#------------------------------------------------------------------------------
#$Date: 2016-03-21 10:23:07 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178648 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/59/4075984.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_4075984
loop_
_publ_author_name
'Shima, Takanori'
'Suzuki, Hiroharu'
_publ_section_title
;
 Heterobimetallic Polyhydride Complex, Cp*Ru(μ-H)4OsCp* (Cp* =
 η5-C5Me5). Synthesis and Reaction with Ethylene
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              3939
_journal_paper_doi               10.1021/om0503996
_journal_volume                  24
_journal_year                    2005
_chemical_formula_sum            'C24 H36 Os Ru'
_chemical_formula_weight         615.80
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                102.120(6)
_cell_angle_beta                 104.308(5)
_cell_angle_gamma                108.693(3)
_cell_formula_units_Z            1
_cell_length_a                   6.8764(6)
_cell_length_b                   8.6346(6)
_cell_length_c                   10.6228(15)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    243(2)
_cell_measurement_theta_max      18
_cell_measurement_theta_min      12
_cell_volume                     549.44(10)
_computing_molecular_graphics    'ORTEX (P.McArdle, 1995)'
_computing_publication_material  'SHELXL-97/2 (Sheldrick,1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      243(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'imaging plate area detector'
_diffrn_measurement_method       'Imaging Plate'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0192
_diffrn_reflns_av_sigmaI/netI    0.0179
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3913
_diffrn_reflns_theta_full        27.44
_diffrn_reflns_theta_max         27.44
_diffrn_reflns_theta_min         2.79
_exptl_absorpt_coefficient_mu    6.468
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.861
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             300
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.806
_refine_diff_density_min         -1.123
_refine_diff_density_rms         0.144
_refine_ls_extinction_coef       0.071(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.163
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     124
_refine_ls_number_reflns         2440
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.163
_refine_ls_R_factor_all          0.0234
_refine_ls_R_factor_gt           0.0226
_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)+(0.0375P)²+0.2490P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0548
_refine_ls_wR_factor_ref         0.0552
_reflns_number_gt                2375
_reflns_number_total             2440
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0503996si20050519_022024.cif
_cod_data_source_block           Ru-Os-bis-ethylidyne_complex_4
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4075984
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_group
Os1 Os 0.029048(18) 0.969398(15) 0.384717(11) 0.02017(9) Uani 0.50 1 d P 1
Ru1A Ru 0.029048(18) 0.969398(15) 0.384717(11) 0.02017(9) Uani 0.50 1 d P 2
C1 C 0.0973(5) 1.1808(4) 0.5215(3) 0.0273(5) Uani 1 1 d . .
C2 C 0.2029(8) 1.3686(4) 0.5447(4) 0.0514(10) Uani 1 1 d . .
C3 C 0.0828(5) 1.0679(4) 0.2086(3) 0.0297(6) Uani 1 1 d . .
C4 C 0.2651(5) 1.0316(4) 0.2707(3) 0.0265(5) Uani 1 1 d . .
C5 C 0.1872(5) 0.8500(4) 0.2543(3) 0.0250(5) Uani 1 1 d . .
C6 C -0.0412(5) 0.7759(4) 0.1802(3) 0.0270(6) Uani 1 1 d . .
C7 C -0.1084(5) 0.9107(4) 0.1582(3) 0.0299(6) Uani 1 1 d . .
C8 C 0.0851(8) 1.2352(5) 0.1905(4) 0.0466(9) Uani 1 1 d . .
H8A H 0.2250 1.3268 0.2475 0.070 Uiso 1 1 calc R .
H8B H -0.0303 1.2591 0.2169 0.070 Uiso 1 1 calc R .
H8C H 0.0619 1.2284 0.0953 0.070 Uiso 1 1 calc R .
C9 C 0.4988(6) 1.1577(5) 0.3324(4) 0.0385(7) Uani 1 1 d . .
H9A H 0.5865 1.1068 0.3816 0.058 Uiso 1 1 calc R .
H9B H 0.5087 1.2616 0.3952 0.058 Uiso 1 1 calc R .
H9C H 0.5521 1.1861 0.2603 0.058 Uiso 1 1 calc R .
C10 C 0.3252(6) 0.7524(5) 0.2942(3) 0.0358(7) Uani 1 1 d . .
H10A H 0.4652 0.8320 0.3617 0.054 Uiso 1 1 calc R .
H10B H 0.3477 0.6938 0.2139 0.054 Uiso 1 1 calc R .
H10C H 0.2519 0.6683 0.3327 0.054 Uiso 1 1 calc R .
C11 C -0.1844(6) 0.5876(5) 0.1271(3) 0.0423(8) Uani 1 1 d . .
