Ruthenium Hydride Complexes of the Hindered Phosphine Ligand Tris(3-diisopropylphosphinopropyl)phosphine
Mohan M. Bhadbhade; Leslie D. Field; Ryan Gilbert-Wilson; Ruth W. Guest; Paul Jensen; Inorganic Chemistry 50 (2011) 6220–6228; doi:10.1021/ic200492w

data_4325519
_publ_section_title
;
 Ruthenium Hydride Complexes of the Hindered Phosphine Ligand
 Tris(3-diisopropylphosphinopropyl)phosphine
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6220
_journal_page_last               6228
_journal_paper_doi               10.1021/ic200492w
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C27 H62 P4 Ru'
_chemical_formula_weight         611.72
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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                 100.723(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.099(2)
_cell_length_b                   17.3858(17)
_cell_length_c                   21.692(3)
_cell_measurement_reflns_used    6163
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.963
_cell_measurement_theta_min      2.343
_cell_volume                     6336.0(13)
_computing_cell_refinement
;
        APEX2(Bruker, 2007, Bruker AXS Inc.,Madison, USA)
;
_computing_data_collection
;
        APEX2(Bruker, 2007, Bruker AXS Inc., Madison, USA)
;
_computing_data_reduction
;
        APEX2(Bruker, 2007, Bruker AXS Inc., Madison, USA)
;
_computing_molecular_graphics    'SHELXTL-Plus. Sheldrick, G. M. (2008)'
_computing_structure_refinement  'SHELXL-97. Sheldrick, G. M. (2008)'
_computing_structure_solution    'SHELXS-97. Sheldrick, G. M. (2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker kappa APEXII CCD Area Detector'
_diffrn_measurement_method       '\f scans, and \w scans with \k offsets'
_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  0.0999
_diffrn_reflns_av_sigmaI/netI    0.0894
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            43788
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    0.711
_exptl_absorpt_correction_T_max  0.9776
_exptl_absorpt_correction_T_min  0.9015
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.283
_exptl_crystal_description       'Large blocks'
_exptl_crystal_F_000             2624
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.441
_refine_diff_density_min         -0.611
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.790
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     617
_refine_ls_number_reflns         11053
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.790
_refine_ls_R_factor_all          0.0770
_refine_ls_R_factor_gt           0.0426
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.5694P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1098
_refine_ls_wR_factor_ref         0.1417
_reflns_number_gt                7444
_reflns_number_total             11053
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200492w_si_001_2.cif
_cod_data_source_block           inp21byc
_cod_original_cell_volume        6335.9(13)
_cod_database_code               4325519