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_4087482
_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         'C47 H35 Fe3 Ru 1+, F6 P 1-, C3 H6 O1'
_chemical_formula_sum            'C50 H41 F6 Fe3 O P Ru'
_chemical_formula_weight         1071.42
_chemical_name_systematic
;
(1,3,5-Tris(ferrocenylethindiyl)-\h^6^-benzene)
(\h^5^-cyclopentadienyl)ruthenium(II) hexafluoridophosphate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                70.777(1)
_cell_angle_beta                 88.675(1)
_cell_angle_gamma                69.777(1)
_cell_formula_units_Z            2
_cell_length_a                   11.6270(3)
_cell_length_b                   12.2072(4)
_cell_length_c                   16.9848(5)
_cell_measurement_reflns_used    7731
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.14
_cell_measurement_theta_min      2.37
_cell_volume                     2124.75(11)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_collection       'APEX2 v.2014.1-1 (Bruker AXS Inc., 2014)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.914
_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  0.0398
_diffrn_reflns_av_unetI/netI     0.0479
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.914
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            33549
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.914
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.000
_diffrn_reflns_theta_min         1.876
_exptl_absorpt_coefficient_mu    1.455
_exptl_absorpt_correction_T_max  0.7467
_exptl_absorpt_correction_T_min  0.6842
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS-2012/1 (Bruker AXS Inc., 2012)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.669
_exptl_crystal_description       plate
_exptl_crystal_F_000             1076
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.159
_refine_diff_density_min         -0.472
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     689
_refine_ls_number_reflns         11324
_refine_ls_number_restraints     101
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0598
_refine_ls_R_factor_gt           0.0403
_refine_ls_shift/su_max          0.001
_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^+1.3612P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0884
_refine_ls_wR_factor_ref         0.0984
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8554
_reflns_number_total             11324
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00160_si_002.cif
_cod_data_source_block           CpRuBzFc3
_cod_original_formula_sum        'C50 H41 F6 Fe3 O1 P Ru'
_cod_database_code               4087482
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.868
_shelx_estimated_absorpt_t_max   0.971
_shelx_res_checksum              82200
_shelx_hkl_checksum              9398