#------------------------------------------------------------------------------
#$Date: 2016-03-21 10:17:04 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178643 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/54/4075497.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_4075497
loop_
_publ_author_name
'Adams, Richard D.'
'Captain, Burjor'
'Zhu, Lei'
_publ_section_title
;
 Cluster Fragmentation and Facile Cleavage of Phenyl Groups from the
 SnPh3Ligand in Reactions of Os3(CO)11(SnPh3)(μ-H) with CO and HSnPh3
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              4183
_journal_paper_doi               10.1021/om0603262
_journal_volume                  25
_journal_year                    2006
_chemical_formula_sum            'C39 H31 O3 Os Sn2'
_chemical_formula_weight         975.22
_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                93.7210(10)
_cell_angle_beta                 109.9430(10)
_cell_angle_gamma                110.1460(10)
_cell_formula_units_Z            2
_cell_length_a                   11.2240(3)
_cell_length_b                   11.3303(3)
_cell_length_c                   16.0970(4)
_cell_measurement_reflns_used    5303
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.22
_cell_measurement_theta_min      2.24
_cell_volume                     1767.59(8)
_computing_cell_refinement       'SAINT+  V6.2 (Bruker, 2001)'
_computing_data_collection       'SMART V5.625 (Bruker, 2001)'
_computing_data_reduction        'SAINT+  V6.2'
_computing_molecular_graphics    'SHELXTL V6.1 (Sheldrick, 1997)'
_computing_publication_material  'SHELXTL V6.1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0135
_diffrn_reflns_av_sigmaI/netI    0.0195
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17792
_diffrn_reflns_theta_full        27.88
_diffrn_reflns_theta_max         27.88
_diffrn_reflns_theta_min         1.38
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    5.022
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.773
_exptl_absorpt_correction_type   SADABS
_exptl_absorpt_process_details   '(SADABS, Bruker, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.832
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             930
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.962
_refine_diff_density_min         -1.156
_refine_diff_density_rms         0.179
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.149
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         8382
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.149
_refine_ls_R_factor_all          0.0232
_refine_ls_R_factor_gt           0.0198
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0322P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0496
_refine_ls_wR_factor_ref         0.0572
_reflns_number_gt                7724
_reflns_number_total             8382
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0603262si20060619_051200.cif
_cod_data_source_block           zlos2sns
_cod_depositor_comments
;
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               4075497
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
Os1 Os 0.376046(10) 0.436378(10) 0.406009(7) 0.03176(4) Uani 1 1 d .
Sn1 Sn 0.621693(19) 0.613108(17) 0.427980(13) 0.03409(5) Uani 1 1 d .
Sn2 Sn 0.31018(2) 0.415643(19) 0.224840(13) 0.03960(5) Uani 1 1 d .
O1 O 0.0869(3) 0.2415(3) 0.36378(19) 0.0667(7) Uani 1 1 d .
O2 O 0.4953(3) 0.2335(3) 0.38700(18) 0.0667(7) Uani 1 1 d .
O3 O 0.2685(3) 0.6523(2) 0.39665(19) 0.0646(7) Uani 1 1 d .
C11 C 0.4514(3) 0.3075(3) 0.3944(2) 0.0428(6) Uani 1 1 d .
C12 C 0.1959(3) 0.3120(3) 0.3800(2) 0.0453(7) Uani 1 1 d .
C13 C 0.3102(3) 0.5738(3) 0.4021(2) 0.0416(6) Uani 1 1 d .
C21 C 0.6730(3) 0.8142(3) 0.4289(2) 0.0429(6) Uani 1 1 d .
C22 C 0.5910(4) 0.8762(3) 0.4388(3) 0.0598(9) Uani 1 1 d .
H22 H 0.5094 0.8295 0.4450 0.072 Uiso 1 1 calc R
C23 C 0.6270(5) 1.0062(4) 0.4398(3) 0.0828(13) Uani 1 1 d .
H23 H 0.5697 1.0458 0.4462 0.099 Uiso 1 1 calc R
C24 C 0.7470(6) 1.0760(4) 0.4313(4) 0.109(2) Uani 1 1 d .
