#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:16:56 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179320 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/17/4321753.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_4321753
loop_
_publ_author_name
'Dieter Sellmann'
'Jürgen Utz'
'Frank W. Heinemann'
_publ_contact_author
; 
        Prof. Dr. D. Sellmann 
        Institut für Anorganische Chemie II 
        Universität Erlangen-Nürnberg 
        Egerlandstr. 1 
        D-91058 Erlangen 
        Bundesrepublik Deutschland 
;
_publ_contact_author_email       SELLMANN@ANORGANIK.CHEMIE.UNI-ERLANGEN.DE
_publ_contact_author_fax         '049 9131 85-7367'
_publ_contact_author_phone       '049 9131 85-7360'
_publ_section_title
;
 Transition-Metal Complexes with Sulfur Ligands. 132.1 Electron-Rich Fe
 and Ru Complexes with [MN₂S₃] Cores Containing the New Pentadentate
 Ligand 'N₂H₂S₃'²⁻ (= 2,2'-Bis(2-mercaptophenylamino)diethyl
 Sulfide(2-))
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              459
_journal_page_last               466
_journal_paper_doi               10.1021/ic980383q
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C38 H43 Cl4 I2 N2 P Ru S3'
_chemical_formula_weight         1151.56
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 109.24(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   33.128(12)
_cell_length_b                   16.252(5)
_cell_length_c                   17.185(7)
_cell_measurement_reflns_used    18
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      12.0
_cell_measurement_theta_min      10.0
_cell_volume                     8736(6)
_computing_cell_refinement       'P3 (Siemens Analytical X-Ray Instr., 1989)'
_computing_data_collection       'P3 (Siemens Analytical X-Ray Instr., 1989)'
_computing_data_reduction
'XDISK (Siemens Analytical X-Ray Instr. , 1989)'
_computing_molecular_graphics
'XP 5.03 (Siemens Analytical X-Ray Instr, 1995)'
_computing_publication_material  'CIFTAB (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL 93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXTL PLUS 4.21/V'
_diffrn_ambient_temperature      200(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       'profile data from ω-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  0.0491
_diffrn_reflns_av_sigmaI/netI    0.0665
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            18249
_diffrn_reflns_theta_max         24.05
_diffrn_reflns_theta_min         2.03
_diffrn_standards_decay_%        2.30
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.227
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.751
_exptl_crystal_description       plate
_exptl_crystal_F_000             4528
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         1.374
_refine_diff_density_min         -1.170
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.881
_refine_ls_goodness_of_fit_obs   1.007
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         6895
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.881
_refine_ls_restrained_S_obs      1.007
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_obs          0.0361
_refine_ls_shift/esd_max         0.011
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0515P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0904
_refine_ls_wR_factor_obs         0.0876
_reflns_number_observed          5063
_reflns_number_total             6895
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic980383q_1.cif
_cod_data_source_block           ju33
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0515P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0515P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        8735.6(55)
_cod_database_code               4321753
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Ru1 Ru 0.159306(12) 0.17051(3) 0.17753(2) 0.01853(10) Uani 1 d . .
I1 I 0.265006(12) 0.33890(2) 0.13536(2) 0.03569(11) Uani 1 d . .
I2 I 0.342003(13) 0.22349(3) 0.46635(2) 0.03759(12) Uani 1 d . .
S1 S 0.14818(4) 0.03521(8) 0.12994(9) 0.0277(3) Uani 1 d . .
S2 S 0.19334(4) 0.14072(9) 0.31681(8) 0.0278(3) Uani 1 d . .
S3 S 0.13133(4) 0.22750(8) 0.04533(8) 0.0245(3) Uani 1 d . .
C1 C 0.1518(2) -0.0436(4) 0.2062(5) 0.046(2) Uani 1 d . .
C2 C 0.1650(2) 0.2140(4) -0.0184(3) 0.0350(14) Uani 1 d . .
