#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/66/4076673.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_4076673
loop_
_publ_author_name
'Deng, Mingli'
'Leong, Weng Kee'
_publ_section_title
;
 Reactions of the Triosmium−Antimony Cluster
 Os3(μ-SbPh2)(μ-H)(μ3,η2-C6H4)(CO)9with Alkynes:  C−C
 Bond Coupling to a Cluster-Bound Phenylene and Catalytic Alkyne
 Cyclotrimerization
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1221
_journal_paper_doi               10.1021/om010911x
_journal_volume                  21
_journal_year                    2002
_chemical_formula_sum            'C40.5 H28.5 O7 Os3 Sb'
_chemical_formula_weight         1319.48
_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                82.1490(10)
_cell_angle_beta                 85.30
_cell_angle_gamma                72.68
_cell_formula_units_Z            2
_cell_length_a                   9.39130(10)
_cell_length_b                   13.52100(10)
_cell_length_c                   16.7683(2)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    223(2)
_cell_volume                     2011.72(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.876
_diffrn_measured_fraction_theta_max 0.876
_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  0.0332
_diffrn_reflns_av_sigmaI/netI    0.0535
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            15383
_diffrn_reflns_theta_full        29.08
_diffrn_reflns_theta_max         29.08
_diffrn_reflns_theta_min         2.12
_exptl_absorpt_coefficient_mu    10.154
_exptl_absorpt_correction_T_max  0.263869
_exptl_absorpt_correction_T_min  0.134745
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.178
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1213
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.593
_refine_diff_density_min         -2.369
_refine_diff_density_rms         0.233
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         9442
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0376
_refine_ls_shift/su_max          0.028
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0442P)²+1.7965P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0893
_refine_ls_wR_factor_ref         0.0967
_reflns_number_gt                7663
_reflns_number_total             9442
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om010911x.cif
_cod_data_source_block           ml8
_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_original_formula_sum        'C40.50 H28.50 O7 Os3 Sb'
_cod_database_code               4076673
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 0.37043(3) 1.18594(2) 0.348912(17) 0.03112(8) Uani 1 1 d .
Os2 Os 0.15082(3) 1.16231(2) 0.238129(16) 0.02841(8) Uani 1 1 d .
Os3 Os 0.39703(3) 1.00751(2) 0.265650(17) 0.03081(8) Uani 1 1 d .
Sb4 Sb 0.17195(5) 1.34188(4) 0.26299(3) 0.03229(11) Uani 1 1 d .
O11 O 0.6256(7) 1.0346(5) 0.4461(4) 0.0578(16) Uani 1 1 d .
O12 O 0.1376(8) 1.1907(6) 0.4907(4) 0.0658(18) Uani 1 1 d .
O13 O 0.5002(9) 1.3625(5) 0.3706(5) 0.088(3) Uani 1 1 d .
O21 O -0.0023(7) 1.2037(5) 0.0795(4) 0.0534(15) Uani 1 1 d .
O22 O -0.1324(6) 1.1816(5) 0.3490(4) 0.0568(16) Uani 1 1 d .
O31 O 0.5185(8) 0.8705(6) 0.1325(4) 0.073(2) Uani 1 1 d .
O32 O 0.6300(8) 0.8468(5) 0.3686(5) 0.077(2) Uani 1 1 d .
C1 C 0.1736(7) 0.9986(5) 0.2663(4) 0.0293(14) Uani 1 1 d .
C2 C 0.2286(8) 0.9470(6) 0.3436(4) 0.0336(15) Uani 1 1 d .
H2A H 0.1860 0.9896 0.3873 0.040 Uiso 1 1 calc R
C10 C 0.4738(7) 1.1524(5) 0.2325(4) 0.0307(15) Uani 1 1 d .
C11 C 0.5262(9) 1.0850(6) 0.4088(5) 0.0413(18) Uani 1 1 d .
C12 C 0.2261(9) 1.1906(6) 0.4400(5) 0.0434(18) Uani 1 1 d .
C13 C 0.4507(9) 1.2969(7) 0.3631(5) 0.050(2) Uani 1 1 d .
