#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:34:46 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179336 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/33/4323367.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_4323367
loop_
_publ_author_name
'Dieter Sellmann'
'Michael W. Wemple'
'Wolfgang Donaubauer'
'Frank W. Heinemann'
_publ_contact_author
;                                                                               
        Dr. F. W. Heinemann                                                     
        Institut für Anorganische Chemie II                                   
        Universität Erlangen-Nürnberg                                       
        Egerlandstr. 1                                                          
        D-91058 Erlangen                                                        
        Bundesrepublik Deutschland                                              
;
_publ_contact_author_email       HEINEMAN@ANORGANIK.CHEMIE.UNI-ERLANGEN.DE
_publ_contact_author_fax         '049 9131 85-7367'
_publ_contact_author_phone       '049 9131 85-7383'
_publ_section_title
;
 Synthesis, Structure, and Reactivity of Ruthenium and Osmium Nitrido
 Complexes with 1,2-Benzenedithiolate Ligands: N- versus S-Alkylation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1397
_journal_page_last               1402
_journal_paper_doi               10.1021/ic961240b
_journal_volume                  36
_journal_year                    1997
_chemical_formula_sum            'C14 H13 Cl2 N Os S4'
_chemical_formula_weight         584.59
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.5520(10)
_cell_length_b                   10.772(2)
_cell_length_c                   19.716(3)
_cell_measurement_reflns_used    18
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      16.0
_cell_measurement_theta_min      14.0
_cell_volume                     1816.3(5)
_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, 1994)
;
_computing_publication_material  'CIFTAB (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_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  0.0312
_diffrn_reflns_av_sigmaI/netI    0.0660
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3479
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.07
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.768
_exptl_absorpt_correction_T_max  0.145
_exptl_absorpt_correction_T_min  0.084
_exptl_absorpt_correction_type   refdelf
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.138
_exptl_crystal_description       prism
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         3.055
_refine_diff_density_min         -2.020
_refine_diff_density_rms         0.201
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.022(13)
_refine_ls_extinction_coef       0.0022(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   0.962
_refine_ls_goodness_of_fit_obs   1.020
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     252
_refine_ls_number_reflns         3204
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.962
_refine_ls_restrained_S_obs      1.020
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_obs          0.0362
_refine_ls_shift/esd_max         -0.035
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0463P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0848
_refine_ls_wR_factor_obs         0.0843
_reflns_number_observed          2845
_reflns_number_total             3204
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic961240b_4.cif
_cod_data_source_block           mw53
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0463P)^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^)+(0.0463P)^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_database_code               4323367
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Os1 Os 0.05438(5) 0.86570(4) 0.42111(2) 0.01732(13) Uani 1 d . .
S1 S 0.0875(3) 0.9162(3) 0.53342(14) 0.0241(6) Uani 1 d . .
S2 S -0.1112(3) 1.0349(2) 0.4141(2) 0.0268(6) Uani 1 d . .
S3 S -0.1271(3) 0.7734(3) 0.3499(2) 0.0266(6) Uani 1 d . .
S4 S 0.1302(3) 0.6576(2) 0.45030(14) 0.0198(6) Uani 1 d . .
N1 N 0.2132(11) 0.9077(9) 0.3807(5) 0.031(2) Uani 1 d . .
C1 C 0.0264(16) 0.6132(14) 0.5278(6) 0.032(3) Uani 1 d . .
C10 C 0.0038(13) 1.0648(11) 0.5437(7) 0.028(3) Uani 1 d . .
C11 C 0.0152(13) 1.1271(12) 0.6061(6) 0.031(3) Uani 1 d . .
C12 C -0.0568(18) 1.2399(11) 0.6128(7) 0.036(3) Uani 1 d . .
C13 C -0.1385(16) 1.2931(11) 0.5621(7) 0.037(3) Uani 1 d . .
C14 C -0.1536(16) 1.2320(12) 0.5000(8) 0.033(3) Uani 1 d . .
C15 C -0.0852(12) 1.1163(11) 0.4893(6) 0.024(3) Uani 1 d . .
C20 C 0.0358(13) 0.5635(9) 0.3885(5) 0.019(2) Uani 1 d . .
C21 C 0.0701(17) 0.4353(10) 0.3856(6) 0.031(3) Uani 1 d . .
C22 C -0.0032(14) 0.3648(13) 0.3384(6) 0.036(3) Uani 1 d . .
C23 C -0.1047(15) 0.4143(11) 0.2929(7) 0.032(3) Uani 1 d . .
C24 C -0.1414(16) 0.5392(12) 0.2952(6) 0.030(3) Uani 1 d . .
C25 C -0.0722(14) 0.6172(11) 0.3447(6) 0.028(3) Uani 1 d . .
C30 C -0.3185(16) 1.0262(17) 0.2492(9) 0.047(4) Uani 1 d . .
Cl1 Cl -0.3754(5) 1.1571(3) 0.2010(2) 0.0500(9) Uani 1 d . .
