#------------------------------------------------------------------------------
#$Date: 2018-09-25 10:31:19 +0300 (Tue, 25 Sep 2018) $
#$Revision: 211151 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/33/91/4339163.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_4339163
loop_
_publ_author_name
'Lai, Siu-Wai'
'Chan, Queenie K.-W.'
'Zhu, Nianyong'
'Che, Chi-Ming'
_publ_section_title
;
 cis-Dicyanoosmium(II) diimine complexes bearing phosphine or sulfoxide
 ligands: spectroscopic and luminescent studies.
;
_journal_issue                   26
_journal_name_full               'Inorganic chemistry'
_journal_page_first              11003
_journal_page_last               11016
_journal_paper_doi               10.1021/ic070290l
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         'C28.50 H29 Cl N4 O2 Os S2'
_chemical_formula_sum            'C28.5 H29 Cl N4 O2 Os S2'
_chemical_formula_weight         749.33
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 117.73(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   25.414(5)
_cell_length_b                   10.516(2)
_cell_length_c                   24.557(5)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    301(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     5809(3)
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      301(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_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  0.0472
_diffrn_reflns_av_sigmaI/netI    0.0633
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            20966
_diffrn_reflns_theta_full        25.65
_diffrn_reflns_theta_max         25.65
_diffrn_reflns_theta_min         2.50
_exptl_absorpt_coefficient_mu    4.659
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.714
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2952
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.769
_refine_diff_density_min         -2.835
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.959
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         5294
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.960
_refine_ls_R_factor_all          0.0490
_refine_ls_R_factor_gt           0.0379
_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)+(0.0565P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0953
_refine_ls_wR_factor_ref         0.0981
_reflns_number_gt                4036
_reflns_number_total             5294
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic070290l-file001.cif
_cod_data_source_block           mar1804_Cpd3d
_cod_depositor_comments
;
 Marking attached hydrogen atoms.

 Antanas Vaitkus,
 2018-09-25
;
_cod_original_cell_volume        5809(2)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C28.50 H29 Cl N4 O2 Os S2'
_cod_database_code               4339163
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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_attached_hydrogens
Os1 Os 0.141113(10) 0.79507(2) 0.100661(9) 0.03558(10) Uani 1 1 d . 0
S1 S 0.22029(7) 0.93239(16) 0.13892(7) 0.0464(4) Uani 1 1 d . 0
S2 S 0.06344(7) 0.65280(15) 0.05667(7) 0.0438(4) Uani 1 1 d . 0
O1 O 0.0676(2) 0.5645(5) 0.0127(2) 0.0761(16) Uani 1 1 d . 0
O2 O 0.2503(2) 0.9494(5) 0.1005(2) 0.0613(13) Uani 1 1 d . 0
N1 N 0.0513(3) 1.0175(6) 0.0858(3) 0.0647(17) Uani 1 1 d . 0
N2 N 0.1656(3) 0.7364(7) 0.2369(3) 0.0718(19) Uani 1 1 d . 0
N3 N 0.1980(2) 0.6515(4) 0.0969(2) 0.0352(11) Uani 1 1 d . 0
N4 N 0.1312(2) 0.8127(4) 0.0106(2) 0.0349(11) Uani 1 1 d . 0
C1 C 0.0844(3) 0.9373(6) 0.0930(3) 0.0456(15) Uani 1 1 d . 0
C2 C 0.1547(3) 0.7582(6) 0.1867(3) 0.0457(15) Uani 1 1 d . 0
