(η6-Arene)−Ruthenium(II) Complexes Containing Methanide and Methandiide Anions of Ph2P(S)CH2P(NR)Ph2: Unprecedented Insertion of Isocyanide into a Ruthenium−Carbene Bond
Cadierno, Victorio; Díez, Josefina; García-Álvarez, Joaquín; Gimeno, José; Organometallics 27 (2008) 1809–; doi:10.1021/om701228a

data_4071049
_publ_section_title
;
 (\h6-Arene)&#x2212;Ruthenium(II) Complexes Containing Methanide and
 Methandiide Anions of Ph2P(&#xE5FB;S)CH2P(&#xE5FB;NR)Ph2: Unprecedented
 Insertion of Isocyanide into a Ruthenium&#x2212;Carbene Bond
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              1809
_journal_paper_doi               10.1021/om701228a
_journal_volume                  27
_journal_year                    2008
_chemical_compound_source        synthesis
_chemical_formula_moiety         'C47 H45 N O3 P3 Ru S, F6 Sb'
_chemical_formula_sum            'C47 H45 F6 N O3 P3 Ru S Sb'
_chemical_formula_weight         1133.63
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 115.9120(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.0192(2)
_cell_length_b                   12.3803(2)
_cell_length_c                   20.9031(2)
_cell_measurement_temperature    100(2)
_cell_volume                     4659.87(11)
_computing_cell_refinement       'Bruker SMART (Bruker 2001)'
_computing_data_collection       'Bruker SMART (Bruker 2001)'
_computing_data_reduction        'Bruker SAINT (Bruker 2000)'
_computing_molecular_graphics    'PLATON (Spek, 2006)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0548
_diffrn_reflns_av_sigmaI/netI    0.0510
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            28909
_diffrn_reflns_theta_full        70.61
_diffrn_reflns_theta_max         70.61
_diffrn_reflns_theta_min         2.55
_exptl_absorpt_coefficient_mu    9.179
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.169337
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick,G.M.,1997-2001)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.616
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2272
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.433
_refine_diff_density_min         -2.364
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     563
_refine_ls_number_reflns         8540
_refine_ls_number_restraints     87
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0704
_refine_ls_R_factor_gt           0.0609
_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^)+(0.0821P)^2^+25.8365P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1586
_refine_ls_wR_factor_ref         0.1684
_reflns_number_gt                7256
_reflns_number_total             8540
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om701228a-file002.cif
_cod_data_source_block           3f
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Empirical' changed to
'empirical' 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_cell_volume        4659.86(10)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4071049