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_4063467
_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         'C33 H33 Cl P2 Ru'
_chemical_formula_sum            'C66 H66 Cl2 P4 Ru2'
_chemical_formula_weight         628.05
_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                 99.227(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.4176(2)
_cell_length_b                   15.3229(3)
_cell_length_c                   19.8384(4)
_cell_measurement_reflns_used    10092
_cell_measurement_temperature    110
_cell_measurement_theta_max      66.2934
_cell_measurement_theta_min      2.2550
_cell_volume                     2825.74(10)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 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 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_details
;
  1 omega  -45.00   13.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -11.6137   77.0000  270.0000    0.0000    0.0000 58

  2 omega  -14.00   39.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       11.6137  -45.0000   90.0000    0.0000    0.0000 53

  3 omega  -67.00   -9.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       11.6137  -77.0000    0.0000    0.0000    0.0000 58

  4 omega   40.00  101.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       11.6137    0.0000  270.0000    0.0000    0.0000 61

  5 omega   -7.00   42.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       11.6137  -63.0000   58.0000    0.0000    0.0000 49

  6 omega -115.00  -62.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -90.0000  -45.0000  240.0000    0.0000    0.0000 53

  7 omega -166.00  -58.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -90.0000  -71.0000  213.0000    0.0000    0.0000 108

  8 omega -114.00  -61.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -90.0000  -77.0000  240.0000    0.0000    0.0000 53

  9 omega -165.00 -111.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -90.0000  -45.0000   60.0000    0.0000    0.0000 54

 10 omega -175.00 -117.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -90.0000    0.0000   60.0000    0.0000    0.0000 58

 11 omega -113.00  -59.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -90.0000  -63.0000   58.0000    0.0000    0.0000 54

 12 omega   20.00  121.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000  -45.0000  210.0000    0.0000    0.0000 101

 13 omega    4.00   64.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000    0.0000    0.0000    0.0000    0.0000 60

 14 omega   69.00  126.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000  -77.0000  120.0000    0.0000    0.0000 57

 15 omega   68.00  121.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000  -45.0000  270.0000    0.0000    0.0000 53

 16 omega   61.00  117.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000   71.0000  146.0000    0.0000    0.0000 56

 17 omega    4.00   62.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000    0.0000   60.0000    0.0000    0.0000 58

 18 omega    9.00   64.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000    0.0000  300.0000    0.0000    0.0000 55

 19 omega  114.00  147.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000   77.0000   90.0000    0.0000    0.0000 33

 20 omega   29.00  123.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000  -71.0000   33.0000    0.0000    0.0000 94

 21 omega   34.00   70.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000  -45.0000   30.0000    0.0000    0.0000 36

 22 omega   72.00  107.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000   45.0000   60.0000    0.0000    0.0000 35

 23 omega  121.00  162.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       93.5000   71.0000  343.0000    0.0000    0.0000 41

;
_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  0.0443
_diffrn_reflns_av_sigmaI/netI    0.0449
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            22037
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        66.44
_diffrn_reflns_theta_max         66.44
_diffrn_reflns_theta_min         2.26
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.581
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61915
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.105
_refine_diff_density_min         -0.880
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details 'Flack H.D. (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.000(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     667
_refine_ls_number_reflns         9598
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0423
_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^)+(0.0641P)^2^+2.2878P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1039
_refine_ls_wR_factor_ref         0.1093
_reflns_number_gt                8199
_reflns_number_total             9598
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om900830a_si_007.cif
_cod_data_source_block           h141
_cod_depositor_comments
;
 Changing the _chemical_formula_sum data item value from
 'C67 H66 L2 P4 R U2' to 'C66 H66 Cl2 P4 Ru2'.

 Antanas Vaitkus,
 2017-01-04

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_original_sg_symbol_H-M      'P 21'
_cod_original_formula_sum        'C66 H66 CL2 P4 RU2'
_cod_database_code               4063467