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_4077583
_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            'C37 H25 Fe2 O6 P'
_chemical_formula_weight         708.24
_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_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.133(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.3078(19)
_cell_length_b                   9.5600(12)
_cell_length_c                   21.656(3)
_cell_measurement_reflns_used    11135
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      29.12
_cell_measurement_theta_min      3.11
_cell_volume                     3168.6(7)
_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 0.997
_diffrn_measured_fraction_theta_max 0.916
_diffrn_measurement_device_type  'Bruker SMART CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Daresbury SRS Station 9.8'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6890
_diffrn_reflns_av_R_equivalents  0.0664
_diffrn_reflns_av_sigmaI/netI    0.0988
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            22243
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.49
_diffrn_reflns_theta_min         2.21
_diffrn_standards_decay_%        65
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.013
_exptl_absorpt_correction_T_max  0.962
_exptl_absorpt_correction_T_min  0.578
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.385
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.890
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         8859
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.890
_refine_ls_R_factor_all          0.0900
_refine_ls_R_factor_gt           0.0526
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0635P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1161
_refine_ls_wR_factor_ref         0.1220
_reflns_number_gt                5372
_reflns_number_total             8859
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0005147.cif
_cod_data_source_block           4
_cod_original_cell_volume        3168.5(7)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4077583