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_4070938
_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         'C32 H42 B Cl2 P Ru, C H2 Cl2'
_chemical_formula_sum            'C33 H44 B Cl4 P Ru'
_chemical_formula_weight         725.33
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.312(4)
_cell_length_b                   13.681(3)
_cell_length_c                   28.015(6)
_cell_measurement_reflns_used    4500
_cell_measurement_temperature    110
_cell_measurement_theta_max      32.1919
_cell_measurement_theta_min      2.8717
_cell_measurement_wavelength     0.71073
_cell_volume                     6635(3)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Oxford-Diffraction XCALIBUR'
_diffrn_measurement_method       \w-\f
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_reflns_av_R_equivalents  0.1356
_diffrn_reflns_av_unetI/netI     0.1497
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            41322
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.88
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.865
_exptl_absorpt_correction_T_max  0.9884
_exptl_absorpt_correction_T_min  0.9768
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            'yellow orange'
_exptl_crystal_density_diffrn    1.452
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2992
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.025
_refine_diff_density_max         2.334
_refine_diff_density_min         -0.815
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         6774
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.1549
_refine_ls_R_factor_gt           0.0766
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0453P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.13
_refine_ls_wR_factor_ref         0.1551
_reflns_number_gt                4118
_reflns_number_total             6774
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om701139a-file001.cif
_cod_data_source_block           pbca
_cod_database_code               4070938