#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:28:34 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179846 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/42/7014223.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_7014223
loop_
_publ_author_name
'Tunik, Sergey P.'
'Khripun, Vassily D.'
'Haukka, Matti'
'Pakkanen, Tapani A.'
_publ_section_title
;
 Reactions of 2,4-hexadiyne-1,6-diol with [H2Os3(CO)9(PR3)] clusters.
 Cyclization of the diyne and reversible exchange of the phosphine
 ligands between different positions of the "Os3C3" framework.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1775
_journal_page_last               1782
_journal_paper_doi               10.1039/b403861b
_journal_year                    2004
_chemical_formula_sum            'C32 H21 O9 Os3 P'
_chemical_formula_weight         1151.06
_chemical_name_common            HOs3(CO)8(C6H5O)PPh3
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                97.2840(10)
_cell_angle_beta                 92.1850(10)
_cell_angle_gamma                101.063(2)
_cell_formula_units_Z            2
_cell_length_a                   9.3420(3)
_cell_length_b                   10.8940(2)
_cell_length_c                   15.4198(5)
_cell_measurement_temperature    150(2)
_cell_volume                     1524.56(8)
_computing_cell_refinement       'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'XP in SHELXTL v.6.12 (Bruker AXS, 2001)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF99 (Beurskens et al., 1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.922
_diffrn_measured_fraction_theta_max 0.922
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_av_sigmaI/netI    0.0384
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14150
_diffrn_reflns_theta_full        26.07
_diffrn_reflns_theta_max         26.07
_diffrn_reflns_theta_min         3.50
_exptl_absorpt_coefficient_mu    12.579
_exptl_absorpt_correction_T_max  0.24790
_exptl_absorpt_correction_T_min  0.15745
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Xprep in Shelxtl v.6.12 (Bruker AXS, 2001)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.507
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.617
_refine_diff_density_min         -1.807
_refine_diff_density_rms         0.163
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.167
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         5566
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.167
_refine_ls_R_factor_all          0.0295
_refine_ls_R_factor_gt           0.0278
_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)+(0.0047P)²+9.9358P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0689
_refine_ls_wR_factor_ref         0.0697
_reflns_number_gt                5334
_reflns_number_total             5566
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b403861b.txt
_cod_data_source_block           Va
_cod_original_cell_volume        1524.56(7)
_cod_database_code               7014223
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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_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
C4 C 0.4071(8) -0.2342(6) 0.1086(5) 0.0324(16) Uani 1 1 d . . .
C5 C 0.4529(8) 0.0222(6) 0.1265(5) 0.0302(16) Uani 1 1 d . . .
C6 C 0.4637(8) -0.1162(7) 0.2757(5) 0.0318(16) Uani 1 1 d . . .
C1 C -0.0263(7) -0.0590(6) 0.3803(4) 0.0237(14) Uani 1 1 d . . .
C3 C 0.2632(7) -0.0196(6) 0.4029(4) 0.0241(14) Uani 1 1 d . . .
C9 C -0.1440(9) -0.3207(6) 0.2130(5) 0.0370(18) Uani 1 1 d . . .
C8 C 0.1350(9) -0.2939(6) 0.3051(5) 0.0344(17) Uani 1 1 d . . .
C7 C 0.0773(8) -0.4014(6) 0.1271(5) 0.0301(15) Uani 1 1 d . . .
C14 C 0.1512(8) -0.1421(6) 0.0901(4) 0.0266(15) Uani 1 1 d . . .
C13 C 0.0210(7) -0.1047(6) 0.1114(4) 0.0237(13) Uani 1 1 d . . .
C12 C -0.0196(7) -0.0590(6) 0.1971(4) 0.0210(13) Uani 1 1 d . . .
C11 C -0.1718(7) -0.0470(6) 0.1860(4) 0.0263(14) Uani 1 1 d . . .
H11 H -0.2315 -0.0229 0.2311 0.032 Uiso 1 1 calc R . .
C10 C -0.2120(9) -0.0769(7) 0.0993(6) 0.0424(19) Uani 1 1 d . . .
H10 H -0.3051 -0.0724 0.0743 0.051 Uiso 1 1 calc R . .
C15 C 0.1410(9) -0.2025(7) -0.0065(5) 0.0355(17) Uani 1 1 d . . .
H15A H 0.0385 -0.2232 -0.0290 0.053 Uiso 1 1 calc R . .
H15B H 0.1810 -0.2797 -0.0108 0.053 Uiso 1 1 calc R . .
H15C H 0.1970 -0.1429 -0.0412 0.053 Uiso 1 1 calc R . .
C20 C -0.0578(7) 0.2309(6) 0.3162(4) 0.0220(13) Uani 1 1 d . . .
C21 C -0.1618(8) 0.1877(6) 0.3740(5) 0.0271(14) Uani 1 1 d . . .
H21 H -0.1341 0.1478 0.4216 0.033 Uiso 1 1 calc R . .
C22 C -0.3063(8) 0.2029(6) 0.3623(5) 0.0318(16) Uani 1 1 d . . .
H22 H -0.3763 0.1738 0.4019 0.038 Uiso 1 1 calc R . .