Cl2 Cl -0.4782(4) 0.9628(3) 0.2935(2) 0.0376(8) Uani 1 d . .
H1A H -0.0752(126) 0.6188(108) 0.5221(52) 0.011(28) Uiso 1 d . .
H1B H 0.0399(118) 0.6581(85) 0.5767(54) 0.019(25) Uiso 1 d . .
H1C H 0.0663(190) 0.5350(142) 0.5520(76) 0.067(49) Uiso 1 d . .
H11 H 0.0670(125) 1.0839(87) 0.6553(52) 0.013(25) Uiso 1 d . .
H12 H -0.0786(178) 1.2823(133) 0.6502(71) 0.055(46) Uiso 1 d . .
H13 H -0.1936(112) 1.3734(106) 0.5673(51) 0.019(26) Uiso 1 d . .
H14 H -0.2046(176) 1.2571(137) 0.4713(74) 0.045(49) Uiso 1 d . .
H21 H 0.1549(122) 0.4039(90) 0.4117(58) 0.017(28) Uiso 1 d . .
H22 H 0.0188(168) 0.2556(132) 0.3423(66) 0.055(43) Uiso 1 d . .
H23 H -0.1664(118) 0.3501(110) 0.2626(54) 0.023(28) Uiso 1 d . .
H24 H -0.1974(143) 0.5509(123) 0.2486(71) 0.044(39) Uiso 1 d . .
H30A H -0.3071(230) 0.9775(186) 0.2094(102) 0.100(76) Uiso 1 d . .
H30B H -0.2675(215) 1.0797(154) 0.3036(99) 0.098(65) 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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Os Os -1.2165 7.6030 '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
_geom_angle_publ_flag
N1 Os1 S1 107.6(4) . . ?
N1 Os1 S2 105.1(4) . . ?
S1 Os1 S2 86.91(11) . . ?
N1 Os1 S3 112.2(4) . . ?
S1 Os1 S3 140.19(11) . . ?
S2 Os1 S3 83.80(10) . . ?
N1 Os1 S4 98.6(4) . . ?
S1 Os1 S4 87.53(10) . . ?
S2 Os1 S4 156.17(10) . . ?
S3 Os1 S4 85.74(10) . . ?
C10 S1 Os1 106.0(4) . . ?
C15 S2 Os1 105.6(4) . . ?
C25 S3 Os1 105.5(4) . . ?
C20 S4 C1 101.7(6) . . ?
C20 S4 Os1 104.2(3) . . ?
C1 S4 Os1 108.2(5) . . ?
S4 C1 H1A 110.7(70) . . ?
S4 C1 H1B 125.0(54) . . ?
H1A C1 H1B 101.0(91) . . ?
S4 C1 H1C 116.2(88) . . ?
H1A C1 H1C 116.4(100) . . ?
H1B C1 H1C 85.3(93) . . ?
C11 C10 C15 120.6(11) . . ?
C11 C10 S1 120.3(9) . . ?
C15 C10 S1 118.9(10) . . ?
C12 C11 C10 118.5(12) . . ?
C12 C11 H11 116.5(50) . . ?
C10 C11 H11 124.4(49) . . ?
C13 C12 C11 122.7(12) . . ?
C13 C12 H12 106.8(97) . . ?
C11 C12 H12 129.1(96) . . ?
C12 C13 C14 119.9(12) . . ?
C12 C13 H13 122.7(61) . . ?
C14 C13 H13 117.3(62) . . ?
C15 C14 C13 121.1(14) . . ?
C15 C14 H14 116.4(100) . . ?
C13 C14 H14 122.4(100) . . ?
C14 C15 C10 117.3(12) . . ?
C14 C15 S2 121.8(10) . . ?
C10 C15 S2 120.9(9) . . ?
C25 C20 C21 121.3(11) . . ?
C25 C20 S4 119.3(8) . . ?
C21 C20 S4 119.4(9) . . ?
C22 C21 C20 118.6(13) . . ?
C22 C21 H21 121.7(64) . . ?
C20 C21 H21 118.9(63) . . ?
C21 C22 C23 122.0(13) . . ?
C21 C22 H22 115.8(67) . . ?
C23 C22 H22 122.0(68) . . ?
C22 C23 C24 120.4(13) . . ?
C22 C23 H23 115.8(61) . . ?
C24 C23 H23 122.9(61) . . ?
C23 C24 C25 120.3(12) . . ?
C23 C24 H24 101.1(74) . . ?
C25 C24 H24 136.6(75) . . ?
C20 C25 C24 117.3(11) . . ?
C20 C25 S3 122.9(9) . . ?
C24 C25 S3 119.9(9) . . ?
Cl2 C30 Cl1 111.3(8) . . ?
Cl2 C30 H30A 106.0(100) . . ?
Cl1 C30 H30A 91.5(100) . . ?
Cl2 C30 H30B 91.3(82) . . ?
Cl1 C30 H30B 100.6(77) . . ?
