Pyramidal Stability of Chiral-at-Metal Half-Sandwich 16-Electron Fragments [CpRu(P−P′)]
Brunner, Henri; Muschiol, Manfred; Tsuno, Takashi; Takahashi, Takemoto; Zabel, Manfred; Organometallics 27 (2008) 3514–; doi:10.1021/om800148r

data_4071400
_publ_section_title
;
 Pyramidal Stability of Chiral-at-Metal Half-Sandwich 16-Electron
 Fragments [CpRu(P&#x2212;P&#x2032;)]
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              3514
_journal_paper_doi               10.1021/om800148r
_journal_volume                  27
_journal_year                    2008
_chemical_absolute_configuration ad
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C36 H33 Br P2 Ru'
_chemical_formula_structural     'C36 H33 Br P2 Ru'
_chemical_formula_sum            'C36 H33 Br P2 Ru'
_chemical_formula_weight         708.53
_chemical_name_systematic        ?
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.45942(10)
_cell_length_b                   15.52669(14)
_cell_length_c                   15.69572(14)
_cell_measurement_reflns_used    35084
_cell_measurement_temperature    150
_cell_measurement_theta_max      62.8450
_cell_measurement_theta_min      2.8073
_cell_volume                     3036.39(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      150
_diffrn_detector_area_resol_mean 10.5431
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
  1 omega  -79.00  -24.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       -1.3492  -75.0000  120.0000    0.0000    0.0000 55

  2 omega  -29.00   22.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       -1.3492   45.0000  240.0000    0.0000    0.0000 51

  3 omega  -79.00  -24.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       -1.3492  -75.0000    0.0000    0.0000    0.0000 55

  4 omega   23.00   74.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       -1.3492   45.0000  240.0000    0.0000    0.0000 51

  5 omega   27.00   78.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -        3.0060   45.0000  120.0000    0.0000    0.0000 51

  6 omega  -39.00    5.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -        3.0060   98.0000  149.0000    0.0000    0.0000 44

  7 omega   26.00   81.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -        3.0060   75.0000  120.0000    0.0000    0.0000 55

  8 omega   26.00   81.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -        3.0060   75.0000    0.0000    0.0000    0.0000 55

  9 phi   -180.00 -120.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
  40.0000    3.0060    0.0000     -        0.0000    0.0000 60

 10 omega   25.00   77.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -        3.0060   59.0000   43.0000    0.0000    0.0000 52

 11 omega   25.00   79.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -        3.0060   70.0000   55.0000    0.0000    0.0000 54

 12 omega -106.00  -51.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -84.2355  -75.0000  120.0000    0.0000    0.0000 55

 13 omega -106.00  -53.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -84.2355  -63.0000  140.0000    0.0000    0.0000 53

 14 omega -108.00  -57.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -84.2355  -43.0000  333.0000    0.0000    0.0000 51

 15 omega -159.00 -108.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -84.2355  -47.0000   62.0000    0.0000    0.0000 51

 16 omega -106.00  -55.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -84.2355  -57.0000   14.0000    0.0000    0.0000 51

 17 omega -107.00  -56.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -84.2355  -47.0000   41.0000    0.0000    0.0000 51

 18 omega  -62.00   -8.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -84.2355   70.0000   75.0000    0.0000    0.0000 54

 19 omega -108.00  -57.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -84.2355  -43.0000  147.0000    0.0000    0.0000 51

 20 omega -100.00  -35.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -84.2355  -18.0000  169.0000    0.0000    0.0000 65

 21 omega -107.00  -56.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -84.2355  -47.0000   62.0000    0.0000    0.0000 51

 22 omega  -62.00  -10.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -84.2355   59.0000  -82.0000    0.0000    0.0000 52

 23 omega -118.00  -62.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -84.2355   75.0000  240.0000    0.0000    0.0000 56

 24 omega -106.00  -53.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -84.2355  -63.0000  157.0000    0.0000    0.0000 53

 25 omega -159.00 -108.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -84.2355  -45.0000  240.0000    0.0000    0.0000 51

 26 omega -106.00  -53.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -84.2355  -63.0000  126.0000    0.0000    0.0000 53

 27 omega -159.00 -108.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -84.2355  -43.0000  147.0000    0.0000    0.0000 51

 28 omega -118.00  -65.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -84.2355  118.0000  258.0000    0.0000    0.0000 53

 29 omega   57.00  108.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       85.8923   53.0000   55.0000    0.0000    0.0000 51

 30 omega    8.00   63.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       85.8923  -75.0000  240.0000    0.0000    0.0000 55

 31 omega   55.00  108.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       85.8923   63.0000  117.0000    0.0000    0.0000 53

 32 omega    3.00   44.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       85.8923  -98.0000 -137.0000    0.0000    0.0000 41

 33 phi     60.00  120.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
  40.0000   85.8923    0.0000     -        0.0000    0.0000 60

 34 omega   54.00  108.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       85.8923   70.0000   55.0000    0.0000    0.0000 54

 35 omega   64.00  119.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       85.8923  -75.0000  240.0000    0.0000    0.0000 55

 36 omega   54.00  108.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       85.8923   70.0000   75.0000    0.0000    0.0000 54

 37 omega   55.00  108.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       85.8923   66.0000  151.0000    0.0000    0.0000 53

 38 omega   45.00   86.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       85.8923  -98.0000 -137.0000    0.0000    0.0000 41

 39 omega   54.00  107.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       85.8923   67.0000   99.0000    0.0000    0.0000 53

 40 omega   45.00   86.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       85.8923  -98.0000 -149.0000    0.0000    0.0000 41

 41 omega    3.00   44.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       85.8923  -98.0000   30.0000    0.0000    0.0000 41

 42 omega   52.00  108.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       85.8923   77.0000   47.0000    0.0000    0.0000 56

 43 omega   54.00  108.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       85.8923   69.0000   86.0000    0.0000    0.0000 54

 44 omega   54.00  108.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       85.8923   70.0000   77.0000    0.0000    0.0000 54

 45 omega   53.00  108.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       85.8923   75.0000  120.0000    0.0000    0.0000 55

 46 omega  109.00  160.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       85.8923   53.0000   55.0000    0.0000    0.0000 51

 47 omega  108.00  162.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       85.8923   70.0000   77.0000    0.0000    0.0000 54

;
_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           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0289
_diffrn_reflns_av_sigmaI/netI    0.0133
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            43053
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        63.11
_diffrn_reflns_theta_max         63.11
_diffrn_reflns_theta_min         4.00
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.892
_exptl_absorpt_correction_T_max  1.14583
_exptl_absorpt_correction_T_min  0.63065
_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 to orange'
_exptl_crystal_density_diffrn    1.550
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.229
_exptl_crystal_size_mid          0.213
_exptl_crystal_size_min          0.147
_refine_diff_density_max         0.606
_refine_diff_density_min         -0.320
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details 'Flack H.D. (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.028(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         4873
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0208
_refine_ls_R_factor_gt           0.0203
_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^)+(0.0357P)^2^+1.2435P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0526
_refine_ls_wR_factor_ref         0.0528
_reflns_number_gt                4736
_reflns_number_total             4873
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om800148r-file003.cif
_cod_data_source_block           norrubr
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               4071400