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#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/08/4300877.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_4300877
loop_
_publ_author_name
'Emma Gallo'
'Alessandro Caselli'
'Fabio Ragaini'
'Simone Fantauzzi'
'Norberto Masciocchi'
'Angelo Sironi'
'Sergio Cenini'
_publ_section_title
;

Structural Determination of Ruthenium-Porphyrin Complexes Relevant to

Catalytic Epoxidation of Olefins

;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2039
_journal_page_last               2049
_journal_paper_doi               10.1021/ic048587w
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C24 H20 N2 O Ru0.5 S'
_chemical_formula_weight         435.01
_chemical_name_systematic
;

 ?

;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2y'
_symmetry_space_group_name_H-M   'I 1 2/m 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                 91.12(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.629(2)
_cell_length_b                   9.3560(10)
_cell_length_c                   14.465(2)
_cell_measurement_temperature    293(2)
_cell_volume                     1979.4(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.939
_diffrn_measured_fraction_theta_max 0.939
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_sigmaI/netI    0.0210
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13697
_diffrn_reflns_theta_full        29.05
_diffrn_reflns_theta_max         29.05
_diffrn_reflns_theta_min         1.96
_exptl_absorpt_coefficient_mu    0.548
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             896
_refine_diff_density_max         1.431
_refine_diff_density_min         -0.465
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         2635
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0359
_refine_ls_R_factor_gt           0.0356
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0594P)²+1.8730P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0936
_refine_ls_wR_factor_ref         0.0938
_reflns_number_gt                2603
_reflns_number_total             2635
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048587wsi20041008_102803.cif
_cod_data_source_block           RuTPPDMSO
_cod_original_formula_sum        'C24 H20 N2 O Ru0.50 S'
_cod_database_code               4300877
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'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
C1 C 0.00590(18) 0.0000 -0.21267(17) 0.0303(5) Uani 1 2 d S . .
C2 C 0.0700(2) 0.0000 -0.28718(19) 0.0377(6) Uani 1 2 d S . .
H2 H 0.0555 0.0000 -0.3501 0.045 Uiso 1 2 calc SR . .
C3 C 0.1545(2) 0.0000 -0.24908(19) 0.0385(6) Uani 1 2 d S . .
H3 H 0.2090 0.0000 -0.2811 0.046 Uiso 1 2 calc SR . .
