#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:52:01 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179132 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/94/4309490.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_4309490
loop_
_publ_author_name
'Te-Wei Chiu'
'Yen-Hsiang Liu'
'Kai-Ming Chi'
'Yuh-Sheng Wen'
'Kuang-Lieh Lu'
_publ_section_title
;
Synthesis, Structure, and Transformation of Novel Osmium Azine and Ylide
Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6425
_journal_page_last               6430
_journal_paper_doi               10.1021/ic050431o
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C29 H17 N2 O10 Os3 P'
_chemical_formula_weight         1155.02
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 121.83(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   32.606(18)
_cell_length_b                   13.1568(18)
_cell_length_c                   17.719(9)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      16.687
_cell_measurement_theta_min      7.332
_cell_volume                     6458(5)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_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, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method       'non-profiled omega/2theta 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    0.0498
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            5686
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.47
_diffrn_standards_decay_%        4
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    11.882
_exptl_absorpt_correction_T_max  0.9977
_exptl_absorpt_correction_T_min  0.3674
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.376
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4224
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.810
_refine_diff_density_min         -1.309
_refine_diff_density_rms         0.177
_refine_ls_extinction_coef       0.000078(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     411
_refine_ls_number_reflns         5686
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0735
_refine_ls_R_factor_gt           0.0361
_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)+(0.0450P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0764
_refine_ls_wR_factor_ref         0.0861
_reflns_number_gt                4150
_reflns_number_total             5686
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050431osi20050607_023949.cif
_cod_data_source_block           i1096
_cod_database_code               4309490
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_disorder_assembly
_atom_site_disorder_group
Os1 Os 0.050695(12) 0.18023(3) 0.66524(3) 0.03350(12) Uani 1 1 d . . .
Os2 Os 0.067058(13) 0.29973(3) 0.54816(2) 0.03474(12) Uani 1 1 d . . .
Os3 Os 0.148308(12) 0.22307(3) 0.71548(2) 0.02945(11) Uani 1 1 d . . .
P1 P 0.18034(8) 0.55211(17) 0.77598(16) 0.0287(5) Uani 1 1 d . . .
O1 O -0.0593(3) 0.1914(7) 0.5567(7) 0.087(3) Uani 1 1 d . . .
O2 O 0.0679(4) 0.0408(6) 0.8166(6) 0.084(3) Uani 1 1 d . . .
O3 O 0.0593(3) 0.3716(6) 0.7734(7) 0.080(3) Uani 1 1 d . . .
O4 O 0.0533(3) -0.0048(6) 0.5626(6) 0.065(2) Uani 1 1 d . . .
O5 O 0.0894(4) 0.4454(8) 0.4406(7) 0.118(4) Uani 1 1 d . . .
O6 O -0.0329(3) 0.3891(6) 0.4758(6) 0.078(3) Uani 1 1 d . . .
O7 O 0.0357(3) 0.1275(7) 0.4098(5) 0.081(3) Uani 1 1 d . . .
O8 O 0.2506(2) 0.2766(5) 0.7655(6) 0.062(2) Uani 1 1 d . . .
O9 O 0.1787(4) 0.1935(7) 0.9079(6) 0.082(3) Uani 1 1 d . . .
O10 O 0.1608(3) -0.0009(5) 0.6883(6) 0.070(3) Uani 1 1 d . . .
N1 N 0.1367(2) 0.3793(5) 0.7195(5) 0.0255(16) Uani 1 1 d . . .
N2 N 0.1699(2) 0.4388(5) 0.7936(5) 0.0305(17) Uani 1 1 d . . .
C1 C -0.0184(4) 0.1873(8) 0.5967(8) 0.053(3) Uani 1 1 d . . .
C2 C 0.0620(4) 0.0944(8) 0.7615(8) 0.050(3) Uani 1 1 d . . .
C3 C 0.0566(3) 0.3038(8) 0.7304(8) 0.046(3) Uani 1 1 d . . .
C4 C 0.0529(3) 0.0645(8) 0.6009(7) 0.043(3) Uani 1 1 d . . .
C5 C 0.0825(5) 0.3873(9) 0.4835(8) 0.065(4) Uani 1 1 d . . .
C6 C 0.0052(4) 0.3550(8) 0.5014(7) 0.050(3) Uani 1 1 d . . .
C7 C 0.0463(4) 0.1905(9) 0.4611(7) 0.048(3) Uani 1 1 d . . .
C8 C 0.2124(3) 0.2566(7) 0.7438(7) 0.042(2) Uani 1 1 d . . .