N1 N 0.22338(13) 0.1500(3) 0.1684(3) 0.0230(10) Uani 1 d . .
N2 N 0.17979(15) 0.2941(3) 0.2119(3) 0.0287(10) Uani 1 d . .
C15 C 0.2264(2) 0.0775(3) 0.1204(3) 0.0259(12) Uani 1 d . .
C14 C 0.2610(2) 0.0688(4) 0.0907(3) 0.0337(14) Uani 1 d . .
C13 C 0.2651(2) -0.0024(5) 0.0504(4) 0.045(2) Uani 1 d . .
C12 C 0.2357(2) -0.0652(4) 0.0391(4) 0.042(2) Uani 1 d . .
C11 C 0.2005(2) -0.0563(4) 0.0650(4) 0.0392(15) Uani 1 d . .
C10 C 0.1956(2) 0.0169(3) 0.1051(3) 0.0282(12) Uani 1 d . .
C25 C 0.1589(2) 0.3575(3) 0.1516(3) 0.0268(12) Uani 1 d . .
C24 C 0.1625(2) 0.4407(4) 0.1721(4) 0.0387(15) Uani 1 d . .
C23 C 0.1469(3) 0.4979(4) 0.1106(5) 0.055(2) Uani 1 d . .
C22 C 0.1287(3) 0.4755(4) 0.0295(5) 0.053(2) Uani 1 d . .
C21 C 0.1242(2) 0.3923(4) 0.0089(4) 0.043(2) Uani 1 d . .
C20 C 0.1396(2) 0.3340(4) 0.0710(4) 0.0290(12) Uani 1 d . .
C16 C 0.2582(2) 0.1471(3) 0.2513(3) 0.0265(12) Uani 1 d . .
C17 C 0.2442(2) 0.1007(4) 0.3133(3) 0.0311(13) Uani 1 d . .
C26 C 0.1851(2) 0.3114(4) 0.2994(4) 0.040(2) Uani 1 d . .
C27 C 0.2098(2) 0.2453(4) 0.3559(3) 0.0342(14) Uani 1 d . .
P1 P 0.09096(4) 0.17882(9) 0.19118(8) 0.0215(3) Uani 1 d . .
C35 C 0.1056(2) 0.0941(4) 0.3420(3) 0.0307(13) Uani 1 d . .
C34 C 0.1021(2) 0.0257(4) 0.3888(4) 0.040(2) Uani 1 d . ..
C33 C 0.0770(2) -0.0412(4) 0.3526(4) 0.042(2) Uani 1 d . .
C32 C 0.0536(2) -0.0377(4) 0.2699(4) 0.0388(15) Uani 1 d . .
C31 C 0.0559(2) 0.0303(4) 0.2227(3) 0.0299(13) Uani 1 d . .
C30 C 0.0823(2) 0.0963(3) 0.2581(3) 0.0254(12) Uani 1 d . .
C45 C 0.0035(2) 0.1922(4) 0.0995(3) 0.0349(14) Uani 1 d . .
C44 C -0.0335(2) 0.1746(5) 0.0347(4) 0.041(2) Uani 1 d . .
C43 C -0.0316(2) 0.1285(4) -0.0312(4) 0.041(2) Uani 1 d . .
C42 C 0.0077(2) 0.0996(4) -0.0327(3) 0.0356(14) Uani 1 d . .
C41 C 0.0445(2) 0.1171(4) 0.0328(3) 0.0274(12) Uani 1 d . .
C40 C 0.0431(2) 0.1638(3) 0.0990(3) 0.0249(11) Uani 1 d . .
C55 C 0.0738(2) 0.2851(4) 0.3089(4) 0.0342(13) Uani 1 d . .
C54 C 0.0639(2) 0.3630(5) 0.3347(4) 0.047(2) Uani 1 d . .
C53 C 0.0563(2) 0.4286(4) 0.2821(5) 0.051(2) Uani 1 d . .
