Ruthenium Complexes with Vinyl, Styryl, and Vinylpyrenyl Ligands: A Case of Non-innocence in Organometallic Chemistry
Jörg Maurer; Michael Linseis; Biprajit Sarkar; Brigitte Schwederski; Mark Niemeyer; Wolfgang Kaim; Stanislav Záliš; Chris Anson; Manfred Zabel; Rainer F. Winter; Journal of the American Chemical Society 130 (2008) 259–268; doi:10.1021/ja075547t

data_4107277
_publ_section_title
;
 Ruthenium Complexes with Vinyl, Styryl, and Vinylpyrenyl Ligands: A Case
 of Non-innocence in Organometallic Chemistry
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              259
_journal_page_last               268
_journal_paper_doi               10.1021/ja075547t
_journal_volume                  130
_journal_year                    2008
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C51 H50 Cl N O3 P2 Ru'
_chemical_formula_structural     'C51 H50 Cl N O3 P2 Ru'
_chemical_formula_sum            'C51 H50 Cl N O3 P2 Ru'
_chemical_formula_weight         923.38
_chemical_name_systematic        ?
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             'May 08 08:40:31 2007'
_audit_creation_method           'PLATON <TABLE ACC> option'
_cell_angle_alpha                90
_cell_angle_beta                 111.9273(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.23180(8)
_cell_length_b                   26.71192(10)
_cell_length_c                   13.38617(10)
_cell_measurement_reflns_used    52345
_cell_measurement_temperature    123
_cell_measurement_theta_max      62.1229
_cell_measurement_theta_min      1.9968
_cell_volume                     4389.03(5)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.30.3 (release 12-05-2006 CrysAlis171 .NET)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.30.3 (release 12-05-2006 CrysAlis171 .NET)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.30.3 (release 12-05-2006 CrysAlis171 .NET)
;
_computing_molecular_graphics    'PLATON (Spek, 1990)'
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-97 (Altomare, 1993)'
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean 10.5431
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_details
;
  1 omega  -25.00   32.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       -1.2571  -75.0000  120.0000    0.0000    0.0000 57

  2 omega   19.00   77.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       -1.2571   75.0000  240.0000    0.0000    0.0000 58

  3 omega   24.00   77.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -        2.5071   45.0000    0.0000    0.0000    0.0000 53

  4 phi     88.00  150.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
  40.0000    2.5071    0.0000     -        0.0000    0.0000 62

  5 omega -116.00  -58.00   1.0000    1.8000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -83.1433   75.0000  240.0000    0.0000    0.0000 58

  6 omega  -62.00   -5.00   1.0000    1.8000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -83.1433   75.0000  240.0000    0.0000    0.0000 57

  7 omega -107.00  -52.00   1.0000    1.8000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -83.1433  -64.0000   53.0000    0.0000    0.0000 55

  8 omega -111.00  -57.00   1.0000    1.8000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -83.1433   45.0000    0.0000    0.0000    0.0000 54

  9 omega -123.00  -69.00   1.0000    1.8000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -83.1433  127.0000  337.0000    0.0000    0.0000 54

 10 omega  -73.00  -20.00   1.0000    1.8000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -83.1433  127.0000  337.0000    0.0000    0.0000 53

 11 omega -161.00 -103.00   1.0000    1.8000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -83.1433  -75.0000  240.0000    0.0000    0.0000 58

 12 omega -113.00  -56.00   1.0000    1.8000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -83.1433  105.0000  324.0000    0.0000    0.0000 57

 13 omega  -61.00   -8.00   1.0000    1.8000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -83.1433   45.0000    0.0000    0.0000    0.0000 53

 14 omega   53.00  109.00   1.0000    1.8000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       84.3933   66.0000  -56.0000    0.0000    0.0000 56

 15 omega  105.00  159.00   1.0000    1.8000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       84.3933   61.0000  -88.0000    0.0000    0.0000 54

 16 omega  105.00  159.00   1.0000    1.8000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       84.3933   60.0000   -4.0000    0.0000    0.0000 54

 17 omega   57.00  110.00   1.0000    1.8000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       84.3933   45.0000  120.0000    0.0000    0.0000 53

 18 omega   53.00   94.00   1.0000    1.8000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       84.3933 -121.0000   58.0000    0.0000    0.0000 41

 19 omega   61.00  118.00   1.0000    1.8000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       84.3933  -75.0000    0.0000    0.0000    0.0000 57

 20 omega   56.00  109.00   1.0000    1.8000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       84.3933   52.0000  174.0000    0.0000    0.0000 53

 21 omega   54.00  109.00   1.0000    1.8000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       84.3933   62.0000  239.0000    0.0000    0.0000 55

 22 omega  105.00  159.00   1.0000    1.8000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       84.3933   62.0000  239.0000    0.0000    0.0000 54

 23 phi     58.00  122.00   1.0000    1.8000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
  40.0000   84.3933    0.0000     -        0.0000    0.0000 64

 24 phi   -122.00  -58.00   1.0000    1.8000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
 -40.0000  -83.1433    0.0000     -        0.0000    0.0000 64

