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_4076671
_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            'C27 H19 O9 Os3 Sb'
_chemical_formula_weight         1179.77
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                   20.1830(4)
_cell_length_b                   13.1745(3)
_cell_length_c                   11.1624(2)
_cell_measurement_reflns_used    7435
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      31.20
_cell_measurement_theta_min      2.39
_cell_volume                     2968.09(10)
_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 0.943
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0742
_diffrn_reflns_av_sigmaI/netI    0.0374
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            27535
_diffrn_reflns_theta_full        31.67
_diffrn_reflns_theta_max         31.67
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    13.751
_exptl_absorpt_correction_T_max  0.382469
_exptl_absorpt_correction_T_min  0.129349
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    2.640
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             2128
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.735
_refine_diff_density_min         -1.778
_refine_diff_density_rms         0.209
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     206
_refine_ls_number_reflns         4904
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0334
_refine_ls_shift/su_max          0.047
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0365P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0710
_refine_ls_wR_factor_ref         0.0735
_reflns_number_gt                4005
_reflns_number_total             4904
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om010911x.cif
_cod_data_source_block           ml13
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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      Pnma
_cod_database_code               4076671