#------------------------------------------------------------------------------
#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/05/7010584.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_7010584
loop_
_publ_author_name
'Maiti, Rabindranath'
'Shang, Maoyu'
'Lappin, A. Graham'
_publ_section_title
;
 The chemistry of ruthenium complexes of 1,2-dicyanoethylene dithiolate
 (mnt2--). Synthesis and characterization of [RuIV/III(mnt)3]2--/3--
 and the derivatives trans-[RuIII(mnt)2(PPh3)2]--,
 trans-[RuIII(mnt)2(py)2]-- and trans-[RuIV(mnt)2(Br)2]2--
;
_journal_issue                   2
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              244
_journal_paper_doi               10.1039/b100603g
_journal_year                    2002
_chemical_formula_moiety         '2(C8 H20 N 1+), (C8 Br2 N4 Ru S4 2-)'
_chemical_formula_sum            'C24 H40 Br2 N6 Ru S4'
_chemical_formula_weight         801.75
_chemical_name_systematic
; 
(Et4N)2Ru[S2C2(CN)2]2Br2 
;
_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                75.457(7)
_cell_angle_beta                 88.446(7)
_cell_angle_gamma                81.798(7)
_cell_formula_units_Z            1
_cell_length_a                   7.2017(6)
_cell_length_b                   9.4615(8)
_cell_length_c                   12.5828(12)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      16
_cell_measurement_theta_min      15
_cell_volume                     821.38(13)
_computing_cell_refinement       'CAD4-ARGUS (Enraf-Nonius, 1994)'
_computing_data_collection       'CAD4-ARGUS (Enraf-Nonius, 1994)'
_computing_data_reduction
;
Chi90s (Boyle, 1997), Xcad4 (Harms, 1996), SHELXTL-v5 (Siemens, 1994)
;
_computing_molecular_graphics    'ORTEP-III for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXTL-v5 (Siemens, 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Enraf-Nonius CAD4'
_diffrn_measurement_method       ω/2θ
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0223
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            2891
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.25
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 200
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.188
_exptl_absorpt_correction_T_max  0.6240
_exptl_absorpt_correction_T_min  0.4260
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
Absorption correction was based on psi-scan data of 6 reflecations 
(North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351).
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.621
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate-like
_exptl_crystal_F_000             404
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.430
_refine_diff_density_min         -0.316
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     169
_refine_ls_number_reflns         2891
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.0322
_refine_ls_R_factor_gt           0.0261
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0343P)²+0.3862P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0632
_refine_ls_wR_factor_ref         0.0657
_reflns_number_gt                2510
_reflns_number_total             2891
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b100603g.txt
_cod_data_source_block           la1806
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 
;
_cod_database_code               7010584
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru Ru 0.5000 0.5000 0.5000 0.03728(10) Uani 1 2 d S . .
Br Br 0.55425(5) 0.24091(3) 0.46364(2) 0.05552(11) Uani 1 1 d . . .
S1 S 0.65891(10) 0.40745(8) 0.66287(5) 0.04253(17) Uani 1 1 d . . .
S2 S 0.22990(10) 0.44168(9) 0.58965(6) 0.04593(18) Uani 1 1 d . . .
C1 C 0.4900(4) 0.3442(3) 0.7524(2) 0.0387(6) Uani 1 1 d . . .
C2 C 0.5433(4) 0.2743(3) 0.8648(2) 0.0461(7) Uani 1 1 d . . .
N1 N 0.5839(4) 0.2174(3) 0.9534(2) 0.0649(8) Uani 1 1 d . . .
C3 C 0.3050(4) 0.3575(3) 0.7204(2) 0.0401(6) Uani 1 1 d . . .
C4 C 0.1703(4) 0.3002(4) 0.7989(2) 0.0501(7) Uani 1 1 d . . .
N2 N 0.0649(4) 0.2531(4) 0.8627(2) 0.0790(10) Uani 1 1 d . . .
N3 N 0.9041(3) 0.8265(2) 0.78117(17) 0.0393(5) Uani 1 1 d . . .
C5 C 0.7571(4) 0.9248(4) 0.8272(3) 0.0546(8) Uani 1 1 d . . .
H5A H 0.8071 1.0142 0.8287 0.066 Uiso 1 1 calc R . .
H5B H 0.7321 0.8749 0.9024 0.066 Uiso 1 1 calc R . .
C6 C 0.5737(5) 0.9668(4) 0.7634(3) 0.0655(9) Uani 1 1 d . . .
H6A H 0.5907 1.0361 0.6948 0.098 Uiso 1 1 calc R . .
H6B H 0.4796 1.0107 0.8053 0.098 Uiso 1 1 calc R . .
H6C H 0.5347 0.8802 0.7495 0.098 Uiso 1 1 calc R . .
C7 C 0.8330(4) 0.6842(3) 0.7789(3) 0.0515(7) Uani 1 1 d . . .
H7A H 0.9304 0.6233 0.7492 0.062 Uiso 1 1 calc R . .
H7B H 0.7258 0.7073 0.7294 0.062 Uiso 1 1 calc R . .
C8 C 0.7759(5) 0.5956(4) 0.8898(3) 0.0616(9) Uani 1 1 d . . .
H8A H 0.7501 0.5013 0.8834 0.092 Uiso 1 1 calc R . .
H8B H 0.6655 0.6477 0.9143 0.092 Uiso 1 1 calc R . .