C9 C 0.1677(4) 0.2050(7) 0.8364(7) 0.040(2) Uani 1 1 d . . .
C10 C 0.1559(3) 0.0832(8) 0.6991(7) 0.045(3) Uani 1 1 d . . .
C11 C 0.0995(3) 0.4105(6) 0.6481(5) 0.0290(19) Uani 1 1 d . . .
H11 H 0.0877 0.4764 0.6409 0.035 Uiso 1 1 calc R . .
C21 C 0.1855(3) 0.5652(6) 0.6791(6) 0.030(2) Uani 1 1 d . . .
C22 C 0.2226(3) 0.5121(7) 0.6794(7) 0.042(2) Uani 1 1 d . . .
H22 H 0.2437 0.4725 0.7282 0.050 Uiso 1 1 calc R . .
C23 C 0.2282(4) 0.5182(9) 0.6068(8) 0.058(3) Uani 1 1 d . . .
H23 H 0.2532 0.4835 0.6072 0.069 Uiso 1 1 calc R . .
C24 C 0.1967(4) 0.5754(10) 0.5349(8) 0.065(3) Uani 1 1 d . . .
H24 H 0.2003 0.5789 0.4862 0.078 Uiso 1 1 calc R . .
C25 C 0.1598(4) 0.6281(10) 0.5334(7) 0.061(3) Uani 1 1 d . . .
H25 H 0.1390 0.6676 0.4843 0.074 Uiso 1 1 calc R . .
C26 C 0.1532(3) 0.6227(9) 0.6045(7) 0.049(3) Uani 1 1 d . . .
H26 H 0.1278 0.6570 0.6027 0.059 Uiso 1 1 calc R . .
C31 C 0.1378(3) 0.6486(7) 0.7649(6) 0.030(2) Uani 1 1 d . . .
C32 C 0.1383(4) 0.7498(7) 0.7429(8) 0.053(3) Uani 1 1 d . . .
H32 H 0.1615 0.7725 0.7313 0.064 Uiso 1 1 calc R . .
C33 C 0.1049(4) 0.8158(8) 0.7384(8) 0.063(3) Uani 1 1 d . . .
H33 H 0.1058 0.8836 0.7247 0.076 Uiso 1 1 calc R . .
C34 C 0.0702(4) 0.7844(9) 0.7536(7) 0.060(3) Uani 1 1 d . . .
H34 H 0.0470 0.8301 0.7477 0.072 Uiso 1 1 calc R . .
C35 C 0.0693(4) 0.6865(9) 0.7772(7) 0.054(3) Uani 1 1 d . . .
H35 H 0.0461 0.6659 0.7896 0.065 Uiso 1 1 calc R . .
C36 C 0.1030(3) 0.6174(8) 0.7830(6) 0.043(2) Uani 1 1 d . . .
H36 H 0.1024 0.5504 0.7989 0.052 Uiso 1 1 calc R . .
C41 C 0.2381(3) 0.5807(7) 0.8735(6) 0.035(2) Uani 1 1 d . . .
C42 C 0.2522(4) 0.6784(8) 0.9073(8) 0.054(3) Uani 1 1 d . . .
H42 H 0.2302 0.7315 0.8823 0.065 Uiso 1 1 calc R . .
C43 C 0.2981(5) 0.6976(11) 0.9769(9) 0.073(4) Uani 1 1 d . . .
H43 H 0.3070 0.7636 0.9982 0.087 Uiso 1 1 calc R . .
C44 C 0.3308(4) 0.6206(13) 1.0154(8) 0.075(4) Uani 1 1 d . . .
H44 H 0.3623 0.6342 1.0608 0.090 Uiso 1 1 calc R . .
C45 C 0.3167(4) 0.5235(11) 0.9865(8) 0.076(4) Uani 1 1 d . . .
H45 H 0.3381 0.4703 1.0156 0.091 Uiso 1 1 calc R . .
C46 C 0.2717(4) 0.5029(9) 0.9155(7) 0.058(3) Uani 1 1 d . . .
H46 H 0.2633 0.4364 0.8951 0.069 Uiso 1 1 calc R . .
H H 0.124(3) 0.243(6) 0.606(5) 0.03(2) Uiso 1 1 d . . .
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'
P P 0.1023 0.0942 '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'
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
_geom_angle_publ_flag
C2 Os1 C1 101.8(5) . . ?
C2 Os1 C4 90.7(4) . . ?
C1 Os1 C4 93.5(4) . . ?
C2 Os1 C3 93.0(4) . . ?
C1 Os1 C3 92.9(4) . . ?