C23 C -0.3474(8) 0.2607(7) 0.2922(5) 0.0353(17) Uani 1 1 d . . .
H23 H -0.4459 0.2697 0.2833 0.042 Uiso 1 1 calc R . .
C24 C -0.2451(9) 0.3044(7) 0.2364(5) 0.0347(17) Uani 1 1 d . . .
H24 H -0.2731 0.3449 0.1893 0.042 Uiso 1 1 calc R . .
C25 C -0.1006(8) 0.2908(6) 0.2475(4) 0.0262(14) Uani 1 1 d . . .
H25 H -0.0311 0.3222 0.2082 0.031 Uiso 1 1 calc R . .
C26 C 0.2295(7) 0.2907(6) 0.2526(4) 0.0214(13) Uani 1 1 d . . .
C27 C 0.2334(8) 0.2391(6) 0.1652(4) 0.0299(15) Uani 1 1 d . . .
H27 H 0.1782 0.1571 0.1446 0.036 Uiso 1 1 calc R . .
C28 C 0.3174(9) 0.3068(7) 0.1083(5) 0.0332(16) Uani 1 1 d . . .
H28 H 0.3194 0.2712 0.0489 0.040 Uiso 1 1 calc R . .
C29 C 0.3980(8) 0.4258(7) 0.1377(5) 0.0317(16) Uani 1 1 d . . .
H29 H 0.4601 0.4701 0.0997 0.038 Uiso 1 1 calc R . .
C30 C 0.3880(8) 0.4805(6) 0.2227(5) 0.0314(16) Uani 1 1 d . . .
H30 H 0.4387 0.5644 0.2418 0.038 Uiso 1 1 calc R . .
C31 C 0.3051(7) 0.4140(6) 0.2799(4) 0.0252(14) Uani 1 1 d . . .
H31 H 0.2994 0.4523 0.3383 0.030 Uiso 1 1 calc R . .
C32 C 0.1997(7) 0.2867(6) 0.4347(4) 0.0208(13) Uani 1 1 d . . .
C33 C 0.3415(8) 0.2798(6) 0.4622(4) 0.0275(14) Uani 1 1 d . . .
H33 H 0.3915 0.2241 0.4285 0.033 Uiso 1 1 calc R . .
C34 C 0.4100(8) 0.3520(7) 0.5371(5) 0.0322(16) Uani 1 1 d . . .
H34 H 0.5076 0.3480 0.5543 0.039 Uiso 1 1 calc R . .
C35 C 0.3359(9) 0.4308(7) 0.5874(5) 0.0345(17) Uani 1 1 d . . .
H35 H 0.3828 0.4810 0.6393 0.041 Uiso 1 1 calc R . .
C36 C 0.1935(9) 0.4367(7) 0.5624(5) 0.0354(17) Uani 1 1 d . . .
H36 H 0.1424 0.4895 0.5978 0.042 Uiso 1 1 calc R . .
C37 C 0.1254(8) 0.3653(6) 0.4854(5) 0.0279(14) Uani 1 1 d . . .
H37 H 0.0284 0.3704 0.4676 0.034 Uiso 1 1 calc R . .
O4 O 0.4582(6) -0.3067(5) 0.0664(4) 0.0412(13) Uani 1 1 d . . .
O5 O 0.5211(6) 0.0959(5) 0.0900(4) 0.0409(13) Uani 1 1 d . . .
O6 O 0.5419(7) -0.1265(6) 0.3317(4) 0.0492(15) Uani 1 1 d . . .
O1 O -0.1210(6) -0.0910(5) 0.4229(3) 0.0366(12) Uani 1 1 d . . .
O3 O 0.3397(6) -0.0280(5) 0.4611(3) 0.0382(12) Uani 1 1 d . . .
O9 O -0.2663(7) -0.3611(6) 0.2169(5) 0.0571(17) Uani 1 1 d . . .
O8 O 0.1828(7) -0.3245(5) 0.3663(3) 0.0432(14) Uani 1 1 d . . .
O7 O 0.0914(7) -0.4920(5) 0.0838(4) 0.0478(15) Uani 1 1 d . . .
O10 O -0.0975(6) -0.1164(5) 0.0491(3) 0.0409(13) Uani 1 1 d . . .
P1 P 0.12503(17) 0.19772(14) 0.32871(10) 0.0183(3) Uani 1 1 d . . .
Os2 Os 0.33166(3) -0.10746(2) 0.177153(17) 0.02322(8) Uani 1 1 d . . .
Os1 Os 0.12668(3) -0.01768(2) 0.306693(15) 0.01763(7) Uani 1 1 d . . .
Os3 Os 0.05629(3) -0.25275(2) 0.199766(16) 0.02115(8) Uani 1 1 d . . .
H1 H 0.2858 0.0325 0.2429 0.050 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
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'
O O 0.0106 0.0060 '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'
Os Os -1.2165 7.6030 '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
O4 C4 Os2 176.8(6) . . ?
O5 C5 Os2 174.9(7) . . ?
O6 C6 Os2 176.9(6) . . ?
O1 C1 Os1 176.2(6) . . ?
O3 C3 Os1 175.7(6) . . ?
O9 C9 Os3 176.7(7) . . ?
