Iron and Ruthenium σ-Polyynyls of the General Formula [{M(dppe)Cp*}‒(C≡C)n‒R]0/+(M = Fe, Ru): An Experimental and Theoretical Investigation
Gendron, Frédéric; Burgun, Alexandre; Skelton, Brian W.; White, Allan H.; Roisnel, Thierry; Bruce, Michael I.; Halet, Jean-François; Lapinte, Claude; Costuas, Karine; Organometallics 31 (2012) 6796–; doi:10.1021/om300584u

data_4079229
_publ_section_title
;
 Iron and Ruthenium \s-Polyynyls of the General Formula
 [{M(dppe)Cp*}--(C\\tb C)n--R]0/+(M = Fe, Ru): An Experimental and
 Theoretical Investigation
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              6796
_journal_paper_doi               10.1021/om300584u
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C45 H48 Fe P2 Si'
_chemical_formula_sum            'C45 H48 Fe P2 Si'
_chemical_formula_weight         734.71
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2011-01-27T16:32:44-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 102.660(10)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   47.893(3)
_cell_length_b                   17.882(2)
_cell_length_c                   20.3130(10)
_cell_measurement_reflns_used    4477
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      67.2641
_cell_measurement_theta_min      3.1172
_cell_volume                     16974(2)
_computing_cell_refinement
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
        (compiled Nov  6 2009,16:24:50)
;
_computing_data_collection
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
        (compiled Nov  6 2009,16:24:50)
;
_computing_data_reduction
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
        (compiled Nov  6 2009,16:24:50)
;
_computing_molecular_graphics    'OrtepII (Johnson, C. K. (1976)'
_computing_publication_material  'WinGX Farrugia, L. J. (1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4738
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Oxford Diffraction Gemini diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0050758784
_diffrn_orient_matrix_UB_12      0.0792806477
_diffrn_orient_matrix_UB_13      0.0131635705
_diffrn_orient_matrix_UB_21      -0.0257035874
_diffrn_orient_matrix_UB_22      0.0337661298
_diffrn_orient_matrix_UB_23      -0.030004213
_diffrn_orient_matrix_UB_31      -0.0731117051
_diffrn_orient_matrix_UB_32      -0.0064042839
_diffrn_orient_matrix_UB_33      0.0042673046
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1288
_diffrn_reflns_av_unetI/netI     0.1536
_diffrn_reflns_limit_h_max       55
_diffrn_reflns_limit_h_min       -56
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            43988
_diffrn_reflns_theta_full        67.18
_diffrn_reflns_theta_max         67.18
_diffrn_reflns_theta_min         3.32
_exptl_absorpt_coefficient_mu    4.035
_exptl_absorpt_correction_T_max  0.913
_exptl_absorpt_correction_T_min  0.398
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
        (compiled Nov  6 2009,16:24:50)
Analytical numeric absorption correction using a multifaceted crystal
                        model based on expressions derived by R.C. Clark & J.S.
        (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)

;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.15
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             6208
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.763
_refine_diff_density_min         -0.792
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.945
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     960
_refine_ls_number_reflns         14952
_refine_ls_number_restraints     114
_refine_ls_restrained_S_all      0.946
_refine_ls_R_factor_all          0.1386
_refine_ls_R_factor_gt           0.0615
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0702P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1399
_refine_ls_wR_factor_ref         0.1741
_reflns_number_gt                7101
_reflns_number_total             14952
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om300584u_si_007.cif
_cod_data_source_block           br1523
_cod_original_sg_symbol_Hall     '-c 2yc'
_cod_original_sg_symbol_H-M      'c 2/c'
_cod_database_code               4079229