 C3A N3 128.5(4) . . ?
N4 C3A N8 123.7(4) . . ?
N3 C3A N8 107.9(4) . . ?
C3A N4 C5 115.6(4) . . ?
C3A N4 Ag2 120.1(3) . . ?
C5 N4 Ag2 123.2(3) . . ?
N4 C5 C6 121.7(5) . . ?
N4 C5 C51 118.3(5) . . ?
C6 C5 C51 120.0(5) . . ?
C5 C51 H51A 109.5 . . ?
C5 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
C5 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C7 C6 C5 122.5(5) . . ?
C7 C6 H6 118.7 . . ?
C5 C6 H6 118.7 . . ?
C6 C7 N8 114.4(5) . . ?
C6 C7 C71 127.7(5) . . ?
N8 C7 C71 117.9(5) . . ?
C7 C71 H71A 109.5 . . ?
C7 C71 H71B 109.5 . . ?
H71A C71 H71B 109.5 . . ?
C7 C71 H71C 109.5 . . ?
H71A C71 H71C 109.5 . . ?
H71B C71 H71C 109.5 . . ?
C3A N8 N1 110.9(4) . . ?
C3A N8 C7 122.1(4) . . ?
N1 N8 C7 127.0(4) . . ?
C12 N11 N18 101.0(4) . . ?
N11 C12 N13 116.7(5) . . ?
N11 C12 H12 121.6 . . ?
N13 C12 H12 121.6 . . ?
C13A N13 C12 102.8(4) . . ?
C13A N13 Ag1 125.6(3) . . ?
C12 N13 Ag1 131.5(4) . . ?
N14 C13A N18 123.4(4) . . ?
N14 C13A N13 128.0(5) . . ?
N18 C13A N13 108.6(4) . . ?
C15 N14 C13A 115.3(4) . . ?
C15 N14 Ag2 123.2(3) . . ?
C13A N14 Ag2 120.9(3) . . ?
N14 C15 C16 122.2(5) . . ?
N14 C15 C151 117.7(5) . . ?
C16 C15 C151 120.2(5) . . ?
C15 C151 H51D 109.5 . . ?
C15 C151 H51E 109.5 . . ?
H51D C151 H51E 109.5 . . ?
C15 C151 H51F 109.5 . . ?
H51D C151 H51F 109.5 . . ?
H51E C151 H51F 109.5 . . ?
C17 C16 C15 121.7(5) . . ?
C17 C16 H16 119.2 . . ?
C15 C16 H16 119.2 . . ?
C16 C17 N18 114.3(5) . . ?
C16 C17 C171 126.2(5) . . ?
N18 C17 C171 119.6(5) . . ?
C17 C171 H71D 109.5 . . ?
C17 C171 H71E 109.5 . . ?
H71D C171 H71E 109.5 . . ?
C17 C171 H71F 109.5 . . ?
H71D C171 H71F 109.5 . . ?
H71E C171 H71F 109.5 . . ?
C13A N18 C17 123.2(5) . . ?
C13A N18 N11 110.8(4) . . ?
C17 N18 N11 126.0(4) . . ?
C8 N9 Ag2 153.5(5) . . ?
N9 C8 C9 178.7(7) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O1 Cl O2 108.6(4) . . ?
O1 Cl O4 111.6(4) . . ?
O2 Cl O4 105.5(5) . . ?
O1 Cl O3 115.4(4) . . ?
O2 Cl O3 105.8(4) . . ?
O4 Cl O3 109.2(4) . . ?
F4 P F2 176.4(6) . . ?
F4 P F3 89.3(5) . . ?
F2 P F3 87.4(5) . . ?
F4 P F1 89.9(4) . . ?
F2 P F1 89.0(4) . . ?
F3 P F1 94.5(3) . . ?
F4 P F5 91.9(5) . . ?
F2 P F5 91.5(4) . . ?
F3 P F5 178.6(4) . . ?
F1 P F5 86.3(3) . . ?
F4 P F6 93.1(4) . . ?
F2 P F6 88.0(4) . . ?
F3 P F6 85.3(3) . . ?
F1 P F6 176.9(4) . . ?