C3 C 0.2769(3) 0.8883(9) 0.2129(3) 0.081(3) Uani 1 1 d . 0
H3A H 0.2922 0.8062 0.2106 0.121 Uiso 1 1 calc R 0
H3B H 0.2606 0.8852 0.2412 0.121 Uiso 1 1 calc R 0
H3C H 0.3084 0.9498 0.2268 0.121 Uiso 1 1 calc R 0
C4 C 0.2029(4) 1.0844(7) 0.1571(4) 0.086(3) Uani 1 1 d . 0
H4A H 0.2389 1.1289 0.1830 0.130 Uiso 1 1 calc R 0
H4B H 0.1794 1.0750 0.1782 0.130 Uiso 1 1 calc R 0
H4C H 0.1807 1.1318 0.1198 0.130 Uiso 1 1 calc R 0
C5 C -0.0069(3) 0.7264(8) 0.0163(5) 0.088(3) Uani 1 1 d . 0
H5A H -0.0075 0.7779 -0.0163 0.132 Uiso 1 1 calc R 0
H5B H -0.0143 0.7790 0.0440 0.132 Uiso 1 1 calc R 0
H5C H -0.0372 0.6624 -0.0008 0.132 Uiso 1 1 calc R 0
C6 C 0.0533(4) 0.5603(9) 0.1103(4) 0.102(4) Uani 1 1 d . 0
H6A H 0.0201 0.5041 0.0891 0.154 Uiso 1 1 calc R 0
H6B H 0.0456 0.6148 0.1372 0.154 Uiso 1 1 calc R 0
H6C H 0.0885 0.5112 0.1341 0.154 Uiso 1 1 calc R 0
C7 C 0.2299(3) 0.5694(6) 0.1422(3) 0.0493(17) Uani 1 1 d . 0
H7 H 0.2287 0.5772 0.1793 0.059 Uiso 1 1 calc R 0
C8 C 0.2639(3) 0.4749(6) 0.1364(3) 0.0510(17) Uani 1 1 d . 0
H8 H 0.2850 0.4202 0.1692 0.061 Uiso 1 1 calc R 0
C9 C 0.2670(3) 0.4603(5) 0.0816(2) 0.0385(14) Uani 1 1 d . 0
C10 C 0.2337(3) 0.5473(5) 0.0350(3) 0.0411(14) Uani 1 1 d . 0
H10 H 0.2351 0.5434 -0.0021 0.049 Uiso 1 1 calc R 0
C11 C 0.1999(3) 0.6365(5) 0.0427(2) 0.0357(13) Uani 1 1 d . 0
C12 C 0.1608(3) 0.7276(5) -0.0065(2) 0.0346(13) Uani 1 1 d . 0
C13 C 0.1518(3) 0.7203(5) -0.0662(2) 0.0377(14) Uani 1 1 d . 0
H13 H 0.1725 0.6608 -0.0768 0.045 Uiso 1 1 calc R 0
C14 C 0.1110(3) 0.8032(5) -0.1115(2) 0.0402(14) Uani 1 1 d . 0
C15 C 0.0826(3) 0.8901(6) -0.0923(3) 0.0468(15) Uani 1 1 d . 0
H15 H 0.0558 0.9470 -0.1207 0.056 Uiso 1 1 calc R 0
C16 C 0.0930(3) 0.8947(5) -0.0324(2) 0.0395(14) Uani 1 1 d . 0
H16 H 0.0734 0.9552 -0.0208 0.047 Uiso 1 1 calc R 0
C17 C 0.3034(3) 0.3580(6) 0.0738(3) 0.0419(14) Uani 1 1 d . 0
C18 C 0.3263(4) 0.2588(7) 0.1156(4) 0.068(2) Uani 1 1 d . 0
H18 H 0.3201 0.2579 0.1500 0.082 Uiso 1 1 calc R 0
C19 C 0.3576(4) 0.1625(8) 0.1071(4) 0.079(3) Uani 1 1 d . 0
H19 H 0.3715 0.0960 0.1353 0.094 Uiso 1 1 calc R 0
C20 C 0.3691(3) 0.1617(7) 0.0583(4) 0.067(2) Uani 1 1 d . 0
H20 H 0.3915 0.0966 0.0536 0.081 Uiso 1 1 calc R 0
C21 C 0.3472(4) 0.2582(7) 0.0161(4) 0.064(2) Uani 1 1 d . 0
H21 H 0.3539 0.2580 -0.0181 0.077 Uiso 1 1 calc R 0
C22 C 0.3152(3) 0.3558(7) 0.0242(3) 0.0587(19) Uani 1 1 d . 0
H22 H 0.3013 0.4217 -0.0043 0.070 Uiso 1 1 calc R 0
C23 C 0.0977(3) 0.7935(6) -0.1765(3) 0.0484(17) Uani 1 1 d . 0
C24 C 0.0869(4) 0.6789(8) -0.2056(3) 0.069(2) Uani 1 1 d . 0
H24 H 0.0902 0.6047 -0.1836 0.082 Uiso 1 1 calc R 0
C25 C 0.0707(4) 0.6715(9) -0.2683(4) 0.086(3) Uani 1 1 d . 0
H25 H 0.0609 0.5935 -0.2884 0.103 Uiso 1 1 calc R 0
C26 C 0.0695(4) 0.7801(10) -0.2999(3) 0.083(3) Uani 1 1 d . 0
H26 H 0.0602 0.7752 -0.3412 0.100 Uiso 1 1 calc R 0
C27 C 0.0816(4) 0.8939(10) -0.2713(3) 0.081(3) Uani 1 1 d . 0
H27 H 0.0810 0.9670 -0.2929 0.097 Uiso 1 1 calc R 0
C28 C 0.0949(3) 0.9025(7) -0.2096(3) 0.064(2) Uani 1 1 d . 0
H28 H 0.1020 0.9816 -0.1905 0.077 Uiso 1 1 calc R 0
C29 C 0.0333(13) 0.2650(19) -0.2469(13) 0.149(10) Uiso 0.50 1 d PD 2
Cl1 Cl 0.0020(4) 0.1803(8) -0.3020(5) 0.235(4) Uiso 0.67 1 d PD 0
Cl2 Cl 0.0000 0.3931(9) -0.2500 0.184(4) Uiso 0.67 2 d SPD 0
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Os Os -1.2165 7.6030 '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'
O O 0.0106 0.0060 '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'
C C 0.0033 0.0016 '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'
H H 0.0000 0.0000 '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
C2 Os1 C1 90.4(3) . .