C4 C 0.14587(18) 0.0000 -0.15024(18) 0.0324(5) Uani 1 2 d S . .
C5 C 0.21831(18) 0.0000 -0.08600(18) 0.0323(5) Uani 1 2 d S . .
C6 C 0.21010(17) 0.0000 0.01006(19) 0.0319(5) Uani 1 2 d S . .
C7 C 0.28476(19) 0.0000 0.0754(2) 0.0406(6) Uani 1 2 d S . .
H7 H 0.3466 0.0000 0.0617 0.049 Uiso 1 2 calc SR . .
C8 C 0.2489(2) 0.0000 0.1609(2) 0.0412(6) Uani 1 2 d S . .
H8 H 0.2817 0.0000 0.2167 0.049 Uiso 1 2 calc SR . .
C9 C 0.15168(18) 0.0000 0.15013(18) 0.0323(5) Uani 1 2 d S . .
C10 C 0.08924(18) 0.0000 0.22270(17) 0.0314(5) Uani 1 2 d S . .
C11 C 0.12891(19) 0.0000 0.31864(18) 0.0347(5) Uani 1 2 d S . .
C12 C 0.1810(3) 0.1184(5) 0.3484(3) 0.0417(10) Uani 0.50 1 d P . .
H12 H 0.1885 0.1962 0.3093 0.050 Uiso 0.50 1 calc PR . .
C13 C 0.2212(4) 0.1191(6) 0.4363(4) 0.0530(13) Uani 0.50 1 d P . .
H13 H 0.2566 0.1962 0.4562 0.064 Uiso 0.50 1 calc PR . .
C14 C 0.2073(3) 0.0000 0.4949(2) 0.0603(10) Uani 1 2 d S . .
H14 H 0.2357 -0.0033 0.5529 0.072 Uiso 1 2 calc SR . .
C15 C 0.1545(5) -0.1053(7) 0.4674(4) 0.0623(15) Uani 0.50 1 d P . .
H15 H 0.1427 -0.1796 0.5081 0.075 Uiso 0.50 1 calc PR . .
C16 C 0.1155(4) -0.1089(5) 0.3785(3) 0.0483(11) Uani 0.50 1 d P . .
H16 H 0.0800 -0.1868 0.3603 0.058 Uiso 0.50 1 calc PR . .
C21 C 0.31312(18) 0.0000 -0.12377(19) 0.0346(5) Uani 1 2 d S . .
C22 C 0.3418(3) -0.1120(5) -0.1745(4) 0.0436(10) Uani 0.50 1 d P . .
H22 H 0.3025 -0.1886 -0.1855 0.052 Uiso 0.50 1 calc PR . .
C23 C 0.4295(4) -0.1147(6) -0.2108(4) 0.0535(13) Uani 0.50 1 d P . .
H23 H 0.4484 -0.1919 -0.2461 0.064 Uiso 0.50 1 calc PR . .
C24 C 0.4887(2) 0.0000 -0.1934(3) 0.0552(9) Uani 1 2 d S . .
H24 H 0.5471 -0.0003 -0.2176 0.066 Uiso 1 2 calc SR . .
C25 C 0.4614(4) 0.1093(6) -0.1425(5) 0.0580(14) Uani 0.50 1 d P . .
H25 H 0.5017 0.1840 -0.1298 0.070 Uiso 0.50 1 calc PR . .
C26 C 0.3731(3) 0.1143(5) -0.1075(4) 0.0490(12) Uani 0.50 1 d P . .
H26 H 0.3543 0.1930 -0.0736 0.059 Uiso 0.50 1 calc PR . .
N1 N 0.05386(15) 0.0000 -0.12927(15) 0.0293(4) Uani 1 2 d S . .
N2 N 0.12907(15) 0.0000 0.05714(16) 0.0322(5) Uani 1 2 d S . .
S S 0.0000 -0.24733(8) 0.0000 0.03905(17) Uani 1 2 d S . .
O O -0.0753(3) -0.3255(4) 0.0292(4) 0.0733(13) Uani 0.50 1 d P . .
C1S C 0.0954(4) -0.3134(6) 0.0802(5) 0.0634(15) Uani 0.50 1 d P . .
C2S C 0.0443(10) -0.3187(7) -0.1025(5) 0.119(4) Uani 0.50 1 d P . .
Ru Ru 0.0000 0.0000 0.0000 0.02457(11) Uani 1 4 d S . .
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'
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
N1 C1 C10 125.3(2) . 5 ?
N1 C1 C2 109.0(2) . . ?
C10 C1 C2 125.7(2) 5 . ?
C3 C2 C1 107.4(2) . . ?
C2 C3 C4 108.1(2) . . ?
N1 C4 C5 125.6(2) . . ?
N1 C4 C3 108.8(2) . . ?
C5 C4 C3 125.6(2) . . ?
C4 C5 C6 125.7(2) . . ?
C4 C5 C21 116.9(2) . . ?
