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_4063465
_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
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_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              428
_journal_paper_doi               10.1021/om900830a
_journal_volume                  29
_journal_year                    2010
_chemical_absolute_configuration ad
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C33 H33 I P2 Ru'
_chemical_formula_sum            'C33 H33 I P2 Ru'
_chemical_formula_weight         719.50
_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                 100.283(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.9397(14)
_cell_length_b                   15.6337(11)
_cell_length_c                   9.4492(6)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    123
_cell_measurement_theta_max      26.91
_cell_measurement_theta_min      2.59
_cell_volume                     2898.3(3)
_computing_cell_refinement       'STOE (1998)'
_computing_data_collection       'STOE (1998)'
_computing_data_reduction        'STOE (1998)'
_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      123(1)
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device_type  'STOE-IPDS diffractometer'
_diffrn_measurement_method       rotation
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0310
_diffrn_reflns_av_sigmaI/netI    0.0565
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            30381
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        26.91
_diffrn_reflns_theta_max         26.91
_diffrn_reflns_theta_min         2.59
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.738
_exptl_absorpt_correction_T_max  0.8243
_exptl_absorpt_correction_T_min  0.7128
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
'analytical from crystal shape (X-SHAPE, X-RED. STOE, 1996)'
_exptl_crystal_colour            'orange to red'
_exptl_crystal_density_diffrn    1.649
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.040
_refine_diff_density_max         1.211
_refine_diff_density_min         -0.409
_refine_diff_density_rms         0.112
_refine_ls_abs_structure_details 'Flack H.D. (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.023(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.904
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     667
_refine_ls_number_reflns         11955
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.904
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0303
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0314P)^2^]         where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0607
_refine_ls_wR_factor_ref         0.0620
_reflns_number_gt                9847
_reflns_number_total             11955
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om900830a_si_005.cif
_cod_data_source_block           h197
_cod_depositor_comments
;
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_database_code               4063465