#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/35/4323581.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_4323581
loop_
_publ_author_name
'Wen-Yann Yeh'
'Charlotte L. Stern'
'Duward F. Shriver'
_publ_contact_author
;
D.F. Shriver
Department of Chemistry
Northwestern University
Evanston, IL 60208-3113, USA
;
_publ_contact_author_email       ' Shriver@chem.nwu.edu '
_publ_contact_author_fax         ' 847-491-7713 '
_publ_contact_author_phone       ' 847-491-5655'
_publ_section_title
;
 Reactions of Triosmium Carbonyl Clusters with Thionylaniline. Crystal
 Structures of Os₃(CO)₉(μ₃-NPh)(μ₃-S),
 Os₃(CO)₉(μ₃,η²-(PhN)₂SO)(μ₃-S), and
 Os₃(CO)₈(NCMe)(μ₃-NPh)(μ₃-S).
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4408
_journal_page_last               4414
_journal_paper_doi               10.1021/ic961153j
_journal_volume                  36
_journal_year                    1997
_chemical_formula_moiety         'C15 H5 N O9 Os3 S '
_chemical_formula_sum            'C15 H5 N O9 Os3 S'
_chemical_formula_weight         945.87
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_audit_creation_date             'Wed Jul 16 10:10:50 1997'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 102.08(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.603(7)
_cell_length_b                   8.679(4)
_cell_length_c                   29.009(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    153.2
_cell_measurement_theta_max      23.2
_cell_measurement_theta_min      20.2
_cell_volume                     4088(3)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_computing_structure_solution    SHELXS86
_diffrn_ambient_temperature      153.2
_diffrn_measurement_device       CAD4
_diffrn_measurement_method       'omega/theta scans'
_diffrn_orient_matrix_UB_11      0.02020
_diffrn_orient_matrix_UB_12      -0.06610
_diffrn_orient_matrix_UB_13      -0.02350
_diffrn_orient_matrix_UB_21      -0.02610
_diffrn_orient_matrix_UB_22      -0.09210
_diffrn_orient_matrix_UB_23      0.01150
_diffrn_orient_matrix_UB_31      -0.05200
_diffrn_orient_matrix_UB_32      0.02070
_diffrn_orient_matrix_UB_33      -0.02360
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           MoKalpha
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  8.01
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            4004
_diffrn_reflns_theta_max         24.97
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 90
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    18.742
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.505
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   Walker&Stuart_DIFABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    3.074
_exptl_crystal_description       platy
_exptl_crystal_F_000             3344.00
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.150
_refine_diff_density_max         2.29
_refine_diff_density_min         -1.72
_refine_ls_extinction_coef       0.37327
_refine_ls_extinction_method     Zachariasen_type_2_Gaussian_isotropic
_refine_ls_goodness_of_fit_obs   2.047
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         2749
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0356
_refine_ls_shift/esd_max         0.0550
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_obs         0.0390
_reflns_number_observed          2749
_reflns_number_total             3873
_reflns_observed_criterion       3.00
_cod_data_source_file            ic961153j_1.cif
_cod_data_source_block           compound1
_cod_original_cell_volume        4087(2)
_cod_original_sg_symbol_H-M      'C 2/c '
_cod_original_formula_sum        'C15 H5 N O9 Os3 S '
_cod_database_code               4323581
loop_
_symmetry_equiv_pos_as_xyz
'   +x,   +y,   +z'
'1/2+x,1/2+y,   +z'
'   -x,   +y,1/2-z'
1/2-x,1/2+y,1/2-z
'   -x,   -y,   -z'
'1/2-x,1/2-y,   -z'
'   +x,   -y,1/2+z'
1/2+x,1/2-y,1/2+z
loop_
_atom_site_label
_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_calc_flag
_atom_site_calc_attached_atom
Os(1) -0.01998(3) 0.40345(7) 0.60432(2) 0.0160(2) Uij ? ?
Os(2) 0.13863(4) 0.44716(6) 0.59232(2) 0.0167(2) Uij ? ?
Os(3) 0.11692(4) 0.13642(6) 0.57485(2) 0.0163(2) Uij ? ?
S 0.0273(2) 0.3305(4) 0.5358(1) 0.0166(10) Uij ? ?
O(1) -0.1429(7) 0.637(1) 0.5523(4) 0.034(3) Uij ? ?
O(2) -0.0333(9) 0.548(2) 0.6982(5) 0.064(5) Uij ? ?
O(3) -0.1570(8) 0.176(1) 0.6049(4) 0.046(4) Uij ? ?
O(4) 0.1342(8) 0.718(1) 0.6586(4) 0.045(4) Uij ? ?
O(5) 0.1780(7) 0.669(1) 0.5189(4) 0.040(4) Uij ? ?
O(6) 0.3180(6) 0.352(1) 0.6314(5) 0.040(4) Uij ? ?
O(7) 0.1769(8) 0.038(1) 0.4862(4) 0.041(4) Uij ? ?