O8 C8 Os3 176.5(6) . . ?
O7 C7 Os3 179.0(7) . . ?
C13 C14 C15 110.5(6) . . ?
C13 C14 Os2 122.5(5) . . ?
C15 C14 Os2 126.9(5) . . ?
C13 C14 Os3 72.1(4) . . ?
C15 C14 Os3 122.4(5) . . ?
Os2 C14 Os3 79.9(2) . . ?
C14 C13 O10 122.5(6) . . ?
C14 C13 C12 127.5(6) . . ?
O10 C13 C12 109.8(6) . . ?
C14 C13 Os3 72.7(4) . . ?
O10 C13 Os3 125.9(4) . . ?
C12 C13 Os3 74.1(3) . . ?
C13 C12 C11 106.1(6) . . ?
C13 C12 Os1 122.5(5) . . ?
C11 C12 Os1 131.3(5) . . ?
C13 C12 Os3 69.8(3) . . ?
C11 C12 Os3 124.0(4) . . ?
Os1 C12 Os3 78.4(2) . . ?
C10 C11 C12 107.0(6) . . ?
C10 C11 H11 126.5 . . ?
C12 C11 H11 126.5 . . ?
C11 C10 O10 112.4(7) . . ?
C11 C10 H10 123.8 . . ?
O10 C10 H10 123.8 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C25 C20 C21 118.7(6) . . ?
C25 C20 P1 122.3(5) . . ?
C21 C20 P1 118.9(5) . . ?
C22 C21 C20 120.4(6) . . ?
C22 C21 H21 119.8 . . ?
C20 C21 H21 119.8 . . ?
C23 C22 C21 119.9(7) . . ?
C23 C22 H22 120.0 . . ?
C21 C22 H22 120.0 . . ?
C24 C23 C22 119.6(7) . . ?
C24 C23 H23 120.2 . . ?
C22 C23 H23 120.2 . . ?
C23 C24 C25 121.2(7) . . ?
C23 C24 H24 119.4 . . ?
C25 C24 H24 119.4 . . ?
C24 C25 C20 120.1(6) . . ?
C24 C25 H25 119.9 . . ?
C20 C25 H25 119.9 . . ?
C31 C26 C27 118.7(6) . . ?
C31 C26 P1 121.2(5) . . ?
C27 C26 P1 120.1(5) . . ?
C28 C27 C26 120.4(6) . . ?
C28 C27 H27 119.8 . . ?
C26 C27 H27 119.8 . . ?
C29 C28 C27 120.2(7) . . ?
C29 C28 H28 119.9 . . ?
C27 C28 H28 119.9 . . ?
C28 C29 C30 119.7(6) . . ?
C28 C29 H29 120.1 . . ?
C30 C29 H29 120.1 . . ?
C31 C30 C29 120.5(6) . . ?
C31 C30 H30 119.7 . . ?
C29 C30 H30 119.7 . . ?
C30 C31 C26 120.3(6) . . ?
C30 C31 H31 119.8 . . ?
C26 C31 H31 119.8 . . ?
C37 C32 C33 119.3(6) . . ?
C37 C32 P1 123.1(5) . . ?
C33 C32 P1 117.5(5) . . ?
C34 C33 C32 121.1(6) . . ?
C34 C33 H33 119.5 . . ?
C32 C33 H33 119.5 . . ?
C33 C34 C35 119.5(7) . . ?
C33 C34 H34 120.2 . . ?
C35 C34 H34 120.2 . . ?
C34 C35 C36 120.3(6) . . ?
C34 C35 H35 119.8 . . ?
C36 C35 H35 119.8 . . ?
C35 C36 C37 120.0(7) . . ?
C35 C36 H36 120.0 . . ?
C37 C36 H36 120.0 . . ?
C32 C37 C36 119.8(7) . . ?
C32 C37 H37 120.1 . . ?
C36 C37 H37 120.1 . . ?
C13 O10 C10 104.5(6) . . ?
C20 P1 C32 104.3(3) . . ?
C20 P1 C26 103.9(3) . . ?
C32 P1 C26 101.5(3) . . ?
C20 P1 Os1 112.8(2) . . ?
C32 P1 Os1 117.5(2) . . ?
C26 P1 Os1 115.2(2) . . ?
C4 Os2 C5 91.5(3) . . ?
C4 Os2 C6 90.1(3) . . ?
C5 Os2 C6 98.5(3) . . ?
C4 Os2 C14 89.4(3) . . ?
C5 Os2 C14 99.5(3) . . ?
C6 Os2 C14 162.0(3) . . ?
C4 Os2 Os3 97.9(2) . . ?
C5 Os2 Os3 151.4(2) . . ?
C6 Os2 Os3 108.4(2) . . ?
C14 Os2 Os3 53.93(16) . . ?
C4 Os2 Os1 153.2(2) . . ?
C5 Os2 Os1 115.18(19) . . ?
C6 Os2 Os1 88.4(2) . . ?
C14 Os2 Os1 84.02(16) . . ?
Os3 Os2 Os1 57.541(8) . . ?
C4 Os2 H1 171.1 . . ?
C5 Os2 H1 80.6 . . ?