H24 H 0.7717 1.1633 0.4317 0.130 Uiso 1 1 calc R
C25 C 0.8308(6) 1.0167(4) 0.4221(4) 0.1043(19) Uani 1 1 d .
H25 H 0.9122 1.0640 0.4158 0.125 Uiso 1 1 calc R
C26 C 0.7954(4) 0.8872(3) 0.4220(3) 0.0648(10) Uani 1 1 d .
H26 H 0.8545 0.8487 0.4173 0.078 Uiso 1 1 calc R
C27 C 0.7561(3) 0.5613(3) 0.37973(19) 0.0409(6) Uani 1 1 d .
C28 C 0.8103(4) 0.4731(4) 0.4138(2) 0.0557(9) Uani 1 1 d .
H28 H 0.7956 0.4412 0.4628 0.067 Uiso 1 1 calc R
C29 C 0.8867(4) 0.4324(4) 0.3750(3) 0.0666(10) Uani 1 1 d .
H29 H 0.9219 0.3729 0.3980 0.080 Uiso 1 1 calc R
C30 C 0.9102(4) 0.4787(4) 0.3038(3) 0.0644(10) Uani 1 1 d .
H30 H 0.9609 0.4506 0.2781 0.077 Uiso 1 1 calc R
C31 C 0.8592(4) 0.5670(4) 0.2698(3) 0.0676(10) Uani 1 1 d .
H31 H 0.8767 0.5998 0.2218 0.081 Uiso 1 1 calc R
C32 C 0.7818(4) 0.6075(3) 0.3069(2) 0.0531(8) Uani 1 1 d .
H32 H 0.7464 0.6665 0.2828 0.064 Uiso 1 1 calc R
C33 C 0.4110(3) 0.5832(3) 0.18013(19) 0.0453(7) Uani 1 1 d .
C34 C 0.4290(4) 0.7051(3) 0.2158(2) 0.0566(8) Uani 1 1 d .
H34 H 0.3941 0.7156 0.2592 0.068 Uiso 1 1 calc R
C35 C 0.4978(5) 0.8126(4) 0.1884(3) 0.0715(11) Uani 1 1 d .
H35 H 0.5087 0.8939 0.2134 0.086 Uiso 1 1 calc R
C36 C 0.5492(4) 0.7981(4) 0.1248(3) 0.0736(11) Uani 1 1 d .
H36 H 0.5964 0.8700 0.1068 0.088 Uiso 1 1 calc R
C37 C 0.5321(5) 0.6802(5) 0.0877(3) 0.0762(12) Uani 1 1 d .
H37 H 0.5660 0.6711 0.0434 0.091 Uiso 1 1 calc R
C38 C 0.4636(4) 0.5715(4) 0.1153(3) 0.0656(10) Uani 1 1 d .
H38 H 0.4535 0.4907 0.0898 0.079 Uiso 1 1 calc R
C39 C 0.3545(4) 0.2672(3) 0.1672(2) 0.0477(7) Uani 1 1 d .
C40 C 0.4880(4) 0.2765(4) 0.1897(3) 0.0656(10) Uani 1 1 d .
H40 H 0.5604 0.3477 0.2312 0.079 Uiso 1 1 calc R
C41 C 0.5160(5) 0.1808(5) 0.1511(3) 0.0804(13) Uani 1 1 d .
H41 H 0.6064 0.1873 0.1683 0.096 Uiso 1 1 calc R
C42 C 0.4125(6) 0.0783(4) 0.0888(3) 0.0817(14) Uani 1 1 d .
H42 H 0.4316 0.0151 0.0626 0.098 Uiso 1 1 calc R
C43 C 0.2792(6) 0.0680(4) 0.0644(3) 0.0894(14) Uani 1 1 d .
H43 H 0.2077 -0.0019 0.0212 0.107 Uiso 1 1 calc R
C44 C 0.2511(5) 0.1620(4) 0.1044(3) 0.0713(11) Uani 1 1 d .
H44 H 0.1602 0.1534 0.0882 0.086 Uiso 1 1 calc R
C45 C 0.0929(3) 0.3673(3) 0.1574(2) 0.0490(7) Uani 1 1 d .
C46 C -0.0042(4) 0.2484(4) 0.1534(3) 0.0630(9) Uani 1 1 d .
