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_4112120
_publ_contact_author_address
;
Laboratoire de Chimie de Coordination
205 Route de Narbonne
31077 Toulouse Cedex 04
;
_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_compound_source        'synthesis as described'
_chemical_formula_moiety         'C30 H60 P2 Ru1'
_chemical_formula_sum            'C30 H60 P2 Ru'
_chemical_formula_weight         583.79
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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
_cell_angle_alpha                90
_cell_angle_beta                 105.139(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.9282(16)
_cell_length_b                   9.4580(7)
_cell_length_c                   21.713(2)
_cell_measurement_reflns_used    7997
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.05
_cell_measurement_theta_min      1.65
_cell_measurement_wavelength     0.71073
_cell_volume                     2959.3(5)
_computing_cell_refinement       'Stoe IPDS software (Stoe, 1996)'
_computing_data_collection       'Stoe IPDS software (Stoe, 1996)'
_computing_data_reduction        'XRED (Stoe, 1.08, 1996)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.946
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_device       'Stoe IPDS'
_diffrn_measurement_method       \f
_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_unetI/netI     0.015
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            22631
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         2.36
_diffrn_standards_decay_%        0.1
_diffrn_standards_interval_time  4
_diffrn_standards_number         200
_exptl_absorpt_coefficient_mu    0.655
_exptl_absorpt_correction_T_max  0.842
_exptl_absorpt_correction_T_min  0.7380
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.31
_exptl_crystal_description       block
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.4625
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.483
_refine_diff_density_min         -0.763
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         5526
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0275
_refine_ls_R_factor_gt           0.0255
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0410P)^2^+2.0328P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0668
_refine_ls_wR_factor_ref         0.07
_reflns_number_gt                5209
_reflns_number_total             5526
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja055126gsi20051018_094223_2.cif
_cod_data_source_block           global
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4112120