Counteranion-Dependent Reaction Pathways in the Protonation of Cationic Ruthenium‒Vinylidene Complexes
Jiménez-Tenorio, Manuel; Puerta, M. Carmen; Valerga, Pedro; Ortuño, Manuel A.; Ujaque, Gregori; Lledós, Agust\?í; Organometallics 33 (2014) 2549–; doi:10.1021/om500179x

data_4083146
_publ_section_title
;
 Counteranion-Dependent Reaction Pathways in the Protonation of Cationic
 Ruthenium--Vinylidene Complexes
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              2549
_journal_paper_doi               10.1021/om500179x
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C29 H40 Br Cl N2 P Ru, B F4, H2 O'
_chemical_formula_sum            'C29 H42 B Br Cl F4 N2 O P Ru'
_chemical_formula_weight         768.86
_chemical_name_common
'[(\h^5^-C~5~Me~5~)Ru{PyNHP(^i^Pr~2~)CH=CHC~6~H~4~Br}Cl][BF~4~]H~2~O'
_chemical_name_systematic
;
{\h^2^-[2-(4-Bromo-phenyl)-vinyl]-di(isopropyl)-(pyridin-2-yl-amine)-
phosphonium-\k^1^ N}-chloro-(\h^5^-pentamethylcyclopentadienyl)-ruthenium(II)
tetrafluoroborate hydrate
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                83.25(3)
_cell_angle_beta                 82.86(3)
_cell_angle_gamma                87.94(3)
_cell_formula_units_Z            2
_cell_length_a                   7.9304(16)
_cell_length_b                   11.059(2)
_cell_length_c                   18.655(4)
_cell_measurement_reflns_used    5082
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.050
_cell_measurement_theta_min      2.215
_cell_volume                     1611.8(6)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics    'ORTEP-3 vers. 1.08 (Farrugia, 2005)'
_computing_publication_material  'SHELXTL (Sheldrick, 2001)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2001)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2001)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '1700 omega scan frames, 0.3 deg, 10 sec'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0275
_diffrn_reflns_av_sigmaI/netI    0.0431
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            11393
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.11
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Bruker SMART APEX'
_diffrn_standards_decay_%        -0.0078
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.907
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.858
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.584
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             780
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.572
_refine_diff_density_min         -0.938
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     386
_refine_ls_number_reflns         5635
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0429
_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^)+(0.0459P)^2^+4.4803P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1041
_refine_ls_wR_factor_ref         0.1068
_reflns_number_gt                5118
_reflns_number_total             5635
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500179x_si_003.cif
_cod_data_source_block           pv0607
_cod_depositor_comments
'Adding full bibliography for 4083146--4083147.cif.'
_cod_database_code               4083146