F5 P F6 93.8(3) . . ?
_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full 25.30
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max 0.695
_refine_diff_density_min -0.612
_refine_diff_density_rms 0.086
#===END
data_AC43
_database_code_depnum_ccdc_archive 'CCDC 819206'
#TrackingRef '- 1-6-crystaldata.CIF'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
[bis(\m-trifluoromethylsulfonate)-bis(\m-5,7-dimethyl-1,2,4-
triazolo[1,5-a]pyrimidine)disilver(I)]
;
_chemical_name_common
;
(bis(mu-trifluoromethylsulfonate)-bis(mu-5,7-dimethyl-1,2,4-
triazolo(1,5-a)pyrimidine)disilver(i))
;
_chemical_melting_point ?
_chemical_formula_moiety 'C8 H8 Ag F3 N4 O3 S'
_chemical_formula_sum 'C8 H8 Ag F3 N4 O3 S'
_chemical_formula_weight 405.11
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'
Ag Ag -0.8971 1.1015 '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'
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'
_symmetry_cell_setting triclinic
_symmetry_Int_Tables_number 2
_symmetry_space_group_name_H-M 'P -1 '
_symmetry_space_group_name_Hall '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 8.3689(2)
_cell_length_b 8.6550(2)
_cell_length_c 9.0743(6)
_cell_angle_alpha 93.984(7)
_cell_angle_beta 94.541(7)
_cell_angle_gamma 112.430(8)
_cell_volume 602.09(4)
_cell_formula_units_Z 2
_cell_measurement_temperature 133(2)
_cell_measurement_reflns_used 69702
_cell_measurement_theta_min 3.2
_cell_measurement_theta_max 52.2
_exptl_crystal_description Block
_exptl_crystal_colour Colorless
_exptl_crystal_size_max 0.20
_exptl_crystal_size_mid 0.11
_exptl_crystal_size_min 0.10
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 2.235
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 396
_exptl_absorpt_coefficient_mu 1.900
_exptl_absorpt_correction_type Multi-scan
_exptl_absorpt_correction_T_min 0.7025
_exptl_absorpt_correction_T_max 0.8327
_exptl_absorpt_process_details '(ABSCOR; Higashi, 1995)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 133(2)
_diffrn_source_power 2.0
_diffrn_source_voltage 50.0
_diffrn_source_current 40.0
_diffrn_measurement_specimen_support Loop
_diffrn_detector RX
_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 'Rigaku R-axis Spider Image plate detector'
_diffrn_measurement_method '\w scans'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 55683
_diffrn_reflns_av_R_equivalents 0.0353
_diffrn_reflns_av_sigmaI/netI 0.0178
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_l_min -13
_diffrn_reflns_limit_l_max 13
_diffrn_reflns_theta_min 3.23
_diffrn_reflns_theta_max 33.14
_reflns_number_total 4585
_reflns_number_gt 4237
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'd*trek, CrystalClear (Rigaku, 2007)'
_computing_cell_refinement 'Fsproc, CrystalClear (Rigaku, 2007)'
_computing_data_reduction 'Fsproc, CrystalClear (Rigaku, 2007)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics 'DIAMOND (Crystal Impact, 2009)'
_computing_publication_material ?
_publ_section_references
;
Crystal Impact (2009). DIAMOND. Version3.2. Crystal Impact GbR, Bonn,
Germany.
Higashi, T. (1995). ABSCOR. Rigaku Corporation, Tokyo, Japan.
Rigaku (2007). CrystalClear (Version SM Expert 2.0 r1).
Rigaku Corporation, Tokyo, Japan.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112--122.
;
_publ_section_exptl_refinement
;
Hydrogen atoms for aromatic CH, aliphatic CH, CH~2~ and methyl groups
were positioned geometrically (C---H = 0.94 \%A for
aromatic CH, C---H = 0.99 \%A for aliphatic CH, C---H = 0.98 \%A for CH~2~,
C---H = 0.97 \%A for CH~3~) and refined using a
riding model (AFIX 43 for aromatic CH, AFIX 13 for aliphatic CH,
AFIX 23 for CH~2~, AFIX 33 or rotating group refinement 137 for CH~3~),
with U~iso~(H) = 1.2U~eq~(CH) and U~iso~(H) = 1.5U~eq~(CH~3~).
