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_4325518
_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         '2(C27 H60 Cl P4 Ru), 2(C24 H20 B), C4 H8 O'
_chemical_formula_sum            'C106 H168 B2 Cl2 O P8 Ru2'
_chemical_formula_weight         2000.82
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                111.889(3)
_cell_angle_beta                 98.687(3)
_cell_angle_gamma                90.272(3)
_cell_formula_units_Z            2
_cell_length_a                   12.280(2)
_cell_length_b                   19.093(4)
_cell_length_c                   23.928(4)
_cell_measurement_reflns_used    7055
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.4752
_cell_measurement_theta_min      2.2927
_cell_volume                     5134.6(16)
_computing_cell_refinement       'SAINT Ver. 6.45  (Bruker-AXS, 2003)'
_computing_data_collection       'SMART Ver. 5.054 (Bruker-AXS, 1998)'
_computing_data_reduction        'SAINT Ver. 6.45'
_computing_molecular_graphics
;
X-Seed (Barbour, 2001), SHELXTL Ver. 6.14 (Bruker-AXS, 2003)
;
_computing_publication_material  'modiCIFer-12162005 (Guzei, 2005)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_crystal_treatment
;
attached with Exxon Paratone N, to a short length 
of fibre supported on a thin piece of copper wire 
inserted in a copper mounting pin.  The crystal was 
quenched in a cold nitrogen gas stream from an 
Oxford Cryosystems Cryostream. 
;
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker CCD-1000 area detector'
_diffrn_measurement_method       \w
_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  0.0245
_diffrn_reflns_av_sigmaI/netI    0.0370
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            49295
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         1.73
_diffrn_standards_decay_%        0.07
_diffrn_standards_number         422
_exptl_absorpt_coefficient_mu    0.517
_exptl_absorpt_correction_T_max  0.890
_exptl_absorpt_correction_T_min  0.712
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS  (Bruker-AXS, 2004)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_description       prism
_exptl_crystal_F_000             2128
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.960
_refine_diff_density_min         -0.560
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1135
_refine_ls_number_reflns         23041
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0322
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0381P)^2^+2.7047P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0754
_refine_ls_wR_factor_ref         0.0851
_reflns_number_gt                18186
_reflns_number_total             23041
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic200492w_si_001_1.cif
_cod_data_source_block           ldf6pj22
_cod_original_sg_symbol_Hall     '-P 1        '
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4325518