Synthesis and Characterization of the Dinuclear Polyhydrides [Os2H7(PPhiPr2)4]+ and [Os2H6(PPhiPr2)4]
Bradley G. Anderson; Sarah A. Hoyte; John L. Spencer; Inorganic Chemistry 48 (2009) 7977–7983; doi:10.1021/ic900111s

data_4302900
_publ_section_title
;
Synthesis and Characterization of the Dinuclear Polyhydrides
[Os2H7(PPhiPr2)4]+ and [Os2H6(PPhiPr2)4]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7977
_journal_page_last               7983
_journal_paper_doi               10.1021/ic900111s
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C48 H82 Os2 P4'
_chemical_formula_sum            'C48 H82 Os2 P4'
_chemical_formula_weight         1163.42
_chemical_name_systematic
tris(\m~2~-Hydrido)-trihydrido-tetrakis(diisopropylphenylphosphine)-di-osmium
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 106.994(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.9836(6)
_cell_length_b                   15.1146(5)
_cell_length_c                   18.9267(6)
_cell_measurement_reflns_used    9594
_cell_measurement_temperature    119
_cell_measurement_theta_max      33.32
_cell_measurement_theta_min      2.37
_cell_volume                     4919.9(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'CCDC Mercury'
_computing_publication_material  'CCDC enCIFer'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      119
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.918
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0493
_diffrn_reflns_av_sigmaI/netI    0.0387
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            179215
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         34.58
_diffrn_reflns_theta_min         1.18
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    5.321
_exptl_absorpt_correction_T_max  0.34
_exptl_absorpt_correction_T_min  0.23503758
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.571
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2328
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_refine_diff_density_max         3.607
_refine_diff_density_min         -1.920
_refine_diff_density_rms         0.177
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     810
_refine_ls_number_reflns         19262
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0318
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0260P)^2^+10.9469P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0617
_refine_ls_wR_factor_ref         0.0715
_reflns_number_gt                15035
_reflns_number_total             19263
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic900111s_si_001_2.cif
_cod_data_source_block           Os2H6P4
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4302900