#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/92/4079248.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_4079248
loop_
_publ_author_name
'Slivarichova, Miriam'
'Reading, Eamonn'
'Haddow, Mairi F.'
'Othman, Hafiizah'
'Owen, Gareth R.'
_publ_section_title
;
 Silver and Palladium Complexes Containing Ditopic N-Heterocyclic
 Carbene--Thione Ligands
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              6595
_journal_paper_doi               10.1021/om300615e
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C18 H26 Ag2 Br4 N8 S2'
_chemical_formula_sum            'C18 H26 Ag2 Br4 N8 S2'
_chemical_formula_weight         953.97
_chemical_name_common            Complex_5.HBr
_chemical_name_systematic
; 
 ? 
;
_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                66.577(2)
_cell_angle_beta                 68.908(2)
_cell_angle_gamma                64.231(2)
_cell_formula_units_Z            1
_cell_length_a                   9.3422(5)
_cell_length_b                   9.4522(5)
_cell_length_c                   10.2640(5)
_cell_measurement_reflns_used    8129
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.56
_cell_measurement_theta_min      2.73
_cell_volume                     729.52(7)
_computing_cell_refinement       'Bruker Apex II'
_computing_data_collection       'Bruker Apex II'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker ShelXTL'
_computing_publication_material  'Bruker ShelXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker Apex II kappa CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0237
_diffrn_reflns_av_sigmaI/netI    0.0219
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            12257
_diffrn_reflns_theta_full        27.56
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         2.50
_exptl_absorpt_coefficient_mu    6.986
_exptl_absorpt_correction_T_max  0.1512
_exptl_absorpt_correction_T_min  0.0829
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.171
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             456
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.594
_refine_diff_density_min         -0.399
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     156
_refine_ls_number_reflns         3344
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0193
_refine_ls_R_factor_gt           0.0173
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0160P)²+0.4420P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0399
_refine_ls_wR_factor_ref         0.0409
_reflns_number_gt                3116
_reflns_number_total             3344
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300615e_si_002.cif
_cod_data_source_block           complex_5.HBr_ms22_0m
_cod_original_sg_symbol_Hall     -P1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4079248
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Ag1 Ag 0.492938(19) 0.583970(19) 0.826709(17) 0.02144(5) Uani 1 1 d .
Br1 Br 0.27193(2) 0.83826(3) 0.69035(2) 0.02255(6) Uani 1 1 d .
Br2 Br 0.40108(2) 0.32629(2) 1.00587(2) 0.01889(5) Uani 1 1 d .
C1 C 0.8923(2) 0.4836(2) 0.7213(2) 0.0161(4) Uani 1 1 d .
C2 C 0.8890(3) 0.2141(2) 0.9007(2) 0.0228(4) Uani 1 1 d .
H2A H 0.7732 0.2498 0.9017 0.034 Uiso 1 1 calc R
H2B H 0.9041 0.1622 1.0008 0.034 Uiso 1 1 calc R
H2C H 0.9532 0.1350 0.8441 0.034 Uiso 1 1 calc R
C3 C 1.0512(2) 0.3799(3) 0.8799(2) 0.0209(4) Uani 1 1 d .
H3 H 1.1024 0.3081 0.9586 0.025 Uiso 1 1 calc R
C4 C 1.0706(2) 0.5224(3) 0.7932(2) 0.0211(4) Uani 1 1 d .
H4 H 1.1386 0.5705 0.7978 0.025 Uiso 1 1 calc R
C5 C 0.9500(3) 0.7430(2) 0.5852(2) 0.0214(4) Uani 1 1 d .
H5A H 0.9227 0.7383 0.5027 0.026 Uiso 1 1 calc R
H5B H 1.0535 0.7661 0.5480 0.026 Uiso 1 1 calc R
C6 C 0.6621(2) 0.9233(2) 0.6477(2) 0.0181(4) Uani 1 1 d .
H6 H 0.6139 0.8754 0.6168 0.022 Uiso 1 1 calc R
C7 C 0.4087(3) 1.1409(3) 0.7240(3) 0.0313(5) Uani 1 1 d .
H7A H 0.3867 1.2301 0.6350 0.047 Uiso 1 1 calc R
H7B H 0.3728 1.1867 0.8055 0.047 Uiso 1 1 calc R
H7C H 0.3494 1.0677 0.7453 0.047 Uiso 1 1 calc R
C8 C 0.6946(3) 1.0831(3) 0.7342(2) 0.0250(5) Uani 1 1 d .
H8 H 0.6709 1.1679 0.7743 0.030 Uiso 1 1 calc R
C9 C 0.8427(3) 0.9745(3) 0.6972(2) 0.0242(5) Uani 1 1 d .
H9 H 0.9433 0.9672 0.7068 0.029 Uiso 1 1 calc R
N1 N 0.9431(2) 0.3554(2) 0.83460(18) 0.0167(3) Uani 1 1 d .
N2 N 0.9720(2) 0.5867(2) 0.69498(18) 0.0177(3) Uani 1 1 d .
N3 N 0.8202(2) 0.8758(2) 0.64258(18) 0.0180(3) Uani 1 1 d .
N4 N 0.5839(2) 1.0486(2) 0.70330(18) 0.0195(4) Uani 1 1 d .
S1 S 0.75901(6) 0.51094(6) 0.62897(5) 0.01910(10) Uani 1 1 d .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
S1 Ag1 Br1 107.070(14) . .