C52 C 0.0586(2) 0.4193(4) 0.2039(5) 0.048(2) Uani 1 d . .
C51 C 0.0681(2) 0.3437(4) 0.1778(4) 0.0371(14) Uani 1 d . .
C50 C 0.0763(2) 0.2757(3) 0.2301(3) 0.0272(12) Uani 1 d . .
C3 C 0.1296(3) 0.7089(5) 0.2387(5) 0.061(2) Uani 1 d . .
H3A H 0.1580(3) 0.7336(5) 0.2672(5) 0.091 Uiso 1 calc R .
H3B H 0.1267(3) 0.7021(5) 0.1798(5) 0.091 Uiso 1 calc R .
Cl1 Cl 0.09018(8) 0.7745(2) 0.2468(2) 0.0890(8) Uani 1 d . .
Cl2 Cl 0.12663(7) 0.61232(13) 0.28161(13) 0.0639(5) Uani 1 d . .
C4 C -0.0080(4) 0.6305(19) 0.0593(9) 0.301(19) Uani 1 d . .
H4A H -0.0289(4) 0.5868(19) 0.0336(9) 0.451 Uiso 1 calc R .
H4B H -0.0178(4) 0.6801(19) 0.0249(9) 0.451 Uiso 1 calc R .
Cl3 Cl -0.0157(2) 0.6514(6) 0.1464(3) 0.285(5) Uani 1 d . .
Cl4 Cl 0.0344(3) 0.6036(5) 0.0435(4) 0.287(4) Uani 1 d . .
H1A H 0.1635 -0.1017 0.1889 0.050 Uiso 1 d . .
H1B H 0.1805 -0.0243 0.2454 0.050 Uiso 1 d . .
H1C H 0.1218 -0.0563 0.2239 0.050 Uiso 1 d . .
H2A H 0.1988 0.2283 0.0191 0.050 Uiso 1 d . .
H2B H 0.1600 0.1538 -0.0353 0.050 Uiso 1 d . .
H2C H 0.1567 0.2416 -0.0554 0.050 Uiso 1 d . .
H1 H 0.2311 0.1985 0.1403 0.050 Uiso 1 d . .
H2 H 0.2120 0.2997 0.1995 0.050 Uiso 1 d . .
H14 H 0.2825 0.1191 0.1080 0.050 Uiso 1 d . .
H13 H 0.2823 -0.0167 0.0217 0.050 Uiso 1 d . .
H12 H 0.2399 -0.1196 0.0117 0.050 Uiso 1 d . .
H11 H 0.1798 -0.0968 0.0663 0.050 Uiso 1 d . .
H24 H 0.1827 0.4496 0.2421 0.050 Uiso 1 d . .
H23 H 0.1443 0.5541 0.1318 0.050 Uiso 1 d . .
H22 H 0.1136 0.5198 -0.0160 0.050 Uiso 1 d . .
H21 H 0.1087 0.3708 -0.0469 0.050 Uiso 1 d . .
H16A H 0.2604 0.1987 0.2592 0.050 Uiso 1 d . .
H16B H 0.2857 0.1315 0.2477 0.050 Uiso 1 d . .
H17A H 0.2620 0.1077 0.3601 0.050 Uiso 1 d . .
H17B H 0.2388 0.0514 0.3008 0.050 Uiso 1 d . .
H26A H 0.1519 0.3117 0.3036 0.050 Uiso 1 d . .
H26B H 0.1971 0.3748 0.3085 0.050 Uiso 1 d . .
H27A H 0.2396 0.2460 0.3781 0.050 Uiso 1 d . .
H27B H 0.2016 0.2438 0.4045 0.050 Uiso 1 d . .
H35 H 0.1303 0.1441 0.3756 0.050 Uiso 1 d . .
H34 H 0.1198 0.0204 0.4510 0.050 Uiso 1 d . .
H33 H 0.0716 -0.0960 0.3777 0.050 Uiso 1 d . .
