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_7110747
_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_sum            'C19 H13 N O10 Ru3 S'
_chemical_formula_weight         750.57
_chemical_name_systematic
;
 (butadiene)(tosylimido)octacarbonyltriruthenium
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2b'
_symmetry_space_group_name_H-M   'P b c 21'
_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                   10.3720(2)
_cell_length_b                   13.5883(2)
_cell_length_c                   16.0282(3)
_cell_measurement_reflns_used    n/a
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      n/a
_cell_measurement_theta_min      n/a
_cell_volume                     2258.98(7)
_computing_cell_refinement       DENZO-SMN
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'RES2INS (Barbour, 1997)'
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '2o phi frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0440
_diffrn_reflns_av_sigmaI/netI    0.0258
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19655
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.80
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count n/a
_diffrn_standards_interval_time  n/a
_diffrn_standards_number         n/a
_exptl_absorpt_coefficient_mu    2.129
_exptl_absorpt_correction_T_max  0.8153
_exptl_absorpt_correction_T_min  0.6754
_exptl_absorpt_correction_type   Scalepack
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.207
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.735
_refine_diff_density_min         -0.683
_refine_diff_density_rms         0.085
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.52(2)
_refine_ls_extinction_coef       0.0020(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.097
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         4203
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0180
_refine_ls_R_factor_gt           0.0179
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0208P)^2^+1.6597P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0455
_refine_ls_wR_factor_ref         0.0456
_reflns_number_gt                4191
_reflns_number_total             4203
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            908706ksup1.cif
_cod_data_source_block           sa255c
_cod_original_sg_symbol_H-M      Pbc21
_cod_database_code               7110747