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_4087480
_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         'C11 H8 I3 Ru 1+, B F4 1-'
_chemical_formula_sum            'C11 H8 B F4 I3 Ru'
_chemical_formula_weight         708.75
_chemical_name_systematic
;
(\h^6^-1,3,5-Triiodobenzene)(\h^5^-cyclopentadienyl)ruthenium(II) 
hexafluoridophosphate  
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_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                 105.779(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.4810(9)
_cell_length_b                   16.883(2)
_cell_length_c                   13.0316(16)
_cell_measurement_reflns_used    16440
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.53
_cell_measurement_theta_min      2.41
_cell_volume                     1583.9(3)
_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 0.984
_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  0.0590
_diffrn_reflns_av_unetI/netI     0.0375
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            18651
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.500
_diffrn_reflns_theta_min         2.413
_exptl_absorpt_coefficient_mu    6.862
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.471
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Bruker AXS)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.972
_exptl_crystal_description       plate
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.158
_refine_diff_density_min         -1.068
_refine_diff_density_rms         0.201
_refine_ls_abs_structure_details
;
 Flack x determined using 2518 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         5460
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0319
_refine_ls_R_factor_gt           0.0316
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0482P)^2^+4.7338P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0806
_refine_ls_wR_factor_ref         0.0808
_reflns_Friedel_coverage         0.934
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.923
_reflns_number_gt                5416
_reflns_number_total             5460
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00160_si_002.cif
_cod_data_source_block           CpRuBzI3
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               4087480
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.204
_shelx_estimated_absorpt_t_max   0.493
_shelx_res_checksum              33276
_shelx_hkl_checksum              83443