#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:19:42 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179241 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/61/4316175.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_4316175
loop_
_publ_author_name
'Richard D. Adams'
'William C. Pearl'
_publ_section_title
;
 Osmium-Bismuth Complexes from the Reaction of Os3(CO)11(NCMe) with BiPh3
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7170
_journal_page_last               7175
_journal_paper_doi               10.1021/ic100994t
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C14 H5 Bi O8 Os2'
_chemical_formula_weight         890.56
_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                94.491(2)
_cell_angle_beta                 106.687(2)
_cell_angle_gamma                104.987(2)
_cell_formula_units_Z            2
_cell_length_a                   9.5596(8)
_cell_length_b                   10.0335(8)
_cell_length_c                   10.7117(9)
_cell_measurement_reflns_used    3518
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      24.87
_cell_measurement_theta_min      2.33
_cell_volume                     937.67(14)
_computing_cell_refinement       'SAINT+  V6.45 (Bruker, 2003)'
_computing_data_collection       'SMART V5.632 (Bruker, 2005)'
_computing_data_reduction        'SAINT+  V6.45'
_computing_molecular_graphics    'SHELXTL V6.1 (Sheldrick, 2000)'
_computing_publication_material  'SHELXTL V6.1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker SMART APEX CCD diffractometer'
_diffrn_measurement_method       'omega 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  0.0375
_diffrn_reflns_av_sigmaI/netI    0.0391
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            15199
_diffrn_reflns_theta_full        28.53
_diffrn_reflns_theta_max         28.53
_diffrn_reflns_theta_min         2.01
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    22.913
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.403
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS, Bruker, 1997)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    3.154
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.371
_refine_diff_density_min         -1.058
_refine_diff_density_rms         0.178
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.970
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         4726
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.970
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0328
_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)+(0.0344P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0663
_refine_ls_wR_factor_ref         0.0735
_reflns_number_gt                3548
_reflns_number_total             4726
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100994t_si_001_1.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multi-scan'
changed to 'multi-scan' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        937.67(13)
_cod_database_code               4316175
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
Os1 Os 0.51887(3) 0.20488(3) 0.23403(3) 0.05152(10) Uani 1 1 d . . .
Os2 Os 0.26581(3) 0.33147(3) 0.16946(3) 0.05255(10) Uani 1 1 d . . .
Bi1 Bi 0.21964(3) 0.04694(3) 0.07614(3) 0.04826(9) Uani 1 1 d . . .
O11 O 0.4319(7) 0.1159(7) 0.4779(6) 0.0764(17) Uani 1 1 d . . .
O12 O 0.6827(9) -0.0179(10) 0.2487(8) 0.119(3) Uani 1 1 d . . .
O13 O 0.5792(8) 0.2687(8) -0.0242(7) 0.096(2) Uani 1 1 d . . .
O14 O 0.7702(10) 0.4657(9) 0.3983(8) 0.129(3) Uani 1 1 d . . .
O21 O 0.1965(9) 0.2605(8) 0.4219(7) 0.097(2) Uani 1 1 d . . .
O22 O 0.4812(9) 0.6202(8) 0.3116(8) 0.103(2) Uani 1 1 d . . .
O23 O 0.3082(9) 0.3826(8) -0.0997(7) 0.098(2) Uani 1 1 d . . .
O24 O -0.0518(8) 0.3714(9) 0.0752(9) 0.115(3) Uani 1 1 d . . .
C1 C 0.1448(8) -0.0771(8) 0.2260(7) 0.0491(17) Uani 1 1 d . . .
C2 C 0.0315(8) -0.0592(9) 0.2787(8) 0.059(2) Uani 1 1 d . . .
H2 H -0.0116 0.0129 0.2588 0.071 Uiso 1 1 calc R . .
C3 C -0.0159(9) -0.1468(10) 0.3590(9) 0.071(2) Uani 1 1 d . . .
H3 H -0.0927 -0.1349 0.3918 0.086 Uiso 1 1 calc R . .
C4 C 0.0465(10) -0.2507(10) 0.3920(9) 0.072(2) Uani 1 1 d . . .
H4 H 0.0143 -0.3085 0.4484 0.086 Uiso 1 1 calc R . .
C5 C 0.1587(10) -0.2703(9) 0.3411(9) 0.071(2) Uani 1 1 d . . .
H5 H 0.2018 -0.3420 0.3628 0.085 Uiso 1 1 calc R . .
C6 C 0.2072(9) -0.1832(9) 0.2579(8) 0.062(2) Uani 1 1 d . . .
H6 H 0.2824 -0.1969 0.2236 0.074 Uiso 1 1 calc R . .
C11 C 0.4594(9) 0.1489(8) 0.3872(9) 0.060(2) Uani 1 1 d . . .
