#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/43/2014338.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_2014338
loop_
_publ_author_name
'Hamamci, Sevim'
'Yilmaz, Veysel T.'
'Büyükgüngör, Orhan'
_publ_section_title
;
 Monoclinic and triclinic concomitant polymorphs of
 di-μ-pyridazine-1κ²N:2κ²N'-bis[(saccharinato)silver(I)]
;
_journal_coeditor_code           GD1419
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m1
_journal_page_last               m3
_journal_paper_doi               10.1107/S0108270105036334
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Ag2 (C7 H4 N O3 S)2 (C4 H4 N2)2]'
_chemical_formula_moiety         'C22 H16 Ag2 N6 O6 S2'
_chemical_formula_sum            'C22 H16 Ag2 N6 O6 S2'
_chemical_formula_weight         740.27
_chemical_name_systematic
;
di-μ-pyridazine-1κ²N:2\kN'-bis[(saccharinato)silver(I)]
;
_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           SHELXL-97
_cell_angle_alpha                73.090(9)
_cell_angle_beta                 83.087(10)
_cell_angle_gamma                71.148(9)
_cell_formula_units_Z            1
_cell_length_a                   7.3231(8)
_cell_length_b                   7.7516(9)
_cell_length_c                   11.5389(14)
_cell_measurement_reflns_used    10253
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.03
_cell_measurement_theta_min      2.88
_cell_volume                     592.82(13)
_computing_cell_refinement       X-AREA
_computing_data_collection       'X-AREA (Stoe & Cie, 2002)'
_computing_data_reduction        'X-RED (Stoe & Cie, 2002)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'STOE IPDS-2'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0991
_diffrn_reflns_av_sigmaI/netI    0.0678
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10253
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         27.57
_diffrn_reflns_theta_min         2.88
_diffrn_standards_decay_%        <2
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.882
_exptl_absorpt_correction_T_max  0.5786
_exptl_absorpt_correction_T_min  0.3682
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(X-RED; Stoe & Cie, 2002)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.074
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'prismatic stick'
_exptl_crystal_F_000             364
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.510
_exptl_crystal_size_min          0.330
_refine_diff_density_max         0.738
_refine_diff_density_min         -1.185
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         2320
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0289
_refine_ls_R_factor_gt           0.0251
_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)+(0.03P)²+0.5506P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0658
_refine_ls_wR_factor_ref         0.0664
_reflns_number_gt                2650
_reflns_number_total             2737
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            gd1419.cif
_cod_data_source_block           II
_cod_original_cell_volume        592.82(12)
_cod_original_sg_symbol_Hall     '-P 1n'
_cod_database_code               2014338
_cod_database_fobs_code          2014338
