Nonclassical vs Classical Metal...H3C-C Interactions: Accurate Characterization of a 14-Electron Ruthenium(II) System by Neutron Diffraction, Database Analysis, Solution Dynamics, and DFT Studies
Walter Baratta; Carlo Mealli; Eberhardt Herdtweck; Andrea Ienco; Sax A. Mason; Pierluigi Rigo; Journal of the American Chemical Society 126 (2004) 5549–5562; doi:10.1021/ja038986a

data_4112530
_publ_contact_author
;
       Dr. Eberhardt Herdtweck,
       Anorganisch-chemisches Institut der
       Technischen Universit\"at M\"unchen,
       Lichtenbergstrasse 4,
       D-85747 Garching bei M\"unchen,
       Germany.
;
_publ_contact_author_email       eberhardt.herdtweck@ch.tum.de
_publ_contact_author_fax         ' +49(0)89 289 13473'
_publ_contact_author_phone       '+49(0)89 289 13143'
_publ_section_title
;
 Nonclassical vs Classical Metal...H3C-C Interactions: Accurate
 Characterization of a 14-Electron Ruthenium(II) System by Neutron
 Diffraction, Database Analysis, Solution Dynamics, and DFT Studies
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5549
_journal_page_last               5562
_journal_paper_doi               10.1021/ja038986a
_journal_volume                  126
_journal_year                    2004
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C40 H38 Cl2 P2 Ru, C7 H8'
_chemical_formula_sum            'C47 H46 Cl2 P2 Ru'
_chemical_formula_weight         844.75
_chemical_name_systematic
;
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             29-Aug-00
_audit_creation_method           'PLATON <TABLE ACC> option'
_audit_update_record
;
  1-Sep-00  Updated by the Author E.H.
  29-Oct-02  Updated by the Author E.H.
            Textwriting by E.H.
            Checkcif    OK
  30-Oct-02  Updated by the Author E.H.
  30-Jul-03  Updated by the Author E.H.
  9-Oct-03  Updated by the Author E.H.
;
_cell_angle_alpha                89.465(6)
_cell_angle_beta                 89.799(6)
_cell_angle_gamma                96.143(6)
_cell_formula_units_Z            2
_cell_length_a                   10.533(1)
_cell_length_b                   12.728(1)
_cell_length_c                   14.913(1)
_cell_measurement_reflns_used    2226
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      45.1
_cell_measurement_theta_min      7.6
_cell_volume                     1987.7(3)
_computing_cell_refinement       ILL-software
_computing_data_collection       ILL-software
_computing_data_reduction        ILL-software
_computing_molecular_graphics    'PLATON PLUTON (Spek, 2001)'
_computing_publication_material  'PLATON (Spek, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1998)'
_computing_structure_solution    'BARK 3066 (Baratta, 1999)'
_diffrn_ambient_temperature      100.0(5)
_diffrn_measurement_device       D19
_diffrn_measurement_method       ' # see _exptl_special_details '
_diffrn_radiation_probe          neutron
_diffrn_radiation_source         ILL
_diffrn_radiation_type           neutron
_diffrn_radiation_wavelength     1.5364
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_sigmaI/netI    0.0391
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5468
_diffrn_reflns_theta_max         56.88
_diffrn_reflns_theta_min         2.95
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.239
_exptl_absorpt_correction_T_max  0.9120
_exptl_absorpt_correction_T_min  0.8595
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
 The intensities were corrected for attenuation by the cylindrical V and Al
 heat shields (minimum and maximum transmission coefficients 0.8624 and
 0.8981 at 1.3072 \%A; 0.8349 and 0.8901 at 1.5364 \%A, and by the crystal
 itself (C47 H46 Cl2 P2 Ru, Formula_Weight =  844.75, F(000) = 872.0,
 mu(neutron)  = 0.221 mm-1 at 1.3072 \%A, 0.239 mm-1 at 1.5364 \%A,
 minimum and maximum transmission coefficients 0.8826 and 0.9181 at
 1.3072 \%A; 0.8595 and 0.9120 at 1.5364 \%A ) with the program D19abs,
 based on the ILL version of the CCSL system ( Matthewman et al, 1982)
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       needle
_exptl_crystal_F_000             872
_exptl_crystal_size_max          3.25
_exptl_crystal_size_mid          0.75
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.720
_refine_diff_density_min         -0.704
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     884
_refine_ls_number_reflns         5468
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0727
_refine_ls_R_factor_gt           0.0641
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
' w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+63.79081P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.1261
_refine_ls_wR_factor_ref         0.1305
_reflns_number_gt                4930
_reflns_number_total             5468
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja038986asi20031010_124309.cif
_cod_data_source_block           BARKN-5001-100
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4112530