Synthesis of the Five-Coordinate Ruthenium(II) Complexes [(PCP)Ru(CO)(L)][BAr'4] {PCP = 2,6-(CH2PtBu2)2C6H3, BAr'4= 3,5-(CF3)2C6H3, L = η1-ClCH2Cl, η1-N2, or μ-Cl-Ru(PCP)(CO)}: Reactions with Phenyldiazomethane and Phenylacetylene
Jubo Zhang; Khaldoon A. Barakat; Thomas R. Cundari; T. Brent Gunnoe; Paul D. Boyle; Jeffrey L. Petersen; Cynthia S. Day; Inorganic Chemistry 44 (2005) 8379–8390; doi:10.1021/ic051074k

data_4309986
_publ_section_title
;
Synthesis of the Five-Coordinate Ruthenium(II) Complexes
[(PCP)Ru(CO)(L)][BAr'4] {PCP = 2,6-(CH2PtBu2)2C6H3, BAr'4=
3,5-(CF3)2C6H3, L = \h1-ClCH2Cl, \h1-N2, or \m-Cl-Ru(PCP)(CO)}:
Reactions with Phenyldiazomethane and Phenylacetylene
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8379
_journal_page_last               8390
_journal_paper_doi               10.1021/ic051074k
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C64 H61 B F24 O P2 Ru'
_chemical_formula_weight         1475.95
_chemical_name_systematic
; 
[(PCP-CHPh)Ru(CO)][BAr'4]
;
_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                73.8410(10)
_cell_angle_beta                 79.9790(10)
_cell_angle_gamma                89.8710(10)
_cell_formula_units_Z            2
_cell_length_a                   12.7936(8)
_cell_length_b                   15.1290(10)
_cell_length_c                   18.1187(11)
_cell_measurement_temperature    295(2)
_cell_volume                     3313.1(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.939
_diffrn_measured_fraction_theta_max 0.939
_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  0.0455
_diffrn_reflns_av_sigmaI/netI    0.0947
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            22237
_diffrn_reflns_theta_full        27.43
_diffrn_reflns_theta_max         27.43
_diffrn_reflns_theta_min         2.08
_exptl_absorpt_coefficient_mu    0.393
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'dark red '
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.460
_refine_diff_density_min         -0.403
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1074
_refine_ls_number_reflns         14198
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      6.027
_refine_ls_R_factor_all          0.0817
_refine_ls_R_factor_gt           0.0624
_refine_ls_shift/su_max          0.104
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1049P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1642
_refine_ls_wR_factor_ref         0.1814
_reflns_number_gt                10903
_reflns_number_total             14198
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic051074ksi20050629_043939_5.cif
_cod_data_source_block           compound-7
_cod_database_code               4309986