C6 Os2 H1 86.9 . . ?
C14 Os2 H1 96.0 . . ?
Os3 Os2 H1 91.0 . . ?
Os1 Os2 H1 35.2 . . ?
C1 Os1 C3 88.6(3) . . ?
C1 Os1 C12 91.0(3) . . ?
C3 Os1 C12 167.0(2) . . ?
C1 Os1 P1 93.99(19) . . ?
C3 Os1 P1 97.62(19) . . ?
C12 Os1 P1 95.40(17) . . ?
C1 Os1 Os3 93.52(19) . . ?
C3 Os1 Os3 111.84(19) . . ?
C12 Os1 Os3 55.18(17) . . ?
P1 Os1 Os3 149.73(4) . . ?
C1 Os1 Os2 148.21(19) . . ?
C3 Os1 Os2 90.85(18) . . ?
C12 Os1 Os2 82.64(17) . . ?
P1 Os1 Os2 117.55(4) . . ?
Os3 Os1 Os2 57.434(8) . . ?
C1 Os1 H1 174.9 . . ?
C3 Os1 H1 87.5 . . ?
C12 Os1 H1 93.5 . . ?
P1 Os1 H1 83.2 . . ?
Os3 Os1 H1 91.0 . . ?
Os2 Os1 H1 35.3 . . ?
C7 Os3 C8 96.7(3) . . ?
C7 Os3 C9 91.5(3) . . ?
C8 Os3 C9 97.9(3) . . ?
C7 Os3 C13 108.3(3) . . ?
C8 Os3 C13 150.1(3) . . ?
C9 Os3 C13 97.7(3) . . ?
C7 Os3 C14 87.1(3) . . ?
C8 Os3 C14 134.7(3) . . ?
C9 Os3 C14 127.2(3) . . ?
C13 Os3 C14 35.2(2) . . ?
C7 Os3 C12 142.6(3) . . ?
C8 Os3 C12 120.7(3) . . ?
C9 Os3 C12 85.4(3) . . ?
C13 Os3 C12 36.1(2) . . ?
C14 Os3 C12 66.1(2) . . ?
C7 Os3 Os2 97.1(2) . . ?
C8 Os3 Os2 88.7(2) . . ?
C9 Os3 Os2 168.5(2) . . ?
C13 Os3 Os2 72.36(17) . . ?
C14 Os3 Os2 46.2(2) . . ?
C12 Os3 Os2 83.05(15) . . ?
C7 Os3 Os1 160.9(2) . . ?
C8 Os3 Os1 77.1(2) . . ?
C9 Os3 Os1 107.1(2) . . ?
C13 Os3 Os1 73.98(15) . . ?
C14 Os3 Os1 84.89(16) . . ?
C12 Os3 Os1 46.40(15) . . ?
Os2 Os3 Os1 65.025(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
C4 O4 1.146(9) . ?
C4 Os2 1.892(7) . ?
C5 O5 1.146(8) . ?
C5 Os2 1.903(7) . ?
C6 O6 1.140(9) . ?
C6 Os2 1.944(8) . ?
C1 O1 1.150(8) . ?
C1 Os1 1.881(7) . ?
C3 O3 1.150(8) . ?
C3 Os1 1.924(7) . ?
C9 O9 1.150(10) . ?
C9 Os3 1.904(8) . ?
C8 O8 1.142(9) . ?
C8 Os3 1.898(8) . ?
C7 O7 1.152(9) . ?
C7 Os3 1.896(7) . ?
C14 C13 1.393(10) . ?
C14 C15 1.542(9) . ?
C14 Os2 2.059(8) . ?
C14 Os3 2.306(6) . ?
C13 O10 1.414(8) . ?
C13 C12 1.442(9) . ?
C13 Os3 2.300(6) . ?
C12 C11 1.458(9) . ?
C12 Os1 2.079(6) . ?
C12 Os3 2.357(6) . ?
C11 C10 1.357(11) . ?
C11 H11 0.9500 . ?
C10 O10 1.443(10) . ?
C10 H10 0.9500 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C20 C25 1.397(9) . ?
C20 C21 1.399(9) . ?
C20 P1 1.820(6) . ?
C21 C22 1.399(10) . ?
C21 H21 0.9500 . ?
C22 C23 1.395(11) . ?
C22 H22 0.9500 . ?
C23 C24 1.368(11) . ?
C23 H23 0.9500 . ?
C24 C25 1.392(10) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C26 C31 1.396(9) . ?
C26 C27 1.398(9) . ?
C26 P1 1.835(6) . ?
C27 C28 1.387(9) . ?
C27 H27 0.9500 . ?
C28 C29 1.379(10) . ?
C28 H28 0.9500 . ?
C29 C30 1.384(10) . ?
C29 H29 0.9500 . ?
C30 C31 1.379(9) . ?
C30 H30 0.9500 . ?
C31 H31 0.9500 . ?
C32 C37 1.388(9) . ?
C32 C33 1.395(9) . ?
C32 P1 1.829(6) . ?
C33 C34 1.373(10) . ?
C33 H33 0.9500 . ?
C34 C35 1.385(11) . ?
C34 H34 0.9500 . ?
