#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/55/2215500.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2215500
loop_
_publ_author_name
'Broker, Grant A.'
'Tiekink, Edward R. T.'
_publ_section_title
;
 catena-Poly[[silver(I)-μ-1,4-di-4-pyridyl-2,3-diazabuta-1,3-diene]
 trifluoromethanesulfonate]
;
_journal_coeditor_code           HB2524
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2442
_journal_page_last               m2442
_journal_paper_doi               10.1107/S1600536807041888
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Ag (C12 H10 N4)] (C F3 S O3)'
_chemical_formula_moiety         'C12 H10 Ag N4 + , C F3 O3 S -'
_chemical_formula_sum            'C13 H10 Ag F3 N4 O3 S'
_chemical_formula_weight         467.18
_chemical_name_systematic
;
catena-Poly[[silver(I)-μ-1,4-di-4-pyridyl-2,3-diazabuta-1,3-diene]
trifluoromethanesulfonate]
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                75.99(3)
_cell_angle_beta                 71.09(3)
_cell_angle_gamma                83.30(3)
_cell_formula_units_Z            2
_cell_length_a                   8.9608(18)
_cell_length_b                   8.9816(18)
_cell_length_c                   10.804(2)
_cell_measurement_reflns_used    1270
_cell_measurement_temperature    98(2)
_cell_measurement_theta_max      30.2
_cell_measurement_theta_min      3.3
_cell_volume                     797.4(3)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC, 2005)'
_computing_data_collection       'CrystalClear (Rigaku/MSC, 2005)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC, 2005)'
_computing_molecular_graphics
;
ORTEPII (Johnson, 1976) and DIAMOND (Brandenburg, 2006)
;
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al.,  1994)'
_diffrn_ambient_temperature      98(2)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'Rigaku AFC12κ/SATURN724'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.036
_diffrn_reflns_av_sigmaI/netI    0.028
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            7718
_diffrn_reflns_theta_full        25.0
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         3.1
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.449
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.845
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.946
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             460
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.47
_refine_diff_density_min         -0.55
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.07
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         2695
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.07
_refine_ls_R_factor_all          0.026
_refine_ls_R_factor_gt           0.025
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0382P)²+0.6435P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.068
_refine_ls_wR_factor_ref         0.068
_reflns_number_gt                2654
_reflns_number_total             2695
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hb2524.cif
_cod_data_source_block           I
_cod_database_code               2215500
_cod_database_fobs_code          2215500
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