C4 Os1 C3 171.7(4) . . ?
C2 Os1 Os2 161.2(3) . . ?
C1 Os1 Os2 96.9(3) . . ?
C4 Os1 Os2 85.7(3) . . ?
C3 Os1 Os2 88.4(3) . . ?
C2 Os1 Os3 100.3(3) . . ?
C1 Os1 Os3 157.9(3) . . ?
C4 Os1 Os3 87.5(3) . . ?
C3 Os1 Os3 84.5(3) . . ?
Os2 Os1 Os3 61.20(3) . . ?
C5 Os2 C6 93.7(5) . . ?
C5 Os2 C7 93.6(5) . . ?
C6 Os2 C7 95.3(5) . . ?
C5 Os2 C11 84.9(4) . . ?
C6 Os2 C11 92.8(4) . . ?
C7 Os2 C11 171.8(4) . . ?
C5 Os2 Os1 173.2(3) . . ?
C6 Os2 Os1 88.0(3) . . ?
C7 Os2 Os1 92.8(3) . . ?
C11 Os2 Os1 88.5(2) . . ?
C5 Os2 Os3 116.1(4) . . ?
C6 Os2 Os3 140.3(4) . . ?
C7 Os2 Os3 107.4(3) . . ?
C11 Os2 Os3 66.4(2) . . ?
Os1 Os2 Os3 59.47(4) . . ?
C5 Os2 H 94(3) . . ?
C6 Os2 H 171(3) . . ?
C7 Os2 H 88(3) . . ?
C11 Os2 H 84(3) . . ?
Os1 Os2 H 84(3) . . ?
Os3 Os2 H 31(3) . . ?
C10 Os3 C9 93.3(4) . . ?
C10 Os3 C8 92.9(4) . . ?
C9 Os3 C8 93.7(4) . . ?
C10 Os3 N1 174.1(4) . . ?
C9 Os3 N1 92.5(3) . . ?
C8 Os3 N1 87.5(3) . . ?
C10 Os3 Os1 88.6(3) . . ?
C9 Os3 Os1 88.9(3) . . ?
C8 Os3 Os1 176.9(3) . . ?
N1 Os3 Os1 90.75(17) . . ?
C10 Os3 Os2 107.5(3) . . ?
C9 Os3 Os2 140.5(3) . . ?
C8 Os3 Os2 117.6(3) . . ?
N1 Os3 Os2 67.26(18) . . ?
Os1 Os3 Os2 59.33(4) . . ?
C10 Os3 H 89(3) . . ?
C9 Os3 H 173(3) . . ?
C8 Os3 H 93(3) . . ?
N1 Os3 H 85(3) . . ?
Os1 Os3 H 85(3) . . ?
Os2 Os3 H 32(3) . . ?
N2 P1 C41 103.3(4) . . ?
N2 P1 C31 116.4(4) . . ?
C41 P1 C31 108.1(4) . . ?
N2 P1 C21 114.1(4) . . ?
C41 P1 C21 108.4(4) . . ?
C31 P1 C21 106.1(4) . . ?
C11 N1 N2 127.2(7) . . ?
C11 N1 Os3 112.0(6) . . ?
N2 N1 Os3 120.7(5) . . ?
N1 N2 P1 118.2(5) . . ?
O1 C1 Os1 179.4(12) . . ?
O2 C2 Os1 177.6(11) . . ?
O3 C3 Os1 174.1(10) . . ?
O4 C4 Os1 178.5(9) . . ?
O5 C5 Os2 175.6(14) . . ?
O6 C6 Os2 177.2(11) . . ?
O7 C7 Os2 177.3(11) . . ?
O8 C8 Os3 176.0(10) . . ?
O9 C9 Os3 179.0(11) . . ?
O10 C10 Os3 178.9(10) . . ?
N1 C11 Os2 114.0(6) . . ?
N1 C11 H11 123.0 . . ?
Os2 C11 H11 123.0 . . ?
C22 C21 C26 119.4(9) . . ?
C22 C21 P1 117.5(7) . . ?
C26 C21 P1 123.1(7) . . ?
C23 C22 C21 120.2(10) . . ?
C23 C22 H22 119.9 . . ?
C21 C22 H22 119.9 . . ?
C24 C23 C22 119.6(11) . . ?
C24 C23 H23 120.2 . . ?
C22 C23 H23 120.2 . . ?
C23 C24 C25 121.0(11) . . ?
C23 C24 H24 119.5 . . ?
C25 C24 H24 119.5 . . ?
C24 C25 C26 120.6(11) . . ?