;
_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^)+(0.0163P)^2^+0.6612P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 4585
_refine_ls_number_parameters 183
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0270
_refine_ls_R_factor_gt 0.0244
_refine_ls_wR_factor_ref 0.0541
_refine_ls_wR_factor_gt 0.0532
_refine_ls_goodness_of_fit_ref 1.165
_refine_ls_restrained_S_all 1.165
_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
Ag Ag 0.305239(15) 0.399819(16) 0.465250(13) 0.01730(4) Uani 1 1 d . . .
N1 N 0.66482(19) 0.83090(19) 0.12436(17) 0.0200(3) Uani 1 1 d . . .
C2 C 0.7299(2) 0.8133(2) 0.2566(2) 0.0201(3) Uani 1 1 d . . .
H21 H 0.8405 0.8898 0.3028 0.024 Uiso 1 1 calc R . .
N3 N 0.62892(17) 0.67896(18) 0.32278(15) 0.0167(2) Uani 1 1 d . . .
C3A C 0.4873(2) 0.6061(2) 0.22440(17) 0.0143(3) Uani 1 1 d . . .
N4 N 0.34237(17) 0.46952(17) 0.23496(15) 0.0148(2) Uani 1 1 d . . .
C5 C 0.2195(2) 0.4213(2) 0.11843(18) 0.0162(3) Uani 1 1 d . . .
C51 C 0.0594(2) 0.2681(2) 0.1246(2) 0.0214(3) Uani 1 1 d . . .
H51A H 0.0165 0.2733 0.2215 0.032 Uiso 1 1 calc R . .
H51B H 0.0867 0.1679 0.1109 0.032 Uiso 1 1 calc R . .
H51C H -0.0302 0.2623 0.0455 0.032 Uiso 1 1 calc R . .
C6 C 0.2392(2) 0.5104(2) -0.00849(18) 0.0182(3) Uani 1 1 d . . .
H61 H 0.1502 0.4708 -0.0900 0.022 Uiso 1 1 calc R . .
C7 C 0.3840(2) 0.6527(2) -0.01610(17) 0.0172(3) Uani 1 1 d . . .
C71 C 0.4153(3) 0.7626(2) -0.1386(2) 0.0232(3) Uani 1 1 d . . .
H71A H 0.4045 0.8680 -0.1052 0.035 Uiso 1 1 calc R . .
H71B H 0.3293 0.7053 -0.2248 0.035 Uiso 1 1 calc R . .
H71C H 0.5326 0.7871 -0.1664 0.035 Uiso 1 1 calc R . .
N8 N 0.50810(18) 0.69569(18) 0.10368(15) 0.0160(2) Uani 1 1 d . . .
S S 0.12324(5) 0.72124(5) 0.42754(4) 0.01527(7) Uani 1 1 d . . .
O11 O 0.01579(16) 0.77724(17) 0.51710(15) 0.0228(2) Uani 1 1 d . . .
O12 O 0.25063(18) 0.67575(17) 0.50953(15) 0.0240(3) Uani 1 1 d . . .
O13 O 0.0326(2) 0.6094(2) 0.29673(17) 0.0325(3) Uani 1 1 d . . .
C11 C 0.2554(3) 0.9130(3) 0.3525(3) 0.0293(4) Uani 1 1 d . . .
F11 F 0.1558(2) 0.9677(2) 0.2662(2) 0.0626(6) Uani 1 1 d . . .
F12 F 0.3449(2) 1.03526(17) 0.4571(2) 0.0551(5) Uani 1 1 d . . .
