Isomerization of Internal Alkynones to Vinylidenes in Tris(pyrazolyl)borate Ruthenium Complexes. Solution and Solid-State Kinetics
de los Ríos, Isaac; Bustelo, Emilio; Puerta, M. Carmen; Valerga, Pedro; Organometallics 29 (2010) 1740–; doi:10.1021/om100084x

data_4065699
_publ_section_title
;
 Isomerization of Internal Alkynones to Vinylidenes in
 Tris(pyrazolyl)borate Ruthenium Complexes. Solution and Solid-State
 Kinetics
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1740
_journal_paper_doi               10.1021/om100084x
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         'C33 H40 B N7 O P Ru, C32 H12 B F24, C6 H5 F'
_chemical_formula_sum            'C71 H57 B2 F25 N7 O P Ru'
_chemical_formula_weight         1652.90
_chemical_name_common
;
[TpRu{=C=C(Ph)COPh}(PMe^i^Pr~2~)(NCCH~3~)][B(C~8~H~3~F~6~)~4~].C~6~H~5~F
;
_chemical_name_systematic
;
Acetonitrile-(2-benzoyl-2-phenyl-ethenylidene)-{hydrogen-tris(pyrazolyl)borato-
\k^3^-N,N',N''}-(diisopropyl-methyl-phosphino)-ruthenium (II)
tetrakis{3,5-bis(trifluoromethyl)phenyl}borate fluoro-benzene solvate
;
_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                108.86(3)
_cell_angle_beta                 105.85(3)
_cell_angle_gamma                93.60(3)
_cell_formula_units_Z            2
_cell_length_a                   12.659(3)
_cell_length_b                   16.205(3)
_cell_length_c                   19.600(4)
_cell_measurement_reflns_used    9792
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.983
_cell_measurement_theta_min      2.224
_cell_volume                     3609.4(17)
_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  0.0238
_diffrn_reflns_av_sigmaI/netI    0.0377
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            25658
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.70
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Bruker SMART APEX'
_diffrn_standards_decay_%        0.0021
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.353
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.839
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            red-orange
_exptl_crystal_density_diffrn    1.521
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1668
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.595
_refine_diff_density_min         -0.975
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1003
_refine_ls_number_reflns         12571
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0535
_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^)+(0.0497P)^2^+8.5616P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1219
_refine_ls_wR_factor_ref         0.1249
_reflns_number_gt                11699
_reflns_number_total             12571
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100084x_si_002.cif
_cod_data_source_block           pv0734
_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_cell_volume        3609.6(12)
_cod_database_code               4065699