#------------------------------------------------------------------------------
#$Date: 2016-03-21 09:00:11 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178615 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/26/4072664.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_4072664
loop_
_publ_author_name
'Gross, Christopher L.'
'Girolami, Gregory S.'
_publ_section_title
;
 Synthesis and Characterization of Osmium Polyhydrides. X-ray Crystal
 Structures of (C5Me5)OsH5and (C5Me5)2Os2H4
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              160
_journal_paper_doi               10.1021/om060920b
_journal_volume                  26
_journal_year                    2007
_chemical_formula_moiety         'C20 H34 Os2'
_chemical_formula_sum            'C20 H34 Os2'
_chemical_formula_weight         654.87
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 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                 108.72(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.098(2)
_cell_length_b                   8.529(2)
_cell_length_c                   12.334(2)
_cell_measurement_temperature    198(2)
_cell_volume                     1006.1(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      198(2)
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 0.959
_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  0.0534
_diffrn_reflns_av_sigmaI/netI    0.0387
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            6455
_diffrn_reflns_theta_full        28.36
_diffrn_reflns_theta_max         28.36
_diffrn_reflns_theta_min         2.13
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    12.614
_exptl_absorpt_correction_T_max  0.7865
_exptl_absorpt_correction_T_min  0.1380
_exptl_absorpt_correction_type   integration
_exptl_crystal_density_diffrn    2.162
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             612
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.567
_refine_diff_density_min         -1.564
_refine_diff_density_rms         0.172
_refine_ls_extinction_coef       0.0022(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     111
_refine_ls_number_reflns         2426
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0297
_refine_ls_R_factor_gt           0.0246
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0250P)²+1.8200P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0599
_refine_ls_wR_factor_ref         0.0631
_reflns_number_gt                2159
_reflns_number_total             2426
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060920bsi20061031_085421.cif
_cod_data_source_block           osabs24
_cod_depositor_comments
;
The following automatic conversions were performed:

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

'_exptl_absorpt_correction_type' value 'Integration'
changed to 'integration' 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_cell_volume        1006.1(3)
_cod_original_sg_symbol_H-M      'P 2/c'
_cod_database_code               4072664
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, 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
Os Os 0.109370(15) 0.238099(19) 0.226517(13) 0.01916(9) Uani 1 1 d D
C1 C 0.3121(4) 0.1252(6) 0.2591(4) 0.0252(9) Uani 1 1 d .
C2 C 0.2350(4) 0.1152(5) 0.1386(4) 0.0234(9) Uani 1 1 d .
C3 C 0.2100(5) 0.2706(5) 0.0941(4) 0.0260(9) Uani 1 1 d .
C4 C 0.2704(5) 0.3755(6) 0.1863(4) 0.0312(10) Uani 1 1 d .
C5 C 0.3335(4) 0.2867(6) 0.2874(4) 0.0283(10) Uani 1 1 d .
C6 C 0.3683(5) -0.0112(7) 0.3355(4) 0.0396(12) Uani 1 1 d .
H6A H 0.4626 -0.0358 0.3344 0.048 Uiso 1 1 calc R
H6B H 0.3073 -0.1021 0.3085 0.048 Uiso 1 1 calc R
H6C H 0.3718 0.0147 0.4138 0.048 Uiso 1 1 calc R
C7 C 0.1969(5) -0.0343(6) 0.0720(4) 0.0340(11) Uani 1 1 d .
H7A H 0.2808 -0.0802 0.0613 0.041 Uiso 1 1 calc R
H7B H 0.1279 -0.0123 -0.0029 0.041 Uiso 1 1 calc R
H7C H 0.1572 -0.1081 0.1140 0.041 Uiso 1 1 calc R
C8 C 0.1417(5) 0.3147(8) -0.0289(4) 0.0419(13) Uani 1 1 d .
H8A H 0.2120 0.3167 -0.0682 0.050 Uiso 1 1 calc R
H8B H 0.0991 0.4188 -0.0332 0.050 Uiso 1 1 calc R
H8C H 0.0692 0.2376 -0.0658 0.050 Uiso 1 1 calc R
C9 C 0.2743(7) 0.5520(6) 0.1764(6) 0.0542(17) Uani 1 1 d .
H9A H 0.3619 0.5836 0.1645 0.065 Uiso 1 1 calc R
H9C H 0.2684 0.6000 0.2469 0.065 Uiso 1 1 calc R
H9B H 0.1950 0.5870 0.1113 0.065 Uiso 1 1 calc R
C10 C 0.4153(5) 0.3491(8) 0.4021(5) 0.0484(15) Uani 1 1 d .
