#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/68/4326827.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_4326827
loop_
_publ_author_name
'Konstantin Livanov'
'Vedichi Madhu'
'Ekambaram Balaraman'
'Linda J. W. Shimon'
'Yael Diskin-Posner'
'Ronny Neumann'
_publ_section_title
;
 Photocatalytic Splitting of CS2 to S8 and a Carbon-Sulfur Polymer
 Catalyzed by a Bimetallic Ruthenium(II) Compound with a Tertiary Amine
 Binding Site: Toward Photocatalytic Splitting of CO2?
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11273
_journal_page_last               11275
_journal_paper_doi               10.1021/ic2008045
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C38 H38 N12 Ru2, 4(B F4), 4(H2 O)'
_chemical_formula_sum            'C38 H46 B4 F16 N12 O4 Ru2'
_chemical_formula_weight         1284.25
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 108.2960(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.3580(2)
_cell_length_b                   18.9180(3)
_cell_length_c                   17.4920(3)
_cell_measurement_reflns_used    7993
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      33.14
_cell_measurement_theta_min      2.55
_cell_volume                     5139.44(14)
_computing_cell_refinement       HKL
_computing_data_collection       'Collect package Bruker-Nonius'
_computing_data_reduction        HKL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-97 (Altmore et al, 1994)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full .998
_diffrn_measured_fraction_theta_max .998
_diffrn_measurement_device_type  'Bruker - Nonius Kappa CCD'
_diffrn_measurement_method       'Omega ans 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  0.036
_diffrn_reflns_av_sigmaI/netI    0.0388
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            10055
_diffrn_reflns_theta_full        33.14
_diffrn_reflns_theta_max         33.14
_diffrn_reflns_theta_min         2.98
_exptl_absorpt_coefficient_mu    0.697
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.660
_exptl_crystal_description       prism
_exptl_crystal_F_000             2568
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.50
_refine_diff_density_max         2.431
_refine_diff_density_min         -1.390
_refine_diff_density_rms         .140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         9799
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0764
_refine_ls_R_factor_gt           0.0535
_refine_ls_shift/su_max          0.041
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0911P)²+11.0249P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1430
_refine_ls_wR_factor_ref         0.1584
_reflns_number_gt                7320
_reflns_number_total             9799
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2008045_si_005.cif
_cod_data_source_block           n277
_cod_original_sg_symbol_Hall     -C2yc
_cod_database_code               4326827
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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
Ru1 Ru 0.425381(12) 0.295331(9) 0.383971(12) 0.01740(7) Uani 1 1 d . . .
N2 N 0.30374(14) 0.26983(12) 0.38079(14) 0.0214(4) Uani 1 1 d . . .
N3 N 0.35540(13) 0.37361(11) 0.30793(13) 0.0182(4) Uani 1 1 d . . .
C4 C 0.2811(2) 0.21000(14) 0.41084(19) 0.0259(5) Uani 1 1 d . . .
H4 H 0.3243 0.1760 0.4351 0.031 Uiso 1 1 calc R . .
C5 C 0.1971(2) 0.19667(16) 0.4075(2) 0.0331(7) Uani 1 1 d . . .
H5 H 0.1828 0.1540 0.4289 0.040 Uiso 1 1 calc R . .
C6 C 0.1341(2) 0.24575(17) 0.3728(2) 0.0338(7) Uani 1 1 d . . .
H6 H 0.0763 0.2377 0.3713 0.041 Uiso 1 1 calc R . .
C7 C 0.15572(19) 0.30695(17) 0.3400(2) 0.0306(6) Uani 1 1 d . . .
H7 H 0.1130 0.3409 0.3147 0.037 Uiso 1 1 calc R . .
C8 C 0.24171(17) 0.31765(14) 0.34503(17) 0.0227(5) Uani 1 1 d . . .
C9 C 0.27240(16) 0.37855(13) 0.30927(16) 0.0215(5) Uani 1 1 d . . .
