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_4071398
_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         'C32 H31 Br P2 Ru'
_chemical_formula_structural     'C32 Br P2 Ru'
_chemical_formula_sum            'C32 H31 Br P2 Ru'
_chemical_formula_weight         658.48
_chemical_name_systematic        ?
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 112.4786(12)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.65602(10)
_cell_length_b                   14.95694(10)
_cell_length_c                   10.48788(10)
_cell_measurement_reflns_used    16128
_cell_measurement_temperature    123
_cell_measurement_theta_max      51.2038
_cell_measurement_theta_min      4.5500
_cell_volume                     1399.62(2)
_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, 1999)'
_diffrn_ambient_temperature      150(1)
_diffrn_detector_area_resol_mean 10.5431
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega  -33.00   22.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -        0.1529   75.0000  240.0000    0.0000    0.0000 55

  2 omega   24.00   75.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -        0.1529   45.0000    0.0000    0.0000    0.0000 51

  3 omega   23.00   78.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -        0.1529   75.0000  120.0000    0.0000    0.0000 55

  4 omega  -51.00    1.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -60.8272  102.0000  328.0000    0.0000    0.0000 52

  5 omega -136.00  -85.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -60.8272  -45.0000  120.0000    0.0000    0.0000 51

  6 omega -135.00  -83.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -60.8272  -62.0000  180.0000    0.0000    0.0000 52

  7 omega  -84.00  -33.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -60.8272  -45.0000  120.0000    0.0000    0.0000 51

  8 omega -109.00  -58.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -60.8272  110.0000  202.0000    0.0000    0.0000 51

  9 omega  -82.00  -28.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -60.8272  -71.0000   46.0000    0.0000    0.0000 54

 10 omega  -83.00  -28.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -60.8272  -75.0000  120.0000    0.0000    0.0000 55

 11 omega  -82.00  -28.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -60.8272  -71.0000  255.0000    0.0000    0.0000 54

 12 omega -137.00  -83.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -60.8272  -71.0000  255.0000    0.0000    0.0000 54

 13 omega  -83.00  -30.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -60.8272  -65.0000   51.0000    0.0000    0.0000 53

 14 omega   98.00  145.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       62.4840   16.0000   66.0000    0.0000    0.0000 47

 15 omega   85.00  140.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       62.4840   74.0000  -85.0000    0.0000    0.0000 55

 16 omega   51.00   98.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       62.4840   16.0000   66.0000    0.0000    0.0000 47

 17 omega  -83.00  -27.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -60.8272  -77.0000  112.0000    0.0000    0.0000 56

 18 omega  -97.00  -39.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -60.8272   25.0000 -177.0000    0.0000    0.0000 58

 19 omega  -97.00  -39.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -60.8272   25.0000  160.0000    0.0000    0.0000 58

 20 omega  -83.00  -28.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -60.8272  -74.0000   18.0000    0.0000    0.0000 55

 21 omega  -38.00   17.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -60.8272   75.0000  120.0000    0.0000    0.0000 55

 22 omega  -83.00  -28.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -60.8272  -75.0000    0.0000    0.0000    0.0000 55

 23 omega  -83.00  -29.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -60.8272  -69.0000    8.0000    0.0000    0.0000 54

 24 omega  -39.00   19.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -60.8272   25.0000  160.0000    0.0000    0.0000 58

 25 omega  -94.00  -39.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -60.8272   75.0000    0.0000    0.0000    0.0000 55

 26 omega  -83.00  -28.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -60.8272  -73.0000  150.0000    0.0000    0.0000 55

 27 omega  -22.00   33.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -        0.1529  -75.0000    0.0000    0.0000    0.0000 55

 28 omega  -78.00  -23.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -        0.1529  -75.0000  120.0000    0.0000    0.0000 55

 29 omega   22.00   80.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -        0.1529   25.0000  160.0000    0.0000    0.0000 58

 30 omega   28.00   85.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       62.4840   78.0000  138.0000    0.0000    0.0000 57

 31 omega   28.00   85.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       62.4840   78.0000  113.0000    0.0000    0.0000 57

 32 omega   29.00   85.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       62.4840   76.0000  141.0000    0.0000    0.0000 56

 33 omega  -94.00  -39.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -60.8272   75.0000  240.0000    0.0000    0.0000 55

 34 omega  -38.00   17.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -60.8272   75.0000    0.0000    0.0000    0.0000 55

 35 omega -104.00  -52.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -60.8272  102.0000  328.0000    0.0000    0.0000 52

 36 omega  -39.00   19.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -60.8272   25.0000 -177.0000    0.0000    0.0000 58

 37 omega  -89.00  -38.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -60.8272   45.0000  120.0000    0.0000    0.0000 51

 38 omega  -37.00   14.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -60.8272   45.0000  120.0000    0.0000    0.0000 51

 39 omega  -84.00  -33.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -60.8272  -45.0000    0.0000    0.0000    0.0000 51

 40 omega  -89.00  -38.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -60.8272   45.0000  240.0000    0.0000    0.0000 51

 41 omega  -83.00  -27.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -60.8272  -77.0000  217.0000    0.0000    0.0000 56

 42 omega  -94.00  -39.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -60.8272   75.0000  120.0000    0.0000    0.0000 55

 43 omega   23.00   78.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -        0.1529   75.0000    0.0000    0.0000    0.0000 55

 44 omega   24.00   75.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -        0.1529   45.0000  120.0000    0.0000    0.0000 51

 45 omega  -75.00  -50.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -        0.1529  -45.0000    0.0000    0.0000    0.0000 25

;
_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  0.0328
_diffrn_reflns_av_sigmaI/netI    0.0169
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            17986
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        51.38
_diffrn_reflns_theta_max         51.38
_diffrn_reflns_theta_min         4.56
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.424
_exptl_absorpt_correction_T_max  1.17771
_exptl_absorpt_correction_T_min  0.73228
_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            orange
_exptl_crystal_density_diffrn    1.5625
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.128
_exptl_crystal_size_mid          0.106
_exptl_crystal_size_min          0.088
_refine_diff_density_max         0.269
_refine_diff_density_min         -0.295
_refine_diff_density_rms         0.043
_refine_ls_abs_structure_details 'Flack H.D. (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.029(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         2986
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0173
_refine_ls_R_factor_gt           0.0168
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0326P)^2^+0.0385P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0425
_refine_ls_wR_factor_ref         0.0426
_reflns_number_gt                2909
_reflns_number_total             2986
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om800148r-file001.cif
_cod_data_source_block           mubr
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_original_sg_symbol_H-M      'P 21'
_cod_database_code               4071398