C35 C36 1.387(11) . ?
C35 H35 0.9500 . ?
C36 C37 1.392(10) . ?
C36 H36 0.9500 . ?
C37 H37 0.9500 . ?
P1 Os1 2.3311(15) . ?
Os2 Os3 2.8090(4) . ?
Os2 Os1 3.0214(3) . ?
Os2 H1 1.8513 . ?
Os1 Os3 2.8123(3) . ?
Os1 H1 1.8470 . ?
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
C15 C14 C13 O10 -3.2(8) . . . . ?
Os2 C14 C13 O10 173.1(4) . . . . ?
Os3 C14 C13 O10 -122.0(6) . . . . ?
C15 C14 C13 C12 171.8(6) . . . . ?
Os2 C14 C13 C12 -11.8(9) . . . . ?
Os3 C14 C13 C12 53.1(6) . . . . ?
C15 C14 C13 Os3 118.7(5) . . . . ?
Os2 C14 C13 Os3 -64.9(4) . . . . ?
C14 C13 C12 C11 -173.5(6) . . . . ?
O10 C13 C12 C11 2.1(7) . . . . ?
Os3 C13 C12 C11 -121.0(5) . . . . ?
C14 C13 C12 Os1 8.3(9) . . . . ?
O10 C13 C12 Os1 -176.2(4) . . . . ?
Os3 C13 C12 Os1 60.8(4) . . . . ?
C14 C13 C12 Os3 -52.5(6) . . . . ?
O10 C13 C12 Os3 123.1(5) . . . . ?
C13 C12 C11 C10 -3.2(7) . . . . ?
Os1 C12 C11 C10 174.8(5) . . . . ?
Os3 C12 C11 C10 -79.5(7) . . . . ?
C12 C11 C10 O10 3.3(8) . . . . ?
C25 C20 C21 C22 0.8(9) . . . . ?
P1 C20 C21 C22 -175.0(5) . . . . ?
C20 C21 C22 C23 0.4(10) . . . . ?
C21 C22 C23 C24 -1.3(10) . . . . ?
C22 C23 C24 C25 0.9(11) . . . . ?
C23 C24 C25 C20 0.3(10) . . . . ?
C21 C20 C25 C24 -1.2(9) . . . . ?
P1 C20 C25 C24 174.5(5) . . . . ?
C31 C26 C27 C28 3.5(10) . . . . ?
P1 C26 C27 C28 -177.1(6) . . . . ?
C26 C27 C28 C29 0.1(12) . . . . ?
C27 C28 C29 C30 -3.8(12) . . . . ?
C28 C29 C30 C31 3.9(11) . . . . ?
C29 C30 C31 C26 -0.3(11) . . . . ?
C27 C26 C31 C30 -3.4(10) . . . . ?
P1 C26 C31 C30 177.2(5) . . . . ?
C37 C32 C33 C34 -1.9(10) . . . . ?
P1 C32 C33 C34 174.4(5) . . . . ?
C32 C33 C34 C35 1.6(11) . . . . ?
C33 C34 C35 C36 0.0(11) . . . . ?
C34 C35 C36 C37 -1.4(12) . . . . ?
C33 C32 C37 C36 0.5(10) . . . . ?
P1 C32 C37 C36 -175.5(5) . . . . ?
C35 C36 C37 C32 1.1(11) . . . . ?
C14 C13 O10 C10 175.6(6) . . . . ?
C12 C13 O10 C10 -0.2(7) . . . . ?
Os3 C13 O10 C10 84.2(6) . . . . ?
C11 C10 O10 C13 -2.0(8) . . . . ?
C25 C20 P1 C32 118.7(5) . . . . ?
C21 C20 P1 C32 -65.6(5) . . . . ?
C25 C20 P1 C26 12.8(6) . . . . ?
C21 C20 P1 C26 -171.6(5) . . . . ?
C25 C20 P1 Os1 -112.6(5) . . . . ?
C21 C20 P1 Os1 63.1(5) . . . . ?
C37 C32 P1 C20 -3.6(6) . . . . ?
C33 C32 P1 C20 -179.7(5) . . . . ?
C37 C32 P1 C26 104.1(6) . . . . ?
C33 C32 P1 C26 -72.0(5) . . . . ?
C37 C32 P1 Os1 -129.3(5) . . . . ?
C33 C32 P1 Os1 54.5(5) . . . . ?
C31 C26 P1 C20 91.3(6) . . . . ?
C27 C26 P1 C20 -88.1(6) . . . . ?
C31 C26 P1 C32 -16.8(6) . . . . ?
C27 C26 P1 C32 163.9(6) . . . . ?
C31 C26 P1 Os1 -144.8(5) . . . . ?
C27 C26 P1 Os1 35.8(6) . . . . ?
O4 C4 Os2 C5 18(13) . . . . ?
O4 C4 Os2 C6 -81(13) . . . . ?
O4 C4 Os2 C14 117(13) . . . . ?
O4 C4 Os2 Os3 171(13) . . . . ?
O4 C4 Os2 Os1 -167(12) . . . . ?
O5 C5 Os2 C4 58(7) . . . . ?
O5 C5 Os2 C6 148(7) . . . . ?
