Nucleophilic Addition Reactions to Allenylidene Complexes of Ruthenium Bearing Hemilabile P,N Ligands: Isolation of the Vinylcarbene Complex [Cp*Ru═CHCH═CPh2(iPr2PNHPy)][PF6]
Hyder, Iqbal; Jiménez-Tenorio, Manuel; Puerta, M. Carmen; Valerga, Pedro; Organometallics 30 (2011) 726–; doi:10.1021/om101013j

data_4063892
_publ_section_title
;
 Nucleophilic Addition Reactions to Allenylidene Complexes of Ruthenium
 Bearing Hemilabile P,N Ligands: Isolation of the Vinylcarbene Complex
 [Cp*Ru&#x2550;CHCH&#x2550;CPh2(iPr2PNHPy)][PF6]
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              726
_journal_paper_doi               10.1021/om101013j
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C41 H49 N3 P Ru S, F6 P, 0.49(C H2 Cl2)'
_chemical_formula_sum            'C41.49 H49.97 Cl0.97 F6 N3 P2 Ru S'
_chemical_formula_weight         934.19
_chemical_name_common
;
[(\h^5^-C~5~Me~5~)Ru{\k^2^-C,N-(=C-CH(SC~5~H~4~N)=CPh~2~}
{\k^1^ P-^i^Pr~2~PNH(C~5~H~4~N)}][PF~6~].0.49 (CH~2~Cl~2~)
;
_chemical_name_systematic
;
{(diisopropyl-phosphanyl)-(pyridin-2-yl)-amine-\k^1^-P}-
{1-(2-mercapto-pyridine)-3,3-diphenyl-prop-2-en-1-ylidene--\k^2^-C,N}-
(pentahapto-pentamethyl-cyclopentadienyl)-ruthenium(II) 
hexafluorophosphate dichloromethane solvate
;
_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                 109.74(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.700(3)
_cell_length_b                   15.636(3)
_cell_length_c                   20.907(4)
_cell_measurement_reflns_used    3679
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.796
_cell_measurement_theta_min      2.442
_cell_volume                     4523.1(18)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0699
_diffrn_reflns_av_sigmaI/netI    0.0635
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            25865
_diffrn_reflns_theta_full        23.03
_diffrn_reflns_theta_max         23.03
_diffrn_reflns_theta_min         1.66
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Bruker SMART APEX'
_diffrn_standards_decay_%        0.0023
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.577
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.838
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            dark-red
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1921.6
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.932
_refine_diff_density_min         -0.957
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     545
_refine_ls_number_reflns         6303
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0887
_refine_ls_R_factor_gt           0.0792
_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^)+(0.0166P)^2^+49.8988P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1474
_refine_ls_wR_factor_ref         0.1521
_reflns_number_gt                5834
_reflns_number_total             6303
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om101013j_si_002.cif
_cod_data_source_block           pv0704
_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               4063892