S1 Ag1 Br2 113.940(14) . .
Br1 Ag1 Br2 116.563(9) . .
S1 Ag1 Br2 100.609(13) . 2_667
Br1 Ag1 Br2 111.695(9) . 2_667
Br2 Ag1 Br2 105.861(8) . 2_667
S1 Ag1 Ag1 119.043(13) . 2_667
Br1 Ag1 Ag1 132.536(10) . 2_667
Br2 Ag1 Ag1 54.443(6) . 2_667
Br2 Ag1 Ag1 51.418(7) 2_667 2_667
Ag1 Br2 Ag1 74.138(8) . 2_667
N1 C1 N2 105.33(16) . .
N1 C1 S1 127.74(15) . .
N2 C1 S1 126.93(15) . .
N1 C2 H2A 109.5 . .
N1 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
N1 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
C4 C3 N1 107.79(18) . .
C4 C3 H3 126.1 . .
N1 C3 H3 126.1 . .
C3 C4 N2 106.67(18) . .
C3 C4 H4 126.7 . .
N2 C4 H4 126.7 . .
N2 C5 N3 111.75(16) . .
N2 C5 H5A 109.3 . .
N3 C5 H5A 109.3 . .
N2 C5 H5B 109.3 . .
N3 C5 H5B 109.3 . .
H5A C5 H5B 107.9 . .
N4 C6 N3 108.12(17) . .
N4 C6 H6 125.9 . .
N3 C6 H6 125.9 . .
N4 C7 H7A 109.5 . .
N4 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
N4 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
C9 C8 N4 107.23(19) . .
C9 C8 H8 126.4 . .
N4 C8 H8 126.4 . .
C8 C9 N3 106.67(19) . .
C8 C9 H9 126.7 . .
N3 C9 H9 126.7 . .
C1 N1 C3 110.07(16) . .
C1 N1 C2 124.66(17) . .
C3 N1 C2 125.26(17) . .
C1 N2 C4 110.14(17) . .
C1 N2 C5 124.30(17) . .
C4 N2 C5 125.51(18) . .
C6 N3 C9 108.90(17) . .
C6 N3 C5 125.73(17) . .
C9 N3 C5 125.36(18) . .
C6 N4 C8 109.07(17) . .
C6 N4 C7 126.01(18) . .
C8 N4 C7 124.88(18) . .
C1 S1 Ag1 97.59(7) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ag1 S1 2.6010(5) .
Ag1 Br1 2.6626(3) .
Ag1 Br2 2.6779(3) .
Ag1 Br2 2.7868(3) 2_667
Ag1 Ag1 3.2952(3) 2_667
Br2 Ag1 2.7869(3) 2_667
C1 N1 1.350(2) .
C1 N2 1.362(3) .
C1 S1 1.700(2) .
C2 N1 1.456(3) .
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C2 H2C 0.9800 .
C3 C4 1.335(3) .
C3 N1 1.384(3) .
C3 H3 0.9500 .
C4 N2 1.389(3) .
C4 H4 0.9500 .
C5 N2 1.439(3) .
C5 N3 1.464(3) .
C5 H5A 0.9900 .
C5 H5B 0.9900 .
C6 N4 1.322(3) .
C6 N3 1.331(3) .
C6 H6 0.9500 .
C7 N4 1.463(3) .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
C8 C9 1.346(3) .
C8 N4 1.374(3) .
C8 H8 0.9500 .
C9 N3 1.378(3) .
C9 H9 0.9500 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
S1 Ag1 Br2 Ag1 109.607(15) . 2_667
Br1 Ag1 Br2 Ag1 -124.869(11) . 2_667
Br2 Ag1 Br2 Ag1 0.0 2_667 2_667
N1 C3 C4 N2 0.7(2) . .
N4 C8 C9 N3 0.6(3) . .
N2 C1 N1 C3 1.0(2) . .
S1 C1 N1 C3 -179.62(15) . .
N2 C1 N1 C2 179.88(17) . .
S1 C1 N1 C2 -0.7(3) . .
C4 C3 N1 C1 -1.1(2) . .
C4 C3 N1 C2 -179.95(18) . .
N1 C1 N2 C4 -0.6(2) . .
S1 C1 N2 C4 -179.97(15) . .
N1 C1 N2 C5 -177.87(17) . .
S1 C1 N2 C5 2.7(3) . .
C3 C4 N2 C1 -0.1(2) . .
C3 C4 N2 C5 177.20(18) . .
N3 C5 N2 C1 90.3(2) . .
N3 C5 N2 C4 -86.6(2) . .
N4 C6 N3 C9 0.1(2) . .
N4 C6 N3 C5 -178.56(17) . .
C8 C9 N3 C6 -0.5(2) . .
C8 C9 N3 C5 178.24(18) . .
N2 C5 N3 C6 -87.2(2) . .
N2 C5 N3 C9 94.4(2) . .
N3 C6 N4 C8 0.2(2) . .
N3 C6 N4 C7 178.06(19) . .
C9 C8 N4 C6 -0.5(2) . .
C9 C8 N4 C7 -178.4(2) . .
N1 C1 S1 Ag1 74.65(18) . .
N2 C1 S1 Ag1 -106.07(17) . .
Br1 Ag1 S1 C1 136.14(7) . .
Br2 Ag1 S1 C1 -93.46(7) . .
Br2 Ag1 S1 C1 19.33(7) 2_667 .
Ag1 Ag1 S1 C1 -32.23(7) 2_667 .
