Reactions of Alkynes with [Fe2(CO)6(μ-PPh2){μ-η1:η2α,β-(H)CαCβCγH2}]: Formation of Diphenylvinylphosphine-Functionalized Vinyl Carbenes via Carbon−Carbon and Carbon−Phosphorus Bond Formation and Hydrogen Migration⊥
Doherty, Simon; Hogarth, Graeme; Waugh, Mark; Clegg, William; Elsegood, Mark R. J.; Organometallics 19 (2000) 4557–; doi:10.1021/om0005147

data_4077581
_publ_section_title
;
 Reactions of Alkynes with
 [Fe2(CO)6(\m-PPh2){\m-\h1:\h2\a,\b-(H)C\aC\bC\gH2}]:&#x00A0; Formation of
 Diphenylvinylphosphine-Functionalized Vinyl Carbenes via
 Carbon&#x2212;Carbon and Carbon&#x2212;Phosphorus Bond Formation and
 Hydrogen Migration&#x22A5;
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              4557
_journal_paper_doi               10.1021/om0005147
_journal_volume                  19
_journal_year                    2000
_chemical_formula_sum            'C35 H23 Fe2 O6 P'
_chemical_formula_weight         682.20
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.8592(12)
_cell_length_b                   10.3433(6)
_cell_length_c                   28.1509(15)
_cell_measurement_reflns_used    17439
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.71
_cell_measurement_theta_min      2.31
_cell_volume                     6073.6(6)
_computing_cell_refinement       'local programs'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measurement_device_type  'Bruker SMART CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0535
_diffrn_reflns_av_sigmaI/netI    0.0453
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            36167
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.89
_diffrn_reflns_theta_min         1.75
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.054
_exptl_absorpt_correction_T_max  0.928
_exptl_absorpt_correction_T_min  0.753
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2784
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.476
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.076
_refine_ls_extinction_coef       0.00009(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         7452
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0693
_refine_ls_R_factor_gt           0.0415
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0295P)^2^+4.3513P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0740
_refine_ls_wR_factor_ref         0.0833
_reflns_number_gt                5514
_reflns_number_total             7452
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0005147.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               4077581