#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:20:08 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179372 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/69/4326966.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_4326966
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 Cl3 N3 O Ru S'
_chemical_formula_weight         936.31
_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                 117.0030(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.5664(17)
_cell_length_b                   17.0892(14)
_cell_length_c                   15.4327(12)
_cell_measurement_reflns_used    6043
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.59
_cell_measurement_theta_min      1.82
_cell_volume                     5067.7(7)
_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      298(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0348
_diffrn_reflns_av_sigmaI/netI    0.0389
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            29824
_diffrn_reflns_theta_full        27.59
_diffrn_reflns_theta_max         27.59
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    0.544
_exptl_absorpt_correction_T_max  0.9476
_exptl_absorpt_correction_T_min  0.9084
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_description       cubic
_exptl_crystal_F_000             1912
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
;
_refine_diff_density_max         1.560
_refine_diff_density_min         -0.654
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.729
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         6043
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.729
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0489
_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)+(0.1489P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1427
_refine_ls_wR_factor_ref         0.1563
_reflns_number_gt                4176
_reflns_number_total             6043
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200977n_si_002_1.cif
_cod_data_source_block           h087r-sr
_cod_database_code               4326966
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
C4 C 1.05210(16) 0.64927(18) 0.9056(2) 0.0550(7) Uani 1 1 d .
Ru1 Ru 0.972536(15) 0.5000 0.724975(19) 0.04644(14) Uani 1 2 d S
S1 S 1.00331(5) 0.5000 0.88486(6) 0.0501(2) Uani 1 2 d S
Cl1 Cl 0.85141(7) 0.5000 0.70159(9) 0.0803(4) Uani 1 2 d S
C1 C 1.0650(2) 0.5000 0.7522(3) 0.0499(9) Uani 1 2 d S
N3 N 0.92962(17) 0.5000 0.5766(2) 0.0506(8) Uani 1 2 d S
N2 N 0.97350(11) 0.62152(14) 0.72829(14) 0.0492(5) Uani 1 1 d .
C15 C 0.94146(15) 0.66854(18) 0.6473(2) 0.0528(7) Uani 1 1 d .
C12 C 1.00532(15) 0.67046(17) 0.8078(2) 0.0520(7) Uani 1 1 d .
C16 C 0.91071(15) 0.64277(19) 0.5506(2) 0.0549(7) Uani 1 1 d .
C3 C 1.06339(16) 0.42593(18) 0.94310(19) 0.0549(7) Uani 1 1 d .
C17 C 0.87978(16) 0.7032(2) 0.4719(2) 0.0614(8) Uani 1 1 d .
C14 C 0.95041(17) 0.74867(19) 0.6775(2) 0.0636(8) Uani 1 1 d .
H14A H 0.9326 0.7919 0.6371 0.076 Uiso 1 1 calc R
C5 C 1.09814(17) 0.71222(18) 0.9719(2) 0.0618(8) Uani 1 1 d .
C24 C 0.90641(16) 0.56460(19) 0.51883(19) 0.0576(7) Uani 1 1 d .
C13 C 0.98923(17) 0.75035(19) 0.7750(2) 0.0647(8) Uani 1 1 d .
H13A H 1.0031 0.7949 0.8139 0.078 Uiso 1 1 calc R
O1 O 1.12227(19) 0.5000 0.7772(3) 0.0812(10) Uani 1 2 d S
C25 C 0.87111(19) 0.5381(2) 0.4187(2) 0.0736(10) Uani 1 1 d .
H25A H 0.8518 0.5700 0.3639 0.088 Uiso 1 1 calc R
C6 C 1.1408(2) 0.7572(2) 0.9467(3) 0.0810(10) Uani 1 1 d .
H6A H 1.1404 0.7504 0.8866 0.097 Uiso 1 1 calc R
C19 C 0.82044(19) 0.7431(2) 0.4583(3) 0.0788(10) Uani 1 1 d .
H19A H 0.8002 0.7330 0.4991 0.095 Uiso 1 1 calc R
C8 C 1.1847(2) 0.8130(2) 1.0123(3) 0.0945(13) Uani 1 1 d .
H8A H 1.2127 0.8436 0.9944 0.113 Uiso 1 1 calc R
C2 C 1.12076(18) 0.45993(19) 1.0226(2) 0.0656(8) Uani 1 1 d .
H2A H 1.1556 0.4304 1.0708 0.079 Uiso 1 1 calc R
C22 C 0.8189(2) 0.8159(2) 0.3243(3) 0.0803(11) Uani 1 1 d .
C18 C 0.90799(19) 0.7197(3) 0.4104(3) 0.0823(11) Uani 1 1 d .
