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
Deng, Mingli; Leong, Weng Kee; Organometallics 21 (2002) 1221–; doi:10.1021/om010911x

data_4076670
_publ_section_title
;
 Reactions of the Triosmium&#x2212;Antimony Cluster
 Os3(\m-SbPh2)(\m-H)(\m3,\h2-C6H4)(CO)9with Alkynes:&#x00A0; C&#x2212;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            'C41.5 H28 Cl O7 Os3 Sb'
_chemical_formula_weight         1366.44
_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                101.0840(10)
_cell_angle_beta                 97.7280(10)
_cell_angle_gamma                97.5030(10)
_cell_formula_units_Z            2
_cell_length_a                   9.23540(10)
_cell_length_b                   10.0936(2)
_cell_length_c                   22.8557(4)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    223(2)
_cell_volume                     2044.86(6)
_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 0.866
_diffrn_measured_fraction_theta_max 0.866
_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  0.0346
_diffrn_reflns_av_sigmaI/netI    0.0586
_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       30
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            17316
_diffrn_reflns_theta_full        29.32
_diffrn_reflns_theta_max         29.32
_diffrn_reflns_theta_min         2.08
_exptl_absorpt_coefficient_mu    10.056
_exptl_absorpt_correction_T_max  0.603955
_exptl_absorpt_correction_T_min  0.337559
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    2.219
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1258
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.304
_refine_diff_density_min         -1.202
_refine_diff_density_rms         0.207
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     513
_refine_ls_number_reflns         9695
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0369
_refine_ls_shift/su_max          0.035
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0239P)^2^+3.3304P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0735
_refine_ls_wR_factor_ref         0.0808
_reflns_number_gt                7768
_reflns_number_total             9695
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om010911x.cif
_cod_data_source_block           ml6
_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        'C41.50 H28 Cl O7 Os3 Sb'
_cod_database_code               4076670