O(8) 0.2644(7) -0.021(1) 0.6377(4) 0.041(4) Uij ? ?
O(9) -0.0005(7) -0.135(1) 0.5719(4) 0.038(4) Uij ? ?
N 0.0841(7) 0.272(1) 0.6277(4) 0.019(3) Uij ? ?
C(1) -0.0948(9) 0.550(2) 0.5726(5) 0.023(4) Uij ? ?
C(2) -0.0266(10) 0.494(2) 0.6636(7) 0.036(5) Uij ? ?
C(3) -0.1041(9) 0.265(2) 0.6059(5) 0.022(4) Uij ? ?
C(4) 0.135(1) 0.618(2) 0.6351(5) 0.031(5) Uij ? ?
C(5) 0.163(1) 0.586(2) 0.5459(6) 0.031(5) Uij ? ?
C(6) 0.2510(10) 0.386(2) 0.6156(6) 0.030(5) Uij ? ?
C(7) 0.153(1) 0.074(2) 0.5188(6) 0.028(5) Uij ? ?
C(8) 0.2074(9) 0.039(2) 0.6143(5) 0.023(4) Uij ? ?
C(9) 0.0447(10) -0.035(2) 0.5734(5) 0.026(5) Uij ? ?
C(10) 0.1098(9) 0.225(2) 0.6768(6) 0.024(4) Uij ? ?
C(11) 0.163(1) 0.313(2) 0.7104(6) 0.044(6) Uij ? ?
C(12) 0.184(1) 0.263(3) 0.7577(7) 0.058(7) Uij ? ?
C(13) 0.155(1) 0.133(3) 0.7712(7) 0.057(7) Uij ? ?
C(14) 0.104(1) 0.042(3) 0.7384(7) 0.060(7) Uij ? ?
C(15) 0.081(1) 0.089(2) 0.6919(6) 0.047(6) Uij ? ?
H(1) 0.1856 0.4060 0.7015 0.0530 Uij ? ?
H(2) 0.2195 0.3243 0.7802 0.0692 Uij ? ?
H(3) 0.1699 0.1019 0.8033 0.0678 Uij ? ?
H(4) 0.0845 -0.0540 0.7477 0.0731 Uij ? ?
H(5) 0.0441 0.0274 0.6700 0.0563 Uij ? ?
loop_
_atom_type_symbol
_atom_type_oxidation_number
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
S 0 8 0.125 0.123 'International Tables'
N 0 8 0.006 0.003 'International Tables'
H 0 40 0.000 0.000 'International Tables'
C 0 120 0.003 0.002 'International Tables'
Os 0 24 -1.216 7.603 'International Tables'
O 0 72 0.011 0.006 'International Tables'
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
-3 -3 -8
5 -3 4
7 -1 5
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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Os(2) Os(1) S 55.78(9) ? ? ? yes
Os(2) Os(1) N 50.2(3) ? ? ? yes
Os(2) Os(1) C(1) 113.4(5) ? ? ? yes
Os(2) Os(1) C(2) 107.1(5) ? ? ? yes
Os(2) Os(1) C(3) 147.0(4) ? ? ? yes
S Os(1) N 74.2(4) ? ? ? yes
S Os(1) C(1) 94.1(5) ? ? ? yes
S Os(1) C(2) 162.6(5) ? ? ? yes
S Os(1) C(3) 103.3(5) ? ? ? yes
N Os(1) C(1) 163.3(6) ? ? ? yes
N Os(1) C(2) 97.6(6) ? ? ? yes
N Os(1) C(3) 102.5(5) ? ? ? yes
C(1) Os(1) C(2) 90.4(7) ? ? ? yes
C(1) Os(1) C(3) 91.6(6) ? ? ? yes
C(2) Os(1) C(3) 93.4(7) ? ? ? yes
Os(1) Os(2) Os(3) 78.26(2) ? ? ? yes
Os(1) Os(2) S 54.10(9) ? ? ? yes
Os(1) Os(2) N 47.8(3) ? ? ? yes
Os(1) Os(2) C(4) 82.3(5) ? ? ? yes
Os(1) Os(2) C(5) 121.6(5) ? ? ? yes
Os(1) Os(2) C(6) 143.3(5) ? ? ? yes
Os(3) Os(2) S 54.12(8) ? ? ? yes
Os(3) Os(2) N 48.8(3) ? ? ? yes
Os(3) Os(2) C(4) 147.6(4) ? ? ? yes
Os(3) Os(2) C(5) 121.8(5) ? ? ? yes
Os(3) Os(2) C(6) 82.9(4) ? ? ? yes
S Os(2) N 71.9(3) ? ? ? yes