H46 H 0.0252 0.1877 0.1802 0.076 Uiso 1 1 calc R
C47 C -0.1432(4) 0.2190(5) 0.1105(3) 0.0803(13) Uani 1 1 d .
H47 H -0.2067 0.1391 0.1086 0.096 Uiso 1 1 calc R
C48 C -0.1878(5) 0.3066(6) 0.0708(3) 0.0892(16) Uani 1 1 d .
H48 H -0.2817 0.2864 0.0420 0.107 Uiso 1 1 calc R
C49 C -0.0958(5) 0.4238(6) 0.0732(3) 0.0817(13) Uani 1 1 d .
H49 H -0.1268 0.4829 0.0454 0.098 Uiso 1 1 calc R
C50 C 0.0445(4) 0.4550(4) 0.1173(2) 0.0618(9) Uani 1 1 d .
H50 H 0.1067 0.5359 0.1199 0.074 Uiso 1 1 calc R
C1S C 0.1870(10) 0.8991(9) 0.2726(8) 0.173(4) Uani 1 1 d .
H1S H 0.2742 0.9150 0.3152 0.207 Uiso 1 1 calc R
C2S C 0.0955(13) 0.9364(7) 0.2961(5) 0.153(4) Uani 1 1 d .
H2S H 0.1215 0.9775 0.3551 0.184 Uiso 1 1 calc R
C3S C -0.0275(9) 0.9142(7) 0.2359(6) 0.122(2) Uani 1 1 d .
H3S H -0.0882 0.9397 0.2523 0.146 Uiso 1 1 calc R
C4S C -0.0651(7) 0.8557(7) 0.1519(6) 0.120(2) Uani 1 1 d .
H4S H -0.1520 0.8415 0.1097 0.144 Uiso 1 1 calc R
C5S C 0.0207(10) 0.8157(7) 0.1257(5) 0.126(2) Uani 1 1 d .
H5S H -0.0074 0.7731 0.0667 0.152 Uiso 1 1 calc R
C6S C 0.1469(9) 0.8397(9) 0.1874(7) 0.145(3) Uani 1 1 d .
H6S H 0.2074 0.8145 0.1706 0.173 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn -0.6537 1.4246 '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
C12 Os1 C13 90.94(13) . .
C12 Os1 C11 93.78(13) . .
C13 Os1 C11 170.80(12) . .
C12 Os1 Sn1 175.18(9) . .
C13 Os1 Sn1 87.68(9) . .
C11 Os1 Sn1 86.96(9) . .
C12 Os1 Sn2 88.54(9) . .
C13 Os1 Sn2 87.35(9) . .
C11 Os1 Sn2 84.88(9) . .
Sn1 Os1 Sn2 86.789(7) . .
C12 Os1 Sn1 75.47(9) . 2_666
C13 Os1 Sn1 98.78(9) . 2_666
C11 Os1 Sn1 90.06(9) . 2_666
Sn1 Os1 Sn1 109.301(6) . 2_666
Sn2 Os1 Sn1 162.888(8) . 2_666
C12 Os1 Os1 128.92(9) . 2_666
C13 Os1 Os1 95.71(9) . 2_666
C11 Os1 Os1 87.47(9) . 2_666
Sn1 Os1 Os1 55.845(5) . 2_666
Sn2 Os1 Os1 142.214(7) . 2_666
Sn1 Os1 Os1 53.456(5) 2_666 2_666
C27 Sn1 C21 106.29(12) . .
C27 Sn1 Os1 120.27(8) . .
C21 Sn1 Os1 126.95(8) . .
C27 Sn1 Os1 117.29(8) . 2_666
C21 Sn1 Os1 110.26(8) . 2_666
Os1 Sn1 Os1 70.699(6) . 2_666
C45 Sn2 C39 106.88(12) . .
C45 Sn2 C33 106.02(13) . .
C39 Sn2 C33 103.92(12) . .
C45 Sn2 Os1 109.35(8) . .
C39 Sn2 Os1 112.83(8) . .
C33 Sn2 Os1 117.15(8) . .
O2 C11 Os1 179.3(3) . .