C6 C5 C21 117.4(2) . . ?
N2 C6 C5 125.6(2) . . ?
N2 C6 C7 109.0(2) . . ?
C5 C6 C7 125.3(2) . . ?
C8 C7 C6 107.4(2) . . ?
C7 C8 C9 107.6(2) . . ?
N2 C9 C10 125.6(2) . . ?
N2 C9 C8 109.0(2) . . ?
C10 C9 C8 125.4(3) . . ?
C1 C10 C9 125.7(2) 5 . ?
C1 C10 C11 117.7(2) 5 . ?
C9 C10 C11 116.6(2) . . ?
C16 C11 C12 118.7(3) . . ?
C16 C11 C10 122.4(3) . . ?
C12 C11 C10 118.9(2) . . ?
C13 C12 C11 120.1(4) . . ?
C12 C13 C14 118.6(4) . . ?
C15 C14 C13 120.1(4) . . ?
C14 C15 C16 121.7(5) . . ?
C11 C16 C15 120.6(5) . . ?
C22 C21 C26 118.9(3) . . ?
C22 C21 C5 119.8(2) . . ?
C26 C21 C5 121.3(2) . . ?
C21 C22 C23 121.0(4) . . ?
C22 C23 C24 119.3(4) . . ?
C25 C24 C23 119.9(4) . . ?
C24 C25 C26 121.1(5) . . ?
C25 C26 C21 119.7(4) . . ?
C1 N1 C4 106.7(2) . . ?
C1 N1 Ru 126.86(18) . . ?
C4 N1 Ru 126.44(18) . . ?
C6 N2 C9 106.8(2) . . ?
C6 N2 Ru 126.58(18) . . ?
C9 N2 Ru 126.58(18) . . ?
O S O 116.8(4) 2 . ?
O S C2S 111.2(4) 2 2 ?
O S C2S 40.6(4) . 2 ?
O S C2S 40.6(4) 2 . ?
O S C2S 111.2(4) . . ?
C2S S C2S 135.5(5) 2 . ?
O S C1S 102.7(3) 2 2 ?
O S C1S 55.9(3) . 2 ?
C2S S C1S 96.5(5) 2 2 ?
C2S S C1S 68.9(5) . 2 ?
O S C1S 55.9(3) 2 . ?
O S C1S 102.7(3) . . ?
C2S S C1S 68.9(5) 2 . ?
C2S S C1S 96.5(5) . . ?
C1S S C1S 142.1(4) 2 . ?
O S Ru 121.62(19) 2 . ?
O S Ru 121.62(19) . . ?
C2S S Ru 112.3(2) 2 . ?
C2S S Ru 112.3(2) . . ?
C1S S Ru 108.97(18) 2 . ?
C1S S Ru 108.97(18) . . ?
C2S O S 87.1(6) 2 . ?
C2S O C1S 165.3(7) 2 2 ?
S O C1S 78.2(3) . 2 ?
O C1S S 45.9(2) 2 . ?
O C2S S 52.3(3) 2 . ?
N1 Ru N1 180.00(12) 5 . ?
N1 Ru N2 89.98(9) 5 . ?
N1 Ru N2 90.02(9) . . ?
N1 Ru N2 90.02(9) 5 5 ?
N1 Ru N2 89.98(9) . 5 ?
N2 Ru N2 180.00(13) . 5 ?
N1 Ru S 90.0 5 . ?
N1 Ru S 90.0 . . ?
N2 Ru S 90.0 . . ?
N2 Ru S 90.0 5 . ?
N1 Ru S 90.0 5 5 ?
N1 Ru S 90.0 . 5 ?
N2 Ru S 90.0 . 5 ?
N2 Ru S 90.0 5 5 ?
S Ru S 180.0 . 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
C1 N1 1.384(3) . ?
C1 C10 1.397(4) 5 ?
C1 C2 1.442(4) . ?
C2 C3 1.343(4) . ?
C3 C4 1.438(4) . ?
C4 N1 1.385(3) . ?
C4 C5 1.396(4) . ?
C5 C6 1.397(4) . ?
C5 C21 1.501(3) . ?
C6 N2 1.379(3) . ?
C6 C7 1.431(4) . ?
C7 C8 1.353(4) . ?
C8 C9 1.428(4) . ?
C9 N2 1.379(3) . ?
C9 C10 1.405(4) . ?
C10 C1 1.397(4) 5 ?
C10 C11 1.494(3) . ?
C11 C16 1.354(5) . ?
C11 C12 1.407(5) . ?
C12 C13 1.390(7) . ?
C13 C14 1.417(6) . ?
C14 C15 1.308(7) . ?
C15 C16 1.397(7) . ?
C21 C22 1.351(5) . ?
C21 C26 1.400(5) . ?
C22 C23 1.395(7) . ?
C23 C24 1.398(6) . ?
C24 C25 1.327(7) . ?
C25 C26 1.397(7) . ?
N1 Ru 2.043(2) . ?
N2 Ru 2.046(2) . ?
S O 1.394(4) 2 ?
S O 1.394(4) . ?
S C2S 1.761(7) 2 ?
S C2S 1.761(7) . ?
S C1S 1.900(5) 2 ?
S C1S 1.900(5) . ?
S Ru 2.3140(7) . ?
O C2S 1.148(10) 2 ?
O C1S 1.607(9) 2 ?
C1S O 1.607(9) 2 ?
C2S O 1.148(10) 2 ?
Ru N1 2.043(2) 5 ?
Ru N2 2.046(2) 5 ?
Ru S 2.3140(7) 5 ?