F13 F 0.36797(19) 0.88628(18) 0.26820(18) 0.0407(3) 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
Ag 0.01622(5) 0.02163(6) 0.01347(6) 0.00579(4) 0.00062(4) 0.00626(4)
N1 0.0175(6) 0.0232(7) 0.0203(7) 0.0078(5) 0.0040(5) 0.0077(5)
C2 0.0164(7) 0.0225(7) 0.0217(8) 0.0076(6) 0.0022(6) 0.0069(6)
N3 0.0148(5) 0.0213(6) 0.0146(6) 0.0049(5) 0.0008(4) 0.0073(5)
C3A 0.0162(6) 0.0185(6) 0.0119(6) 0.0044(5) 0.0029(5) 0.0101(5)
N4 0.0151(5) 0.0183(6) 0.0128(6) 0.0031(4) 0.0018(4) 0.0083(5)
C5 0.0174(6) 0.0193(7) 0.0142(6) 0.0012(5) 0.0010(5) 0.0101(5)
C51 0.0180(7) 0.0228(8) 0.0209(8) 0.0027(6) -0.0006(6) 0.0056(6)
C6 0.0202(7) 0.0242(7) 0.0130(7) 0.0016(6) -0.0009(5) 0.0123(6)
C7 0.0218(7) 0.0229(7) 0.0124(6) 0.0036(5) 0.0026(5) 0.0146(6)
C71 0.0300(8) 0.0300(9) 0.0153(7) 0.0096(6) 0.0039(6) 0.0167(7)
N8 0.0164(6) 0.0205(6) 0.0141(6) 0.0061(5) 0.0036(4) 0.0096(5)
S 0.01423(15) 0.01622(16) 0.01467(16) 0.00183(13) 0.00040(12) 0.00538(13)
O11 0.0183(5) 0.0271(6) 0.0242(6) 0.0048(5) 0.0082(5) 0.0087(5)
O12 0.0281(6) 0.0269(6) 0.0212(6) 0.0039(5) -0.0023(5) 0.0162(5)
O13 0.0283(7) 0.0377(8) 0.0260(7) -0.0110(6) -0.0099(5) 0.0116(6)
C11 0.0295(9) 0.0258(9) 0.0436(12) 0.0151(8) 0.0212(8) 0.0176(7)
F11 0.0589(10) 0.0767(12) 0.0900(14) 0.0674(11) 0.0425(10) 0.0517(10)
F12 0.0459(8) 0.0187(6) 0.0901(13) -0.0093(7) 0.0327(9) -0.0015(6)
F13 0.0443(7) 0.0382(7) 0.0571(9) 0.0235(6) 0.0374(7) 0.0264(6)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ag N3 2.1839(14) 2_666 ?
Ag N4 2.2277(13) . ?
Ag O11 2.5598(13) 2_566 ?
Ag O12 2.6081(13) . ?
Ag Ag 3.0398(4) 2_666 ?
N1 C2 1.321(2) . ?
N1 N8 1.373(2) . ?
C2 N3 1.362(2) . ?
C2 H21 0.9500 . ?
N3 C3A 1.335(2) . ?
N3 Ag 2.1839(14) 2_666 ?
C3A N4 1.348(2) . ?
C3A N8 1.370(2) . ?
N4 C5 1.337(2) . ?
C5 C6 1.416(2) . ?
C5 C51 1.491(2) . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C6 C7 1.369(2) . ?
C6 H61 0.9500 . ?
C7 N8 1.367(2) . ?
C7 C71 1.487(2) . ?
C71 H71A 0.9800 . ?
C71 H71B 0.9800 . ?
C71 H71C 0.9800 . ?
S O13 1.4349(14) . ?
S O12 1.4424(13) . ?
S O11 1.4483(13) . ?
S C11 1.821(2) . ?
O11 Ag 2.5598(13) 2_566 ?
C11 F12 1.314(3) . ?
C11 F13 1.335(2) . ?
C11 F11 1.335(3) . ?
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 Ag N4 155.91(5) 2_666 . ?
N3 Ag O11 88.87(5) 2_666 2_566 ?
N4 Ag O11 110.23(5) . 2_566 ?
N3 Ag O12 110.30(5) 2_666 . ?
N4 Ag O12 84.81(5) . . ?
O11 Ag O12 90.68(4) 2_566 . ?
N3 Ag Ag 76.19(4) 2_666 2_666 ?
N4 Ag Ag 85.47(4) . 2_666 ?
O11 Ag Ag 164.28(3) 2_566 2_666 ?
O12 Ag Ag 89.98(3) . 2_666 ?