H11A H -0.3306 0.5723 0.1268 0.063 Uiso 1 1 calc R .
H11B H -0.1259 0.5291 0.1856 0.063 Uiso 1 1 calc R .
H11C H -0.1894 0.5397 0.0347 0.063 Uiso 1 1 calc R .
C12 C -0.3321(6) 0.8880(6) 0.0732(4) 0.0464(9) Uani 1 1 d . .
H12A H -0.4359 0.7735 0.0588 0.070 Uiso 1 1 calc R .
H12B H -0.3294 0.9027 -0.0145 0.070 Uiso 1 1 calc R .
H12C H -0.3751 0.9733 0.1206 0.070 Uiso 1 1 calc R .
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'
Ru Ru -1.2594 0.8363 '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
C1 Os1 C1 96.46(12) . 2_576
C1 Os1 C7 126.45(12) . .
C1 Os1 C7 122.21(13) 2_576 .
C1 Os1 C5 139.22(12) . .
C1 Os1 C5 111.13(11) 2_576 .
C7 Os1 C5 62.06(10) . .
C1 Os1 C4 106.03(12) . .
C1 Os1 C4 146.22(12) 2_576 .
C7 Os1 C4 62.07(11) . .
C5 Os1 C4 37.39(10) . .
C1 Os1 C3 100.54(12) . .
C1 Os1 C3 159.27(13) 2_576 .
C7 Os1 C3 37.12(12) . .
C5 Os1 C3 61.72(11) . .
C4 Os1 C3 36.73(11) . .
C1 Os1 C6 161.46(12) . .
C1 Os1 C6 100.99(12) 2_576 .
C7 Os1 C6 36.78(11) . .
C5 Os1 C6 36.73(10) . .
C4 Os1 C6 61.49(11) . .
C3 Os1 C6 61.11(11) . .
C1 Os1 Os1 48.28(9) . 2_576
C1 Os1 Os1 48.18(9) 2_576 2_576
C7 Os1 Os1 147.79(8) . 2_576
C5 Os1 Os1 147.01(7) . 2_576
C4 Os1 Os1 146.25(7) . 2_576
C3 Os1 Os1 147.12(8) . 2_576
C6 Os1 Os1 148.69(8) . 2_576
C2 C1 Os1 137.9(2) . .
C2 C1 Ru1A 138.5(2) . 2_576
Os1 C1 Ru1A 83.54(11) . 2_576
C2 C1 Os1 138.5(2) . 2_576
Os1 C1 Os1 83.54(11) . 2_576
Ru1A C1 Os1 0.000(7) 2_576 2_576
C4 C3 C7 107.9(3) . .
C4 C3 C8 127.4(3) . .
C7 C3 C8 124.6(3) . .
C4 C3 Os1 70.87(15) . .
C7 C3 Os1 70.01(16) . .
C8 C3 Os1 127.1(2) . .
C3 C4 C5 107.8(3) . .
C3 C4 C9 125.9(3) . .
C5 C4 C9 126.1(3) . .
C3 C4 Os1 72.39(16) . .
C5 C4 Os1 70.93(15) . .
C9 C4 Os1 125.8(2) . .
C6 C5 C4 107.8(2) . .
C6 C5 C10 125.7(3) . .
C4 C5 C10 126.2(3) . .
C6 C5 Os1 72.93(15) . .
C4 C5 Os1 71.69(15) . .
C10 C5 Os1 126.0(2) . .
C7 C6 C5 108.3(3) . .
C7 C6 C11 125.6(3) . .
C5 C6 C11 126.0(3) . .
C7 C6 Os1 70.02(15) . .
C5 C6 Os1 70.34(15) . .
C11 C6 Os1 128.1(2) . .
C6 C7 C3 108.0(3) . .
C6 C7 C12 125.9(3) . .
C3 C7 C12 125.1(3) . .
C6 C7 Os1 73.21(15) . .
C3 C7 Os1 72.87(16) . .
C12 C7 Os1 128.5(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Os1 C1 1.914(3) .
Os1 C1 1.917(3) 2_576
Os1 C7 2.235(3) .
Os1 C5 2.243(3) .
Os1 C4 2.253(3) .
Os1 C3 2.273(3) .
Os1 C6 2.277(3) .
Os1 Os1 2.5521(4) 2_576
C1 C2 1.485(4) .
C1 Ru1A 1.917(3) 2_576
C1 Os1 1.917(3) 2_576
C3 C4 1.426(4) .
C3 C7 1.435(5) .
C3 C8 1.493(4) .
C4 C5 1.441(4) .
C4 C9 1.502(4) .
C5 C6 1.424(4) .
C5 C10 1.502(4) .