C20 C 0.3660(8) 1.1539(5) 0.1774(4) 0.0329(15) Uani 1 1 d .
C21 C 0.0532(8) 1.1881(6) 0.1420(5) 0.0402(18) Uani 1 1 d .
C22 C -0.0300(8) 1.1770(6) 0.3070(5) 0.0371(16) Uani 1 1 d .
C30 C 0.4070(10) 1.1534(7) 0.0934(5) 0.047(2) Uani 1 1 d .
H30A H 0.3361 1.1569 0.0567 0.057 Uiso 1 1 calc R
C31 C 0.4693(9) 0.9199(7) 0.1851(5) 0.0461(19) Uani 1 1 d .
C32 C 0.5444(9) 0.9102(6) 0.3282(5) 0.0456(19) Uani 1 1 d .
C40 C 0.5532(10) 1.1478(7) 0.0667(6) 0.054(2) Uani 1 1 d .
H40A H 0.5798 1.1479 0.0120 0.065 Uiso 1 1 calc R
C50 C 0.6601(9) 1.1419(7) 0.1218(6) 0.054(2) Uani 1 1 d .
H50A H 0.7575 1.1376 0.1031 0.065 Uiso 1 1 calc R
C60 C 0.6252(9) 1.1424(6) 0.2023(5) 0.0450(19) Uani 1 1 d .
H60A H 0.6992 1.1361 0.2378 0.054 Uiso 1 1 calc R
C101 C 0.1007(7) 0.9476(5) 0.2138(4) 0.0317(15) Uani 1 1 d .
C102 C -0.0114(8) 0.9044(6) 0.2487(5) 0.0427(18) Uani 1 1 d .
H10A H -0.0331 0.9028 0.3039 0.051 Uiso 1 1 calc R
C103 C -0.0907(10) 0.8636(7) 0.2014(6) 0.052(2) Uani 1 1 d .
H10B H -0.1648 0.8350 0.2251 0.063 Uiso 1 1 calc R
C104 C -0.0586(11) 0.8659(7) 0.1186(6) 0.054(2) Uani 1 1 d .
H10C H -0.1132 0.8410 0.0865 0.065 Uiso 1 1 calc R
C105 C 0.0554(10) 0.9056(6) 0.0849(5) 0.048(2) Uani 1 1 d .
H10D H 0.0816 0.9025 0.0304 0.058 Uiso 1 1 calc R
C106 C 0.1306(9) 0.9493(5) 0.1300(5) 0.0400(18) Uani 1 1 d .
H10E H 0.2016 0.9803 0.1053 0.048 Uiso 1 1 calc R
C201 C 0.2593(8) 0.8329(5) 0.3707(4) 0.0331(15) Uani 1 1 d .
C202 C 0.3088(9) 0.7549(6) 0.3197(5) 0.0440(18) Uani 1 1 d .
H20A H 0.3234 0.7737 0.2649 0.053 Uiso 1 1 calc R
C203 C 0.3369(9) 0.6504(6) 0.3486(6) 0.048(2) Uani 1 1 d .
H20B H 0.3696 0.5999 0.3133 0.058 Uiso 1 1 calc R
C204 C 0.3160(10) 0.6210(6) 0.4304(6) 0.053(2) Uani 1 1 d .
H20C H 0.3382 0.5509 0.4509 0.064 Uiso 1 1 calc R
C205 C 0.2619(10) 0.6978(7) 0.4806(6) 0.052(2) Uani 1 1 d .
H20D H 0.2431 0.6788 0.5350 0.062 Uiso 1 1 calc R
C206 C 0.2346(9) 0.8028(6) 0.4520(5) 0.0408(17) Uani 1 1 d .
H20E H 0.1998 0.8531 0.4873 0.049 Uiso 1 1 calc R
C411 C 0.2673(9) 1.4491(6) 0.1899(5) 0.0451(19) Uani 1 1 d .
C412 C 0.4065(13) 1.4139(8) 0.1526(8) 0.094(4) Uani 1 1 d .