C10 C 0.22125(18) 0.43737(15) 0.2799(2) 0.0278(6) Uani 1 1 d . . .
H10 H 0.1641 0.4395 0.2824 0.033 Uiso 1 1 calc R . .
C11 C 0.25431(19) 0.49290(15) 0.2469(2) 0.0309(6) Uani 1 1 d . . .
H11 H 0.2211 0.5343 0.2285 0.037 Uiso 1 1 calc R . .
C12 C 0.33644(18) 0.48697(14) 0.24123(18) 0.0257(5) Uani 1 1 d . . .
H12 H 0.3597 0.5238 0.2175 0.031 Uiso 1 1 calc R . .
C13 C 0.38476(16) 0.42664(12) 0.27047(16) 0.0189(4) Uani 1 1 d . . .
C14 C 0.46769(16) 0.42006(12) 0.25976(15) 0.0191(4) Uani 1 1 d . . .
N15 N 0.48273(15) 0.22140(12) 0.46861(15) 0.0238(4) Uani 1 1 d . . .
C16 C 0.51634(19) 0.18577(15) 0.52204(19) 0.0277(5) Uani 1 1 d . . .
C17 C 0.5588(3) 0.14199(19) 0.5924(2) 0.0410(8) Uani 1 1 d . . .
H17A H 0.6017 0.1704 0.6323 0.062 Uiso 1 1 calc R . .
H17B H 0.5873 0.1019 0.5758 0.062 Uiso 1 1 calc R . .
H17C H 0.5158 0.1244 0.6161 0.062 Uiso 1 1 calc R . .
N18 N 0.54966(14) 0.32103(11) 0.39266(13) 0.0201(4) Uani 1 1 d . . .
C19 C 0.62138(18) 0.33342(14) 0.41091(17) 0.0239(5) Uani 1 1 d . . .
C20 C 0.71274(19) 0.35087(18) 0.4342(2) 0.0364(7) Uani 1 1 d . . .
H20A H 0.7203 0.3956 0.4090 0.055 Uiso 1 1 calc R . .
H20B H 0.7437 0.3132 0.4165 0.055 Uiso 1 1 calc R . .
H20C H 0.7355 0.3556 0.4929 0.055 Uiso 1 1 calc R . .
N21 N 0.43534(15) 0.36660(11) 0.47248(14) 0.0218(4) Uani 1 1 d . . .
C22 C 0.4430(2) 0.41126(15) 0.51826(18) 0.0283(6) Uani 1 1 d . . .
C23 C 0.4542(3) 0.4686(2) 0.5761(2) 0.0470(9) Uani 1 1 d . . .
H23A H 0.5137 0.4858 0.5911 0.070 Uiso 1 1 calc R . .
H23B H 0.4420 0.4513 0.6241 0.070 Uiso 1 1 calc R . .
H23C H 0.4146 0.5072 0.5518 0.070 Uiso 1 1 calc R . .
N24 N 0.41197(14) 0.22700(11) 0.29216(14) 0.0210(4) Uani 1 1 d . . .
C25 C 0.39756(17) 0.18889(14) 0.23923(18) 0.0238(5) Uani 1 1 d . . .
C26 C 0.3814(2) 0.14000(18) 0.1720(2) 0.0348(7) Uani 1 1 d . . .
H26A H 0.4149 0.0967 0.1898 0.052 Uiso 1 1 calc R . .
H26B H 0.3983 0.1620 0.1286 0.052 Uiso 1 1 calc R . .
H26C H 0.3199 0.1283 0.1524 0.052 Uiso 1 1 calc R . .
B27 B 0.3290(2) 0.02377(18) 0.5024(2) 0.0302(7) Uani 1 1 d . . .
F28 F 0.36508(18) -0.04171(12) 0.52871(19) 0.0676(7) Uani 1 1 d . A .