O5 C5 Os2 C14 -32(7) . . . . ?
O5 C5 Os2 Os3 -52(7) . . . . ?
O5 C5 Os2 Os1 -119(7) . . . . ?
O6 C6 Os2 C4 -18(13) . . . . ?
O6 C6 Os2 C5 -109(13) . . . . ?
O6 C6 Os2 C14 71(13) . . . . ?
O6 C6 Os2 Os3 81(13) . . . . ?
O6 C6 Os2 Os1 136(13) . . . . ?
C13 C14 Os2 C4 161.3(5) . . . . ?
C15 C14 Os2 C4 -23.0(6) . . . . ?
Os3 C14 Os2 C4 100.2(2) . . . . ?
C13 C14 Os2 C5 -107.2(5) . . . . ?
C15 C14 Os2 C5 68.5(6) . . . . ?
Os3 C14 Os2 C5 -168.3(2) . . . . ?
C13 C14 Os2 C6 72.9(10) . . . . ?
C15 C14 Os2 C6 -111.4(9) . . . . ?
Os3 C14 Os2 C6 11.8(9) . . . . ?
C13 C14 Os2 Os3 61.1(5) . . . . ?
C15 C14 Os2 Os3 -123.1(6) . . . . ?
C13 C14 Os2 Os1 7.4(5) . . . . ?
C15 C14 Os2 Os1 -176.9(5) . . . . ?
Os3 C14 Os2 Os1 -53.75(11) . . . . ?
O1 C1 Os1 C3 -102(9) . . . . ?
O1 C1 Os1 C12 65(9) . . . . ?
O1 C1 Os1 P1 160(9) . . . . ?
O1 C1 Os1 Os3 9(9) . . . . ?
O1 C1 Os1 Os2 -13(9) . . . . ?
O3 C3 Os1 C1 50(7) . . . . ?
O3 C3 Os1 C12 -38(8) . . . . ?
O3 C3 Os1 P1 144(7) . . . . ?
O3 C3 Os1 Os3 -43(8) . . . . ?
O3 C3 Os1 Os2 -98(7) . . . . ?
C13 C12 Os1 C1 -150.3(5) . . . . ?
C11 C12 Os1 C1 31.9(6) . . . . ?
Os3 C12 Os1 C1 -93.6(2) . . . . ?
C13 C12 Os1 C3 -62.2(13) . . . . ?
C11 C12 Os1 C3 120.1(11) . . . . ?
Os3 C12 Os1 C3 -5.4(12) . . . . ?
C13 C12 Os1 P1 115.6(5) . . . . ?
C11 C12 Os1 P1 -62.2(6) . . . . ?
Os3 C12 Os1 P1 172.30(11) . . . . ?
C13 C12 Os1 Os3 -56.7(4) . . . . ?
C11 C12 Os1 Os3 125.5(6) . . . . ?
C13 C12 Os1 Os2 -1.6(5) . . . . ?
C11 C12 Os1 Os2 -179.4(6) . . . . ?
Os3 C12 Os1 Os2 55.16(11) . . . . ?
C20 P1 Os1 C1 -48.1(3) . . . . ?
C32 P1 Os1 C1 73.4(3) . . . . ?
C26 P1 Os1 C1 -167.1(3) . . . . ?
C20 P1 Os1 C3 -137.2(3) . . . . ?
C32 P1 Os1 C3 -15.7(3) . . . . ?
C26 P1 Os1 C3 103.8(3) . . . . ?
C20 P1 Os1 C12 43.3(3) . . . . ?
C32 P1 Os1 C12 164.8(3) . . . . ?
C26 P1 Os1 C12 -75.7(3) . . . . ?
C20 P1 Os1 Os3 55.9(2) . . . . ?
C32 P1 Os1 Os3 177.4(2) . . . . ?
C26 P1 Os1 Os3 -63.1(3) . . . . ?
C20 P1 Os1 Os2 127.8(2) . . . . ?
C32 P1 Os1 Os2 -110.7(2) . . . . ?
C26 P1 Os1 Os2 8.8(2) . . . . ?
C4 Os2 Os1 C1 0.7(6) . . . . ?
C5 Os2 Os1 C1 175.1(5) . . . . ?
C6 Os2 Os1 C1 -86.2(4) . . . . ?
C14 Os2 Os1 C1 77.4(4) . . . . ?
Os3 Os2 Os1 C1 26.8(4) . . . . ?
C4 Os2 Os1 C3 89.5(6) . . . . ?
C5 Os2 Os1 C3 -96.2(3) . . . . ?
C6 Os2 Os1 C3 2.5(3) . . . . ?
C14 Os2 Os1 C3 166.2(3) . . . . ?
Os3 Os2 Os1 C3 115.6(2) . . . . ?
C4 Os2 Os1 C12 -79.2(6) . . . . ?
C5 Os2 Os1 C12 95.2(3) . . . . ?
C6 Os2 Os1 C12 -166.2(3) . . . . ?
C14 Os2 Os1 C12 -2.5(2) . . . . ?
Os3 Os2 Os1 C12 -53.08(16) . . . . ?
C4 Os2 Os1 P1 -171.5(5) . . . . ?
