#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:20:08 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179372 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/69/4326967.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_4326967
loop_
_publ_author_name
'Chuan-Hung Chuang'
'Chen-Kuo Ou'
'Shan-Tung Liu'
'Anil Kumar'
'Wei-Min Ching'
'Pei-Chun Chiang'
'Mira Anne C. dela Rosa'
'Chen-Hsiung Hung'
_publ_section_title
;
 Ruthenium Complexes of Thiaporphyrin and Dithiaporphyrin
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11947
_journal_page_last               11957
_journal_paper_doi               10.1021/ic200977n
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C50 H38 Cl2 N4 O4 Ru S'
_chemical_formula_weight         962.87
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 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                 119.1450(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.6857(13)
_cell_length_b                   17.1532(11)
_cell_length_c                   15.5257(9)
_cell_measurement_reflns_used    6196
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.56
_cell_measurement_theta_min      1.79
_cell_volume                     5276.6(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  '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  0.0269
_diffrn_reflns_av_sigmaI/netI    0.0390
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            16683
_diffrn_reflns_theta_full        27.56
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    0.480
_exptl_absorpt_correction_T_max  0.9314
_exptl_absorpt_correction_T_min  0.9101
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'Dark Brown'
_exptl_crystal_density_diffrn    1.212
_exptl_crystal_description       cubic
_exptl_crystal_F_000             1968
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_platon_squeeze_details
;
;
_refine_diff_density_max         0.931
_refine_diff_density_min         -0.403
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.751
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         6194
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.751
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_gt           0.0536
_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)+(0.1990P)²+0.8512P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1885
_refine_ls_wR_factor_ref         0.1989
_reflns_number_gt                4505
_reflns_number_total             6194
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200977n_si_002_2.cif
_cod_data_source_block           h027_m-sr
_cod_database_code               4326967
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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
Ru1 Ru 0.478004(17) 0.0000 0.72651(2) 0.04696(17) Uani 1 2 d S . .
S1 S 0.50536(6) 0.0000 0.88620(8) 0.0491(3) Uani 1 2 d S . .
N1 N 0.4357(2) 0.0000 0.5759(3) 0.0525(9) Uani 1 2 d S . .
N2 N 0.47809(12) 0.12158(17) 0.72982(17) 0.0500(6) Uani 1 1 d . . .
N3 N 0.3408(4) 0.0267(4) 0.7126(5) 0.0748(19) Uani 0.50 1 d P . .
O1 O 0.6239(2) 0.0000 0.7873(3) 0.0829(12) Uani 1 2 d S . .
O2 O 0.3752(2) 0.0000 0.6914(4) 0.1023(17) Uani 1 2 d S . .
O3 O 0.3643(4) 0.0871(4) 0.7597(6) 0.103(2) Uani 0.50 1 d P . .
O4 O 0.2814(3) 0.0000 0.6896(6) 0.137(2) Uani 1 2 d S . .
C1 C 0.5668(3) 0.0000 0.7594(3) 0.0538(11) Uani 1 2 d S . .
C2 C 0.56353(18) -0.0740(2) 0.9481(2) 0.0543(8) Uani 1 1 d . . .
C3 C 0.6187(2) -0.0402(2) 1.0321(3) 0.0628(9) Uani 1 1 d . . .
H3 H 0.6520 -0.0697 1.0827 0.075 Uiso 1 1 calc R . .
C4 C 0.55351(17) 0.1484(2) 0.9108(2) 0.0527(7) Uani 1 1 d . . .
C5 C 0.50747(18) 0.1694(2) 0.8102(2) 0.0532(7) Uani 1 1 d . . .
C6 C 0.4921(2) 0.2485(2) 0.7774(3) 0.0615(9) Uani 1 1 d . . .
H6 H 0.5061 0.2925 0.8176 0.074 Uiso 1 1 calc R . .
C7 C 0.4538(2) 0.2483(2) 0.6781(3) 0.0655(9) Uani 1 1 d . . .
H7 H 0.4355 0.2915 0.6374 0.079 Uiso 1 1 calc R . .
C8 C 0.44684(17) 0.1674(2) 0.6477(2) 0.0526(7) Uani 1 1 d . . .
C9 C 0.41686(17) 0.1415(2) 0.5496(2) 0.0572(8) Uani 1 1 d . . .