F29A F 0.3839(3) 0.0783(2) 0.5376(4) 0.0676(7) Uani 0.570(6) 1 d P A 1
F30A F 0.2510(4) 0.0331(3) 0.5129(4) 0.0719(14) Uani 0.570(6) 1 d P A 1
F31A F 0.3200(4) 0.0250(4) 0.4231(3) 0.0719(14) Uani 0.570(6) 1 d P A 1
F29B F 0.3527(6) 0.0638(5) 0.5690(6) 0.083(2) Uiso 0.430(6) 1 d P A 2
F30B F 0.2412(4) 0.0224(3) 0.4665(4) 0.0551(17) Uiso 0.430(6) 1 d P A 2
F31B F 0.3681(5) 0.0578(4) 0.4504(5) 0.070(2) Uiso 0.430(6) 1 d P A 2
B32 B 0.1529(3) 0.1695(2) 0.1455(3) 0.0424(9) Uani 1 1 d . . .
F33 F 0.07296(14) 0.19299(13) 0.15144(15) 0.0468(5) Uani 1 1 d . . .
F34 F 0.20639(15) 0.15429(13) 0.22079(15) 0.0502(6) Uani 1 1 d . . .
F35 F 0.14069(19) 0.10730(16) 0.09867(18) 0.0657(7) Uani 1 1 d . . .
F36 F 0.1850(2) 0.21891(17) 0.1061(3) 0.0833(11) Uani 1 1 d . . .
O37 O 0.0000 0.43837(18) 0.2500 0.0351(7) Uani 1 2 d S . .
H37 H 0.0163 0.4691 0.2251 0.046(13) Uiso 1 1 d R . .
O38 O 0.0000 0.11193(19) 0.2500 0.0472(9) Uani 1 2 d S . .
H38 H 0.0328 0.1362 0.2409 0.047(13) Uiso 1 1 d R . .
O39 O 0.4658(2) 0.03679(14) 0.35929(17) 0.0451(6) Uani 1 1 d . . .
H39A H 0.4237 0.0374 0.3830 0.046(13) Uiso 1 1 d R . .
H39B H 0.5156 0.0381 0.3950 0.11(2) Uiso 1 1 d R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 .8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B .0013 .0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F .0171 .0103 '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
N24 Ru1 N21 177.53(9) .
N24 Ru1 N2 88.01(9) .
N21 Ru1 N2 91.27(9) .
N24 Ru1 N15 92.79(10) .
N21 Ru1 N15 89.62(10) .
N2 Ru1 N15 94.61(9) .
N24 Ru1 N18 93.92(9) .
N21 Ru1 N18 86.87(9) .
N2 Ru1 N18 177.45(9) .
N15 Ru1 N18 83.64(9) .
N24 Ru1 N3 92.68(9) .
N21 Ru1 N3 84.87(9) .
N2 Ru1 N3 79.26(9) .
N15 Ru1 N3 171.63(9) .
N18 Ru1 N3 102.29(8) .
C4 N2 C8 118.9(2) .
C4 N2 Ru1 125.1(2) .
C8 N2 Ru1 116.01(17) .
C13 N3 C9 117.3(2) .
C13 N3 Ru1 128.67(17) .
C9 N3 Ru1 112.83(17) .
N2 C4 C5 121.9(3) .
N2 C4 H4 119.1 .
C5 C4 H4 119.1 .
C6 C5 C4 119.5(3) .
C6 C5 H5 120.2 .
C4 C5 H5 120.2 .
C5 C6 C7 119.5(3) .
C5 C6 H6 120.3 .
C7 C6 H6 120.3 .
C6 C7 C8 118.6(3) .
C6 C7 H7 120.7 .
C8 C7 H7 120.7 .
N2 C8 C7 121.7(3) .
N2 C8 C9 114.4(2) .
C7 C8 C9 123.9(3) .
N3 C9 C10 122.3(2) .
N3 C9 C8 115.2(2) .