H32 H 0.0402 -0.0924 0.2442 0.050 Uiso 1 d . .
H31 H 0.0326 0.0430 0.1608 0.050 Uiso 1 d . .
H45 H 0.0037 0.2259 0.1474 0.050 Uiso 1 d . .
H44 H -0.0669 0.1952 0.0248 0.050 Uiso 1 d . .
H43 H -0.0561 0.1244 -0.0797 0.050 Uiso 1 d . .
H42 H 0.0103 0.0577 -0.0781 0.050 Uiso 1 d . .
H41 H 0.0680 0.0978 0.0271 0.050 Uiso 1 d . .
H55 H 0.0771 0.2301 0.3474 0.050 Uiso 1 d . .
H54 H 0.0634 0.3609 0.3959 0.050 Uiso 1 d . .
H53 H 0.0508 0.4863 0.3045 0.050 Uiso 1 d . .
H52 H 0.0598 0.4767 0.1745 0.050 Uiso 1 d . .
H51 H 0.0697 0.3362 0.1223 0.050 Uiso 1 d . .
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'
P P 0.1023 0.0942 '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'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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
N2 Ru1 N1 86.3(2) . . ?
N2 Ru1 S1 168.71(13) . . ?
N1 Ru1 S1 82.95(12) . . ?
N2 Ru1 S2 84.80(13) . . ?
N1 Ru1 S2 83.72(12) . . ?
S1 Ru1 S2 97.53(6) . . ?
N2 Ru1 S3 83.39(13) . . ?
N1 Ru1 S3 94.21(12) . . ?
S1 Ru1 S3 93.81(6) . . ?
S2 Ru1 S3 168.12(5) . . ?
N2 Ru1 P1 98.42(13) . . ?
N1 Ru1 P1 174.39(12) . . ?
S1 Ru1 P1 92.46(5) . . ?
S2 Ru1 P1 93.73(7) . . ?
S3 Ru1 P1 89.30(6) . . ?
C10 S1 C1 101.7(3) . . ?
C10 S1 Ru1 101.0(2) . . ?
C1 S1 Ru1 116.7(3) . . ?
C17 S2 C27 100.1(3) . . ?
C17 S2 Ru1 100.3(2) . . ?
C27 S2 Ru1 99.6(2) . . ?
C20 S3 C2 101.0(3) . . ?
C20 S3 Ru1 99.4(2) . . ?
C2 S3 Ru1 114.3(2) . . ?
C15 N1 C16 109.5(4) . . ?
C15 N1 Ru1 114.1(3) . . ?
C16 N1 Ru1 113.1(3) . . ?
C25 N2 C26 117.1(5) . . ?
C25 N2 Ru1 115.6(3) . . ?
C26 N2 Ru1 112.3(4) . . ?
C10 C15 C14 119.9(5) . . ?
C10 C15 N1 120.0(5) . . ?
C14 C15 N1 120.0(5) . . ?
C13 C14 C15 119.4(6) . . ?
C14 C13 C12 120.7(6) . . ?
C13 C12 C11 120.5(6) . . ?
C12 C11 C10 119.3(6) . . ?
C15 C10 C11 120.0(5) . . ?
C15 C10 S1 119.3(4) . . ?
C11 C10 S1 120.6(4) . . ?
C20 C25 C24 119.9(6) . . ?
C20 C25 N2 118.1(5) . . ?
C24 C25 N2 121.5(5) . . ?
C23 C24 C25 118.9(6) . . ?
C22 C23 C24 122.0(6) . . ?
C23 C22 C21 119.3(7) . . ?
C20 C21 C22 119.0(6) . . ?
C25 C20 C21 120.9(6) . . ?
C25 C20 S3 120.1(4) . . ?
C21 C20 S3 118.9(5) . . ?
C17 C16 N1 111.5(4) . . ?
C16 C17 S2 110.5(4) . . ?
N2 C26 C27 112.3(5) . . ?
C26 C27 S2 113.1(4) . . ?