H41A H 0.4565 1.3429 0.1569 0.113 Uiso 1 1 calc R
C413 C 0.4721(17) 1.4858(12) 0.1082(11) 0.151(8) Uani 1 1 d .
H41B H 0.5672 1.4627 0.0844 0.181 Uiso 1 1 calc R
C414 C 0.3956(16) 1.5908(11) 0.0998(10) 0.130(7) Uani 1 1 d .
H41C H 0.4389 1.6383 0.0696 0.156 Uiso 1 1 calc R
C415 C 0.2597(13) 1.6244(8) 0.1348(8) 0.085(4) Uani 1 1 d .
H41D H 0.2092 1.6953 0.1289 0.102 Uiso 1 1 calc R
C416 C 0.1926(10) 1.5550(7) 0.1798(6) 0.059(3) Uani 1 1 d .
H41E H 0.0975 1.5796 0.2033 0.071 Uiso 1 1 calc R
C421 C -0.0033(9) 1.4465(6) 0.3248(5) 0.0425(18) Uani 1 1 d .
C422 C 0.0299(14) 1.5131(9) 0.3726(7) 0.087(4) Uani 1 1 d .
H42A H 0.1286 1.5103 0.3788 0.104 Uiso 1 1 calc R
C423 C -0.085(2) 1.5832(11) 0.4107(10) 0.123(6) Uani 1 1 d .
H42B H -0.0637 1.6274 0.4429 0.148 Uiso 1 1 calc R
C424 C -0.2295(18) 1.5874(9) 0.4009(10) 0.112(6) Uani 1 1 d .
H42C H -0.3066 1.6353 0.4260 0.134 Uiso 1 1 calc R
C425 C -0.2620(12) 1.5226(10) 0.3548(9) 0.093(4) Uani 1 1 d .
H42D H -0.3611 1.5257 0.3494 0.111 Uiso 1 1 calc R
C426 C -0.1508(10) 1.4527(7) 0.3164(7) 0.064(3) Uani 1 1 d .
H42E H -0.1746 1.4092 0.2845 0.077 Uiso 1 1 calc R
C100 C 0.767(2) 0.6212(16) 0.1188(13) 0.067(5) Uiso 0.50 1 d P
H10F H 0.7143 0.5953 0.1646 0.101 Uiso 0.50 1 calc PR
H10G H 0.6959 0.6660 0.0816 0.101 Uiso 0.50 1 calc PR
H10H H 0.8269 0.6597 0.1362 0.101 Uiso 0.50 1 calc PR
C200 C 0.859(3) 0.5368(18) 0.0806(14) 0.075(6) Uiso 0.50 1 d P
H20F H 0.9208 0.4914 0.1223 0.089 Uiso 0.50 1 calc PR
H20G H 0.7924 0.4991 0.0671 0.089 Uiso 0.50 1 calc PR
C300 C 0.948(2) 0.5411(16) 0.0173(13) 0.068(5) Uiso 0.50 1 d P
H30B H 1.0048 0.5867 0.0283 0.082 Uiso 0.50 1 calc PR
H30C H 0.8834 0.5793 -0.0258 0.082 Uiso 0.50 1 calc PR
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'
Sb Sb -0.5866 1.5461 '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_3
C13 Os1 C11 91.7(3) .
C13 Os1 C12 101.9(4) .
C11 Os1 C12 92.5(3) .
C13 Os1 C10 98.3(3) .
C11 Os1 C10 95.1(3) .
C12 Os1 C10 158.2(3) .
C13 Os1 Sb4 82.2(3) .
C11 Os1 Sb4 173.5(2) .
C12 Os1 Sb4 90.8(2) .
C10 Os1 Sb4 83.88(18) .
C13 Os1 Os3 146.9(3) .
C11 Os1 Os3 80.8(2) .
C12 Os1 Os3 110.5(2) .
C10 Os1 Os3 51.00(16) .
Sb4 Os1 Os3 103.286(14) .
C13 Os1 Os2 134.3(3) .
C11 Os1 Os2 131.8(2) .