C10 C9 C8 122.5(2) .
C11 C10 C9 119.5(2) .
C11 C10 H10 120.3 .
C9 C10 H10 120.3 .
C12 C11 C10 118.9(3) .
C12 C11 H11 120.6 .
C10 C11 H11 120.6 .
C11 C12 C13 119.5(3) .
C11 C12 H12 120.2 .
C13 C12 H12 120.2 .
N3 C13 C12 122.3(2) .
N3 C13 C14 119.3(2) .
C12 C13 C14 118.4(2) .
C14 C14 C13 170.2(3) 2_655
C16 N15 Ru1 172.6(2) .
N15 C16 C17 178.0(3) .
C16 C17 H17A 109.5 .
C16 C17 H17B 109.5 .
H17A C17 H17B 109.5 .
C16 C17 H17C 109.5 .
H17A C17 H17C 109.5 .
H17B C17 H17C 109.5 .
C19 N18 Ru1 168.5(2) .
N18 C19 C20 178.8(3) .
C19 C20 H20A 109.5 .
C19 C20 H20B 109.5 .
H20A C20 H20B 109.5 .
C19 C20 H20C 109.5 .
H20A C20 H20C 109.5 .
H20B C20 H20C 109.5 .
C22 N21 Ru1 173.9(2) .
N21 C22 C23 178.8(3) .
C22 C23 H23A 109.5 .
C22 C23 H23B 109.5 .
H23A C23 H23B 109.5 .
C22 C23 H23C 109.5 .
H23A C23 H23C 109.5 .
H23B C23 H23C 109.5 .
C25 N24 Ru1 174.6(2) .
N24 C25 C26 178.6(3) .
C25 C26 H26A 109.5 .
C25 C26 H26B 109.5 .
H26A C26 H26B 109.5 .
C25 C26 H26C 109.5 .
H26A C26 H26C 109.5 .
H26B C26 H26C 109.5 .
F29B B27 F31A 142.4(6) .
F29B B27 F30A 80.6(5) .
F31A B27 F30A 109.5(4) .
F29B B27 F30B 112.5(5) .
F31A B27 F30B 76.7(4) .
F31A B27 F29A 107.0(5) .
F30A B27 F29A 110.5(5) .
F30B B27 F29A 131.1(4) .
F29B B27 F28 103.9(5) .
F31A B27 F28 104.7(4) .
F30A B27 F28 113.1(4) .
F30B B27 F28 114.2(4) .
F29A B27 F28 111.7(3) .
F29B B27 F31B 103.6(6) .
F30A B27 F31B 131.3(5) .
F30B B27 F31B 109.4(5) .
F29A B27 F31B 65.5(4) .
F28 B27 F31B 112.7(4) .
F36 B32 F34 113.7(4) .
F36 B32 F35 106.6(4) .
F34 B32 F35 108.3(3) .
F36 B32 F33 109.5(3) .
F34 B32 F33 108.8(3) .
F35 B32 F33 109.8(3) .
H39A O39 H39B 110.5 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ru1 N24 2.019(2) .
Ru1 N21 2.021(2) .
Ru1 N2 2.031(2) .
Ru1 N15 2.039(2) .
Ru1 N18 2.049(2) .
Ru1 N3 2.078(2) .
N2 C4 1.348(3) .
N2 C8 1.357(4) .
N3 C13 1.365(3) .
N3 C9 1.368(3) .
C4 C5 1.381(4) .
C4 H4 0.9500 .
C5 C6 1.378(5) .
C5 H5 0.9500 .
C6 C7 1.386(4) .
C6 H6 0.9500 .
C7 C8 1.396(4) .
C7 H7 0.9500 .
C8 C9 1.472(4) .
C9 C10 1.390(4) .
C10 C11 1.388(4) .
C10 H10 0.9500 .
C11 C12 1.382(4) .
C11 H11 0.9500 .
C12 C13 1.391(4) .