C2 Os1 N4 173.3(2) . .
C1 Os1 N4 96.1(2) . .
C2 Os1 N3 97.0(2) . .
C1 Os1 N3 172.7(2) . .
N4 Os1 N3 76.60(17) . .
C2 Os1 S1 90.11(19) . .
C1 Os1 S1 91.39(19) . .
N4 Os1 S1 91.59(13) . .
N3 Os1 S1 88.86(14) . .
C2 Os1 S2 93.33(19) . .
C1 Os1 S2 91.05(18) . .
N4 Os1 S2 84.71(13) . .
N3 Os1 S2 88.28(14) . .
S1 Os1 S2 175.77(6) . .
O2 S1 C4 108.4(4) . .
O2 S1 C3 105.8(3) . .
C4 S1 C3 99.0(4) . .
O2 S1 Os1 115.53(19) . .
C4 S1 Os1 113.4(3) . .
C3 S1 Os1 113.2(3) . .
O1 S2 C6 106.8(4) . .
O1 S2 C5 105.4(4) . .
C6 S2 C5 101.6(5) . .
O1 S2 Os1 114.6(2) . .
C6 S2 Os1 113.7(3) . .
C5 S2 Os1 113.6(3) . .
C7 N3 C11 117.0(5) . .
C7 N3 Os1 125.6(4) . .
C11 N3 Os1 117.3(4) . .
C12 N4 C16 118.6(5) . .
C12 N4 Os1 116.9(3) . .
C16 N4 Os1 124.1(4) . .
N1 C1 Os1 176.8(5) . .
N2 C2 Os1 176.4(6) . .
S1 C3 H3A 109.5 . .
S1 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
S1 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
S1 C4 H4A 109.5 . .
S1 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
S1 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
S2 C5 H5A 109.5 . .
S2 C5 H5B 109.5 . .
H5A C5 H5B 109.5 . .
S2 C5 H5C 109.5 . .
H5A C5 H5C 109.5 . .
H5B C5 H5C 109.5 . .
S2 C6 H6A 109.5 . .
S2 C6 H6B 109.5 . .
H6A C6 H6B 109.5 . .
S2 C6 H6C 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
N3 C7 C8 123.3(6) . .
N3 C7 H7 118.4 . .
C8 C7 H7 118.4 . .
C7 C8 C9 120.2(5) . .
C7 C8 H8 119.9 . .
C9 C8 H8 119.9 . .
C8 C9 C10 115.7(5) . .
C8 C9 C17 121.4(5) . .
C10 C9 C17 122.9(5) . .
C11 C10 C9 121.6(6) . .
C11 C10 H10 119.2 . .
C9 C10 H10 119.2 . .
C10 C11 N3 122.2(5) . .
C10 C11 C12 124.1(5) . .
N3 C11 C12 113.7(5) . .
N4 C12 C13 121.7(5) . .
N4 C12 C11 115.3(5) . .
C13 C12 C11 122.8(5) . .
C12 C13 C14 120.1(5) . .
C12 C13 H13 120.0 . .
C14 C13 H13 120.0 . .
C15 C14 C13 116.7(5) . .
C15 C14 C23 121.6(5) . .
C13 C14 C23 121.6(5) . .
C16 C15 C14 121.4(5) . .
C16 C15 H15 119.3 . .
C14 C15 H15 119.3 . .
N4 C16 C15 121.4(5) . .
N4 C16 H16 119.3 . .
C15 C16 H16 119.3 . .
C22 C17 C18 116.7(6) . .
C22 C17 C9 121.8(5) . .
C18 C17 C9 121.5(6) . .