C2 N1 N8 101.64(13) . . ?
N1 C2 N3 115.96(15) . . ?
N1 C2 H21 122.0 . . ?
N3 C2 H21 122.0 . . ?
C3A N3 C2 103.38(13) . . ?
C3A N3 Ag 129.49(11) . 2_666 ?
C2 N3 Ag 127.07(11) . 2_666 ?
N3 C3A N4 128.69(14) . . ?
N3 C3A N8 108.64(14) . . ?
N4 C3A N8 122.67(14) . . ?
C5 N4 C3A 116.50(14) . . ?
C5 N4 Ag 126.31(11) . . ?
C3A N4 Ag 114.59(10) . . ?
N4 C5 C6 121.83(15) . . ?
N4 C5 C51 117.95(15) . . ?
C6 C5 C51 120.22(15) . . ?
C5 C51 H51A 109.5 . . ?
C5 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
C5 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C7 C6 C5 121.33(15) . . ?
C7 C6 H61 119.3 . . ?
C5 C6 H61 119.3 . . ?
N8 C7 C6 115.03(14) . . ?
N8 C7 C71 118.51(15) . . ?
C6 C7 C71 126.45(15) . . ?
C7 C71 H71A 109.5 . . ?
C7 C71 H71B 109.5 . . ?
H71A C71 H71B 109.5 . . ?
C7 C71 H71C 109.5 . . ?
H71A C71 H71C 109.5 . . ?
H71B C71 H71C 109.5 . . ?
C7 N8 C3A 122.58(14) . . ?
C7 N8 N1 127.04(14) . . ?
C3A N8 N1 110.37(13) . . ?
O13 S O12 114.80(9) . . ?
O13 S O11 115.20(9) . . ?
O12 S O11 115.39(8) . . ?
O13 S C11 103.13(11) . . ?
O12 S C11 103.25(9) . . ?
O11 S C11 102.47(8) . . ?
S O11 Ag 123.38(8) . 2_566 ?
S O12 Ag 127.46(8) . . ?
F12 C11 F13 107.70(18) . . ?
F12 C11 F11 107.59(19) . . ?
F13 C11 F11 106.94(18) . . ?
F12 C11 S 112.48(16) . . ?
F13 C11 S 111.12(13) . . ?
F11 C11 S 110.76(15) . . ?
_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full 33.14
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max 0.861
_refine_diff_density_min -0.681
_refine_diff_density_rms 0.104
#===END
data_acad
_database_code_depnum_ccdc_archive 'CCDC 819207'
#TrackingRef '- 1-6-crystaldata.CIF'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
catena-[bis(\m-1,2,4-triazolo[1,5-a]pyrimidine)disilver(I)]
bis(hexafluorophosphate) hexahydrate
;
_chemical_name_common
;
catena-(bis(mu-1,2,4-triazolo(1,5-a)pyrimidine)disilver(i))
bis(hexafluorophosphate) hexahydrate
;
_chemical_melting_point ?