C12 H12 0.9500 .
C13 C14 1.432(3) .
C14 C14 1.208(5) 2_655
N15 C16 1.143(4) .
C16 C17 1.465(5) .
C17 H17A 0.9800 .
C17 H17B 0.9800 .
C17 H17C 0.9800 .
N18 C19 1.139(3) .
C19 C20 1.458(4) .
C20 H20A 0.9800 .
C20 H20B 0.9800 .
C20 H20C 0.9800 .
N21 C22 1.144(4) .
C22 C23 1.454(4) .
C23 H23A 0.9800 .
C23 H23B 0.9800 .
C23 H23C 0.9800 .
N24 C25 1.138(4) .
C25 C26 1.453(4) .
C26 H26A 0.9800 .
C26 H26B 0.9800 .
C26 H26C 0.9800 .
B27 F29B 1.340(9) .
B27 F31A 1.349(6) .
B27 F30A 1.356(6) .
B27 F30B 1.375(7) .
B27 F29A 1.380(6) .
B27 F28 1.387(4) .
B27 F31B 1.420(9) .
B32 F36 1.359(5) .
B32 F34 1.364(5) .
B32 F35 1.412(6) .
B32 F33 1.415(4) .
O37 H37 0.8200 .
O38 H38 0.7598 .
O39 H39A 0.9088 .
O39 H39B 0.8572 .
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
N24 Ru1 N2 C4 77.1(2)
N21 Ru1 N2 C4 -105.2(2)
N15 Ru1 N2 C4 -15.5(2)
N3 Ru1 N2 C4 170.2(2)
N24 Ru1 N2 C8 -102.6(2)
N21 Ru1 N2 C8 75.0(2)
N15 Ru1 N2 C8 164.71(19)
N3 Ru1 N2 C8 -9.54(19)
N24 Ru1 N3 C13 -91.9(2)
N21 Ru1 N3 C13 88.3(2)
N2 Ru1 N3 C13 -179.4(2)
N18 Ru1 N3 C13 2.7(2)
N24 Ru1 N3 C9 101.18(18)
N21 Ru1 N3 C9 -78.55(18)
N2 Ru1 N3 C9 13.72(17)
N18 Ru1 N3 C9 -164.21(17)
C8 N2 C4 C5 -1.1(4)
Ru1 N2 C4 C5 179.1(2)
N2 C4 C5 C6 -0.3(5)
C4 C5 C6 C7 1.6(5)
C5 C6 C7 C8 -1.5(5)
C4 N2 C8 C7 1.2(4)
Ru1 N2 C8 C7 -179.0(2)
C4 N2 C8 C9 -175.9(2)
Ru1 N2 C8 C9 3.9(3)
C6 C7 C8 N2 0.1(4)
C6 C7 C8 C9 176.9(3)
C13 N3 C9 C10 -5.1(4)
Ru1 N3 C9 C10 163.4(2)
C13 N3 C9 C8 175.7(2)
Ru1 N3 C9 C8 -15.8(3)
N2 C8 C9 N3 8.2(3)
C7 C8 C9 N3 -168.8(3)
N2 C8 C9 C10 -171.0(3)
C7 C8 C9 C10 12.0(4)
N3 C9 C10 C11 1.0(4)
C8 C9 C10 C11 -179.9(3)
C9 C10 C11 C12 2.5(5)
C10 C11 C12 C13 -1.7(5)
C9 N3 C13 C12 6.0(4)
Ru1 N3 C13 C12 -160.4(2)
C9 N3 C13 C14 -173.2(2)
Ru1 N3 C13 C14 20.4(3)
C11 C12 C13 N3 -2.7(4)
C11 C12 C13 C14 176.5(3)
N24 Ru1 N18 C19 -131.9(11)
N21 Ru1 N18 C19 50.4(11)
N15 Ru1 N18 C19 -39.6(11)
N3 Ru1 N18 C19 134.5(11)
