Proton-Controlled Regioselective Synthesis of [Cp*(dppe)Fe‒C\τb C-1-(η6-C10H7)Ru(η5-Cp](PF6) and Electron-Driven Haptotropic Rearrangement of the (η5-Cp)Ru+Arenophile
Makhoul, Rim; Sahnoune, Hiba; Davin, Thomas; Kahlal, Samia; Dorcet, Vincent; Roisnel, Thierry; Halet, Jean-François; Hamon, Jean-René; Lapinte, Claude; Organometallics 33 (2014) 4792–; doi:10.1021/om500047k

data_4082886
_publ_section_title
;
 Proton-Controlled Regioselective Synthesis of [Cp*(dppe)Fe--C\\tb
 C-1-(\h6-C10H7)Ru(\h5-Cp](PF6) and Electron-Driven Haptotropic
 Rearrangement of the (\h5-Cp)Ru+Arenophile
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              4792
_journal_paper_doi               10.1021/om500047k
_journal_volume                  33
_journal_year                    2014
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C53 H51 Fe P2 Ru, F6 P'
_chemical_formula_sum            'C53 H51 F6 Fe P3 Ru'
_chemical_formula_weight         1051.77
_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
_cell_angle_alpha                90
_cell_angle_beta                 92.692(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.3298(5)
_cell_length_b                   23.7633(8)
_cell_length_c                   17.4117(6)
_cell_measurement_reflns_used    5794
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.48
_cell_measurement_theta_min      2.27
_cell_measurement_wavelength     0.71073
_cell_volume                     4682.6(3)
_computing_cell_refinement       'Bruker APEX2 (Bruker, 2006)'
_computing_data_collection       'Bruker APEX2 (Bruker, 2006)'
_computing_data_reduction        'Bruker APEX2 (Bruker, 2006)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material
;
           WinGX publication routines (Farrugia, 2012),
           CRYSCAL (T. Roisnel, local program)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'APEXII, Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thin slices'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0641
_diffrn_reflns_av_unetI/netI     0.0841
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            37116
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    0.795
_exptl_absorpt_correction_T_max  0.961
_exptl_absorpt_correction_T_min  0.887
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       stick
_exptl_crystal_F_000             2152
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         5.639
_refine_diff_density_min         -3.044
_refine_diff_density_rms         0.177
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     510
_refine_ls_number_reflns         10659
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.1744
_refine_ls_R_factor_gt           0.119
_refine_ls_shift/su_max          0.028
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1745P)^2^+56.0086P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3099
_refine_ls_wR_factor_ref         0.351
_reflns_number_gt                6593
_reflns_number_total             10659
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500047k_si_001.cif
_cod_data_source_block           RM0118_2
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4082886