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_4077582
_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            'C30 H21 Fe2 O6 P'
_chemical_formula_weight         620.14
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   'geom except H3&33 coords freely refined'
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                109.143(2)
_cell_angle_beta                 99.880(2)
_cell_angle_gamma                104.577(2)
_cell_formula_units_Z            4
_cell_length_a                   12.5509(6)
_cell_length_b                   15.3144(8)
_cell_length_c                   15.9483(8)
_cell_measurement_reflns_used    14709
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.83
_cell_measurement_theta_min      2.61
_cell_volume                     2692.3(2)
_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 0.987
_diffrn_measured_fraction_theta_max 0.888
_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  0.0159
_diffrn_reflns_av_sigmaI/netI    0.0330
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            22404
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.03
_diffrn_reflns_theta_min         1.41
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.180
_exptl_absorpt_correction_T_max  0.726
_exptl_absorpt_correction_T_min  0.460
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.530
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.78
_exptl_crystal_size_mid          0.58
_exptl_crystal_size_min          0.29
_refine_diff_density_max         0.545
_refine_diff_density_min         -0.347
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     711
_refine_ls_number_reflns         12746
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0302
_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^)+(0.0440P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0721
_refine_ls_wR_factor_ref         0.0736
_reflns_number_gt                9987
_reflns_number_total             12746
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0005147.cif
_cod_data_source_block           3a
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4077582