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_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
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
C1 0.2961(4) 0.6328(3) 0.8038(3) 0.0184(5) Uani d . 1 . . C
C2 0.2856(4) 0.7137(4) 0.8978(3) 0.0206(5) Uani d . 1 . . C
H2 0.3318 0.6410 0.9739 0.025 Uiso calc R 1 . . H
C3 0.2027(4) 0.9086(4) 0.8727(3) 0.0236(6) Uani d . 1 . . C
H3 0.1949 0.9686 0.9330 0.028 Uiso calc R 1 . . H
C4 0.1310(4) 1.0157(4) 0.7585(3) 0.0241(6) Uani d . 1 . . C
H4 0.0743 1.1458 0.7444 0.029 Uiso calc R 1 . . H
C5 0.1428(4) 0.9318(4) 0.6657(3) 0.0212(5) Uani d . 1 . . C
H5 0.0949 1.0036 0.5897 0.025 Uiso calc R 1 . . H
C6 0.2285(4) 0.7371(4) 0.6895(2) 0.0187(5) Uani d . 1 . . C
C7 0.2542(4) 0.6145(3) 0.6054(3) 0.0192(5) Uani d . 1 . . C
C8 0.2204(4) 0.4099(4) 0.3283(3) 0.0205(5) Uani d . 1 . . C
H8 0.1923 0.5083 0.3648 0.025 Uiso calc R 1 . . H
C9 0.1538(4) 0.4492(4) 0.2127(3) 0.0216(5) Uani d . 1 . . C
H9 0.0847 0.5715 0.1719 0.026 Uiso calc R 1 . . H
C10 0.1926(4) 0.3040(4) 0.1612(3) 0.0223(5) Uani d . 1 . . C
H10 0.1497 0.3229 0.0846 0.027 Uiso calc R 1 . . H
C11 0.2997(4) 0.1248(4) 0.2281(3) 0.0214(5) Uani d . 1 . . C
H11 0.3274 0.0237 0.1942 0.026 Uiso calc R 1 . . H
N1 0.3338(3) 0.4268(3) 0.6626(2) 0.0201(4) Uani d . 1 . . N
N2 0.3230(3) 0.2371(3) 0.3892(2) 0.0198(4) Uani d . 1 . . N
N3 0.3635(3) 0.0922(3) 0.3375(2) 0.0205(5) Uani d . 1 . . N
O1 0.2573(3) 0.2919(2) 0.88383(18) 0.0223(4) Uani d . 1 . . O
O2 0.5813(3) 0.3087(3) 0.82572(19) 0.0241(4) Uani d . 1 . . O
O3 0.2102(3) 0.6773(3) 0.49987(18) 0.0252(4) Uani d . 1 . . O
S1 0.37842(9) 0.39200(8) 0.80332(6) 0.01781(14) Uani d . 1 . . S
Ag1 0.44028(3) 0.19733(2) 0.571644(17) 0.02225(9) Uani d . 1 . . Ag
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'
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
C2 C1 C6 . . 123.0(2) ?
C2 C1 S1 . . 129.7(2) ?
C6 C1 S1 . . 107.2(2) ?
C1 C2 C3 . . 116.8(3) ?
C1 C2 H2 . . 121.6 ?
C3 C2 H2 . . 121.6 ?
C2 C3 C4 . . 121.0(3) ?
C2 C3 H3 . . 119.5 ?
C4 C3 H3 . . 119.5 ?
C5 C4 C3 . . 121.2(2) ?
C5 C4 H4 . . 119.4 ?
C3 C4 H4 . . 119.4 ?
C4 C5 C6 . . 118.1(3) ?
C4 C5 H5 . . 121.0 ?
C6 C5 H5 . . 121.0 ?
C1 C6 C5 . . 119.9(3) ?
C1 C6 C7 . . 112.2(2) ?
C5 C6 C7 . . 127.9(3) ?
O3 C7 N1 . . 125.2(3) ?
O3 C7 C6 . . 123.2(2) ?
N1 C7 C6 . . 111.6(2) ?
N2 C8 C9 . . 122.8(2) ?
N2 C8 H8 . . 118.6 ?
C9 C8 H8 . . 118.6 ?
C10 C9 C8 . . 118.1(2) ?
C10 C9 H9 . . 120.9 ?
C8 C9 H9 . . 120.9 ?
C9 C10 C11 . . 117.3(3) ?
C9 C10 H10 . . 121.3 ?
C11 C10 H10 . . 121.3 ?
N3 C11 C10 . . 123.1(2) ?
N3 C11 H11 . . 118.4 ?
C10 C11 H11 . . 118.4 ?
C7 N1 S1 . . 112.50(19) ?
C7 N1 Ag1 . . 125.13(19) ?
S1 N1 Ag1 . . 121.53(11) ?
C8 N2 N3 . . 119.1(2) ?
C8 N2 Ag1 . . 119.04(18) ?
N3 N2 Ag1 . . 121.71(16) ?
C11 N3 N2 . . 119.4(2) ?
C11 N3 Ag1 . 2_656 119.65(17) ?
N2 N3 Ag1 . 2_656 120.72(17) ?
O2 S1 O1 . . 114.46(11) ?
O2 S1 N1 . . 111.56(12) ?
O1 S1 N1 . . 111.23(12) ?
O2 S1 C1 . . 112.10(12) ?
O1 S1 C1 . . 109.65(12) ?
N1 S1 C1 . . 96.45(12) ?
N1 Ag1 N2 . . 119.53(8) yes
N1 Ag1 N3 . 2_656 122.52(9) yes
N3 Ag1 N2 2_656 . 117.54(8) yes
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
C1 C2 . 1.385(4) ?
C1 C6 . 1.384(4) ?
C1 S1 . 1.768(2) ?
C2 C3 . 1.390(4) ?
C2 H2 . 0.9300 ?