H18A H 0.9472 0.6927 0.4166 0.099 Uiso 1 1 calc R
C7 C 1.1006(2) 0.7240(2) 1.0618(3) 0.0776(10) Uani 1 1 d .
H7A H 1.0724 0.6942 1.0800 0.093 Uiso 1 1 calc R
C20 C 0.8780(2) 0.7774(3) 0.3377(3) 0.0914(13) Uani 1 1 d .
H20A H 0.8988 0.7893 0.2982 0.110 Uiso 1 1 calc R
C21 C 0.7904(2) 0.7982(3) 0.3847(3) 0.0919(13) Uani 1 1 d .
H21A H 0.7499 0.8236 0.3764 0.110 Uiso 1 1 calc R
C9 C 1.1449(2) 0.7800(3) 1.1259(3) 0.0934(13) Uani 1 1 d .
H9A H 1.1453 0.7876 1.1858 0.112 Uiso 1 1 calc R
C10 C 1.1877(2) 0.8237(3) 1.1014(4) 0.0992(14) Uani 1 1 d .
C23 C 0.7854(3) 0.8764(3) 0.2430(3) 0.1182(18) Uani 1 1 d .
H23A H 0.7447 0.8977 0.2444 0.177 Uiso 1 1 calc R
H23B H 0.7725 0.8517 0.1813 0.177 Uiso 1 1 calc R
H23C H 0.8181 0.9177 0.2523 0.177 Uiso 1 1 calc R
C11 C 1.2369(3) 0.8829(3) 1.1735(5) 0.155(3) Uani 1 1 d .
H11A H 1.2629 0.9089 1.1454 0.232 Uiso 1 1 calc R
H11B H 1.2683 0.8564 1.2319 0.232 Uiso 1 1 calc R
H11C H 1.2105 0.9208 1.1888 0.232 Uiso 1 1 calc R
Cl2 Cl 0.8198(2) 0.91907(17) 0.6142(3) 0.2869(18) Uani 1 1 d .
C26 C 0.7953(8) 1.0000 0.5396(8) 0.234(7) Uani 1 2 d S
H26A H 0.8182 1.0000 0.4981 0.281 Uiso 1 2 calc SR
H26B H 0.7454 1.0000 0.4988 0.281 Uiso 1 2 calc SR
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'
Ru Ru -1.2594 0.8363 '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'
Cl Cl 0.1484 0.1585 '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'
H H 0.0000 0.0000 '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'
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
C3 C4 C12 125.6(3) 6_565 .
C3 C4 C5 116.3(2) 6_565 .
C12 C4 C5 117.9(3) . .
C1 Ru1 N3 98.49(15) . .
C1 Ru1 N2 89.81(6) . .
N3 Ru1 N2 91.26(5) . .
C1 Ru1 N2 89.81(6) . 6_565
N3 Ru1 N2 91.26(5) . 6_565
N2 Ru1 N2 177.48(10) . 6_565
C1 Ru1 S1 90.03(12) . .
N3 Ru1 S1 171.47(10) . .
N2 Ru1 S1 88.76(5) . .
N2 Ru1 S1 88.76(5) 6_565 .
C1 Ru1 Cl1 175.78(12) . .
N3 Ru1 Cl1 85.72(10) . .
N2 Ru1 Cl1 90.10(6) . .
N2 Ru1 Cl1 90.10(6) 6_565 .
S1 Ru1 Cl1 85.75(4) . .
C3 S1 C3 93.3(2) . 6_565
C3 S1 Ru1 110.28(10) . .
C3 S1 Ru1 110.28(10) 6_565 .
O1 C1 Ru1 173.7(4) . .
C24 N3 C24 108.2(3) 6_565 .
C24 N3 Ru1 125.27(16) 6_565 .
C24 N3 Ru1 125.27(16) . .
C15 N2 C12 107.1(3) . .
C15 N2 Ru1 124.42(18) . .
C12 N2 Ru1 128.46(17) . .
N2 C15 C16 125.6(3) . .
N2 C15 C14 109.0(2) . .
C16 C15 C14 125.2(3) . .
N2 C12 C4 127.7(3) . .
N2 C12 C13 108.5(2) . .
C4 C12 C13 123.5(3) . .
C15 C16 C24 126.3(3) . .
C15 C16 C17 117.9(3) . .
C24 C16 C17 115.8(3) . .
C4 C3 C2 131.5(3) 6_565 .
C4 C3 S1 120.7(2) 6_565 .
C2 C3 S1 107.6(2) . .
C19 C17 C18 117.7(3) . .
C19 C17 C16 120.3(3) . .
C18 C17 C16 121.9(3) . .
C13 C14 C15 107.9(3) . .
C13 C14 H14A 126.1 . .
C15 C14 H14A 126.1 . .
C6 C5 C7 118.4(3) . .
C6 C5 C4 121.6(3) . .