_chemical_formula_moiety 'C5 H4 Ag N4 O0.12, F6 P'
_chemical_formula_sum 'C5 H4 Ag F6 N4 O0.12 P'
_chemical_formula_weight 374.91
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting trigonal
_symmetry_space_group_name_H-M 'R -3'
_symmetry_space_group_name_Hall '-R 3'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
_cell_length_a 26.0272(3)
_cell_length_b 26.0272(3)
_cell_length_c 11.0746(2)
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 120.00
_cell_volume 6497.01(16)
_cell_formula_units_Z 18
_cell_measurement_temperature 103(2)
_cell_measurement_reflns_used 9913
_cell_measurement_theta_min 2.578
_cell_measurement_theta_max 29.7
_exptl_crystal_description block
_exptl_crystal_colour colorless
_exptl_crystal_size_max 0.08
_exptl_crystal_size_mid 0.05
_exptl_crystal_size_min 0.05
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.725
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 3222
_exptl_absorpt_coefficient_mu 1.557
_exptl_absorpt_correction_type Multi-scan
_exptl_absorpt_correction_T_min 0.8921
_exptl_absorpt_correction_T_max 0.9262
_exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)'
_exptl_special_details
;
with 3 H2O crystal water per formula unit
54 H2O per cell included for calculation:
_chemical_formula_moiety 'C5 H10 Ag N4 O3 (P F6)'
_chemical_formula_sum 'C5 H10 Ag F6 N4 O3 P'
_chemical_formula_weight 427.01
_exptl_crystal_density_diffrn 1.964
_exptl_crystal_F_000 3744
_exptl_absorpt_correction_T_min 0.8904
_exptl_absorpt_correction_T_max 0.9250
;
_diffrn_ambient_temperature 103(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'microfocus sealed tube'
_diffrn_radiation_monochromator 'multilayer mirror optics'
_diffrn_measurement_device_type 'Bruker APEX2 CCD area detector'
_diffrn_measurement_method '\w scans and \f scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 3592
_diffrn_reflns_av_R_equivalents 0.0000
_diffrn_reflns_av_sigmaI/netI 0.0162
_diffrn_reflns_limit_h_min -34
_diffrn_reflns_limit_h_max 16
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_k_max 34
_diffrn_reflns_limit_l_min 0
_diffrn_reflns_limit_l_max 14
_diffrn_reflns_theta_min 1.56
_diffrn_reflns_theta_max 28.28
_reflns_number_total 3592
_reflns_number_gt 3041
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'APEX2 (Bruker, 2006)'
_computing_cell_refinement 'SAINT (Bruker, 2006)'
_computing_data_reduction SAINT
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'DIAMOND (Crystal Impact, 2009)'
_computing_publication_material ?
_publ_section_references
;
Bruker (2006). APEX2 (Version 2.1-0) and SAINT.
Bruker Analytical X-ray Systems, Madison, Wisconsin, USA.
Crystal Impact (2009). DIAMOND. Version 3.2. Crystal Impact GbR, Bonn,
Germany.
Sheldrick, G. M. (1996). SADABS. University of G\"ottingen, Germany.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112--122.
;
_publ_section_exptl_refinement
;
Hydrogen atoms for aromatic CH, aliphatic CH and CH~2~
were positioned geometrically (C---H = 0.94 \%A for
aromatic CH, C---H = 0.99 \%A for aliphatic CH, C---H = 0.98 \%A for CH~2~)
and refined using a
riding model (AFIX 43 for aromatic CH, AFIX 13 for aliphatic CH,
AFIX 23 for CH~2~),
with U~iso~(H) = 1.2U~eq~(CH).
The largest residual Fourier peak (1.06 e \%A^-3^) is
found within 0.8 \%A of the Ag atom. The deepest hole (-0.95) is 0.73
\%A from the Ag atom.
;
_platon_calc_solv_details
;
Note: Expected volumes for solvent molecules are:
A hydrogen bonded H2O-molecule 40 Ang^3^
rea #GridPoint VolPerc. Vol(A^3^) X(av) Y(av) Z(av)
#-----------------------------------------------------
1 120136[ 55980] 11 747[ 347.9] 0.000 0.000-0.010
2 120136[ 55980] 11 747[ 347.9] 0.333 0.667-0.066
3 120136[ 55980] 11 747[ 347.9] 0.667 0.333 0.042
Each of the three solvent accessible voids of 747 Ang^3^
fits 18 water molecules
The voids fit a total of 54 water molecules per cell
;
_platon_squeeze_details
;
# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
Nr of gridpoints at least 1.20 Ang. from nearest vdWaals
Surface= 167508
N: Total Potential Solvent Accessible Void Vol ..2244.3 Ang^3^
N: Water Count / Cell = 54 - To be included in D(calc),
F000 and Mol.Wght.
;
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 -0.010 739 318 .
2 0.333 0.667 -0.068 750 318 .
3 0.667 0.333 0.043 750 318 .
_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^)+(0.0296P)^2^+12.7529P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 3592
_refine_ls_number_parameters 159
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0309
_refine_ls_R_factor_gt 0.0256
_refine_ls_wR_factor_ref 0.0630
_refine_ls_wR_factor_gt 0.0612
_refine_ls_goodness_of_fit_ref 1.066
_refine_ls_restrained_S_all 1.066
_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
Ag Ag 0.446243(7) 0.461321(8) 0.574994(14) 0.03309(7) Uani 1 1 d . . .
