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_4067450
_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 H32 O22 Os6 P2 S2'
_chemical_formula_weight         2276.04
_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                112.96
_cell_angle_beta                 103.163(3)
_cell_angle_gamma                105.503(3)
_cell_formula_units_Z            2
_cell_length_a                   13.5001(15)
_cell_length_b                   16.0441(16)
_cell_length_c                   16.7391(16)
_cell_measurement_temperature    100(2)
_cell_volume                     2983.3(5)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'Nonius Collect'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'XSeed (Barbour, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '2o phi + omega frames'
_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  0.1442
_diffrn_reflns_av_sigmaI/netI    0.1199
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16593
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.75
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    12.927
_exptl_absorpt_correction_T_max  0.4245
_exptl_absorpt_correction_T_min  0.1126
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.534
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2076
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         6.522
_refine_diff_density_min         -7.327
_refine_diff_density_rms         0.709
_refine_ls_extinction_coef       0.0009(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_ref   1.099
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     758
_refine_ls_number_reflns         10441
_refine_ls_number_restraints     504
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.1092
_refine_ls_R_factor_gt           0.0960
_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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2543
_refine_ls_wR_factor_ref         0.2723
_reflns_number_gt                8690
_reflns_number_total             10441
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900966c_si_001.cif
_cod_data_source_block           comp1
_cod_original_cell_volume        2983.1(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4067450