C24 C25 H25 119.7 . . ?
C26 C25 H25 119.7 . . ?
C25 C26 C21 119.2(10) . . ?
C25 C26 H26 120.4 . . ?
C21 C26 H26 120.4 . . ?
C32 C31 C36 118.5(9) . . ?
C32 C31 P1 125.4(7) . . ?
C36 C31 P1 116.0(7) . . ?
C33 C32 C31 119.9(11) . . ?
C33 C32 H32 120.0 . . ?
C31 C32 H32 120.0 . . ?
C34 C33 C32 121.3(11) . . ?
C34 C33 H33 119.4 . . ?
C32 C33 H33 119.4 . . ?
C33 C34 C35 120.4(11) . . ?
C33 C34 H34 119.8 . . ?
C35 C34 H34 119.8 . . ?
C34 C35 C36 119.7(11) . . ?
C34 C35 H35 120.1 . . ?
C36 C35 H35 120.1 . . ?
C35 C36 C31 120.1(10) . . ?
C35 C36 H36 120.0 . . ?
C31 C36 H36 120.0 . . ?
C42 C41 C46 117.5(9) . . ?
C42 C41 P1 123.2(8) . . ?
C46 C41 P1 119.3(7) . . ?
C43 C42 C41 121.0(11) . . ?
C43 C42 H42 119.5 . . ?
C41 C42 H42 119.5 . . ?
C44 C43 C42 120.5(12) . . ?
C44 C43 H43 119.8 . . ?
C42 C43 H43 119.8 . . ?
C45 C44 C43 119.3(11) . . ?
C45 C44 H44 120.4 . . ?
C43 C44 H44 120.4 . . ?
C44 C45 C46 121.2(12) . . ?
C44 C45 H45 119.4 . . ?
C46 C45 H45 119.4 . . ?
C45 C46 C41 120.4(11) . . ?
C45 C46 H46 119.8 . . ?
C41 C46 H46 119.8 . . ?
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 C2 1.913(13) . ?
Os1 C1 1.916(11) . ?
Os1 C4 1.927(11) . ?
Os1 C3 1.944(11) . ?
Os1 Os2 2.8683(11) . ?
Os1 Os3 2.8725(18) . ?
Os2 C5 1.873(12) . ?
Os2 C6 1.876(11) . ?
Os2 C7 1.950(11) . ?
Os2 C11 2.097(9) . ?
Os2 Os3 2.9225(17) . ?
Os2 H 1.75(8) . ?
Os3 C10 1.899(10) . ?
Os3 C9 1.901(10) . ?
Os3 C8 1.925(10) . ?
Os3 N1 2.098(6) . ?
Os3 H 1.69(8) . ?
P1 N2 1.596(7) . ?
P1 C41 1.800(9) . ?
P1 C31 1.812(9) . ?
P1 C21 1.818(9) . ?
O1 C1 1.135(12) . ?
O2 C2 1.134(13) . ?
O3 C3 1.147(12) . ?
O4 C4 1.140(12) . ?
O5 C5 1.179(13) . ?
O6 C6 1.165(12) . ?
O7 C7 1.140(12) . ?
O8 C8 1.126(11) . ?
O9 C9 1.131(12) . ?
O10 C10 1.148(11) . ?
N1 C11 1.275(10) . ?
N1 N2 1.417(9) . ?
C11 H11 0.9300 . ?
C21 C22 1.397(12) . ?
C21 C26 1.400(13) . ?
C22 C23 1.393(14) . ?
C22 H22 0.9300 . ?
C23 C24 1.365(15) . ?
C23 H23 0.9300 . ?
C24 C25 1.379(16) . ?
C24 H24 0.9300 . ?
C25 C26 1.385(15) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
C31 C32 1.390(13) . ?
C31 C36 1.393(12) . ?
C32 C33 1.363(15) . ?
C32 H32 0.9300 . ?
C33 C34 1.356(16) . ?
C33 H33 0.9300 . ?
C34 C35 1.360(15) . ?
C34 H34 0.9300 . ?
C35 C36 1.389(13) . ?
C35 H35 0.9300 . ?
C36 H36 0.9300 . ?
C41 C42 1.391(13) . ?
C41 C46 1.393(14) . ?
C42 C43 1.370(15) . ?
C42 H42 0.9300 . ?
C43 C44 1.363(18) . ?
C43 H43 0.9300 . ?
C44 C45 1.363(18) . ?
C44 H44 0.9300 . ?
C45 C46 1.365(14) . ?
C45 H45 0.9300 . ?
C46 H46 0.9300 . ?
