Reversible Insertion of Carbenes into Ruthenium-Silicon Bonds
María J. Bernal; Olga Torres; Marta Martín; Eduardo Sola; Journal of the American Chemical Society 135 (2013) 19008–19015; doi:10.1021/ja410822p

data_4121356
_publ_contact_author_address
;
  Dr. Marta Mart\'in
  Departamento de Qu\'imica Inorg\'anica - I.C.M.A.
  Facultad de Ciencias
  Universidad de Zaragoza - C.S.I.C.
  50009 Zaragoza, Spain
;
_publ_contact_author_email       martam@unizar.es
_publ_contact_author_fax         '+34 956 761187'
_publ_contact_author_name        'Dr. Marta Mart\'in'
_publ_contact_author_phone       '+34 976 762026'
_publ_section_title
;
 Reversible Insertion of Carbenes into Ruthenium-Silicon Bonds
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              19008
_journal_page_last               19015
_journal_paper_doi               10.1021/ja410822p
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C33 H45 Cl P2 Ru Si'
_chemical_formula_sum            'C33 H45 Cl P2 Ru Si'
_chemical_formula_weight         668.24
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.731(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.422(2)
_cell_length_b                   15.902(2)
_cell_length_c                   13.8473(19)
_cell_measurement_reflns_used    2641
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      22.20
_cell_measurement_theta_min      2.38
_cell_volume                     3174.3(7)
_computing_cell_refinement       'SAINT+ v. 6.01 (Bruker AXS, 2000)'
_computing_data_collection       'SMART v. 5.611 (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT+ v. 6.01 (Bruker AXS, 2000)'
_computing_molecular_graphics    'XP program, SHELXTL v6.10, Bruker2000'
_computing_publication_material  'XCIF program, SHELXTLv6.10,BrukerAXS'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       '\w rotations with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0865
_diffrn_reflns_av_sigmaI/netI    0.1383
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            27419
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.50
_diffrn_reflns_theta_min         1.91
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    0.738
_exptl_absorpt_correction_T_max  0.936
_exptl_absorpt_correction_T_min  0.609
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  SADABS: Area-Detector Absorption Correction. (1996)  Bruker-AXS 
  within SAINT+ package, v. 6.01.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.898
_refine_diff_density_min         -1.033
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.802
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         7560
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.802
_refine_ls_R_factor_all          0.0920
_refine_ls_R_factor_gt           0.0412
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0100P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0608
_refine_ls_wR_factor_ref         0.0700
_reflns_number_gt                4227
_reflns_number_total             7560
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja410822p_si_002_3.cif
_cod_data_source_block           mar200b
_cod_original_cell_volume        3174.3(8)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4121356