O1 C12 Os1 177.4(3) . .
O3 C13 Os1 177.5(3) . .
C22 C21 C26 117.7(3) . .
C22 C21 Sn1 122.9(2) . .
C26 C21 Sn1 119.5(2) . .
C21 C22 C23 121.7(4) . .
C24 C23 C22 119.7(4) . .
C23 C24 C25 119.7(4) . .
C24 C25 C26 120.6(4) . .
C25 C26 C21 120.7(4) . .
C28 C27 C32 118.0(3) . .
C28 C27 Sn1 121.9(2) . .
C32 C27 Sn1 119.9(2) . .
C27 C28 C29 120.3(3) . .
C30 C29 C28 120.7(3) . .
C29 C30 C31 120.0(3) . .
C30 C31 C32 120.2(3) . .
C31 C32 C27 120.9(3) . .
C34 C33 C38 117.5(3) . .
C34 C33 Sn2 122.3(2) . .
C38 C33 Sn2 120.2(3) . .
C33 C34 C35 121.7(3) . .
C36 C35 C34 119.5(4) . .
C37 C36 C35 120.4(4) . .
C36 C37 C38 120.5(4) . .
C33 C38 C37 120.4(4) . .
C44 C39 C40 117.7(3) . .
C44 C39 Sn2 121.0(3) . .
C40 C39 Sn2 121.3(3) . .
C39 C40 C41 120.9(4) . .
C42 C41 C40 120.4(4) . .
C41 C42 C43 119.7(4) . .
C42 C43 C44 119.9(4) . .
C39 C44 C43 121.4(4) . .
C50 C45 C46 117.5(3) . .
C50 C45 Sn2 120.8(3) . .
C46 C45 Sn2 121.7(3) . .
C47 C46 C45 121.1(4) . .
C48 C47 C46 120.1(5) . .
C47 C48 C49 120.4(4) . .
C48 C49 C50 120.0(4) . .
C45 C50 C49 120.9(4) . .
C6S C1S C2S 118.4(9) . .
C3S C2S C1S 120.7(8) . .
C2S C3S C4S 119.9(8) . .
C3S C4S C5S 121.5(7) . .
C6S C5S C4S 118.2(7) . .
C1S C6S C5S 121.1(8) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Os1 C12 1.906(3) .
Os1 C13 1.936(3) .
Os1 C11 1.951(3) .
Os1 Sn1 2.6789(2) .
Os1 Sn2 2.7253(2) .
Os1 Sn1 2.7593(2) 2_666
Os1 Os1 3.1471(2) 2_666
Sn1 C27 2.139(3) .
Sn1 C21 2.147(3) .
Sn1 Os1 2.7593(2) 2_666
Sn2 C45 2.150(3) .
Sn2 C39 2.151(3) .
Sn2 C33 2.158(3) .
O1 C12 1.133(4) .
O2 C11 1.127(3) .
O3 C13 1.134(3) .
C21 C22 1.376(4) .
C21 C26 1.385(5) .
C22 C23 1.384(5) .
C23 C24 1.365(7) .
C24 C25 1.369(7) .
C25 C26 1.381(5) .
C27 C28 1.390(4) .
C27 C32 1.393(4) .
C28 C29 1.392(5) .
C29 C30 1.359(5) .
C30 C31 1.371(5) .
C31 C32 1.383(5) .
C33 C34 1.379(5) .
C33 C38 1.384(5) .
C34 C35 1.388(5) .
C35 C36 1.363(6) .
C36 C37 1.349(6) .
C37 C38 1.399(5) .
C39 C44 1.372(5) .
C39 C40 1.380(5) .
C40 C41 1.393(5) .
C41 C42 1.352(7) .
C42 C43 1.371(7) .
C43 C44 1.388(5) .
C45 C50 1.384(5) .
C45 C46 1.392(5) .
C46 C47 1.379(5) .
C47 C48 1.360(7) .
C48 C49 1.361(7) .
C49 C50 1.389(6) .
C1S C6S 1.337(11) .
C1S C2S 1.384(12) .
C2S C3S 1.314(10) .
C3S C4S 1.322(9) .
C4S C5S 1.365(9) .
C5S C6S 1.344(10) .