C3 C4 . 1.397(4) ?
C3 H3 . 0.9300 ?
C4 C5 . 1.387(4) ?
C4 H4 . 0.9300 ?
C5 C6 . 1.391(4) ?
C5 H5 . 0.9300 ?
C6 C7 . 1.503(4) ?
C7 O3 . 1.213(4) ?
C7 N1 . 1.371(3) ?
C8 N2 . 1.334(3) ?
C8 C9 . 1.391(4) ?
C8 H8 . 0.9300 ?
C9 C10 . 1.357(4) ?
C9 H9 . 0.9300 ?
C10 C11 . 1.400(4) ?
C10 H10 . 0.9300 ?
C11 N3 . 1.324(4) ?
C11 H11 . 0.9300 ?
N1 S1 . 1.623(2) ?
N2 N3 . 1.356(3) ?
O2 S1 . 1.438(2) ?
O1 S1 . 1.4418(19) ?
N1 Ag1 . 2.206(2) yes
N2 Ag1 . 2.270(2) yes
N3 Ag1 2_656 2.261(2) yes
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
C3 H3 O1 1_565 0.93 2.58 3.163(3) 121
C8 H8 O3 . 0.93 2.35 3.236(3) 160
C9 H9 O1 2_566 0.93 2.47 3.152(3) 131
C10 H10 O1 1_554 0.93 2.41 3.203(4) 143
C11 H11 O2 2_656 0.93 2.52 3.410(3) 161
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_4
_geom_torsion
C6 C1 C2 C3 . -0.1(4)
S1 C1 C2 C3 . -176.2(2)
C1 C2 C3 C4 . 1.1(4)
C2 C3 C4 C5 . -1.0(4)
C3 C4 C5 C6 . 0.0(4)
C2 C1 C6 C5 . -1.0(4)
S1 C1 C6 C5 . 175.9(2)
C2 C1 C6 C7 . -179.0(2)
S1 C1 C6 C7 . -2.1(3)
C4 C5 C6 C1 . 1.0(4)
C4 C5 C6 C7 . 178.6(2)
C1 C6 C7 O3 . -177.7(2)
C5 C6 C7 O3 . 4.5(4)
C1 C6 C7 N1 . 1.8(3)
C5 C6 C7 N1 . -176.0(2)
N2 C8 C9 C10 . 1.2(4)
C8 C9 C10 C11 . -0.8(4)
C9 C10 C11 N3 . -0.1(4)
O3 C7 N1 S1 . 179.0(2)
C6 C7 N1 S1 . -0.5(3)
O3 C7 N1 Ag1 . 9.4(4)
C6 C7 N1 Ag1 . -170.09(16)
C9 C8 N2 N3 . -0.6(4)
C9 C8 N2 Ag1 . 175.75(19)
C10 C11 N3 N2 . 0.7(4)
C10 C11 N3 Ag1 2_656 -174.0(2)
C8 N2 N3 C11 . -0.4(4)
Ag1 N2 N3 C11 . -176.60(18)
C8 N2 N3 Ag1 2_656 174.24(18)
Ag1 N2 N3 Ag1 2_656 -2.0(3)
C7 N1 S1 O2 . -117.49(19)
Ag1 N1 S1 O2 . 52.53(16)
C7 N1 S1 O1 . 113.38(19)
Ag1 N1 S1 O1 . -76.60(16)
C7 N1 S1 C1 . -0.6(2)
Ag1 N1 S1 C1 . 169.38(13)
C2 C1 S1 O2 . -65.3(3)
C6 C1 S1 O2 . 118.06(19)
C2 C1 S1 O1 . 62.9(3)
C6 C1 S1 O1 . -113.66(19)
C2 C1 S1 N1 . 178.2(2)
C6 C1 S1 N1 . 1.6(2)
C7 N1 Ag1 N3 2_656 163.75(19)
S1 N1 Ag1 N3 2_656 -4.96(18)
C7 N1 Ag1 N2 . -23.8(2)
S1 N1 Ag1 N2 . 167.46(12)
C8 N2 Ag1 N1 . 12.9(2)
N3 N2 Ag1 N1 . -170.85(17)
C8 N2 Ag1 N3 2_656 -174.31(18)
N3 N2 Ag1 N3 2_656 1.9(2)
