Stille Cross-Coupling Reaction with Cationic [(η5-Cp)(η6-C6H6‒xIx)Ru]+ Complexes as Key for Ethynyl-Bridged Homo- and Heteronuclear Sandwich Compounds
Ziemann, Elisabeth A.; Baljak, Sladjana; Steffens, Stefan; Stein, Timo; Van Steerteghem, Nick; Asselberghs, Inge; Clays, Koen; Heck, Jürgen; Organometallics 34 (2015) 1692–; doi:10.1021/acs.organomet.5b00160

data_4087481
_publ_section_title
;
 Stille Cross-Coupling Reaction with Cationic [(\h5-Cp)(\h6-C6H6--xIx)Ru]+
 Complexes as Key for Ethynyl-Bridged Homo- and Heteronuclear Sandwich
 Compounds
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              1692
_journal_paper_doi               10.1021/acs.organomet.5b00160
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C23 H19 Fe Ru 1+, F6 P 1-'
_chemical_formula_sum            'C23 H19 F6 Fe P Ru'
_chemical_formula_weight         597.27
_chemical_name_systematic
;
(Ferrocenylethindiyl-\h^6^-benzene)(\h^5^-cyclopentadienyl)
ruthenium(II) hexafluoridophosphate
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   18.7608(9)
_cell_length_b                   48.464(2)
_cell_length_c                   9.2144(4)
_cell_measurement_reflns_used    8689
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.5
_cell_measurement_theta_min      2.5
_cell_volume                     8377.9(6)
_computing_cell_refinement       'SAINT (Bruker AXS, 2008)'
_computing_data_collection       'SMART (Bruker AXS, 2008)'
_computing_data_reduction        'SAINT (Bruker AXS, 2008)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart APEX CCD area detector'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'Incoatec microfocus'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0508
_diffrn_reflns_av_unetI/netI     0.0279
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       73
_diffrn_reflns_limit_k_min       -72
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            55277
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.480
_diffrn_reflns_theta_min         2.328
_exptl_absorpt_coefficient_mu    1.552
_exptl_absorpt_correction_T_max  0.8991
_exptl_absorpt_correction_T_min  0.5109
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Bruker AXS)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.894
_exptl_crystal_description       plate
_exptl_crystal_F_000             4736
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.999
_refine_diff_density_min         -0.593
_refine_diff_density_rms         0.102
_refine_ls_abs_structure_details
;
 Flack x determined using 3362 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.014(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         7548
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0296
_refine_ls_R_factor_gt           0.0289
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0422P)^2^+3.9833P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0678
_refine_ls_wR_factor_ref         0.0680
_reflns_Friedel_coverage         0.895
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                7364
_reflns_number_total             7548
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00160_si_002.cif
_cod_data_source_block           CpRuBzFc
_cod_original_cell_volume        8377.9(7)
_cod_database_code               4087481
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.511
_shelx_estimated_absorpt_t_max   0.899
_shelx_res_checksum              77812
_shelx_hkl_checksum              39408