Reactions of [Ru(CO)2(PPh3)3] with Alkynylphosphonium Salts: A Phosphinoallene Complex
Ang, Wee Han; Cordiner, Richard L.; Hill, Anthony F.; Perry, Tamara L.; Wagler, Jörg; Organometallics 28 (2009) 5568–; doi:10.1021/om900621v

data_4070124
_publ_section_title
;
 Reactions of [Ru(CO)2(PPh3)3] with Alkynylphosphonium Salts: A
 Phosphinoallene Complex
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              5568
_journal_paper_doi               10.1021/om900621v
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety
'C59 H48 O2 P3 Ru, 0.5(F6 P), 0.5(C H2 Cl2), 0.5(C H2 Cl2), 0.5(Br),'
_chemical_formula_sum            'C60 H50 Br0.5 Cl2 F3 O2 P3.5 Ru'
_chemical_formula_weight         1180.32
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 107.0630(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.4415(3)
_cell_length_b                   12.2233(3)
_cell_length_c                   27.9952(6)
_cell_measurement_reflns_used    76339
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.022
_cell_measurement_theta_min      2.546
_cell_volume                     5378.5(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Nonius Collect, KappaCCD'
_computing_data_reduction
'Denzo and Scalepak (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEP32 for windows (Farugia)'
_computing_publication_material  'Ciftab (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Nonius Kappa CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0703
_diffrn_reflns_av_sigmaI/netI    0.0529
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            45044
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.59
_exptl_absorpt_coefficient_mu    0.920
_exptl_absorpt_correction_T_max  0.955
_exptl_absorpt_correction_T_min  0.818
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SORTAV
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2404
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.544
_refine_diff_density_min         -0.579
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     748
_refine_ls_number_reflns         9349
_refine_ls_number_restraints     47
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0624
_refine_ls_R_factor_gt           0.0417
_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^)+(0.0323P)^2^+7.9420P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0833
_refine_ls_wR_factor_ref         0.0886
_reflns_number_gt                7414
_reflns_number_total             9349
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900621v_si_001.cif
_cod_data_source_block           tlp00101
_cod_original_sg_symbol_Hall     -P2yc
_cod_original_sg_symbol_H-M      P2/c
_cod_original_formula_sum        'C60 H50 Br0.50 Cl2 F3 O2 P3.50 Ru'
_cod_database_code               4070124