C10 C 0.41313(18) 0.0654(2) 0.5180(2) 0.0545(8) Uani 1 1 d . . .
C11 C 0.3786(2) 0.0391(2) 0.4161(3) 0.0708(10) Uani 1 1 d . . .
H11 H 0.3598 0.0710 0.3606 0.085 Uiso 1 1 calc R . .
C12 C 0.38607(18) 0.2017(2) 0.4698(2) 0.0617(9) Uani 1 1 d . . .
C13 C 0.3295(2) 0.2439(3) 0.4554(3) 0.0761(11) Uani 1 1 d . . .
H13 H 0.3113 0.2364 0.4969 0.091 Uiso 1 1 calc R . .
C14 C 0.4124(2) 0.2177(3) 0.4072(3) 0.0754(11) Uani 1 1 d . . .
H14 H 0.4516 0.1926 0.4178 0.090 Uiso 1 1 calc R . .
C15 C 0.3004(2) 0.2978(3) 0.3775(3) 0.0825(13) Uani 1 1 d . . .
H15 H 0.2624 0.3254 0.3680 0.099 Uiso 1 1 calc R . .
C16 C 0.3826(2) 0.2688(3) 0.3317(3) 0.0775(11) Uani 1 1 d . . .
H16 H 0.4005 0.2760 0.2895 0.093 Uiso 1 1 calc R . .
C17 C 0.3258(2) 0.3107(3) 0.3162(3) 0.0790(12) Uani 1 1 d . . .
C18 C 0.2920(3) 0.3687(3) 0.2311(4) 0.1110(19) Uani 1 1 d . . .
H18A H 0.3256 0.4026 0.2309 0.166 Uiso 1 1 calc R . .
H18B H 0.2595 0.3991 0.2393 0.166 Uiso 1 1 calc R . .
H18C H 0.2697 0.3409 0.1698 0.166 Uiso 1 1 calc R . .
C19 C 0.59874(19) 0.2105(2) 0.9782(3) 0.0594(8) Uani 1 1 d . . .
C20 C 0.6017(2) 0.2243(2) 1.0682(3) 0.0695(10) Uani 1 1 d . . .
H20 H 0.5745 0.1953 1.0858 0.083 Uiso 1 1 calc R . .
C21 C 0.6407(2) 0.2533(3) 0.9567(3) 0.0751(11) Uani 1 1 d . . .
H21 H 0.6392 0.2457 0.8963 0.090 Uiso 1 1 calc R . .
C22 C 0.6447(2) 0.2808(3) 1.1328(3) 0.0830(13) Uani 1 1 d . . .
H22 H 0.6447 0.2901 1.1918 0.100 Uiso 1 1 calc R . .
C23 C 0.6849(2) 0.3069(3) 1.0211(4) 0.0874(13) Uani 1 1 d . . .
H23 H 0.7141 0.3332 1.0050 0.105 Uiso 1 1 calc R . .
C24 C 0.6867(2) 0.3225(3) 1.1107(4) 0.0855(13) Uani 1 1 d . . .
C25 C 0.7355(3) 0.3806(3) 1.1821(5) 0.129(2) Uani 1 1 d . . .
H25A H 0.7114 0.4261 1.1836 0.193 Uiso 1 1 calc R . .
H25B H 0.7677 0.3950 1.1616 0.193 Uiso 1 1 calc R . .
H25C H 0.7587 0.3578 1.2467 0.193 Uiso 1 1 calc R . .
C26 C 0.1929(10) 1.0042(9) 0.445(3) 0.225(3) Uani 0.25 1 d PD A -1
H26A H 0.1786 1.0381 0.3886 0.270 Uiso 0.25 1 calc PR A -1
H26B H 0.2226 1.0339 0.5038 0.270 Uiso 0.25 1 calc PR A -1
Cl2 Cl 0.1213(6) 0.9738(6) 0.4537(11) 0.225(3) Uani 0.25 1 d PD A -1
Cl1 Cl 0.2377(10) 0.9239(15) 0.434(2) 0.225(3) Uani 0.25 1 d PD A -1
C26A C 0.195(2) 1.0000 0.461(2) 0.225(3) Uani 0.50 2 d SPD . 2
H26O H 0.1516 1.0000 0.4596 0.270 Uiso 0.50 2 calc SPR . 2
H26W H 0.2297 1.0000 0.5300 0.270 Uiso 0.50 2 calc SPR . 2
Cl3 Cl 0.2020(5) 0.9130(6) 0.4057(10) 0.225(3) Uani 0.50 1 d PD . 2
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'
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
C1 Ru1 N1 99.13(18) . .