C50 P1 C30 106.3(3) . . ?
C50 P1 C40 99.8(2) . . ?
C30 P1 C40 99.9(2) . . ?
C50 P1 Ru1 117.6(2) . . ?
C30 P1 Ru1 111.8(2) . . ?
C40 P1 Ru1 119.1(2) . . ?
C30 C35 C34 119.5(6) . . ?
C33 C34 C35 121.1(5) . . ?
C32 C33 C34 118.8(6) . . ?
C33 C32 C31 121.0(6) . . ?
C32 C31 C30 120.5(5) . . ?
C31 C30 C35 119.1(5) . . ?
C31 C30 P1 119.4(4) . . ?
C35 C30 P1 121.0(4) . . ?
C44 C45 C40 120.7(5) . . ?
C43 C44 C45 120.3(6) . . ?
C44 C43 C42 119.7(5) . . ?
C41 C42 C43 119.4(5) . . ?
C40 C41 C42 121.6(5) . . ?
C41 C40 C45 118.3(5) . . ?
C41 C40 P1 121.8(4) . . ?
C45 C40 P1 119.5(4) . . ?
C50 C55 C54 119.8(6) . . ?
C53 C54 C55 120.1(6) . . ?
C54 C53 C52 120.2(6) . . ?
C51 C52 C53 120.3(6) . . ?
C52 C51 C50 120.9(6) . . ?
C55 C50 C51 118.6(5) . . ?
C55 C50 P1 123.8(4) . . ?
C51 C50 P1 117.6(4) . . ?
Cl1 C3 Cl2 111.8(4) . . ?
Cl4 C4 Cl3 129.2(9) . . ?
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
Ru1 N2 2.139(5) . ?
Ru1 N1 2.205(4) . ?
Ru1 S1 2.333(2) . ?
Ru1 S2 2.336(2) . ?
Ru1 S3 2.343(2) . ?
Ru1 P1 2.356(2) . ?
S1 C10 1.784(6) . ?
S1 C1 1.808(6) . ?
S2 C17 1.826(6) . ?
S2 C27 1.842(6) . ?
S3 C20 1.784(6) . ?
S3 C2 1.815(6) . ?
N1 C15 1.461(7) . ?
N1 C16 1.510(7) . ?
N2 C25 1.465(7) . ?
N2 C26 1.481(7) . ?
C15 C10 1.378(8) . ?
C15 C14 1.409(8) . ?
C14 C13 1.377(9) . ?
C13 C12 1.381(10) . ?
C12 C11 1.385(9) . ?
C11 C10 1.411(8) . ?
C25 C20 1.374(8) . ?
C25 C24 1.391(8) . ?
C24 C23 1.375(10) . ?
C23 C22 1.373(11) . ?
C22 C21 1.394(10) . ?
C21 C20 1.392(8) . ?
C16 C17 1.497(8) . ?
C26 C27 1.497(9) . ?
P1 C50 1.837(6) . ?
P1 C30 1.850(5) . ?
P1 C40 1.851(5) . ?
C35 C30 1.394(7) . ?
C35 C34 1.399(8) . ?
C34 C33 1.385(9) . ?
C33 C32 1.379(9) . ?
C32 C31 1.387(8) . ?
C31 C30 1.391(8) . ?
C45 C44 1.387(8) . ?
C45 C40 1.394(7) . ?
C44 C43 1.376(9) . ?
C43 C42 1.393(8) . ?
C42 C41 1.388(8) . ?
C41 C40 1.379(8) . ?
C55 C50 1.393(8) . ?
C55 C54 1.415(9) . ?
C54 C53 1.366(10) . ?
C53 C52 1.380(10) . ?
C52 C51 1.380(9) . ?
C51 C50 1.394(8) . ?
C3 Cl1 1.727(8) . ?
C3 Cl2 1.751(8) . ?
C4 Cl4 1.577(15) . ?
C4 Cl3 1.64(2) . ?
