#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/96/4339660.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4339660
loop_
_publ_author_name
'Räisänen, Minna T'
'Runeberg, Nino'
'Klinga, Martti'
'Nieger, Martin'
'Bolte, Michael'
'Pyykkö, Pekka'
'Leskelä, Markku'
'Repo, Timo'
_publ_section_title
;
 Coordination of pyridinethiols in gold(I) complexes.
;
_journal_issue                   23
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9954
_journal_page_last               9960
_journal_paper_doi               10.1021/ic700453t
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         '4(C10 H10 N2 S2), 8 Cl, 2(C  O)'
_chemical_formula_sum            'C10.5 H10 Cl2 N2 O0.5 S2'
_chemical_formula_weight         307.23
_chemical_name_systematic
; 
 bis(2-pyridinium)disulfide dichloride methanol solvate 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.73(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.389(1)
_cell_length_b                   11.128(1)
_cell_length_c                   23.774(2)
_cell_measurement_reflns_used    2127
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.40
_cell_measurement_theta_min      4.30
_cell_volume                     1425.6(3)
_computing_cell_refinement       'COLLECT (Nonius, 2002)'
_computing_data_collection       'COLLECT (Nonius, 2002)'
_computing_data_reduction        'COLLECT (Nonius, 2002)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997)'
_computing_publication_material  'SHELXTL (Sheldrick, 1997)'
_computing_structure_refinement  'SHELX97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR2002 (Burla et al., 2003)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.907
_diffrn_measured_fraction_theta_max 0.907
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'Omega and Phi 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  0.0788
_diffrn_reflns_av_sigmaI/netI    0.0701
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            8229
_diffrn_reflns_theta_full        24.40
_diffrn_reflns_theta_max         24.40
_diffrn_reflns_theta_min         4.30
_exptl_absorpt_coefficient_mu    0.730
_exptl_absorpt_correction_T_max  0.9784
_exptl_absorpt_correction_T_min  0.7115
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            pale_yellow
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.550
_refine_diff_density_min         -0.462
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         2127
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0880
_refine_ls_R_factor_gt           0.0489
_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)+(0.0700P)²+0.3300P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1216
_refine_ls_wR_factor_ref         0.1409
_reflns_number_gt                1464
_reflns_number_total             2127
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic700453t-file001.cif
_cod_data_source_block           cos366-2y
_cod_original_sg_symbol_Hall     'P 2(1)/n'
_cod_original_sg_symbol_H-M      'P 2(1)/n'
_cod_original_formula_sum        'C10.50 H10 Cl2 N2 O0.50 S2'
_cod_database_code               4339660
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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
Cl1 Cl 1.01640(16) 0.80453(9) 0.06363(3) 0.0381(2) Uani 1 1 d . . .
Cl2 Cl -0.33287(14) 0.68504(9) 0.28103(4) 0.0361(2) Uani 1 1 d . . .
S1 S 0.51093(14) 0.87516(9) 0.17729(3) 0.0290(2) Uani 1 1 d . . .
N1 N 0.6446(4) 1.0000(3) 0.08808(10) 0.0284(7) Uani 1 1 d . . .
H1A H 0.7554 0.9420 0.0867 0.034 Uiso 1 1 calc R . .
S2 S 0.15861(14) 0.85619(9) 0.20626(3) 0.0302(2) Uani 1 1 d . . .
N2 N -0.0156(4) 0.8994(3) 0.30671(10) 0.0285(7) Uani 1 1 d . . .
H2B H -0.1183 0.8421 0.2959 0.034 Uiso 1 1 calc R . .
C1 C 0.4738(5) 0.9977(3) 0.12951(12) 0.0278(9) Uani 1 1 d . . .
C2 C 0.6508(6) 1.0877(4) 0.04901(13) 0.0365(10) Uani 1 1 d . . .
H2A H 0.7759 1.0870 0.0212 0.044 Uiso 1 1 calc R . .
C3 C 0.4802(7) 1.1767(4) 0.04909(16) 0.0427(11) Uani 1 1 d . . .