C1 Ru1 N2 90.31(7) . .
N1 Ru1 N2 91.28(6) . .
C1 Ru1 N2 90.31(7) . 6
N1 Ru1 N2 91.28(6) . 6
N2 Ru1 N2 177.23(13) . 6
C1 Ru1 O2 178.83(18) . .
N1 Ru1 O2 82.04(18) . .
N2 Ru1 O2 89.66(7) . .
N2 Ru1 O2 89.66(7) 6 .
C1 Ru1 S1 91.01(14) . .
N1 Ru1 S1 169.86(12) . .
N2 Ru1 S1 88.64(6) . .
N2 Ru1 S1 88.65(6) 6 .
O2 Ru1 S1 87.82(14) . .
C2 S1 C2 93.5(2) 6 .
C2 S1 Ru1 109.70(12) 6 .
C2 S1 Ru1 109.70(12) . .
C10 N1 C10 109.7(4) . 6
C10 N1 Ru1 124.47(19) . .
C10 N1 Ru1 124.47(19) 6 .
C8 N2 C5 107.9(3) . .
C8 N2 Ru1 124.0(2) . .
C5 N2 Ru1 128.1(2) . .
N3 N3 O2 65.0(4) 6 .
N3 N3 O3 147.4(5) 6 .
O2 N3 O3 111.7(7) . .
N3 N3 O4 69.3(3) 6 .
O2 N3 O4 124.8(7) . .
O3 N3 O4 123.5(7) . .
N3 O2 N3 50.0(8) 6 .
N3 O2 Ru1 141.7(5) 6 .
N3 O2 Ru1 141.7(5) . .
N3 O4 N3 41.3(6) . 6
O1 C1 Ru1 174.9(4) . .
C4 C2 C3 131.1(3) 6 .
C4 C2 S1 121.2(3) 6 .
C3 C2 S1 107.5(3) . .
C3 C3 C2 114.1(2) 6 .
C3 C3 H3 122.9 6 .
C2 C3 H3 122.9 . .
C2 C4 C5 125.0(3) 6 .
C2 C4 C19 116.8(3) 6 .
C5 C4 C19 117.9(3) . .
N2 C5 C6 108.6(3) . .
N2 C5 C4 127.9(3) . .
C6 C5 C4 123.0(3) . .
C7 C6 C5 108.2(3) . .
C7 C6 H6 125.9 . .
C5 C6 H6 125.9 . .
C6 C7 C8 106.3(3) . .
C6 C7 H7 126.8 . .
C8 C7 H7 126.8 . .
N2 C8 C9 126.0(3) . .
N2 C8 C7 108.8(3) . .
C9 C8 C7 125.1(3) . .
C10 C9 C8 126.7(3) . .
C10 C9 C12 115.7(3) . .
C8 C9 C12 117.6(3) . .
N1 C10 C9 126.9(3) . .
N1 C10 C11 107.0(3) . .
C9 C10 C11 125.9(3) . .
C11 C11 C10 108.1(2) 6 .
C11 C11 H11 126.0 6 .
C10 C11 H11 126.0 . .
C13 C12 C14 117.3(4) . .
C13 C12 C9 120.8(4) . .
C14 C12 C9 121.8(3) . .
C12 C13 C15 119.4(4) . .
C12 C13 H13 120.3 . .
C15 C13 H13 120.3 . .
C16 C14 C12 122.1(4) . .
C16 C14 H14 118.9 . .
C12 C14 H14 118.9 . .
C17 C15 C13 122.0(4) . .
C17 C15 H15 119.0 . .
C13 C15 H15 119.0 . .
C14 C16 C17 120.9(4) . .
C14 C16 H16 119.5 . .
C17 C16 H16 119.5 . .
C15 C17 C16 118.1(4) . .
C15 C17 C18 120.6(5) . .
C16 C17 C18 121.3(5) . .
C17 C18 H18A 109.5 . .
C17 C18 H18B 109.5 . .
H18A C18 H18B 109.5 . .
C17 C18 H18C 109.5 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
C20 C19 C21 117.3(4) . .
