Reductive coupling of alkynes to give ruthenium and osmium clusters of the type [M3(1,3-diene)(μ3-X)(CO)8] containing μ-η2,η2- or η4-1,3-diene
Ali, Shahbano; Deeming, Antony J.; Hogarth, Graeme; Mehta, Nikesh A.; Steed, Jonathan W.; Chemical Communications  (1999) 2541–; doi:10.1039/a908706k

data_7110748
_publ_section_title
;
 Reductive coupling of alkynes to give ruthenium and osmium clusters of
 the type [M3(1,3-diene)(\m3-X)(CO)8] containing \m-\h2,\h2- or
 \h4-1,3-diene
;
_journal_issue                   24
_journal_name_full               'Chemical Communications'
_journal_page_first              2541
_journal_paper_doi               10.1039/a908706k
_journal_year                    1999
_chemical_formula_structural     Os3(S)(Ph2C4H4)(CO)8
_chemical_formula_sum            'C24 H14 O8 Os3 S'
_chemical_formula_weight         1033.01
_chemical_name_systematic
;
 Octacarbonyl(1,3-diphenylbutadiene)(sulfido)triosmium
;
_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
_cell_angle_alpha                91.58(3)
_cell_angle_beta                 108.82(3)
_cell_angle_gamma                104.51(3)
_cell_formula_units_Z            2
_cell_length_a                   9.406(2)
_cell_length_b                   10.615(2)
_cell_length_c                   13.885(3)
_cell_measurement_reflns_used    33
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14.0
_cell_measurement_theta_min      8.4
_cell_volume                     1261.5(6)
_computing_cell_refinement       SHELXTL-PLUS
_computing_data_collection       SHELXTL-PLUS
_computing_data_reduction        SHELXTL-PLUS
_computing_molecular_graphics    SHELXTL-PLUS
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      291(2)
_diffrn_measurement_device       'Nicolet R3v/m'
_diffrn_measurement_method       'omega-2theta 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  0.0271
_diffrn_reflns_av_sigmaI/netI    0.0307
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4713
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         2.65
_diffrn_standards_decay_%        zero
_diffrn_standards_interval_count 'every 97 reflections'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    15.201
_exptl_absorpt_correction_T_max  0.975
_exptl_absorpt_correction_T_min  0.275
_exptl_absorpt_correction_type   psi-scans
_exptl_crystal_colour            yellow/orange
_exptl_crystal_density_diffrn    2.720
_exptl_crystal_description       block
_exptl_crystal_F_000             932
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.16
_refine_diff_density_max         3.176
_refine_diff_density_min         -4.835
_refine_diff_density_rms         0.386
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.060
_refine_ls_goodness_of_fit_obs   1.072
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         4417
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_restrained_S_obs      1.072
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_obs          0.0501
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1019P)^2^+10.0612P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1453
_refine_ls_wR_factor_obs         0.1344
_reflns_number_observed          3864
_reflns_number_total             4421
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            908706ksup1.cif
_cod_data_source_block           str658
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1019P)^2^+10.0612P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1019P)^2^+10.0612P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1261.4(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7110748