H8C H 0.8760 0.5818 0.9418 0.092 Uiso 1 1 calc R . .
C9 C 0.9510(5) 0.8984(4) 0.6639(2) 0.0571(8) Uani 1 1 d . . .
H9A H 0.8380 0.9166 0.6194 0.069 Uiso 1 1 calc R . .
H9B H 1.0410 0.8295 0.6368 0.069 Uiso 1 1 calc R . .
C10 C 1.0309(6) 1.0429(4) 0.6473(3) 0.0715(10) Uani 1 1 d . . .
H10A H 1.0363 1.0886 0.5702 0.107 Uiso 1 1 calc R . .
H10B H 1.1549 1.0237 0.6785 0.107 Uiso 1 1 calc R . .
H10C H 0.9518 1.1076 0.6828 0.107 Uiso 1 1 calc R . .
C11 C 1.0748(4) 0.7950(4) 0.8564(2) 0.0518(7) Uani 1 1 d . . .
H11A H 1.1252 0.8864 0.8503 0.062 Uiso 1 1 calc R . .
H11B H 1.0348 0.7612 0.9316 0.062 Uiso 1 1 calc R . .
C12 C 1.2297(4) 0.6815(4) 0.8325(3) 0.0606(9) Uani 1 1 d . . .
H12A H 1.1891 0.5860 0.8518 0.091 Uiso 1 1 calc R . .
H12B H 1.3394 0.6796 0.8749 0.091 Uiso 1 1 calc R . .
H12C H 1.2589 0.7069 0.7558 0.091 Uiso 1 1 calc R . .
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'
Ru Ru -1.2594 0.8363 '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
_geom_angle_publ_flag
S1 Ru S1 180.0 2_666 . ?
S1 Ru S2 91.28(3) 2_666 . ?
S1 Ru S2 88.72(3) . . ?
S1 Ru S2 88.72(3) 2_666 2_666 ?
S1 Ru S2 91.28(3) . 2_666 ?
S2 Ru S2 180.0 . 2_666 ?
S1 Ru Br 90.52(2) 2_666 . ?
S1 Ru Br 89.48(2) . . ?
S2 Ru Br 88.73(2) . . ?
S2 Ru Br 91.27(2) 2_666 . ?
S1 Ru Br 89.48(2) 2_666 2_666 ?
S1 Ru Br 90.52(2) . 2_666 ?
S2 Ru Br 91.27(2) . 2_666 ?
S2 Ru Br 88.73(2) 2_666 2_666 ?
Br Ru Br 180.0 . 2_666 ?
C1 S1 Ru 103.49(9) . . ?
C3 S2 Ru 103.34(10) . . ?
C3 C1 C2 119.4(2) . . ?
C3 C1 S1 122.1(2) . . ?
C2 C1 S1 118.5(2) . . ?
N1 C2 C1 179.0(3) . . ?
C1 C3 C4 119.5(2) . . ?
C1 C3 S2 122.2(2) . . ?
C4 C3 S2 118.2(2) . . ?
N2 C4 C3 178.9(4) . . ?
C5 N3 C9 111.4(2) . . ?
C5 N3 C7 110.5(2) . . ?
C9 N3 C7 106.4(2) . . ?
C5 N3 C11 106.5(2) . . ?
C9 N3 C11 111.6(2) . . ?
C7 N3 C11 110.4(2) . . ?
N3 C5 C6 114.3(3) . . ?
N3 C5 H5A 108.7 . . ?
C6 C5 H5A 108.7 . . ?
N3 C5 H5B 108.7 . . ?
C6 C5 H5B 108.7 . . ?
H5A C5 H5B 107.6 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N3 C7 C8 114.6(2) . . ?
N3 C7 H7A 108.6 . . ?
C8 C7 H7A 108.6 . . ?
N3 C7 H7B 108.6 . . ?
C8 C7 H7B 108.6 . . ?
H7A C7 H7B 107.6 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N3 C9 C10 115.4(3) . . ?
N3 C9 H9A 108.4 . . ?
C10 C9 H9A 108.4 . . ?
N3 C9 H9B 108.4 . . ?
C10 C9 H9B 108.4 . . ?
H9A C9 H9B 107.5 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 N3 114.6(2) . . ?
C12 C11 H11A 108.6 . . ?
N3 C11 H11A 108.6 . . ?
C12 C11 H11B 108.6 . . ?
N3 C11 H11B 108.6 . . ?
H11A C11 H11B 107.6 . . ?
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 . . ?
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
Ru S1 2.2840(7) 2_666 ?
Ru S1 2.2840(7) . ?
Ru S2 2.2881(7) . ?
Ru S2 2.2881(7) 2_666 ?
Ru Br 2.5790(4) . ?
Ru Br 2.5790(4) 2_666 ?
S1 C1 1.704(3) . ?
S2 C3 1.704(3) . ?
C1 C3 1.382(4) . ?
C1 C2 1.439(4) . ?
C2 N1 1.136(4) . ?
C3 C4 1.428(4) . ?
C4 N2 1.141(4) . ?
N3 C5 1.509(4) . ?
N3 C9 1.513(3) . ?
N3 C7 1.514(4) . ?
N3 C11 1.521(4) . ?
C5 C6 1.515(5) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 C8 1.515(4) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 C10 1.522(5) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 C12 1.514(4) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