C20 C19 C4 120.3(4) . .
C21 C19 C4 122.3(3) . .
C19 C20 C22 121.0(4) . .
C19 C20 H20 119.5 . .
C22 C20 H20 119.5 . .
C23 C21 C19 122.2(4) . .
C23 C21 H21 118.9 . .
C19 C21 H21 118.9 . .
C24 C22 C20 121.0(4) . .
C24 C22 H22 119.5 . .
C20 C22 H22 119.5 . .
C21 C23 C24 120.7(4) . .
C21 C23 H23 119.6 . .
C24 C23 H23 119.6 . .
C22 C24 C23 117.7(4) . .
C22 C24 C25 121.3(5) . .
C23 C24 C25 121.0(5) . .
C24 C25 H25A 109.5 . .
C24 C25 H25B 109.5 . .
H25A C25 H25B 109.5 . .
C24 C25 H25C 109.5 . .
H25A C25 H25C 109.5 . .
H25B C25 H25C 109.5 . .
Cl1 C26 Cl2 111.71(9) . .
Cl1 C26 H26A 109.3 . .
Cl2 C26 H26A 109.3 . .
Cl1 C26 H26B 109.3 . .
Cl2 C26 H26B 109.3 . .
H26A C26 H26B 107.9 . .
Cl3 C26A Cl3 115.0(13) 6_575 .
Cl3 C26A H26O 108.5 6_575 .
Cl3 C26A H26O 108.5 . .
Cl3 C26A H26W 108.5 6_575 .
Cl3 C26A H26W 108.5 . .
H26O C26A H26W 107.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ru1 C1 1.822(5) .
Ru1 N1 2.050(4) .
Ru1 N2 2.086(3) .
Ru1 N2 2.086(3) 6
Ru1 O2 2.120(5) .
Ru1 S1 2.2436(11) .
S1 C2 1.744(3) 6
S1 C2 1.744(3) .
N1 C10 1.371(4) .
N1 C10 1.371(4) 6
N2 C8 1.365(4) .
N2 C5 1.365(4) .
N3 N3 0.917(14) 6
N3 O2 1.085(7) .
N3 O3 1.229(9) .
N3 O4 1.300(8) .
O1 C1 1.148(6) .
O2 N3 1.085(7) 6
O4 N3 1.300(8) 6
C2 C4 1.372(5) 6
C2 C3 1.419(5) .
C3 C3 1.380(7) 6
C3 H3 0.9300 .
C4 C2 1.373(5) 6
C4 C5 1.440(4) .
C4 C19 1.496(5) .
C5 C6 1.432(5) .
C6 C7 1.352(6) .
C6 H6 0.9300 .
C7 C8 1.450(5) .
C7 H7 0.9300 .
C8 C9 1.405(5) .
C9 C10 1.382(5) .
C9 C12 1.499(5) .
C10 C11 1.453(5) .
C11 C11 1.342(8) 6
C11 H11 0.9300 .
C12 C13 1.393(5) .
C12 C14 1.392(6) .
C13 C15 1.405(6) .
C13 H13 0.9300 .
C14 C16 1.351(5) .
C14 H14 0.9300 .
C15 C17 1.351(7) .
C15 H15 0.9300 .
C16 C17 1.391(6) .
C16 H16 0.9300 .
C17 C18 1.528(6) .
C18 H18A 0.9600 .
C18 H18B 0.9600 .
C18 H18C 0.9600 .
C19 C20 1.388(5) .
C19 C21 1.365(6) .
C20 C22 1.394(6) .
C20 H20 0.9300 .
C21 C23 1.369(6) .
C21 H21 0.9300 .
C22 C24 1.362(7) .
C22 H22 0.9300 .
C23 C24 1.399(7) .
C23 H23 0.9300 .
C24 C25 1.501(6) .
C25 H25A 0.9600 .
C25 H25B 0.9600 .
C25 H25C 0.9600 .
C26 Cl1 1.7700(10) .
C26 Cl2 1.7700(10) .
C26 H26A 0.9700 .
C26 H26B 0.9700 .
C26A Cl3 1.7698(10) 6_575
C26A Cl3 1.7698(10) .
C26A H26O 0.9700 .
C26A H26W 0.9700 .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 -0.007 511 71 ' '
2 0.500 0.500 -0.003 511 71 ' '