C12 Os1 Os2 91.0(2) .
C10 Os1 Os2 68.76(17) .
Sb4 Os1 Os2 53.693(12) .
Os3 Os1 Os2 53.263(9) .
C21 Os2 C22 95.0(3) .
C21 Os2 C1 99.5(3) .
C22 Os2 C1 83.3(3) .
C21 Os2 C20 93.2(3) .
C22 Os2 C20 170.7(3) .
C1 Os2 C20 99.6(3) .
C21 Os2 Sb4 104.7(2) .
C22 Os2 Sb4 92.6(2) .
C1 Os2 Sb4 155.75(19) .
C20 Os2 Sb4 81.12(18) .
C21 Os2 Os3 122.5(2) .
C22 Os2 Os3 122.7(2) .
C1 Os2 Os3 51.76(17) .
C20 Os2 Os3 55.12(19) .
Sb4 Os2 Os3 113.875(15) .
C21 Os2 Os1 154.7(2) .
C22 Os2 Os1 102.8(2) .
C1 Os2 Os1 100.34(18) .
C20 Os2 Os1 68.06(18) .
Sb4 Os2 Os1 57.159(13) .
Os3 Os2 Os1 61.216(9) .
C31 Os3 C32 85.0(4) .
C31 Os3 C1 94.7(3) .
C32 Os3 C1 122.6(3) .
C31 Os3 C2 107.9(3) .
C32 Os3 C2 87.3(3) .
C1 Os3 C2 38.4(3) .
C31 Os3 C20 93.0(3) .
C32 Os3 C20 140.4(3) .
C1 Os3 C20 97.0(3) .
C2 Os3 C20 130.2(3) .
C31 Os3 C10 108.2(3) .
C32 Os3 C10 107.2(3) .
C1 Os3 C10 126.7(2) .
C2 Os3 C10 142.0(2) .
C20 Os3 C10 36.5(2) .
C31 Os3 Os2 117.3(3) .
C32 Os3 Os2 156.3(3) .
C1 Os3 Os2 52.18(18) .
C2 Os3 Os2 78.72(19) .
C20 Os3 Os2 51.72(17) .
C10 Os3 Os2 74.64(17) .
C31 Os3 Os1 155.3(2) .
C32 Os3 Os1 97.7(2) .
C1 Os3 Os1 104.16(17) .
C2 Os3 Os1 96.76(17) .
C20 Os3 Os1 69.25(17) .
C10 Os3 Os1 47.45(18) .
Os2 Os3 Os1 65.521(10) .
C411 Sb4 C421 100.4(3) .
C411 Sb4 Os2 131.0(2) .
C421 Sb4 Os2 120.8(2) .
C411 Sb4 Os1 114.3(2) .
C421 Sb4 Os1 119.2(2) .
Os2 Sb4 Os1 69.147(14) .
C2 C1 C101 121.3(6) .
C2 C1 Os3 74.7(4) .
C101 C1 Os3 131.4(5) .
C2 C1 Os2 118.7(4) .
C101 C1 Os2 118.6(5) .
Os3 C1 Os2 76.1(2) .
C1 C2 C201 125.5(6) .
C1 C2 Os3 66.9(4) .
C201 C2 Os3 120.5(5) .
C20 C10 C60 118.4(7) .
C20 C10 Os1 111.0(5) .
C60 C10 Os1 130.1(5) .
C20 C10 Os3 71.5(4) .
C60 C10 Os3 119.7(5) .
Os1 C10 Os3 81.5(2) .
O11 C11 Os1 171.7(7) .
O12 C12 Os1 176.0(7) .
O13 C13 Os1 178.9(9) .
C10 C20 C30 119.5(7) .
C10 C20 Os2 111.3(5) .
C30 C20 Os2 129.1(6) .
C10 C20 Os3 72.0(4) .
C30 C20 Os3 123.7(5) .
Os2 C20 Os3 73.2(2) .
O21 C21 Os2 177.0(7) .
O22 C22 Os2 177.1(7) .
C40 C30 C20 119.9(8) .
