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_4079226
_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         'C46 H44 P2 Ru'
_chemical_formula_sum            'C46 H44 P2 Ru'
_chemical_formula_weight         759.82
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2008-06-29T09:48:53-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 107.285(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6501(4)
_cell_length_b                   35.7310(13)
_cell_length_c                   10.2532(3)
_cell_measurement_reflns_used    21482
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      32.5281
_cell_measurement_theta_min      2.6296
_cell_volume                     3725.5(2)
_computing_cell_refinement
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
        (compiled Jan 10 2008,16:37:18)
;
_computing_data_collection
;
        CrysAlis CCD, Oxford Diffraction Ltd.,
        Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
        (compiled Jan 10 2008,16:37:18)
;
_computing_data_reduction
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
        (compiled Jan 10 2008,16:37:18)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean 16.0009
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device_type
;
 Oxford Diffraction Xcalibur diffractometer
;
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0236723188
_diffrn_orient_matrix_UB_12      0.0032750378
_diffrn_orient_matrix_UB_13      -0.0686728541
_diffrn_orient_matrix_UB_21      0.0228217421
_diffrn_orient_matrix_UB_22      -0.0180239311
_diffrn_orient_matrix_UB_23      -0.0115654084
_diffrn_orient_matrix_UB_31      -0.0644800771
_diffrn_orient_matrix_UB_32      -0.0075850126
_diffrn_orient_matrix_UB_33      -0.0021301407
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0481
_diffrn_reflns_av_unetI/netI     0.061
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       53
_diffrn_reflns_limit_k_min       -53
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            58066
_diffrn_reflns_theta_full        32
_diffrn_reflns_theta_max         32.63
_diffrn_reflns_theta_min         2.63
_exptl_absorpt_coefficient_mu    0.539
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.99088
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
        (compiled Jan 10 2008,16:37:18)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1576
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.327
_refine_diff_density_min         -0.384
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.942
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     447
_refine_ls_number_reflns         13019
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.942
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_gt           0.0371
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0408P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0774
_refine_ls_wR_factor_ref         0.0813
_reflns_number_gt                9594
_reflns_number_total             13019
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            om300584u_si_001.cif
_cod_data_source_block           br1430a
_cod_original_sg_symbol_Hall     -p_2ybc
_cod_database_code               4079226