N1 N 0.60307(10) 0.67690(8) 0.69684(16) 0.0371(5) Uani 1 1 d . . .
C2 C 0.60347(10) 0.65385(9) 0.59070(18) 0.0301(5) Uani 1 1 d . . .
H21 H 0.6304 0.6766 0.5283 0.036 Uiso 1 1 calc R . .
N3 N 0.56322(8) 0.59611(8) 0.57714(14) 0.0249(4) Uani 1 1 d . . .
C3A C 0.53529(9) 0.58104(9) 0.68323(17) 0.0245(4) Uani 1 1 d . . .
N4 N 0.49125(8) 0.52821(8) 0.71900(15) 0.0309(4) Uani 1 1 d . . .
C5 C 0.47320(12) 0.52529(11) 0.8324(2) 0.0420(6) Uani 1 1 d . . .
H51 H 0.4423 0.4883 0.8615 0.050 Uiso 1 1 calc R . .
C6 C 0.49726(12) 0.57383(12) 0.9112(2) 0.0447(7) Uani 1 1 d . . .
H61 H 0.4830 0.5693 0.9917 0.054 Uiso 1 1 calc R . .
C7 C 0.54103(12) 0.62735(11) 0.87199(19) 0.0398(6) Uani 1 1 d . . .
H71 H 0.5579 0.6614 0.9225 0.048 Uiso 1 1 calc R . .
N8 N 0.55935(9) 0.62945(8) 0.75668(15) 0.0299(4) Uani 1 1 d . . .
O1W O 0.4319(9) 0.5238(9) 0.4635(17) 0.063(7) Uiso 0.121(8) 1 d P . .
P P 0.43450(3) 0.32088(3) 0.77647(5) 0.03536(15) Uani 1 1 d . . .
F1 F 0.48859(8) 0.34220(9) 0.86690(15) 0.0564(5) Uani 1 1 d . . .
F2 F 0.37986(9) 0.30013(9) 0.68593(14) 0.0638(5) Uani 1 1 d . . .
F3 F 0.47478(10) 0.32509(14) 0.66672(17) 0.1008(9) Uani 1 1 d . . .
F4 F 0.44935(10) 0.38716(9) 0.7599(2) 0.0772(6) Uani 1 1 d . . .
F5 F 0.41750(12) 0.25411(9) 0.7951(2) 0.0888(8) Uani 1 1 d . . .
F6 F 0.39244(8) 0.31493(9) 0.88577(13) 0.0584(5) 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
Ag 0.02770(10) 0.02904(10) 0.02124(9) -0.01103(6) 0.00918(6) -0.00178(7)
N1 0.0519(13) 0.0223(9) 0.0201(8) -0.0038(7) 0.0071(8) 0.0057(9)
C2 0.0378(12) 0.0225(11) 0.0182(9) -0.0021(8) 0.0049(8) 0.0062(9)
N3 0.0283(9) 0.0229(9) 0.0155(7) -0.0037(6) 0.0018(6) 0.0068(7)
C3A 0.0266(10) 0.0248(10) 0.0162(8) -0.0066(7) -0.0014(7) 0.0085(9)
N4 0.0306(10) 0.0269(9) 0.0191(8) -0.0062(7) 0.0055(7) 0.0024(8)
C5 0.0412(14) 0.0351(13) 0.0228(10) -0.0060(9) 0.0110(10) -0.0013(11)
C6 0.0522(16) 0.0406(14) 0.0188(10) -0.0078(9) 0.0099(10) 0.0063(12)
C7 0.0513(15) 0.0337(13) 0.0188(10) -0.0102(9) 0.0054(10) 0.0094(11)
N8 0.0372(11) 0.0225(9) 0.0175(8) -0.0054(7) 0.0028(7) 0.0055(8)
P 0.0467(4) 0.0442(4) 0.0190(2) -0.0084(2) -0.0036(2) 0.0256(3)
F1 0.0545(10) 0.0835(13) 0.0446(9) -0.0229(8) -0.0172(8) 0.0445(10)
F2 0.0687(12) 0.0888(14) 0.0328(8) -0.0174(8) -0.0207(8) 0.0386(11)
F3 0.0801(15) 0.181(3) 0.0414(10) -0.0269(13) 0.0131(10) 0.0653(17)
F4 0.0922(16) 0.0481(11) 0.0817(14) 0.0083(10) -0.0189(12) 0.0278(11)
F5 0.146(2) 0.0516(12) 0.0806(14) -0.0269(10) -0.0393(14) 0.0581(14)
F6 0.0548(10) 0.0875(13) 0.0283(7) -0.0122(8) 0.0013(7) 0.0323(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
Ag N3 2.1831(16) 10_666 ?