O31 C31 Os3 175.4(8) .
O32 C32 Os3 176.1(8) .
C30 C40 C50 120.2(8) .
C60 C50 C40 121.6(8) .
C50 C60 C10 120.2(8) .
C102 C101 C106 118.4(7) .
C102 C101 C1 118.3(7) .
C106 C101 C1 123.0(6) .
C103 C102 C101 120.6(8) .
C104 C103 C102 119.9(8) .
C105 C104 C103 119.3(7) .
C106 C105 C104 121.4(8) .
C105 C106 C101 120.2(8) .
C206 C201 C202 117.9(7) .
C206 C201 C2 117.7(6) .
C202 C201 C2 124.4(7) .
C203 C202 C201 121.7(8) .
C202 C203 C204 119.8(8) .
C205 C204 C203 118.7(8) .
C204 C205 C206 121.6(9) .
C201 C206 C205 120.1(8) .
C412 C411 C416 119.1(8) .
C412 C411 Sb4 119.9(6) .
C416 C411 Sb4 121.0(7) .
C411 C412 C413 119.5(11) .
C414 C413 C412 120.1(12) .
C415 C414 C413 120.1(11) .
C414 C415 C416 121.0(10) .
C411 C416 C415 120.1(10) .
C426 C421 C422 119.0(9) .
C426 C421 Sb4 121.1(7) .
C422 C421 Sb4 119.9(7) .
C423 C422 C421 119.6(12) .
C424 C423 C422 119.8(13) .
C425 C424 C423 120.7(12) .
C424 C425 C426 120.7(11) .
C425 C426 C421 120.1(10) .
C300 C200 C100 127(2) .
C200 C300 C300 129(3) 2_765
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Os1 C13 1.917(8) .
Os1 C11 1.921(8) .
Os1 C12 1.951(9) .
Os1 C10 2.150(7) .
Os1 Sb4 2.6957(5) .
Os1 Os3 2.8873(4) .
Os1 Os2 2.9983(4) .
Os2 C21 1.860(8) .
Os2 C22 1.948(8) .
Os2 C1 2.149(6) .
Os2 C20 2.165(7) .
Os2 Sb4 2.5855(5) .
Os2 Os3 2.6401(4) .
Os3 C31 1.869(8) .
Os3 C32 1.877(8) .
Os3 C1 2.137(6) .
Os3 C2 2.240(7) .
Os3 C20 2.263(7) .
Os3 C10 2.269(6) .
Sb4 C411 2.125(8) .
Sb4 C421 2.126(8) .
O11 C11 1.152(9) .
O12 C12 1.140(10) .
O13 C13 1.141(9) .
O21 C21 1.175(9) .
O22 C22 1.136(9) .
O31 C31 1.161(10) .
O32 C32 1.166(10) .
C1 C2 1.443(10) .
C1 C101 1.505(9) .
C2 C201 1.495(9) .
C10 C20 1.420(9) .
C10 C60 1.444(10) .
C20 C30 1.430(10) .
C30 C40 1.392(11) .
C40 C50 1.398(12) .
C50 C60 1.362(12) .
C101 C102 1.402(10) .
C101 C106 1.407(10) .
C102 C103 1.395(10) .
C103 C104 1.394(13) .
C104 C105 1.383(12) .
C105 C106 1.372(10) .
C201 C206 1.389(10) .
C201 C202 1.397(10) .
C202 C203 1.383(11) .
C203 C204 1.391(12) .
C204 C205 1.378(12) .
C205 C206 1.390(11) .
C411 C412 1.380(13) .
C411 C416 1.387(11) .
C412 C413 1.400(15) .
C413 C414 1.381(18) .
C414 C415 1.337(17) .
C415 C416 1.388(13) .
C421 C426 1.380(11) .
C421 C422 1.399(12) .
C422 C423 1.383(16) .
C423 C424 1.36(2) .
C424 C425 1.36(2) .
C425 C426 1.366(14) .
C100 C200 1.41(3) .
C200 C300 1.30(3) .
C300 C300 1.40(4) 2_765
