Synthesis and Reactivity of Ruthenium Arene Complexes Incorporating Novel Ph2PCH2CH2BR2Ligands. Easy Access to the Four-Membered Ruthenacycle [(p-cymene)RuCl(κC,P-CH2CH2PPh2)]
Vergnaud, Jérôme; Grellier, Mary; Bouhadir, Ghenwa; Vendier, Laure; Sabo-Etienne, Sylviane; Bourissou, Didier; Organometallics 27 (2008) 1140–; doi:10.1021/om701139a

data_4070939
_publ_section_title
;
 Synthesis and Reactivity of Ruthenium Arene Complexes Incorporating Novel
 Ph2PCH2CH2BR2Ligands. Easy Access to the Four-Membered Ruthenacycle
 [(p-cymene)RuCl(\kC,P-CH2CH2PPh2)]
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1140
_journal_paper_doi               10.1021/om701139a
_journal_volume                  27
_journal_year                    2008
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C24 H28 Cl P Ru'
_chemical_formula_sum            'C24 H28 Cl P Ru'
_chemical_formula_weight         483.95
_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
_cell_angle_alpha                77.024(4)
_cell_angle_beta                 73.311(4)
_cell_angle_gamma                82.677(4)
_cell_formula_units_Z            2
_cell_length_a                   7.9420(4)
_cell_length_b                   11.1756(5)
_cell_length_c                   13.0715(6)
_cell_measurement_temperature    110
_cell_measurement_theta_max      32.0473
_cell_measurement_theta_min      2.6781
_cell_measurement_wavelength     0.71073
_cell_volume                     1080.47(9)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_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    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      110
_diffrn_measured_fraction_theta_full 0.913
_diffrn_measured_fraction_theta_max 0.913
_diffrn_measurement_device_type  'Oxford-Diffraction XCALIBUR'
_diffrn_measurement_method       \w-\f
_diffrn_orient_matrix_UB_11      -0.0326983853
_diffrn_orient_matrix_UB_12      0.0623054668
_diffrn_orient_matrix_UB_13      -0.0106447701
_diffrn_orient_matrix_UB_21      -0.0814599504
_diffrn_orient_matrix_UB_22      -0.0192428123
_diffrn_orient_matrix_UB_23      -0.0001962585
_diffrn_orient_matrix_UB_31      -0.0317428907
_diffrn_orient_matrix_UB_32      -0.0015679312
_diffrn_orient_matrix_UB_33      0.0567623249
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_av_unetI/netI     0.1117
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11845
_diffrn_reflns_theta_full        32.09
_diffrn_reflns_theta_max         32.09
_diffrn_reflns_theta_min         3.32
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.93
_exptl_absorpt_correction_T_max  0.925
_exptl_absorpt_correction_T_min  0.811
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET)
        (compiled Aug 28 2006,13:05:05)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.945
_refine_diff_density_min         -0.937
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.917
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         6909
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.917
_refine_ls_R_factor_all          0.058
_refine_ls_R_factor_gt           0.0316
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0188P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0545
_refine_ls_wR_factor_ref         0.0589
_reflns_number_gt                4629
_reflns_number_total             6909
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om701139a-file002.cif
_cod_data_source_block           jvo270307
_cod_database_code               4070939