C5 Os2 Os1 P1 2.9(3) . . . . ?
C6 Os2 Os1 P1 101.6(2) . . . . ?
C14 Os2 Os1 P1 -94.77(17) . . . . ?
Os3 Os2 Os1 P1 -145.35(5) . . . . ?
C4 Os2 Os1 Os3 -26.1(5) . . . . ?
C5 Os2 Os1 Os3 148.2(3) . . . . ?
C6 Os2 Os1 Os3 -113.1(2) . . . . ?
C14 Os2 Os1 Os3 50.58(16) . . . . ?
O7 C7 Os3 C8 -16(44) . . . . ?
O7 C7 Os3 C9 -114(44) . . . . ?
O7 C7 Os3 C13 147(44) . . . . ?
O7 C7 Os3 C14 119(44) . . . . ?
O7 C7 Os3 C12 162(44) . . . . ?
O7 C7 Os3 Os2 74(44) . . . . ?
O7 C7 Os3 Os1 54(45) . . . . ?
O8 C8 Os3 C7 -5(12) . . . . ?
O8 C8 Os3 C9 88(12) . . . . ?
O8 C8 Os3 C13 -152(11) . . . . ?
O8 C8 Os3 C14 -97(12) . . . . ?
O8 C8 Os3 C12 177(12) . . . . ?
O8 C8 Os3 Os2 -102(12) . . . . ?
O8 C8 Os3 Os1 -167(12) . . . . ?
O9 C9 Os3 C7 -70(12) . . . . ?
O9 C9 Os3 C8 -167(12) . . . . ?
O9 C9 Os3 C13 38(12) . . . . ?
O9 C9 Os3 C14 17(12) . . . . ?
O9 C9 Os3 C12 72(12) . . . . ?
O9 C9 Os3 Os2 68(13) . . . . ?
O9 C9 Os3 Os1 114(12) . . . . ?
C14 C13 Os3 C7 -55.9(5) . . . . ?
O10 C13 Os3 C7 62.1(6) . . . . ?
C12 C13 Os3 C7 165.4(4) . . . . ?
C14 C13 Os3 C8 89.1(7) . . . . ?
O10 C13 Os3 C8 -152.9(6) . . . . ?
C12 C13 Os3 C8 -49.6(7) . . . . ?
C14 C13 Os3 C9 -150.1(4) . . . . ?
O10 C13 Os3 C9 -32.0(6) . . . . ?
C12 C13 Os3 C9 71.2(4) . . . . ?
O10 C13 Os3 C14 118.0(7) . . . . ?
C12 C13 Os3 C14 -138.7(6) . . . . ?
C14 C13 Os3 C12 138.7(6) . . . . ?
O10 C13 Os3 C12 -103.3(7) . . . . ?
C14 C13 Os3 Os2 36.0(4) . . . . ?
O10 C13 Os3 Os2 154.0(6) . . . . ?
C12 C13 Os3 Os2 -102.8(4) . . . . ?
C14 C13 Os3 Os1 104.3(4) . . . . ?
O10 C13 Os3 Os1 -137.7(6) . . . . ?
C12 C13 Os3 Os1 -34.5(3) . . . . ?
C13 C14 Os3 C7 128.1(4) . . . . ?
C15 C14 Os3 C7 24.7(6) . . . . ?
Os2 C14 Os3 C7 -102.8(3) . . . . ?
C13 C14 Os3 C8 -135.5(4) . . . . ?
C15 C14 Os3 C8 121.2(6) . . . . ?
Os2 C14 Os3 C8 -6.3(4) . . . . ?
C13 C14 Os3 C9 38.4(5) . . . . ?
C15 C14 Os3 C9 -65.0(7) . . . . ?
Os2 C14 Os3 C9 167.5(3) . . . . ?
C15 C14 Os3 C13 -103.4(7) . . . . ?
Os2 C14 Os3 C13 129.2(4) . . . . ?
C13 C14 Os3 C12 -25.1(4) . . . . ?
C15 C14 Os3 C12 -128.5(6) . . . . ?
Os2 C14 Os3 C12 104.0(2) . . . . ?
C13 C14 Os3 Os2 -129.2(4) . . . . ?
C15 C14 Os3 Os2 127.5(6) . . . . ?
C13 C14 Os3 Os1 -69.3(4) . . . . ?
C15 C14 Os3 Os1 -172.6(6) . . . . ?
Os2 C14 Os3 Os1 59.89(13) . . . . ?
C13 C12 Os3 C7 -23.2(6) . . . . ?
C11 C12 Os3 C7 73.0(7) . . . . ?
Os1 C12 Os3 C7 -154.6(4) . . . . ?
C13 C12 Os3 C8 153.8(4) . . . . ?
C11 C12 Os3 C8 -110.0(6) . . . . ?
Os1 C12 Os3 C8 22.5(4) . . . . ?
C13 C12 Os3 C9 -109.8(4) . . . . ?
C11 C12 Os3 C9 -13.5(6) . . . . ?
Os1 C12 Os3 C9 118.9(3) . . . . ?
C11 C12 Os3 C13 96.2(6) . . . . ?
Os1 C12 Os3 C13 -131.3(4) . . . . ?
