Internal Alkyne Isomerization to Vinylidene versus Stable π-Alkyne: Theoretical and Experimental Study on the Divergence of Analogous Cp*Ru and TpRu Systems
Singh, Vinay K.; Bustelo, Emilio; de los Ríos, Isaac; Macías-Arce, Ignacio; Puerta, M. Carmen; Valerga, Pedro; Ortuño, Manuel Ángel; Ujaque, Gregori; Lledós, Agustí; Organometallics 30 (2011) 4014–; doi:10.1021/om200273v

data_4064692
_publ_section_title
;
 Internal Alkyne Isomerization to Vinylidene versus Stable \p-Alkyne:
 Theoretical and Experimental Study on the Divergence of Analogous Cp*Ru
 and TpRu Systems
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              4014
_journal_paper_doi               10.1021/om200273v
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C20 H28 B Cl N7 P Ru S'
_chemical_formula_sum            'C20 H28 B Cl N7 P Ru S'
_chemical_formula_weight         576.86
_chemical_name_systematic
; 
chloro-{hydrogen-tris(pyrazolyl)borato-\k^3^-N,N',N''}-{2-(diisopropyl-
phosphanyl-mercapto)-pyridine-\k^2^-P,N}-ruthenium(II)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 92.76(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   30.334(6)
_cell_length_b                   10.568(2)
_cell_length_c                   15.019(3)
_cell_measurement_reflns_used    4011
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.966
_cell_measurement_theta_min      2.349
_cell_volume                     4809.1(16)
_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 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0760
_diffrn_reflns_av_sigmaI/netI    0.0729
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            29934
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         0.67
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Bruker SMART APEX'
_diffrn_standards_decay_%        0.0012
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.940
_exptl_absorpt_correction_T_max  0.960
_exptl_absorpt_correction_T_min  0.603
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.593
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2352
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.52
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.998
_refine_diff_density_min         -0.476
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     585
_refine_ls_number_reflns         8374
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0860
_refine_ls_R_factor_gt           0.0625
_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^)+(0.0492P)^2^+14.3646P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1191
_refine_ls_wR_factor_ref         0.1295
_reflns_number_gt                6835
_reflns_number_total             8374
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200273v_si_002.cif
_cod_data_source_block           pv0806
_cod_depositor_comments
;
 Replacing the "\K" substring with the "\k" substring in the
 values of the _chemical_name_common and _chemical_name_systematic
 data items.

 Antanas Vaitkus,
 2017-03-29
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4064692