Cationic Osmium(II) Acetyl Complexes Bearing Pyrazolylmethane Ligands: Intramolecular and Interionic Structure and Isolation of an Intermediate Containing the “Os−I−Ag” Moiety
Bellachioma, Gianfranco; Cardaci, Giuseppe; Macchioni, Alceo; Valentini, Francesco; Zuccaccia, Cristiano; Foresti, Elisabetta; Sabatino, Piera; Organometallics 19 (2000) 4320–; doi:10.1021/om000344y

data_4077529
_publ_section_title
;
 Cationic Osmium(II) Acetyl Complexes Bearing Pyrazolylmethane
 Ligands:&#x00A0; Intramolecular and Interionic Structure and Isolation of
 an Intermediate Containing the &#x201C;Os&#x2212;I&#x2212;Ag&#x201D;
 Moiety
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              4320
_journal_paper_doi               10.1021/om000344y
_journal_volume                  19
_journal_year                    2000
_chemical_formula_sum            'C10 H21 F3 O6 Os P2 S'
_chemical_formula_weight         578.47
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 106.87
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.742
_cell_length_b                   23.683
_cell_length_c                   10.049
_cell_measurement_temperature    293(2)
_cell_volume                     1990.979
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0249
_diffrn_reflns_av_sigmaI/netI    0.0317
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3686
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         2.58
_exptl_absorpt_coefficient_mu    6.716
_exptl_crystal_density_diffrn    1.930
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1112
_refine_diff_density_max         1.072
_refine_diff_density_min         -1.228
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.354
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     206
_refine_ls_number_reflns         3485
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.354
_refine_ls_R_factor_all          0.0659
_refine_ls_R_factor_gt           0.0405
_refine_ls_shift/su_max          0.231
_refine_ls_shift/su_mean         0.026
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0496P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1003
_refine_ls_wR_factor_ref         0.1069
_reflns_number_gt                2568
_reflns_number_total             3485
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om000344y.cif
_cod_data_source_block           osass
_cod_original_cell_volume        1991.0
_cod_database_code               4077529