H3A H 0.4831 1.2382 0.0214 0.051 Uiso 1 1 calc R . .
C4 C 0.3006(7) 1.1766(4) 0.09045(16) 0.0415(10) Uani 1 1 d . . .
H4A H 0.1778 1.2379 0.0907 0.050 Uiso 1 1 calc R . .
C5 C 0.2986(6) 1.0887(4) 0.13114(14) 0.0325(9) Uani 1 1 d . . .
H5A H 0.1785 1.0904 0.1600 0.039 Uiso 1 1 calc R . .
C6 C 0.1708(5) 0.9303(3) 0.27224(12) 0.0256(8) Uani 1 1 d . . .
C7 C -0.0516(7) 0.9527(4) 0.35726(14) 0.0437(11) Uani 1 1 d . . .
H7A H -0.1868 0.9286 0.3799 0.052 Uiso 1 1 calc R . .
C8 C 0.1045(7) 1.0401(4) 0.37547(16) 0.0490(12) Uani 1 1 d . . .
H8A H 0.0770 1.0798 0.4102 0.059 Uiso 1 1 calc R . .
C9 C 0.3064(7) 1.0707(4) 0.34228(15) 0.0445(11) Uani 1 1 d . . .
H9A H 0.4227 1.1286 0.3556 0.053 Uiso 1 1 calc R . .
C10 C 0.3394(6) 1.0177(3) 0.29021(14) 0.0323(9) Uani 1 1 d . . .
H10A H 0.4743 1.0405 0.2672 0.039 Uiso 1 1 calc R . .
C21 C 0.4506(18) 0.9949(13) 0.5046(5) 0.070(3) Uiso 0.50 1 d PD A -1
O22 O 0.5862(16) 0.9037(10) 0.4716(4) 0.121(3) Uiso 0.50 1 d PD A -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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
C1 S1 S2 101.35(11)
C2 N1 C1 122.4(3)
C2 N1 H1A 118.8
C1 N1 H1A 118.8
C6 S2 S1 103.10(11)
C6 N2 C7 122.9(3)
C6 N2 H2B 118.6
C7 N2 H2B 118.6
N1 C1 C5 118.4(3)
N1 C1 S1 113.9(2)
C5 C1 S1 127.7(2)
N1 C2 C3 120.5(3)
N1 C2 H2A 119.8
C3 C2 H2A 119.8
C2 C3 C4 118.7(4)
C2 C3 H3A 120.6
C4 C3 H3A 120.6
C5 C4 C3 120.7(4)
C5 C4 H4A 119.7
C3 C4 H4A 119.7
C4 C5 C1 119.3(3)
C4 C5 H5A 120.4
C1 C5 H5A 120.4
N2 C6 C10 118.6(3)
N2 C6 S2 113.6(2)
C10 C6 S2 127.7(2)
C8 C7 N2 120.2(3)
C8 C7 H7A 119.9
N2 C7 H7A 119.9
C7 C8 C9 118.7(4)
C7 C8 H8A 120.6
C9 C8 H8A 120.6
C10 C9 C8 120.8(4)
C10 C9 H9A 119.6
C8 C9 H9A 119.6
C9 C10 C6 118.7(3)
C9 C10 H10A 120.7
C6 C10 H10A 120.7
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
S1 C1 1.785(4)
S1 S2 2.0389(11)
N1 C2 1.348(5)
N1 C1 1.357(4)
N1 H1A 0.8800
S2 C6 1.773(3)
N2 C6 1.349(4)
N2 C7 1.356(4)
N2 H2B 0.8800
C1 C5 1.385(5)
C2 C3 1.351(5)
C2 H2A 0.9500
C3 C4 1.389(5)
C3 H3A 0.9500
C4 C5 1.376(5)
C4 H4A 0.9500
C5 H5A 0.9500
C6 C10 1.395(5)
C7 C8 1.353(6)
C7 H7A 0.9500
C8 C9 1.394(5)
C8 H8A 0.9500
C9 C10 1.385(5)
C9 H9A 0.9500
C10 H10A 0.9500
C21 O22 1.481(16)
