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_4325520
_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_moiety         '(C27 H63 P4 Ru), (C24 H20 B),0.5(C2 H6 O)'
_chemical_formula_sum            'C52 H86 B O P4 Ru'
_chemical_formula_weight         962.97
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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                 105.8920(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.4283(7)
_cell_length_b                   17.7729(6)
_cell_length_c                   18.1170(6)
_cell_measurement_reflns_used    9894
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.233
_cell_measurement_theta_min      2.274
_cell_volume                     5087.6(3)
_computing_cell_refinement       '<i>APEX2</i>  '
_computing_data_collection       '<i>APEX2</i> (Bruker, 2007)'
_computing_data_reduction        '<i>APEX2</i>  '
_computing_molecular_graphics    '<i>SHELXTL-Plus</i> (Sheldrick, 2008)'
_computing_structure_refinement  '<i>SHELXL-97</i> (Sheldrick, 2008)'
_computing_structure_solution    '<i>SHELXS-97</i> (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0563
_diffrn_reflns_av_sigmaI/netI    0.0496
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            60017
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.57
_exptl_absorpt_coefficient_mu    0.469
_exptl_absorpt_correction_T_max  0.9692
_exptl_absorpt_correction_T_min  0.8833
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2001)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.257
_exptl_crystal_description       'Square plates'
_exptl_crystal_F_000             2060
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.777
_refine_diff_density_min         -0.735
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     565
_refine_ls_number_reflns         11057
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0662
_refine_ls_R_factor_gt           0.0460
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0208P)^2^+9.4450P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0931
_refine_ls_wR_factor_ref         0.1007
_reflns_number_gt                8606
_reflns_number_total             11057
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200492w_si_001_3.cif
_cod_data_source_block           fulldata
_cod_database_code               4325520