Ag N4 2.2151(17) . ?
Ag O1W 2.218(19) . ?
Ag N1 2.4137(19) 14_456 ?
Ag Ag 3.0016(3) 10_666 ?
N1 C2 1.322(3) . ?
N1 N8 1.362(3) . ?
N1 Ag 2.4136(19) 15_556 ?
C2 N3 1.343(3) . ?
N3 C3A 1.333(2) . ?
N3 Ag 2.1831(16) 10_666 ?
C3A N4 1.336(3) . ?
C3A N8 1.361(3) . ?
N4 C5 1.330(3) . ?
C5 C6 1.399(3) . ?
C6 C7 1.356(4) . ?
C7 N8 1.355(3) . ?
P F3 1.5727(19) . ?
P F5 1.578(2) . ?
P F4 1.579(2) . ?
P F1 1.5847(17) . ?
P F6 1.5870(16) . ?
P F2 1.5974(17) . ?
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 Ag N4 158.13(7) 10_666 . ?
N3 Ag O1W 94.0(5) 10_666 . ?
N4 Ag O1W 92.4(5) . . ?
N3 Ag N1 96.03(7) 10_666 14_456 ?
N4 Ag N1 104.58(7) . 14_456 ?
O1W Ag N1 92.4(5) . 14_456 ?
N3 Ag Ag 77.31(5) 10_666 10_666 ?
N4 Ag Ag 85.52(5) . 10_666 ?
O1W Ag Ag 69.1(5) . 10_666 ?
N1 Ag Ag 159.48(5) 14_456 10_666 ?
C2 N1 N8 102.34(17) . . ?
C2 N1 Ag 129.41(15) . 15_556 ?
N8 N1 Ag 127.17(13) . 15_556 ?
N1 C2 N3 115.37(19) . . ?
C3A N3 C2 103.66(16) . . ?
C3A N3 Ag 128.35(14) . 10_666 ?
C2 N3 Ag 127.61(14) . 10_666 ?
N3 C3A N4 128.68(18) . . ?
N3 C3A N8 108.87(18) . . ?
N4 C3A N8 122.44(18) . . ?
C5 N4 C3A 115.81(19) . . ?
C5 N4 Ag 127.03(16) . . ?
C3A N4 Ag 116.09(13) . . ?
N4 C5 C6 123.5(2) . . ?
C7 C6 C5 119.6(2) . . ?
N8 C7 C6 116.2(2) . . ?
C7 N8 C3A 122.43(19) . . ?
C7 N8 N1 127.82(18) . . ?
C3A N8 N1 109.75(16) . . ?
F3 P F5 89.31(15) . . ?
F3 P F4 92.50(15) . . ?
F5 P F4 177.97(14) . . ?
F3 P F1 91.12(11) . . ?
F5 P F1 90.79(11) . . ?
F4 P F1 90.07(11) . . ?
F3 P F6 178.41(13) . . ?
F5 P F6 89.59(13) . . ?
F4 P F6 88.57(12) . . ?
F1 P F6 90.05(9) . . ?
F3 P F2 89.33(11) . . ?
F5 P F2 89.88(12) . . ?
F4 P F2 89.24(11) . . ?
F1 P F2 179.19(11) . . ?
F6 P F2 89.52(10) . . ?
_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full 28.28
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max 1.065
_refine_diff_density_min -0.955
_refine_diff_density_rms 0.070
#===END