Ag Ag 0.36832(2) 0.36786(2) 0.060832(18) 0.02608(10) Uani d . 1
S S1 0.26232(8) 0.68538(8) 0.79915(7) 0.02863(17) Uani d . 1
F F1 -0.0358(2) 0.7776(2) 0.8486(2) 0.0571(5) Uani d . 1
F F2 0.1221(3) 0.9605(2) 0.7756(2) 0.0600(6) Uani d . 1
F F3 0.0766(3) 0.8337(2) 0.9775(2) 0.0568(6) Uani d . 1
O O1 0.2826(3) 0.7020(3) 0.6605(2) 0.0583(7) Uani d . 1
O O2 0.2017(3) 0.5404(2) 0.8843(3) 0.0469(6) Uani d . 1
O O3 0.3899(3) 0.7370(3) 0.8300(2) 0.0436(5) Uani d . 1
N N1 0.2426(3) 0.4890(2) 0.2149(2) 0.0215(4) Uani d . 1
N N2 -0.1451(3) 0.8152(2) 0.5065(2) 0.0247(5) Uani d . 1
N N3 -0.1980(3) 0.8996(3) 0.6078(2) 0.0273(5) Uani d . 1
N N4 -0.5349(3) 1.2325(2) 0.9117(2) 0.0219(4) Uani d . 1
C C1 0.3015(3) 0.5068(3) 0.3104(3) 0.0234(5) Uani d . 1
H H1 0.4007 0.4581 0.3132 0.028 Uiso calc R 1
C C2 0.2238(3) 0.5927(3) 0.4042(3) 0.0223(5) Uani d . 1
H H2 0.2690 0.6028 0.4700 0.027 Uiso calc R 1
C C3 0.0771(3) 0.6650(3) 0.4012(2) 0.0215(5) Uani d . 1
C C4 0.0148(3) 0.6433(3) 0.3041(3) 0.0236(5) Uani d . 1
H H4 -0.0855 0.6882 0.3005 0.028 Uiso calc R 1
C C5 0.1001(3) 0.5563(3) 0.2138(3) 0.0251(5) Uani d . 1
H H5 0.0568 0.5430 0.1479 0.030 Uiso calc R 1
C C6 -0.0050(3) 0.7582(3) 0.4990(3) 0.0231(5) Uani d . 1
H H6 0.0462 0.7768 0.5580 0.028 Uiso calc R 1
C C7 -0.3364(3) 0.9599(3) 0.6199(3) 0.0277(6) Uani d . 1
H H7 -0.3941 0.9449 0.5644 0.033 Uiso calc R 1
C C8 -0.4057(3) 1.0528(3) 0.7210(3) 0.0237(5) Uani d . 1
C C9 -0.3297(3) 1.0618(3) 0.8132(3) 0.0225(5) Uani d . 1
H H9 -0.2320 1.0071 0.8118 0.027 Uiso calc R 1
C C10 -0.3976(3) 1.1503(3) 0.9058(2) 0.0216(5) Uani d . 1
H H10 -0.3455 1.1540 0.9689 0.026 Uiso calc R 1
C C11 -0.6086(3) 1.2238(3) 0.8233(3) 0.0289(6) Uani d . 1
H H11 -0.7058 1.2803 0.8266 0.035 Uiso calc R 1
C C12 -0.5486(3) 1.1358(3) 0.7276(3) 0.0299(6) Uani d . 1
H H12 -0.6042 1.1321 0.6671 0.036 Uiso calc R 1
C C13 0.0992(3) 0.8217(3) 0.8526(3) 0.0298(6) Uani d . 1
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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 Ag N4 . 1_644 172.36(8) y
N1 Ag Ag . 2_665 89.29(6) ?
N4 Ag Ag 1_644 2_665 97.80(6) ?
O1 S1 O3 . . 115.54(16) ?
O1 S1 O2 . . 115.44(17) ?
O3 S1 O2 . . 113.75(15) ?
O1 S1 C13 . . 103.95(14) ?
O3 S1 C13 . . 103.31(13) ?
O2 S1 C13 . . 102.47(14) ?
C5 N1 C1 . . 118.0(2) ?
C5 N1 Ag . . 118.75(17) ?
C1 N1 Ag . . 123.24(17) ?
C6 N2 N3 . . 110.3(2) ?
C7 N3 N2 . . 113.4(2) ?
C11 N4 C10 . . 117.7(2) ?
C11 N4 Ag . 1_466 122.05(17) ?
C10 N4 Ag . 1_466 120.26(17) ?
N1 C1 C2 . . 122.8(2) ?
N1 C1 H1 . . 118.6 ?
C2 C1 H1 . . 118.6 ?
C1 C2 C3 . . 119.1(2) ?
C1 C2 H2 . . 120.5 ?
C3 C2 H2 . . 120.5 ?
C4 C3 C2 . . 118.0(2) ?
C4 C3 C6 . . 122.6(2) ?
C2 C3 C6 . . 119.4(2) ?
C5 C4 C3 . . 119.4(2) ?
C5 C4 H4 . . 120.3 ?
C3 C4 H4 . . 120.3 ?
N1 C5 C4 . . 122.8(2) ?
N1 C5 H5 . . 118.6 ?
C4 C5 H5 . . 118.6 ?
N2 C6 C3 . . 121.0(2) ?
N2 C6 H6 . . 119.5 ?
C3 C6 H6 . . 119.5 ?
N3 C7 C8 . . 119.1(2) ?
N3 C7 H7 . . 120.4 ?
C8 C7 H7 . . 120.4 ?
C12 C8 C9 . . 117.9(2) ?
C12 C8 C7 . . 121.2(2) ?
C9 C8 C7 . . 121.0(2) ?
C10 C9 C8 . . 119.4(2) ?
C10 C9 H9 . . 120.3 ?
C8 C9 H9 . . 120.3 ?
N4 C10 C9 . . 123.1(2) ?
N4 C10 H10 . . 118.4 ?
C9 C10 H10 . . 118.4 ?
N4 C11 C12 . . 122.7(2) ?
N4 C11 H11 . . 118.6 ?
C12 C11 H11 . . 118.6 ?
C11 C12 C8 . . 119.3(2) ?
