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_4079228
_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 P2 Ru Si, 1/4(C6 H14)'
_chemical_formula_sum            'C46.5 H51.5 P2 Ru Si'
_chemical_formula_weight         801.48
_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             2011-06-23T11:41:05-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 102.174(5)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   48.476(14)
_cell_length_b                   18.052(6)
_cell_length_c                   20.193(6)
_cell_measurement_reflns_used    6352
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.53
_cell_measurement_theta_min      2.31
_cell_volume                     17273(9)
_computing_cell_refinement       'Siemens SAINT (Siemens, 1995)'
_computing_data_collection       'Siemens SMART (Siemens, 1995)'
_computing_data_reduction        'xtal ADDREF SORTRF'
_computing_molecular_graphics    'OrtepII (Johnson, C. K. (1976)'
_computing_publication_material  'WinGX Farrugia, L. J. (1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    Sir92
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type
;
        Bruker SMART CCD diffractometer
;
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.072
_diffrn_reflns_av_unetI/netI     0.0794
_diffrn_reflns_limit_h_max       61
_diffrn_reflns_limit_h_min       -63
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            68019
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.59
_diffrn_reflns_theta_min         1.21
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.494
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  .84
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS; Sheldrick, 1996
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.233
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       bar
_exptl_crystal_F_000             6696
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.501
_refine_diff_density_min         -0.74
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     925
_refine_ls_number_reflns         19746
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.099
_refine_ls_R_factor_gt           0.0603
_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^)+(0.0709P)^2^+54.1096P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.138
_refine_ls_wR_factor_ref         0.1567
_reflns_number_gt                13480
_reflns_number_total             19746
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om300584u_si_005.cif
_cod_data_source_block           br1092
_cod_original_sg_symbol_Hall     '-c 2yc'
_cod_original_sg_symbol_H-M      C_1_2/c_1
_cod_original_formula_sum        'C46.50 H51.50 P2 Ru Si'
_cod_database_code               4079228