H10C H 0.5144 0.3547 0.4084 0.058 Uiso 1 1 calc R
H10A H 0.4038 0.2795 0.4617 0.058 Uiso 1 1 calc R
H10B H 0.3814 0.4542 0.4118 0.058 Uiso 1 1 calc R
H1 H 0.0000 0.372(5) 0.2500 0.073 Uiso 1 2 d SD
H3 H -0.062(3) 0.235(7) 0.156(3) 0.073 Uiso 1 1 d D
H2 H 0.0000 0.106(5) 0.2500 0.073 Uiso 1 2 d SD
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'
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 Os C2 38.61(16) . .
C1 Os C5 38.00(17) . .
C2 Os C5 63.83(17) . .
C1 Os C4 63.62(19) . .
C2 Os C4 63.36(18) . .
C5 Os C4 38.02(19) . .
C1 Os C3 64.03(17) . .
C2 Os C3 37.94(16) . .
C5 Os C3 63.69(18) . .
C4 Os C3 37.80(17) . .
C1 Os Os 144.97(12) . 2
C2 Os Os 145.76(12) . 2
C5 Os Os 146.09(12) . 2
C4 Os Os 147.55(13) . 2
C3 Os Os 147.07(13) . 2
C1 Os H1 154.2(6) . .
C2 Os H1 158.8(6) . .
C5 Os H1 118.5(8) . .
C4 Os H1 104.6(11) . .
C3 Os H1 121.9(8) . .
Os Os H1 43.0(10) 2 .
C1 Os H3 147.6(17) . .
C2 Os H3 113.7(13) . .
C5 Os H3 165.5(16) . .
C4 Os H3 127.5(15) . .
C3 Os H3 105.1(10) . .
Os Os H3 42.7(10) 2 .
H1 Os H3 58.1(18) . .
C1 Os H2 107.7(10) . .
C2 Os H2 106.5(10) . .
C5 Os H2 137.7(7) . .
C4 Os H2 169.7(10) . .
C3 Os H2 134.7(7) . .
Os Os H2 42.6(10) 2 .
H1 Os H2 85.6(15) . .
H3 Os H2 56.6(18) . .
C5 C1 C2 107.5(4) . .
C5 C1 C6 127.2(4) . .
C2 C1 C6 125.1(4) . .
C5 C1 Os 71.1(2) . .
C2 C1 Os 70.8(2) . .
C6 C1 Os 127.3(3) . .
C3 C2 C1 108.2(4) . .
C3 C2 C7 126.7(4) . .
C1 C2 C7 125.0(4) . .
C3 C2 Os 71.7(2) . .
C1 C2 Os 70.6(2) . .
C7 C2 Os 126.4(3) . .
C4 C3 C2 107.5(4) . .
C4 C3 C8 126.2(5) . .
C2 C3 C8 126.2(5) . .
C4 C3 Os 70.6(2) . .
C2 C3 Os 70.4(2) . .
C8 C3 Os 127.6(3) . .
C3 C4 C5 108.8(4) . .
C3 C4 C9 125.3(5) . .
C5 C4 C9 125.7(5) . .
C3 C4 Os 71.6(3) . .
C5 C4 Os 70.9(2) . .
C9 C4 Os 126.3(3) . .
C1 C5 C4 108.0(4) . .
C1 C5 C10 125.1(5) . .
C4 C5 C10 126.8(5) . .
C1 C5 Os 70.9(2) . .
C4 C5 Os 71.1(3) . .
C10 C5 Os 126.3(3) . .
C1 C6 H6A 109.5 . .
C1 C6 H6B 109.5 . .
H6A C6 H6B 109.5 . .
C1 C6 H6C 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
C2 C7 H7A 109.5 . .
C2 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
C2 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
C3 C8 H8A 109.5 . .
C3 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
C3 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
C4 C9 H9A 109.5 . .
C4 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
C4 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
H9C C9 H9B 109.5 . .
C5 C10 H10C 109.5 . .
C5 C10 H10A 109.5 . .
H10C C10 H10A 109.5 . .
C5 C10 H10B 109.5 . .
H10C C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Os C1 2.180(4) .
Os C2 2.183(4) .
Os C5 2.184(4) .
Os C4 2.187(4) .
Os C3 2.201(4) .
Os Os 2.4568(6) 2
Os H1 1.68(3) .
Os H3 1.67(3) .
Os H2 1.67(3) .
C1 C5 1.421(6) .
C1 C2 1.442(6) .
C1 C6 1.490(7) .
C2 C3 1.425(6) .
C2 C7 1.498(6) .
C3 C4 1.421(7) .
C3 C8 1.499(7) .
C4 C5 1.423(7) .
C4 C9 1.512(7) .
C5 C10 1.489(7) .
C6 H6A 0.9800 .
C6 H6B 0.9800 .
C6 H6C 0.9800 .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
C9 H9A 0.9800 .
C9 H9C 0.9800 .
C9 H9B 0.9800 .
C10 H10C 0.9800 .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
