Synthesis, Neutron Structure, and Reactivity of the Bis(dihydrogen) Complex RuH2(η2-H2)2(PCyp3)2 Stabilized by Two Tricyclopentylphosphines
Mary Grellier; Laure Vendier; Bruno Chaudret; Alberto Albinati; Silvia Rizzato; Sax Mason; Sylviane Sabo-Etienne; Journal of the American Chemical Society 127 (2005) 17592–17593; doi:10.1021/ja055126g

data_4112119
_publ_contact_author_address
;
 Laboratoire de Chimie de Coordination
 205 Route de Narbonne
 31077 Toulouse Cedex 04
;
_publ_contact_author_email       sabo@lcc-toulouse.fr
_publ_contact_author_name        'Sylviane Sabo-Etienne'
_publ_section_title
;
 Synthesis, Neutron Structure, and Reactivity of the Bis(dihydrogen)
 Complex RuH2(\h2-H2)2(PCyp3)2 Stabilized by Two Tricyclopentylphosphines
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17592
_journal_page_last               17593
_journal_paper_doi               10.1021/ja055126g
_journal_volume                  127
_journal_year                    2005
_chemical_formula_sum            'C30 H60 P2 Ru'
_chemical_formula_weight         583.82
_chemical_name_common            Ru(H)2(eta2-H2)2[P(C5H27)3]2
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000(2)
_cell_angle_beta                 105.3771(17)
_cell_angle_gamma                90.000(2)
_cell_formula_units_Z            4
_cell_length_a                   14.8322(9)
_cell_length_b                   9.4259(6)
_cell_length_c                   21.6790(14)
_cell_measurement_reflns_used    1979
_cell_measurement_temperature    20(1)
_cell_measurement_theta_max      45.81
_cell_measurement_theta_min      21.08
_cell_volume                     2922.4(3)
_computing_cell_refinement       'ILL RAFD9'
_computing_data_collection       'ILL HKLGEN, MAD'
_computing_data_reduction        'ILL Retreat'
_computing_molecular_graphics
'ORTEP for Windows v1.074 (L.J. Farrugia 1997)'
_computing_publication_material
'WinGX v1.64.05(L.J. Farrugia,J. Appl. Cryst.,1999,32, 837)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      20(2)
_diffrn_detector_area_resol_mean '2 to 3 mm'
_diffrn_measured_fraction_theta_full 0.855
_diffrn_measured_fraction_theta_max 0.855
_diffrn_measurement_device_type  'D19 multidetector-diffractometer'
_diffrn_measurement_method       'omega step-scans'
_diffrn_radiation_monochromator  'Ge (115)'
_diffrn_radiation_probe          neutron
_diffrn_radiation_source         'ILL High Flux Reactor'
_diffrn_radiation_type           neutron
_diffrn_radiation_wavelength     1.31600
_diffrn_reflns_av_R_equivalents  0.0756
_diffrn_reflns_av_sigmaI/netI    0.0640
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12878
_diffrn_reflns_theta_full        63.02
_diffrn_reflns_theta_max         63.02
_diffrn_reflns_theta_min         2.77
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  '12 hours'
_diffrn_standards_number         6
_exptl_absorpt_correction_T_max  0.9641
_exptl_absorpt_correction_T_min  0.8993
_exptl_absorpt_correction_type   'analytic, attenuation by cans'
_exptl_absorpt_process_details   'program D19abscan'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_density_method    n.a.
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             -3
_exptl_crystal_size_max          2.1
_exptl_crystal_size_mid          2.0
_exptl_crystal_size_min          2.0
_refine_diff_density_max         0.115
_refine_diff_density_min         -0.094
_refine_diff_density_rms         0.023
_refine_ls_extinction_coef       0.0
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     838
_refine_ls_number_reflns         6498
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0779
_refine_ls_R_factor_gt           0.0521
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0613P)^2^+0.3583P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1207
_refine_ls_wR_factor_ref         0.1440
_reflns_number_gt                4979
_reflns_number_total             6498
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja055126gsi20051018_094223_1.cif
_cod_data_source_block           ruh6
_cod_database_code               4112119