C6 C7 1.424(4) .
C6 C11 1.498(4) .
C7 C12 1.505(4) .
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_4
C1 Os1 C1 C2 178.3(5) 2_576 .
C7 Os1 C1 C2 -43.1(5) . .
C5 Os1 C1 C2 44.9(5) . .
C4 Os1 C1 C2 23.8(4) . .
C3 Os1 C1 C2 -13.6(4) . .
C6 Os1 C1 C2 -21.4(7) . .
Os1 Os1 C1 C2 178.3(5) 2_576 .
C1 Os1 C1 Ru1A 0.0 2_576 2_576
C7 Os1 C1 Ru1A 138.65(12) . 2_576
C5 Os1 C1 Ru1A -133.38(13) . 2_576
C4 Os1 C1 Ru1A -154.54(10) . 2_576
C3 Os1 C1 Ru1A 168.09(11) . 2_576
C6 Os1 C1 Ru1A 160.3(3) . 2_576
Os1 Os1 C1 Ru1A 0.0 2_576 2_576
C1 Os1 C1 Os1 0.0 2_576 2_576
C7 Os1 C1 Os1 138.65(12) . 2_576
C5 Os1 C1 Os1 -133.38(13) . 2_576
C4 Os1 C1 Os1 -154.54(10) . 2_576
C3 Os1 C1 Os1 168.09(11) . 2_576
C6 Os1 C1 Os1 160.3(3) . 2_576
C1 Os1 C3 C4 102.7(2) . .
C1 Os1 C3 C4 -112.7(3) 2_576 .
C7 Os1 C3 C4 -118.2(3) . .
C5 Os1 C3 C4 -38.03(17) . .
C6 Os1 C3 C4 -80.09(19) . .
Os1 Os1 C3 C4 119.21(17) 2_576 .
C1 Os1 C3 C7 -139.07(18) . .
C1 Os1 C3 C7 5.5(4) 2_576 .
C5 Os1 C3 C7 80.17(19) . .
C4 Os1 C3 C7 118.2(3) . .
C6 Os1 C3 C7 38.12(17) . .
Os1 Os1 C3 C7 -122.58(17) 2_576 .
C1 Os1 C3 C8 -20.2(3) . .
C1 Os1 C3 C8 124.3(4) 2_576 .
C7 Os1 C3 C8 118.8(4) . .
C5 Os1 C3 C8 -161.0(4) . .
C4 Os1 C3 C8 -123.0(4) . .
C6 Os1 C3 C8 156.9(4) . .
Os1 Os1 C3 C8 -3.8(4) 2_576 .
C7 C3 C4 C5 2.0(3) . .
C8 C3 C4 C5 -174.9(3) . .
Os1 C3 C4 C5 62.49(18) . .
C7 C3 C4 C9 177.7(3) . .
C8 C3 C4 C9 0.8(5) . .
Os1 C3 C4 C9 -121.8(3) . .
C7 C3 C4 Os1 -60.50(19) . .
C8 C3 C4 Os1 122.6(3) . .
C1 Os1 C4 C3 -86.2(2) . .
C1 Os1 C4 C3 144.0(2) 2_576 .
C7 Os1 C4 C3 37.01(18) . .
C5 Os1 C4 C3 116.7(2) . .
C6 Os1 C4 C3 78.97(19) . .
Os1 Os1 C4 C3 -121.45(17) 2_576 .
C1 Os1 C4 C5 157.16(17) . .
C1 Os1 C4 C5 27.3(3) 2_576 .
C7 Os1 C4 C5 -79.66(18) . .
C3 Os1 C4 C5 -116.7(2) . .
C6 Os1 C4 C5 -37.71(16) . .
Os1 Os1 C4 C5 121.87(16) 2_576 .
C1 Os1 C4 C9 35.9(3) . .
C1 Os1 C4 C9 -93.9(3) 2_576 .
C7 Os1 C4 C9 159.1(3) . .
C5 Os1 C4 C9 -121.3(3) . .
C3 Os1 C4 C9 122.0(4) . .
C6 Os1 C4 C9 -159.0(3) . .
Os1 Os1 C4 C9 0.6(4) 2_576 .
C3 C4 C5 C6 1.0(3) . .
C9 C4 C5 C6 -174.7(3) . .
Os1 C4 C5 C6 64.46(18) . .
C3 C4 C5 C10 174.9(3) . .
C9 C4 C5 C10 -0.8(4) . .
Os1 C4 C5 C10 -121.6(3) . .
C3 C4 C5 Os1 -63.45(19) . .
C9 C4 C5 Os1 120.9(3) . .
C1 Os1 C5 C6 -150.9(2) . .