H30A C30 H30B 153.8(100) . . ?
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
Os1 N1 1.639(9) . ?
Os1 S1 2.298(3) . ?
Os1 S2 2.312(3) . ?
Os1 S3 2.318(3) . ?
Os1 S4 2.403(3) . ?
S1 C10 1.765(12) . ?
S2 C15 1.737(12) . ?
S3 C25 1.750(12) . ?
S4 C20 1.780(11) . ?
S4 C1 1.831(13) . ?
C1 H1A 0.88(10) . ?
C1 H1B 1.08(10) . ?
C1 H1C 1.03(15) . ?
C10 C11 1.41(2) . ?
C10 C15 1.43(2) . ?
C11 C12 1.37(2) . ?
C11 H11 1.16(10) . ?
C12 C13 1.35(2) . ?
C12 H12 0.89(14) . ?
C13 C14 1.40(2) . ?
C13 H13 0.99(11) . ?
C14 C15 1.39(2) . ?
C14 H14 0.76(14) . ?
C20 C25 1.39(2) . ?
C20 C21 1.413(15) . ?
C21 C22 1.35(2) . ?
C21 H21 0.95(11) . ?
C22 C23 1.36(2) . ?
C22 H22 1.19(14) . ?
C23 C24 1.38(2) . ?
C23 H23 1.06(11) . ?
C24 C25 1.42(2) . ?
C24 H24 1.04(14) . ?
C30 Cl2 1.760(14) . ?
C30 Cl1 1.767(15) . ?
C30 H30A 0.95(19) . ?
C30 H30B 1.29(19) . ?
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 Os1 S1 C10 93.7(6) . . . . ?
S2 Os1 S1 C10 -11.2(4) . . . . ?
S3 Os1 S1 C10 -87.7(4) . . . . ?
S4 Os1 S1 C10 -168.1(4) . . . . ?
N1 Os1 S2 C15 -96.2(5) . . . . ?
S1 Os1 S2 C15 11.2(4) . . . . ?
S3 Os1 S2 C15 152.4(4) . . . . ?
S4 Os1 S2 C15 87.9(4) . . . . ?
N1 Os1 S3 C25 84.4(6) . . . . ?
S1 Os1 S3 C25 -94.2(4) . . . . ?
S2 Os1 S3 C25 -171.8(4) . . . . ?
S4 Os1 S3 C25 -13.2(4) . . . . ?
N1 Os1 S4 C20 -99.8(5) . . . . ?
S1 Os1 S4 C20 152.8(4) . . . . ?
S2 Os1 S4 C20 76.2(5) . . . . ?
S3 Os1 S4 C20 12.1(4) . . . . ?
N1 Os1 S4 C1 152.5(6) . . . . ?
S1 Os1 S4 C1 45.1(4) . . . . ?
S2 Os1 S4 C1 -31.5(5) . . . . ?
S3 Os1 S4 C1 -95.6(5) . . . . ?
Os1 S1 C10 C11 -175.2(9) . . . . ?
Os1 S1 C10 C15 9.5(10) . . . . ?
C15 C10 C11 C12 -2.1(18) . . . . ?
S1 C10 C11 C12 -177.3(10) . . . . ?
C10 C11 C12 C13 0.4(20) . . . . ?
C11 C12 C13 C14 0.7(21) . . . . ?
C12 C13 C14 C15 -0.1(20) . . . . ?
C13 C14 C15 C10 -1.6(18) . . . . ?
C13 C14 C15 S2 176.5(10) . . . . ?
C11 C10 C15 C14 2.7(16) . . . . ?
S1 C10 C15 C14 178.0(9) . . . . ?
C11 C10 C15 S2 -175.4(9) . . . . ?
S1 C10 C15 S2 -0.1(13) . . . . ?
Os1 S2 C15 C14 172.7(9) . . . . ?
Os1 S2 C15 C10 -9.2(10) . . . . ?
C1 S4 C20 C25 104.0(10) . . . . ?
Os1 S4 C20 C25 -8.5(10) . . . . ?
C1 S4 C20 C21 -75.0(11) . . . . ?
Os1 S4 C20 C21 172.5(9) . . . . ?
C25 C20 C21 C22 0.8(18) . . . . ?
S4 C20 C21 C22 179.7(9) . . . . ?
C20 C21 C22 C23 1.9(19) . . . . ?
C21 C22 C23 C24 -2.7(20) . . . . ?
C22 C23 C24 C25 0.7(19) . . . . ?
C21 C20 C25 C24 -2.6(17) . . . . ?
S4 C20 C25 C24 178.5(9) . . . . ?
C21 C20 C25 S3 176.0(9) . . . . ?
S4 C20 C25 S3 -3.0(14) . . . . ?
C23 C24 C25 C20 1.9(18) . . . . ?
C23 C24 C25 S3 -176.8(10) . . . . ?
Os1 S3 C25 C20 13.2(11) . . . . ?
Os1 S3 C25 C24 -168.3(9) . . . . ?