C7 C5 C4 120.0(3) . .
N3 C24 C16 126.3(2) . .
N3 C24 C25 107.6(3) . .
C16 C24 C25 125.9(3) . .
C14 C13 C12 107.4(3) . .
C14 C13 H13A 126.3 . .
C12 C13 H13A 126.3 . .
C25 C25 C24 108.20(19) 6_565 .
C25 C25 H25A 125.9 6_565 .
C24 C25 H25A 125.9 . .
C5 C6 C8 119.5(4) . .
C5 C6 H6A 120.2 . .
C8 C6 H6A 120.2 . .
C21 C19 C17 121.1(4) . .
C21 C19 H19A 119.4 . .
C17 C19 H19A 119.4 . .
C10 C8 C6 122.0(4) . .
C10 C8 H8A 119.0 . .
C6 C8 H8A 119.0 . .
C2 C2 C3 114.30(18) 6_565 .
C2 C2 H2A 122.9 6_565 .
C3 C2 H2A 122.9 . .
C20 C22 C21 118.1(3) . .
C20 C22 C23 120.6(4) . .
C21 C22 C23 121.3(4) . .
C17 C18 C20 120.5(4) . .
C17 C18 H18A 119.7 . .
C20 C18 H18A 119.7 . .
C9 C7 C5 121.0(4) . .
C9 C7 H7A 119.5 . .
C5 C7 H7A 119.5 . .
C22 C20 C18 121.1(4) . .
C22 C20 H20A 119.4 . .
C18 C20 H20A 119.4 . .
C19 C21 C22 121.4(4) . .
C19 C21 H21A 119.3 . .
C22 C21 H21A 119.3 . .
C7 C9 C10 120.6(4) . .
C7 C9 H9A 119.7 . .
C10 C9 H9A 119.7 . .
C8 C10 C9 118.5(4) . .
C8 C10 C11 121.8(5) . .
C9 C10 C11 119.7(5) . .
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 . .
C10 C11 H11A 109.5 . .
C10 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
C10 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
Cl2 C26 Cl2 106.9(6) 6_575 .
Cl2 C26 H26A 110.3 6_575 .
Cl2 C26 H26A 110.3 . .
Cl2 C26 H26B 110.3 6_575 .
Cl2 C26 H26B 110.3 . .
H26A C26 H26B 108.6 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C4 C3 1.385(4) 6_565
C4 C12 1.430(4) .
C4 C5 1.505(4) .
Ru1 C1 1.843(4) .
Ru1 N3 2.044(3) .
Ru1 N2 2.077(2) .
Ru1 N2 2.077(2) 6_565
Ru1 S1 2.2453(10) .
Ru1 Cl1 2.4694(14) .
S1 C3 1.741(3) .
S1 C3 1.741(3) 6_565
C1 O1 1.114(5) .
N3 C24 1.363(3) 6_565
N3 C24 1.363(3) .
N2 C15 1.378(3) .
N2 C12 1.383(3) .
C15 C16 1.401(4) .
C15 C14 1.431(4) .
C12 C13 1.443(4) .
C16 C24 1.412(4) .
C16 C17 1.500(4) .
C3 C4 1.385(4) 6_565
C3 C2 1.412(4) .
C17 C19 1.380(5) .
C17 C18 1.370(5) .
C14 C13 1.349(5) .
C14 H14A 0.9300 .
C5 C6 1.384(5) .
C5 C7 1.379(5) .
C24 C25 1.451(4) .
C13 H13A 0.9300 .
C25 C25 1.301(7) 6_565
C25 H25A 0.9300 .
C6 C8 1.400(5) .
C6 H6A 0.9300 .
C19 C21 1.389(5) .
C19 H19A 0.9300 .
C8 C10 1.360(6) .
C8 H8A 0.9300 .
C2 C2 1.369(6) 6_565
C2 H2A 0.9300 .
C22 C20 1.364(6) .
C22 C21 1.362(6) .
C22 C23 1.531(5) .
C18 C20 1.410(5) .
C18 H18A 0.9300 .
C7 C9 1.396(5) .
C7 H7A 0.9300 .
C20 H20A 0.9300 .
C21 H21A 0.9300 .
C9 C10 1.368(7) .
C9 H9A 0.9300 .
C10 C11 1.521(6) .
C23 H23A 0.9600 .
C23 H23B 0.9600 .
C23 H23C 0.9600 .
C11 H11A 0.9600 .
C11 H11B 0.9600 .
C11 H11C 0.9600 .
Cl2 C26 1.722(7) .
C26 Cl2 1.721(7) 6_575
C26 H26A 0.9700 .
C26 H26B 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 -0.016 512 70 ' '
2 0.500 0.500 -0.013 512 70 ' '