C19 C18 C17 121.4(8) . .
C19 C18 H18 119.3 . .
C17 C18 H18 119.3 . .
C20 C19 C18 121.3(7) . .
C20 C19 H19 119.4 . .
C18 C19 H19 119.4 . .
C19 C20 C21 118.9(7) . .
C19 C20 H20 120.5 . .
C21 C20 H20 120.5 . .
C20 C21 C22 120.0(8) . .
C20 C21 H21 120.0 . .
C22 C21 H21 120.0 . .
C21 C22 C17 121.6(7) . .
C21 C22 H22 119.2 . .
C17 C22 H22 119.2 . .
C24 C23 C28 118.7(7) . .
C24 C23 C14 121.3(6) . .
C28 C23 C14 120.0(6) . .
C23 C24 C25 120.8(8) . .
C23 C24 H24 119.6 . .
C25 C24 H24 119.6 . .
C26 C25 C24 119.6(8) . .
C26 C25 H25 120.2 . .
C24 C25 H25 120.2 . .
C27 C26 C25 120.3(8) . .
C27 C26 H26 119.8 . .
C25 C26 H26 119.8 . .
C26 C27 C28 120.3(8) . .
C26 C27 H27 119.8 . .
C28 C27 H27 119.8 . .
C23 C28 C27 120.2(7) . .
C23 C28 H28 119.9 . .
C27 C28 H28 119.9 . .
Cl1 C29 Cl2 114.6(19) . .
Cl1 C29 C29 79.8(19) . 2_554
Cl2 C29 C29 58.9(10) . 2_554
Cl1 C29 Cl1 94.6(16) . 2_554
Cl2 C29 Cl1 91.7(12) . 2_554
C29 C29 Cl1 47.4(11) 2_554 2_554
C29 Cl1 C29 52.8(17) . 2_554
C29 Cl2 C29 62(2) 2_554 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Os1 C2 2.014(7) .
Os1 C1 2.025(7) .
Os1 N4 2.116(5) .
Os1 N3 2.123(5) .
Os1 S1 2.2930(17) .
Os1 S2 2.3059(17) .
S1 O2 1.475(5) .
S1 C4 1.771(7) .
S1 C3 1.775(7) .
S2 O1 1.465(5) .
S2 C6 1.751(8) .
S2 C5 1.769(8) .
N1 C1 1.145(8) .
N2 C2 1.152(8) .
N3 C7 1.341(7) .
N3 C11 1.362(7) .
N4 C12 1.354(7) .
N4 C16 1.359(7) .
C3 H3A 0.9600 .
C3 H3B 0.9600 .
C3 H3C 0.9600 .
C4 H4A 0.9600 .
C4 H4B 0.9600 .
C4 H4C 0.9600 .
C5 H5A 0.9600 .
C5 H5B 0.9600 .
C5 H5C 0.9600 .
C6 H6A 0.9600 .
C6 H6B 0.9600 .
C6 H6C 0.9600 .
C7 C8 1.367(8) .
C7 H7 0.9300 .
C8 C9 1.394(8) .
C8 H8 0.9300 .
C9 C10 1.399(8) .
C9 C17 1.488(8) .
C10 C11 1.344(8) .
C10 H10 0.9300 .
C11 C12 1.500(7) .
C12 C13 1.377(8) .
C13 C14 1.413(7) .
C13 H13 0.9300 .
C14 C15 1.377(8) .
C14 C23 1.473(8) .
C15 C16 1.370(8) .
C15 H15 0.9300 .
C16 H16 0.9300 .
C17 C22 1.384(9) .
C17 C18 1.386(9) .
C18 C19 1.363(11) .
C18 H18 0.9300 .
C19 C20 1.360(11) .
C19 H19 0.9300 .
C20 C21 1.371(11) .
C20 H20 0.9300 .
C21 C22 1.381(10) .
C21 H21 0.9300 .
C22 H22 0.9300 .
C23 C24 1.363(9) .
C23 C28 1.388(9) .
C24 C25 1.398(10) .
C24 H24 0.9300 .
C25 C26 1.373(12) .
C25 H25 0.9300 .
C26 C27 1.348(12) .
C26 H26 0.9300 .
C27 C28 1.393(10) .
C27 H27 0.9300 .
C28 H28 0.9300 .
C29 Cl1 1.502(19) .
C29 Cl2 1.574(18) .
C29 C29 1.63(5) 2_554
C29 Cl1 2.01(3) 2_554
Cl1 C29 2.01(3) 2_554
Cl2 C29 1.574(18) 2_554
