Synthesis and Characterization of Osmium(IV) Polyhydride Complexes of Stoichiometry (C5Me5)OsH3(L). Crystal Structures of (C5Me5)OsH3(AsPh3) and (C5Me5)OsH3(PPh3)
Gross, Christopher L.; Girolami, Gregory S.; Organometallics 25 (2006) 4792–; doi:10.1021/om060463z

data_4074209
_publ_section_title
;
 Synthesis and Characterization of Osmium(IV) Polyhydride Complexes of
 Stoichiometry (C5Me5)OsH3(L). Crystal Structures of (C5Me5)OsH3(AsPh3)
 and (C5Me5)OsH3(PPh3)
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              4792
_journal_paper_doi               10.1021/om060463z
_journal_volume                  25
_journal_year                    2006
_chemical_formula_sum            'C28 H33 As Os'
_chemical_formula_weight         634.66
_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                93.04
_cell_angle_beta                 101.0950(10)
_cell_angle_gamma                113.8560(10)
_cell_formula_units_Z            2
_cell_length_a                   8.5812(3)
_cell_length_b                   9.2527(3)
_cell_length_c                   17.3789(6)
_cell_measurement_reflns_used    4582
_cell_measurement_temperature    198(2)
_cell_volume                     1225.16(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      198(2)
_diffrn_measured_fraction_theta_full 0.918
_diffrn_measured_fraction_theta_max 0.918
_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  0.0348
_diffrn_reflns_av_sigmaI/netI    0.0429
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            7930
_diffrn_reflns_theta_full        28.24
_diffrn_reflns_theta_max         28.24
_diffrn_reflns_theta_min         2.41
_exptl_absorpt_coefficient_mu    6.556
_exptl_absorpt_correction_T_max  0.690
_exptl_absorpt_correction_T_min  0.132
_exptl_absorpt_correction_type   integration
_exptl_crystal_density_diffrn    1.720
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             620
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.722
_refine_diff_density_min         -1.189
_refine_diff_density_rms         0.104
_refine_ls_extinction_coef       0.0039(3)
_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   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     387
_refine_ls_number_reflns         5559
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0268
_refine_ls_shift/su_max          0.024
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0167P)^2^+1.5603P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0575
_refine_ls_wR_factor_ref         0.0615
_reflns_number_gt                4874
_reflns_number_total             5559
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060463zsi20060526_113928.cif
_cod_data_source_block           osh3abs
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4074209