C12 C 0.6213(10) 0.0661(11) 0.2416(10) 0.079(3) Uani 1 1 d . . .
C13 C 0.5534(10) 0.2451(10) 0.0686(10) 0.069(2) Uani 1 1 d . . .
C14 C 0.6764(11) 0.3704(12) 0.3381(10) 0.086(3) Uani 1 1 d . . .
C21 C 0.2229(10) 0.2832(9) 0.3285(9) 0.067(2) Uani 1 1 d . . .
C22 C 0.4015(11) 0.5140(11) 0.2587(10) 0.074(3) Uani 1 1 d . . .
C23 C 0.2940(10) 0.3616(9) 0.0001(9) 0.067(2) Uani 1 1 d . . .
C24 C 0.0689(11) 0.3576(10) 0.1092(9) 0.075(2) Uani 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'
Os Os -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Bi Bi -4.1077 10.2566 '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
C12 Os1 C14 103.7(5) . . ?
C12 Os1 C13 91.1(4) . . ?
C14 Os1 C13 93.8(4) . . ?
C12 Os1 C11 89.5(4) . . ?
C14 Os1 C11 92.9(4) . . ?
C13 Os1 C11 172.9(3) . . ?
C12 Os1 Bi1 100.7(3) . . ?
C14 Os1 Bi1 155.6(3) . . ?
C13 Os1 Bi1 86.0(3) . . ?
C11 Os1 Bi1 87.0(2) . . ?
C12 Os1 Os2 159.1(3) . . ?
C14 Os1 Os2 97.1(3) . . ?
C13 Os1 Os2 88.8(3) . . ?
C11 Os1 Os2 88.0(2) . . ?
Bi1 Os1 Os2 58.500(12) . . ?
C24 Os2 C21 88.1(4) . . ?
C24 Os2 C22 104.9(4) . . ?
C21 Os2 C22 92.5(4) . . ?
C24 Os2 C23 90.1(4) . . ?
C21 Os2 C23 174.1(4) . . ?
C22 Os2 C23 93.4(4) . . ?
C24 Os2 Bi1 104.9(3) . . ?
C21 Os2 Bi1 90.6(3) . . ?
C22 Os2 Bi1 150.1(3) . . ?
C23 Os2 Bi1 84.4(3) . . ?
C24 Os2 Os1 163.3(3) . . ?
C21 Os2 Os1 89.4(2) . . ?
C22 Os2 Os1 91.7(3) . . ?
C23 Os2 Os1 90.8(3) . . ?
Bi1 Os2 Os1 58.614(11) . . ?
C1 Bi1 Os2 106.79(19) . . ?
C1 Bi1 Os1 99.83(18) . . ?
Os2 Bi1 Os1 62.886(11) . . ?
C6 C1 C2 118.6(7) . . ?
C6 C1 Bi1 116.8(5) . . ?
C2 C1 Bi1 124.3(6) . . ?
C3 C2 C1 120.3(8) . . ?
C4 C3 C2 121.3(8) . . ?
C3 C4 C5 119.4(8) . . ?
C4 C5 C6 120.1(8) . . ?
C1 C6 C5 120.2(7) . . ?
O11 C11 Os1 176.7(8) . . ?
O12 C12 Os1 178.6(9) . . ?
O13 C13 Os1 177.2(8) . . ?
O14 C14 Os1 178.6(11) . . ?
O21 C21 Os2 176.9(8) . . ?
O22 C22 Os2 179.5(11) . . ?
O23 C23 Os2 177.7(9) . . ?
O24 C24 Os2 178.1(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
Os1 C12 1.892(10) . ?
Os1 C14 1.929(11) . ?
Os1 C13 1.947(9) . ?
Os1 C11 1.961(9) . ?
Os1 Bi1 2.8305(4) . ?
Os1 Os2 2.9512(5) . ?
Os2 C24 1.900(10) . ?
Os2 C21 1.932(9) . ?
Os2 C22 1.933(11) . ?
Os2 C23 1.944(9) . ?
Os2 Bi1 2.8270(5) . ?
Bi1 C1 2.269(7) . ?
O11 C11 1.130(9) . ?
O12 C12 1.141(11) . ?
O13 C13 1.119(10) . ?
O14 C14 1.123(10) . ?
O21 C21 1.127(10) . ?
O22 C22 1.129(10) . ?
O23 C23 1.145(10) . ?
O24 C24 1.154(10) . ?
C1 C6 1.369(10) . ?
C1 C2 1.400(10) . ?
C2 C3 1.362(11) . ?
C3 C4 1.351(12) . ?
C4 C5 1.384(11) . ?
C5 C6 1.388(11) . ?