C13 C12 Os3 C14 24.6(4) . . . . ?
C11 C12 Os3 C14 120.8(6) . . . . ?
Os1 C12 Os3 C14 -106.7(3) . . . . ?
C13 C12 Os3 Os2 69.4(4) . . . . ?
C11 C12 Os3 Os2 165.7(5) . . . . ?
Os1 C12 Os3 Os2 -61.89(14) . . . . ?
C13 C12 Os3 Os1 131.3(4) . . . . ?
C11 C12 Os3 Os1 -132.4(6) . . . . ?
C4 Os2 Os3 C7 -4.5(3) . . . . ?
C5 Os2 Os3 C7 103.5(4) . . . . ?
C6 Os2 Os3 C7 -97.2(3) . . . . ?
C14 Os2 Os3 C7 79.0(3) . . . . ?
Os1 Os2 Os3 C7 -172.9(2) . . . . ?
C4 Os2 Os3 C8 92.0(3) . . . . ?
C5 Os2 Os3 C8 -159.9(4) . . . . ?
C6 Os2 Os3 C8 -0.7(3) . . . . ?
C14 Os2 Os3 C8 175.5(3) . . . . ?
Os1 Os2 Os3 C8 -76.4(2) . . . . ?
C4 Os2 Os3 C9 -142.8(12) . . . . ?
C5 Os2 Os3 C9 -34.7(12) . . . . ?
C6 Os2 Os3 C9 124.5(12) . . . . ?
C14 Os2 Os3 C9 -59.3(12) . . . . ?
Os1 Os2 Os3 C9 48.8(12) . . . . ?
C4 Os2 Os3 C13 -111.5(3) . . . . ?
C5 Os2 Os3 C13 -3.4(4) . . . . ?
C6 Os2 Os3 C13 155.8(3) . . . . ?
C14 Os2 Os3 C13 -28.0(3) . . . . ?
Os1 Os2 Os3 C13 80.13(17) . . . . ?
C4 Os2 Os3 C14 -83.5(3) . . . . ?
C5 Os2 Os3 C14 24.6(4) . . . . ?
C6 Os2 Os3 C14 -176.2(3) . . . . ?
Os1 Os2 Os3 C14 108.1(2) . . . . ?
C4 Os2 Os3 C12 -146.8(3) . . . . ?
C5 Os2 Os3 C12 -38.7(4) . . . . ?
C6 Os2 Os3 C12 120.5(3) . . . . ?
C14 Os2 Os3 C12 -63.3(3) . . . . ?
Os1 Os2 Os3 C12 44.80(15) . . . . ?
C4 Os2 Os3 Os1 168.4(2) . . . . ?
C5 Os2 Os3 Os1 -83.5(4) . . . . ?
C6 Os2 Os3 Os1 75.7(2) . . . . ?
C14 Os2 Os3 Os1 -108.1(2) . . . . ?
C1 Os1 Os3 C7 -144.2(7) . . . . ?
C3 Os1 Os3 C7 -54.3(7) . . . . ?
C12 Os1 Os3 C7 127.0(7) . . . . ?
P1 Os1 Os3 C7 111.7(6) . . . . ?
Os2 Os1 Os3 C7 22.0(6) . . . . ?
C1 Os1 Os3 C8 -71.5(3) . . . . ?
C3 Os1 Os3 C8 18.4(3) . . . . ?
C12 Os1 Os3 C8 -160.3(3) . . . . ?
P1 Os1 Os3 C8 -175.7(3) . . . . ?
Os2 Os1 Os3 C8 94.7(2) . . . . ?
C1 Os1 Os3 C9 22.9(3) . . . . ?
C3 Os1 Os3 C9 112.8(3) . . . . ?
C12 Os1 Os3 C9 -65.9(3) . . . . ?
P1 Os1 Os3 C9 -81.3(3) . . . . ?
Os2 Os1 Os3 C9 -170.9(2) . . . . ?
C1 Os1 Os3 C13 116.1(3) . . . . ?
C3 Os1 Os3 C13 -153.9(3) . . . . ?
C12 Os1 Os3 C13 27.4(3) . . . . ?
P1 Os1 Os3 C13 12.0(2) . . . . ?
Os2 Os1 Os3 C13 -77.64(18) . . . . ?
C1 Os1 Os3 C14 150.3(3) . . . . ?
C3 Os1 Os3 C14 -119.8(3) . . . . ?
C12 Os1 Os3 C14 61.5(3) . . . . ?
P1 Os1 Os3 C14 46.1(2) . . . . ?
Os2 Os1 Os3 C14 -43.53(18) . . . . ?
C1 Os1 Os3 C12 88.8(3) . . . . ?
C3 Os1 Os3 C12 178.7(3) . . . . ?
P1 Os1 Os3 C12 -15.3(2) . . . . ?
Os2 Os1 Os3 C12 -105.0(2) . . . . ?
C1 Os1 Os3 Os2 -166.21(19) . . . . ?
C3 Os1 Os3 Os2 -76.3(2) . . . . ?
C12 Os1 Os3 Os2 105.0(2) . . . . ?
P1 Os1 Os3 Os2 89.68(8) . . . . ?