 25 phi     28.00   92.00   1.0000    1.8000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
 -40.0000  -83.1433    0.0000     -        0.0000    0.0000 64

 26 phi     58.00  122.00   1.0000    1.8000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
 -40.0000  -83.1433    0.0000     -        0.0000    0.0000 64

 27 phi    -92.00  -28.00   1.0000    1.8000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
 -40.0000  -83.1433    0.0000     -        0.0000    0.0000 64

 28 phi     -2.00   62.00   1.0000    1.8000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
 -40.0000  -83.1433    0.0000     -        0.0000    0.0000 64

 29 phi    -32.00   32.00   1.0000    1.8000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
 -40.0000  -83.1433    0.0000     -        0.0000    0.0000 64

 30 phi   -150.00  -88.00   1.0000    1.8000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
 -40.0000  -83.1433    0.0000     -        0.0000    0.0000 62

 31 phi   -180.00 -118.00   1.0000    1.8000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
 -40.0000  -83.1433    0.0000     -        0.0000    0.0000 62

 32 phi     88.00  150.00   1.0000    1.8000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
 -40.0000  -83.1433    0.0000     -        0.0000    0.0000 62

 33 phi    118.00  180.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
 -40.0000   -1.2571    0.0000     -        0.0000    0.0000 62

 34 phi     28.00   92.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
 -40.0000   -1.2571    0.0000     -        0.0000    0.0000 64

 35 phi     28.00   92.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
  40.0000    2.5071    0.0000     -        0.0000    0.0000 64

 36 omega   23.00   80.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -        2.5071   75.0000  240.0000    0.0000    0.0000 57

 37 phi   -122.00  -58.00   1.0000    1.8000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
  40.0000   84.3933    0.0000     -        0.0000    0.0000 64

 38 phi    -92.00  -28.00   1.0000    1.8000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
  40.0000   84.3933    0.0000     -        0.0000    0.0000 64

 39 phi    -32.00   32.00   1.0000    1.8000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
  40.0000   84.3933    0.0000     -        0.0000    0.0000 64

 40 phi     28.00   92.00   1.0000    1.8000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
  40.0000   84.3933    0.0000     -        0.0000    0.0000 64

 41 phi    -62.00    2.00   1.0000    1.8000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
  40.0000   84.3933    0.0000     -        0.0000    0.0000 64

 42 phi     -2.00   62.00   1.0000    1.8000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
  40.0000   84.3933    0.0000     -        0.0000    0.0000 64

 43 phi   -150.00  -88.00   1.0000    1.8000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
  40.0000   84.3933    0.0000     -        0.0000    0.0000 62

 44 phi   -180.00 -118.00   1.0000    1.8000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
  40.0000   84.3933    0.0000     -        0.0000    0.0000 62

 45 phi     88.00  150.00   1.0000    1.8000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
  40.0000   84.3933    0.0000     -        0.0000    0.0000 62

 46 phi    118.00  180.00   1.0000    1.8000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
  40.0000   84.3933    0.0000     -        0.0000    0.0000 62

 47 phi    -62.00    2.00   1.0000    1.8000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
 -40.0000  -83.1433    0.0000     -        0.0000    0.0000 64

 48 phi    118.00  180.00   1.0000    1.8000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
 -40.0000  -83.1433    0.0000     -        0.0000    0.0000 62

 49 omega -161.00 -103.00   1.0000    1.8000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -83.1433  -75.0000    0.0000    0.0000    0.0000 58

 50 omega -161.00 -103.00   1.0000    1.8000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -83.1433  -75.0000    0.0000    0.0000    0.0000 58

 51 omega -161.00 -103.00   1.0000    1.8000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -83.1433  -75.0000    0.0000    0.0000    0.0000 58

 52 omega -161.00 -103.00   1.0000    1.8000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -83.1433  -75.0000    0.0000    0.0000    0.0000 58

 53 omega -107.00  -50.00   1.0000    1.8000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -83.1433  -75.0000  240.0000    0.0000    0.0000 57

 54 omega -116.00  -58.00   1.0000    1.8000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -83.1433   75.0000    0.0000    0.0000    0.0000 58

 55 omega -116.00  -87.00   1.0000    1.8000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -83.1433   75.0000    0.0000    0.0000    0.0000 29

;
_diffrn_measurement_device_type  'Oxford Diffraction Gemini Ultra'
_diffrn_measurement_method       omega-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0349
_diffrn_reflns_av_sigmaI/netI    0.0182
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            81848
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        63.34
_diffrn_reflns_theta_max         63.34
_diffrn_reflns_theta_min         3.31
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.484
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.11184
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.30.3 (release 12-05-2006 CrysAlis171 .NET)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1912
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.130
_refine_diff_density_max         1.936
_refine_diff_density_min         -0.688
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     534
_refine_ls_number_reflns         6910
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0336
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0677P)^2^+1.2615P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0932
_refine_ls_wR_factor_ref         0.0966
_reflns_number_gt                5949
_reflns_number_total             6910
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja075547tsi20070921_093159.cif
_cod_data_source_block           ml10
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4107277