Pyramidal Stability of 16-Electron Half-Sandwich Intermediates [CpRu(P−P)]+with P−P Ligands Forming Four- to Six-Membered Chelate Rings
Brunner, Henri; Muschiol, Manfred; Tsuno, Takashi; Takahashi, Takemoto; Zabel, Manfred; Organometallics 29 (2010) 428–; doi:10.1021/om900830a

data_4063463
_publ_section_title
;
 Pyramidal Stability of 16-Electron Half-Sandwich Intermediates
 [CpRu(P&#x2212;P)]+with P&#x2212;P Ligands Forming Four- to Six-Membered
 Chelate Rings
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              428
_journal_paper_doi               10.1021/om900830a
_journal_volume                  29
_journal_year                    2010
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C31 H29 I P2 Ru'
_chemical_formula_sum            'C31 H29 I P2 Ru'
_chemical_formula_weight         691.45
_chemical_name_systematic        ?
_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
_cell_angle_alpha                78.325(4)
_cell_angle_beta                 88.954(4)
_cell_angle_gamma                76.134(4)
_cell_formula_units_Z            2
_cell_length_a                   9.4185(5)
_cell_length_b                   9.5250(4)
_cell_length_c                   15.8005(7)
_cell_measurement_reflns_used    7988
_cell_measurement_temperature    110
_cell_measurement_theta_max      66.5144
_cell_measurement_theta_min      2.8535
_cell_volume                     1347.02(11)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.30 (release 18-06-2008 CrysAlis171 .NET)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.30 (release 18-06-2008 CrysAlis171 .NET)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.30 (release 18-06-2008 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, 1999)'
_diffrn_ambient_temperature      110
_diffrn_detector_area_resol_mean 10.5431
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_details
;
  1 omega  -63.00  -10.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       11.6137  -45.0000  270.0000    0.0000    0.0000 53

  2 omega  -37.00   16.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -11.6137  -45.0000   90.0000    0.0000    0.0000 53

  3 omega  -45.00   13.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -11.6137   77.0000   60.0000    0.0000    0.0000 58

  4 omega  -90.00  -32.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -11.6137  -77.0000  240.0000    0.0000    0.0000 58

  5 omega  -45.00   13.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -11.6137   77.0000    0.0000    0.0000    0.0000 58

  6 omega  -37.00   16.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -11.6137  -45.0000  210.0000    0.0000    0.0000 53

  7 omega -115.00  -61.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -90.0000  109.0000  219.0000    0.0000    0.0000 54

  8 omega -119.00  -64.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -90.0000  119.0000  344.0000    0.0000    0.0000 55

  9 omega -114.00  -60.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -90.0000  108.0000   86.0000    0.0000    0.0000 54

 10 omega  -69.00  -11.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -90.0000   77.0000  300.0000    0.0000    0.0000 58

 11 omega -111.00  -57.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -90.0000   99.0000  308.0000    0.0000    0.0000 54

 12 omega -112.00  -58.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -90.0000  102.0000  161.0000    0.0000    0.0000 54

 13 omega -124.00  -11.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -90.0000   77.0000  240.0000    0.0000    0.0000 113

 14 omega -115.00  -62.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -90.0000  -45.0000  330.0000    0.0000    0.0000 53

 15 omega   68.00  121.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000  -45.0000   30.0000    0.0000    0.0000 53

 16 omega   66.00  119.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000   45.0000  210.0000    0.0000    0.0000 53

 17 omega   66.00  168.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000   45.0000   90.0000    0.0000    0.0000 102

 18 omega   66.00  119.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000   45.0000   60.0000    0.0000    0.0000 53

 19 omega  114.00  172.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000   77.0000  120.0000    0.0000    0.0000 58

 20 omega   19.00   72.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000  -45.0000  210.0000    0.0000    0.0000 53

 21 omega   15.00   73.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000  -77.0000   60.0000    0.0000    0.0000 58

 22 omega   60.00  122.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000    0.0000  240.0000    0.0000    0.0000 62

 23 omega   69.00  127.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000  -77.0000  270.0000    0.0000    0.0000 58

 24 omega -178.00   -1.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -90.0000    0.0000    0.0000    0.0000    0.0000 177

 25 omega -178.00  -13.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -90.0000    0.0000   30.0000    0.0000    0.0000 165

;
_diffrn_measurement_device_type  'Oxford Diffraction Gemini Ultra'
_diffrn_measurement_method       omega-scan
_diffrn_radiation_monochromator  mirror
_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  0.0347
_diffrn_reflns_av_sigmaI/netI    0.0327
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13547
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        66.76
_diffrn_reflns_theta_max         66.76
_diffrn_reflns_theta_min         2.86
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    14.961
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.31353
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.30 (release 18-06-2008 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'orange to brown'
_exptl_crystal_density_diffrn    1.705
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       'flat rod'
_exptl_crystal_F_000             684
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.814
_refine_diff_density_min         -0.713
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         4620
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0297
_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^)+(0.0535P)^2^]         where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0747
_refine_ls_wR_factor_ref         0.0774
_reflns_number_gt                3961
_reflns_number_total             4620
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om900830a_si_003.cif
_cod_data_source_block           h246
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1673 2011-04-08 12:14:43Z adriana 
;
_cod_database_code               4063463