C11 C12 H12 . . 120.4 ?
C8 C12 H12 . . 120.4 ?
F2 C13 F3 . . 107.5(2) ?
F2 C13 F1 . . 106.6(2) ?
F3 C13 F1 . . 107.1(3) ?
F2 C13 S1 . . 112.5(2) ?
F3 C13 S1 . . 111.70(18) ?
F1 C13 S1 . . 111.1(2) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ag N1 . 2.144(2) y
Ag N4 1_644 2.150(2) y
Ag Ag 2_665 3.2738(13) n
S1 O1 . 1.422(2) ?
S1 O3 . 1.442(2) ?
S1 O2 . 1.449(3) ?
S1 C13 . 1.830(3) ?
F1 C13 . 1.333(3) ?
F2 C13 . 1.317(3) ?
F3 C13 . 1.328(3) ?
N1 C5 . 1.350(3) ?
N1 C1 . 1.351(3) ?
N2 C6 . 1.284(4) ?
N2 N3 . 1.407(3) ?
N3 C7 . 1.273(4) ?
N4 C11 . 1.346(3) ?
N4 C10 . 1.350(3) ?
N4 Ag 1_466 2.150(2) ?
C1 C2 . 1.379(4) ?
C1 H1 . 0.9500 ?
C2 C3 . 1.403(4) ?
C2 H2 . 0.9500 ?
C3 C4 . 1.397(4) ?
C3 C6 . 1.463(3) ?
C4 C5 . 1.376(4) ?
C4 H4 . 0.9500 ?
C5 H5 . 0.9500 ?
C6 H6 . 0.9500 ?
C7 C8 . 1.469(4) ?
C7 H7 . 0.9500 ?
C8 C12 . 1.395(4) ?
C8 C9 . 1.397(4) ?
C9 C10 . 1.372(4) ?
C9 H9 . 0.9500 ?
C10 H10 . 0.9500 ?
C11 C12 . 1.385(4) ?
C11 H11 . 0.9500 ?
C12 H12 . 0.9500 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
C2 H2 O1 1_555 0.95 2.47 3.360(4) 155 y
C10 H10 O3 2_577 0.95 2.49 3.274(3) 139 y
C11 H11 O2 1_465 0.95 2.54 3.235(4) 130 y
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_site_symmetry_1
_geom_torsion
Ag Ag N1 C5 2_665 111.84(19)
Ag Ag N1 C1 2_665 -65.45(19)
C6 N2 N3 C7 . 179.7(2)
C5 N1 C1 C2 . -1.3(4)
Ag N1 C1 C2 . 176.01(19)
N1 C1 C2 C3 . 0.1(4)
C1 C2 C3 C4 . 1.4(4)
C1 C2 C3 C6 . -179.1(2)
C2 C3 C4 C5 . -1.7(4)
C6 C3 C4 C5 . 178.9(2)
C1 N1 C5 C4 . 1.0(4)
Ag N1 C5 C4 . -176.4(2)
C3 C4 C5 N1 . 0.4(4)
N3 N2 C6 C3 . 180.0(2)
C4 C3 C6 N2 . 5.4(4)
C2 C3 C6 N2 . -174.0(2)
N2 N3 C7 C8 . -179.3(2)
N3 C7 C8 C12 . 172.3(3)
N3 C7 C8 C9 . -7.2(4)
C12 C8 C9 C10 . 0.2(4)
C7 C8 C9 C10 . 179.7(2)
C11 N4 C10 C9 . 1.2(4)
Ag N4 C10 C9 1_466 179.98(19)
C8 C9 C10 N4 . -1.0(4)
C10 N4 C11 C12 . -0.5(4)
Ag N4 C11 C12 1_466 -179.3(2)
N4 C11 C12 C8 . -0.3(4)
C9 C8 C12 C11 . 0.5(4)
C7 C8 C12 C11 . -179.1(3)
O1 S1 C13 F2 . -51.7(3)
O3 S1 C13 F2 . 69.4(2)
O2 S1 C13 F2 . -172.2(2)
O1 S1 C13 F3 . -172.7(2)
O3 S1 C13 F3 . -51.7(2)
O2 S1 C13 F3 . 66.7(2)
O1 S1 C13 F1 . 67.8(2)
O3 S1 C13 F1 . -171.2(2)
O2 S1 C13 F1 . -52.7(2)
