#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:19:42 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179241 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/61/4316176.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_4316176
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            'C16 H10 O4 Os'
_chemical_formula_weight         456.44
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.7405(3)
_cell_length_b                   12.6633(5)
_cell_length_c                   15.6545(6)
_cell_measurement_reflns_used    6413
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      2.60
_cell_volume                     1534.46(10)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0410
_diffrn_reflns_av_sigmaI/netI    0.0309
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            24383
_diffrn_reflns_theta_full        28.33
_diffrn_reflns_theta_max         28.33
_diffrn_reflns_theta_min         2.07
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    8.321
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.736
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS, Bruker, 1997)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.976
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.870
_refine_diff_density_min         -0.595
_refine_diff_density_rms         0.097
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.007(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         3815
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_gt           0.0265
_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)+(0.0253P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0513
_refine_ls_wR_factor_ref         0.0536
_reflns_number_gt                3396
_reflns_number_total             3815
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100994t_si_001_2.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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_database_code               4316176
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -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 0.94356(2) 0.450520(16) 0.159521(12) 0.04729(6) Uani 1 1 d . . .
O13 O 0.7511(7) 0.4789(4) 0.3296(3) 0.0934(15) Uani 1 1 d . . .
O14 O 1.0306(6) 0.2138(3) 0.1852(3) 0.0746(12) Uani 1 1 d . . .
O15 O 1.0444(5) 0.4555(3) -0.0310(2) 0.0687(9) Uani 1 1 d . . .
O16 O 1.2911(6) 0.5345(5) 0.2295(4) 0.1068(17) Uani 1 1 d . . .
C1 C 0.6946(6) 0.3949(4) 0.1122(3) 0.0464(11) Uani 1 1 d . . .
C2 C 0.6191(6) 0.4361(5) 0.0388(3) 0.0527(12) Uani 1 1 d . . .
H2 H 0.6708 0.4928 0.0111 0.063 Uiso 1 1 calc R . .
C3 C 0.4665(7) 0.3932(5) 0.0062(4) 0.0626(15) Uani 1 1 d . . .
H3 H 0.4179 0.4217 -0.0430 0.075 Uiso 1 1 calc R . .
C4 C 0.3877(7) 0.3099(5) 0.0457(4) 0.0686(17) Uani 1 1 d . . .
H4 H 0.2878 0.2807 0.0225 0.082 Uiso 1 1 calc R . .
C5 C 0.4555(8) 0.2698(4) 0.1187(4) 0.0667(15) Uani 1 1 d . . .
H5 H 0.4000 0.2150 0.1471 0.080 Uiso 1 1 calc R . .
C6 C 0.6097(6) 0.3115(4) 0.1510(4) 0.0549(12) Uani 1 1 d . . .
H6 H 0.6567 0.2821 0.2003 0.066 Uiso 1 1 calc R . .
C7 C 0.8696(7) 0.6131(4) 0.1336(3) 0.0525(13) Uani 1 1 d . . .
C8 C 0.7060(8) 0.6521(5) 0.1518(4) 0.0686(15) Uani 1 1 d . . .
H8 H 0.6224 0.6071 0.1741 0.082 Uiso 1 1 calc R . .
C9 C 0.6658(11) 0.7570(6) 0.1374(4) 0.088(2) Uani 1 1 d . . .
H9 H 0.5567 0.7819 0.1518 0.106 Uiso 1 1 calc R . .
C10 C 0.7825(14) 0.8239(6) 0.1026(5) 0.102(3) Uani 1 1 d . . .
H10 H 0.7534 0.8942 0.0933 0.123 Uiso 1 1 calc R . .
C11 C 0.9438(14) 0.7877(5) 0.0811(4) 0.091(2) Uani 1 1 d . . .
H11 H 1.0242 0.8328 0.0563 0.110 Uiso 1 1 calc R . .
C12 C 0.9855(9) 0.6826(5) 0.0969(4) 0.0724(18) Uani 1 1 d . . .
H12 H 1.0949 0.6584 0.0823 0.087 Uiso 1 1 calc R . .
C13 C 0.8283(8) 0.4671(4) 0.2693(4) 0.0609(14) Uani 1 1 d . . .
C14 C 1.0015(6) 0.3018(5) 0.1777(3) 0.0548(13) Uani 1 1 d . . .
C15 C 1.0134(6) 0.4509(4) 0.0402(4) 0.0524(11) Uani 1 1 d . . .
C16 C 1.1655(9) 0.5034(5) 0.2033(4) 0.0717(16) 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'
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
C15 Os1 C13 167.1(2) . . ?
C15 Os1 C14 94.5(2) . . ?
C13 Os1 C14 94.6(2) . . ?
C15 Os1 C16 95.2(2) . . ?
C13 Os1 C16 93.2(2) . . ?
C14 Os1 C16 94.4(2) . . ?
C15 Os1 C7 83.7(2) . . ?
C13 Os1 C7 86.7(2) . . ?
C14 Os1 C7 176.8(2) . . ?
C16 Os1 C7 88.4(2) . . ?
C15 Os1 C1 85.43(18) . . ?
C13 Os1 C1 85.9(2) . . ?
C14 Os1 C1 86.61(19) . . ?
C16 Os1 C1 178.7(2) . . ?
C7 Os1 C1 90.6(2) . . ?
C6 C1 C2 116.7(5) . . ?
C6 C1 Os1 121.1(4) . . ?
C2 C1 Os1 122.0(4) . . ?
C1 C2 C3 120.8(5) . . ?
C4 C3 C2 120.9(6) . . ?
C5 C4 C3 119.8(5) . . ?
C4 C5 C6 119.6(5) . . ?
C1 C6 C5 122.3(5) . . ?
C12 C7 C8 116.8(5) . . ?
C12 C7 Os1 120.7(4) . . ?
C8 C7 Os1 122.5(4) . . ?
C9 C8 C7 120.9(6) . . ?
C10 C9 C8 121.2(7) . . ?
C9 C10 C11 119.8(7) . . ?
C10 C11 C12 119.2(8) . . ?
C7 C12 C11 122.2(7) . . ?
O13 C13 Os1 175.0(5) . . ?
O14 C14 Os1 176.9(5) . . ?
O15 C15 Os1 175.2(5) . . ?
O16 C16 Os1 178.8(7) . . ?
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 C15 1.945(6) . ?
Os1 C13 1.947(6) . ?
Os1 C14 1.957(6) . ?
Os1 C16 1.967(7) . ?
Os1 C7 2.175(5) . ?
Os1 C1 2.182(5) . ?
O13 C13 1.128(7) . ?
O14 C14 1.143(6) . ?
O15 C15 1.141(6) . ?
O16 C16 1.127(7) . ?
C1 C6 1.385(7) . ?
C1 C2 1.390(7) . ?
C2 C3 1.397(7) . ?
C3 C4 1.366(8) . ?
C4 C5 1.357(9) . ?
C5 C6 1.399(8) . ?
C7 C12 1.381(8) . ?
C7 C8 1.389(8) . ?
C8 C9 1.382(8) . ?
C9 C10 1.353(11) . ?
C10 C11 1.372(11) . ?
C11 C12 1.391(9) . ?
