Reactions of [Ru(CO)2(PPh3)3] with Alkynylphosphonium Salts: Phosphaallenylidene vs Phosphonioacetylide Coordination
Cordiner, Richard L.; Hill, Anthony F.; Wagler, Jörg; Organometallics 28 (2009) 4880–; doi:10.1021/om9003384

data_4069655
_publ_section_title
;
 Reactions of [Ru(CO)2(PPh3)3] with Alkynylphosphonium Salts:
 Phosphaallenylidene vs Phosphonioacetylide Coordination
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              4880
_journal_paper_doi               10.1021/om9003384
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C58 H46 O2 P3 Ru, C H2 Cl2, C F3 O3 S'
_chemical_formula_sum            'C60 H48 Cl2 F3 O5 P3 Ru S'
_chemical_formula_weight         1202.92
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                86.3740(10)
_cell_angle_beta                 78.064(2)
_cell_angle_gamma                79.451(2)
_cell_formula_units_Z            2
_cell_length_a                   10.0272(2)
_cell_length_b                   14.6376(4)
_cell_length_c                   19.3095(7)
_cell_measurement_reflns_used    98580
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      2.546
_cell_volume                     2725.05(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0753
_diffrn_reflns_av_sigmaI/netI    0.0487
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            34494
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.55
_exptl_absorpt_coefficient_mu    0.572
_exptl_absorpt_correction_T_max  0.983
_exptl_absorpt_correction_T_min  0.804
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SORTAV
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.466
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1228
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.616
_refine_diff_density_min         -0.985
_refine_diff_density_rms         0.126
_refine_ls_extinction_coef       0.0080(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     696
_refine_ls_number_reflns         34494
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0747
_refine_ls_R_factor_gt           0.0619
_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^)+(0.0920P)^2^+12.8691P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1684
_refine_ls_wR_factor_ref         0.1768
_reflns_number_gt                8225
_reflns_number_total             9482
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om9003384_si_001.cif
_cod_data_source_block           rc02902_5
_cod_original_sg_symbol_Hall     -P1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4069655