Synthesis, Characterization, and Novel Fluxional Mechanisms of Triosmium Clusters Containing the Highly Flexible Ligand Ph2PC2H4SC2H4SC2H4PPh2(PSSP)
Persson, Roger; Stchedroff, Marc J.; Uebersezig, Bettina; Gobetto, Roberto; Steed, Jonathan W.; Prince, Paul D.; Monari, Magda; Nordlander, Ebbe; Organometallics 29 (2010) 2223–; doi:10.1021/om900966c

data_4067452
_publ_section_title
;
 Synthesis, Characterization, and Novel Fluxional Mechanisms of Triosmium
 Clusters Containing the Highly Flexible Ligand
 Ph2PC2H4SC2H4SC2H4PPh2(PSSP)
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              2223
_journal_paper_doi               10.1021/om900966c
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C52 H34 Cl6 O20 Os6 P2 S2'
_chemical_formula_weight         2458.75
_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                109.6240(10)
_cell_angle_beta                 99.645(2)
_cell_angle_gamma                104.675(2)
_cell_formula_units_Z            2
_cell_length_a                   13.9222(6)
_cell_length_b                   15.5954(7)
_cell_length_c                   17.5669(8)
_cell_measurement_temperature    293(2)
_cell_volume                     3339.2(3)
_computing_cell_refinement       SMART
_computing_data_collection       SMART
_computing_data_reduction        SAINT+
_computing_molecular_graphics    'ORTEP-3 (Farrugia 2004)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-97 (Giacovazzo, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART 2000 CCD'
_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  0.0746
_diffrn_reflns_av_sigmaI/netI    0.1132
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            45638
_diffrn_reflns_theta_full        29.99
_diffrn_reflns_theta_max         29.99
_diffrn_reflns_theta_min         2.56
_exptl_absorpt_coefficient_mu    11.789
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.70
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.445
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2252
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.23
_refine_diff_density_max         3.336
_refine_diff_density_min         -1.762
_refine_diff_density_rms         0.252
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.901
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     806
_refine_ls_number_reflns         19363
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.901
_refine_ls_R_factor_all          0.1024
_refine_ls_R_factor_gt           0.0471
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0404P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1002
_refine_ls_wR_factor_ref         0.1143
_reflns_number_gt                10563
_reflns_number_total             19363
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900966c_si_001.cif
_cod_data_source_block           compd4
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4067452