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_4071401
_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 I P2 Ru), (C H2 Cl2)'
_chemical_formula_structural     'C36 H33 I P2 Ru, (C H2 Cl2)'
_chemical_formula_sum            'C37 H35 Cl2 I P2 Ru'
_chemical_formula_weight         840.46
_chemical_name_systematic        ?
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      5
_symmetry_space_group_name_Hall  'I 2y'
_symmetry_space_group_name_H-M   'I 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 112.352(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.3029(3)
_cell_length_b                   11.3714(3)
_cell_length_c                   20.1949(4)
_cell_measurement_reflns_used    17545
_cell_measurement_temperature    123
_cell_measurement_theta_max      28.9545
_cell_measurement_theta_min      3.0577
_cell_volume                     3462.57(14)
_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(1)
_diffrn_detector_area_resol_mean 10.5431
_diffrn_measured_fraction_theta_full 0.934
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measurement_details
;
  1 omega  -33.00   18.00   1.0000   25.9000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -10.0296  -45.0000  120.0000    0.0000    0.0000 51

  2 omega  -85.00  -34.00   1.0000   25.9000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -10.0296  -45.0000  120.0000    0.0000    0.0000 51

  3 omega  -33.00   18.00   1.0000   25.9000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -10.0296  -45.0000    0.0000    0.0000    0.0000 51

  4 omega  -32.00   21.00   1.0000   25.9000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -10.0296  -65.0000  163.0000    0.0000    0.0000 53

  5 phi   -180.00 -120.00   1.0000   25.9000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
 -40.0000  -10.0296    0.0000     -        0.0000    0.0000 60

  6 omega  -85.00  -34.00   1.0000   25.9000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -10.0296  -45.0000    0.0000    0.0000    0.0000 51

  7 omega   34.00   89.00   1.0000   25.9000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       11.3358   75.0000    0.0000    0.0000    0.0000 55

  8 omega  -11.00   45.00   1.0000   25.9000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       11.3358  -77.0000  278.0000    0.0000    0.0000 56

  9 omega  -56.00  -11.00   1.0000   25.9000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       11.3358  -75.0000  120.0000    0.0000    0.0000 45

 10 omega   54.00   82.00   1.0000   25.9000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       11.3358   45.0000  240.0000    0.0000    0.0000 28

 11 omega  -11.00   45.00   1.0000   25.9000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       11.3358  -75.0000  120.0000    0.0000    0.0000 56

 12 omega  -67.00  -11.00   1.0000   25.9000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       11.3358  -77.0000  278.0000    0.0000    0.0000 56

 13 omega    8.00   37.00   1.0000   25.9000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       11.3358  -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 (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0452
_diffrn_reflns_av_sigmaI/netI    0.0486
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            28060
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        29.00
_diffrn_reflns_theta_max         29.00
_diffrn_reflns_theta_min         3.08
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.617
_exptl_absorpt_correction_T_max  1.07793
_exptl_absorpt_correction_T_min  0.91776
_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    1.612
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'plate like'
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.856
_refine_diff_density_min         -0.665
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details 'Flack H.D. (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.014(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.976
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         8136
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.975
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0316
_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^)+(0.0391P)^2^]         where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0653
_refine_ls_wR_factor_ref         0.0674
_reflns_number_gt                6864
_reflns_number_total             8136
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om800148r-file004.cif
_cod_data_source_block           runori1
_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      'I 2'
_cod_database_code               4071401