C1 Os1 C5 C6 79.9(2) 2_576 .
C7 Os1 C5 C6 -36.37(18) . .
C4 Os1 C5 C6 -116.0(2) . .
C3 Os1 C5 C6 -78.67(19) . .
Os1 Os1 C5 C6 124.02(16) 2_576 .
C1 Os1 C5 C4 -34.8(2) . .
C1 Os1 C5 C4 -164.11(17) 2_576 .
C7 Os1 C5 C4 79.67(18) . .
C3 Os1 C5 C4 37.36(17) . .
C6 Os1 C5 C4 116.0(2) . .
Os1 Os1 C5 C4 -119.95(16) 2_576 .
C1 Os1 C5 C10 87.1(3) . .
C1 Os1 C5 C10 -42.2(3) 2_576 .
C7 Os1 C5 C10 -158.4(3) . .
C4 Os1 C5 C10 121.9(3) . .
C3 Os1 C5 C10 159.3(3) . .
C6 Os1 C5 C10 -122.1(3) . .
Os1 Os1 C5 C10 2.0(4) 2_576 .
C4 C5 C6 C7 -3.7(3) . .
C10 C5 C6 C7 -177.6(3) . .
Os1 C5 C6 C7 59.99(19) . .
C4 C5 C6 C11 173.0(3) . .
C10 C5 C6 C11 -0.9(5) . .
Os1 C5 C6 C11 -123.3(3) . .
C4 C5 C6 Os1 -63.64(18) . .
C10 C5 C6 Os1 122.4(3) . .
C1 Os1 C6 C7 -29.7(4) . .
C1 Os1 C6 C7 130.32(19) 2_576 .
C5 Os1 C6 C7 -119.0(3) . .
C4 Os1 C6 C7 -80.58(19) . .
C3 Os1 C6 C7 -38.48(18) . .
Os1 Os1 C6 C7 121.32(18) 2_576 .
C1 Os1 C6 C5 89.2(4) . .
C1 Os1 C6 C5 -110.72(19) 2_576 .
C7 Os1 C6 C5 119.0(3) . .
C4 Os1 C6 C5 38.38(16) . .
C3 Os1 C6 C5 80.48(19) . .
Os1 Os1 C6 C5 -119.72(17) 2_576 .
C1 Os1 C6 C11 -149.9(4) . .
C1 Os1 C6 C11 10.2(3) 2_576 .
C7 Os1 C6 C11 -120.1(4) . .
C5 Os1 C6 C11 120.9(4) . .
C4 Os1 C6 C11 159.3(3) . .
C3 Os1 C6 C11 -158.6(3) . .
Os1 Os1 C6 C11 1.2(4) 2_576 .
C5 C6 C7 C3 4.9(3) . .
C11 C6 C7 C3 -171.8(3) . .
Os1 C6 C7 C3 65.08(19) . .
C5 C6 C7 C12 174.0(3) . .
C11 C6 C7 C12 -2.7(5) . .
Os1 C6 C7 C12 -125.8(3) . .
C5 C6 C7 Os1 -60.19(18) . .
C11 C6 C7 Os1 123.1(3) . .
C4 C3 C7 C6 -4.2(3) . .
C8 C3 C7 C6 172.8(3) . .
Os1 C3 C7 C6 -65.30(19) . .
C4 C3 C7 C12 -173.5(3) . .
C8 C3 C7 C12 3.5(5) . .
Os1 C3 C7 C12 125.4(3) . .
C4 C3 C7 Os1 61.05(19) . .
C8 C3 C7 Os1 -121.9(3) . .
C1 Os1 C7 C6 168.69(17) . .
C1 Os1 C7 C6 -62.2(2) 2_576 .
C5 Os1 C7 C6 36.32(17) . .
C4 Os1 C7 C6 78.87(18) . .
C3 Os1 C7 C6 115.5(3) . .
Os1 Os1 C7 C6 -123.62(17) 2_576 .
C1 Os1 C7 C3 53.2(2) . .
C1 Os1 C7 C3 -177.69(17) 2_576 .
C5 Os1 C7 C3 -79.17(19) . .
C4 Os1 C7 C3 -36.62(17) . .
C6 Os1 C7 C3 -115.5(3) . .
Os1 Os1 C7 C3 120.89(18) 2_576 .
C1 Os1 C7 C12 -68.4(4) . .
C1 Os1 C7 C12 60.7(4) 2_576 .
C5 Os1 C7 C12 159.2(4) . .
C4 Os1 C7 C12 -158.2(4) . .
C3 Os1 C7 C12 -121.6(4) . .
C6 Os1 C7 C12 122.9(4) . .
Os1 Os1 C7 C12 -0.7(4) 2_576 .