S Os(2) C(4) 129.1(5) ? ? ? yes
S Os(2) C(5) 91.8(5) ? ? ? yes
S Os(2) C(6) 132.1(5) ? ? ? yes
N Os(2) C(4) 99.3(6) ? ? ? yes
N Os(2) C(5) 163.6(6) ? ? ? yes
N Os(2) C(6) 96.6(6) ? ? ? yes
C(4) Os(2) C(5) 90.4(7) ? ? ? yes
C(4) Os(2) C(6) 98.3(7) ? ? ? yes
C(5) Os(2) C(6) 95.1(7) ? ? ? yes
Os(2) Os(3) S 55.77(9) ? ? ? yes
Os(2) Os(3) N 50.0(3) ? ? ? yes
Os(2) Os(3) C(7) 112.4(5) ? ? ? yes
Os(2) Os(3) C(8) 105.7(4) ? ? ? yes
Os(2) Os(3) C(9) 145.7(5) ? ? ? yes
S Os(3) N 73.5(3) ? ? ? yes
S Os(3) C(7) 94.0(4) ? ? ? yes
S Os(3) C(8) 161.4(4) ? ? ? yes
S Os(3) C(9) 102.4(4) ? ? ? yes
N Os(3) C(7) 162.1(5) ? ? ? yes
N Os(3) C(8) 96.0(6) ? ? ? yes
N Os(3) C(9) 101.3(6) ? ? ? yes
C(7) Os(3) C(8) 92.2(6) ? ? ? yes
C(7) Os(3) C(9) 93.8(7) ? ? ? yes
C(8) Os(3) C(9) 94.7(6) ? ? ? yes
Os(1) S Os(2) 70.1(1) ? ? ? yes
Os(1) S Os(3) 94.2(1) ? ? ? yes
Os(2) S Os(3) 70.1(1) ? ? ? yes
Os(1) N Os(2) 82.0(4) ? ? ? yes
Os(1) N Os(3) 113.5(6) ? ? ? yes
Os(1) N C(10) 122.1(9) ? ? ? yes
Os(2) N Os(3) 81.2(4) ? ? ? yes
Os(2) N C(10) 127.0(9) ? ? ? yes
Os(3) N C(10) 119.3(9) ? ? ? yes
Os(1) C(1) O(1) 177(1) ? ? ? yes
Os(1) C(2) O(2) 177(1) ? ? ? yes
Os(1) C(3) O(3) 177(1) ? ? ? yes
Os(2) C(4) O(4) 177(1) ? ? ? yes
Os(2) C(5) O(5) 179(1) ? ? ? yes
Os(2) C(6) O(6) 177(1) ? ? ? yes
Os(3) C(7) O(7) 177(1) ? ? ? yes
Os(3) C(8) O(8) 178(1) ? ? ? yes
Os(3) C(9) O(9) 178(1) ? ? ? yes
N C(10) C(11) 122(1) ? ? ? yes
N C(10) C(15) 119(1) ? ? ? yes
C(11) C(10) C(15) 117(1) ? ? ? yes
C(10) C(11) C(12) 120(1) ? ? ? yes
C(11) C(12) C(13) 121(2) ? ? ? yes
C(12) C(13) C(14) 119(1) ? ? ? yes
C(13) C(14) C(15) 120(1) ? ? ? yes
C(10) C(15) C(14) 121(1) ? ? ? yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Os(1) Os(2) 2.754(1) ? ? yes
Os(1) S 2.372(4) ? ? yes
Os(1) N 2.06(1) ? ? yes
Os(1) C(1) 1.88(2) ? ? yes
Os(1) C(2) 1.91(2) ? ? yes
Os(1) C(3) 1.85(2) ? ? yes
Os(2) Os(3) 2.7538(8) ? ? yes
Os(2) S 2.421(4) ? ? yes
Os(2) N 2.14(1) ? ? yes
Os(2) C(4) 1.94(2) ? ? yes
Os(2) C(5) 1.92(2) ? ? yes
Os(2) C(6) 1.92(2) ? ? yes
Os(3) S 2.373(4) ? ? yes
Os(3) N 2.10(1) ? ? yes
Os(3) C(7) 1.92(2) ? ? yes
Os(3) C(8) 1.89(2) ? ? yes
Os(3) C(9) 1.90(2) ? ? yes
O(1) C(1) 1.17(2) ? ? yes
O(2) C(2) 1.14(2) ? ? yes
O(3) C(3) 1.16(2) ? ? yes
O(4) C(4) 1.11(2) ? ? yes
O(5) C(5) 1.13(2) ? ? yes
O(6) C(6) 1.15(2) ? ? yes
O(7) C(7) 1.14(2) ? ? yes
O(8) C(8) 1.16(2) ? ? yes
O(9) C(9) 1.14(2) ? ? yes
N C(10) 1.46(2) ? ? yes
C(10) C(11) 1.40(2) ? ? yes
C(10) C(15) 1.38(2) ? ? yes
C(11) C(12) 1.41(2) ? ? yes
C(12) C(13) 1.31(3) ? ? yes
C(13) C(14) 1.39(3) ? ? yes
C(14) C(15) 1.39(2) ? ? yes
