Regioselective Addition oftert-BuN⋮C to the α Carbon Atom of the Allenyl Ligand in [Fe2(CO)6(μ-PPh2){μ-η1:η2α,β-(H)CαCβCγH2}]: Formation of [Fe2(CO)6(μ-PPh2){μ-η1:η1-(tert-BuN⋮C)CCCH3}] and [Fe2(CO)6(μ-PPh2)(μ-η1:η2-{tert-BuNHC(O)CH2}CCH2)] via Competitive 1,3-Hydrogen Migration and Hydrolysis of the Reactive Allene-Bridged Intermediate [Fe2(CO)6(μ-PPh2){μ-η1:η1-(tert-BuNC)HCCCH2}]
Doherty, Simon; Hogarth, Graeme; Waugh, Mark; Scanlan, Tom H.; Clegg, William; Elsegood, Mark R. J.; Organometallics 18 (1999) 3178–; doi:10.1021/om9901630

data_4077786
_publ_section_title
;
 Regioselective Addition oftert-BuN&#x22EE;C to the \a Carbon Atom of the
 Allenyl Ligand in
 [Fe2(CO)6(\m-PPh2){\m-\h1:\h2\a,\b-(H)C\aC\bC\gH2}]:&#x00A0; Formation of
 [Fe2(CO)6(\m-PPh2){\m-\h1:\h1-(tert-BuN&#x22EE;C)CCCH3}] and
 [Fe2(CO)6(\m-PPh2)(\m-\h1:\h2-{tert-BuNHC(O)CH2}CCH2)] via Competitive
 1,3-Hydrogen Migration and Hydrolysis of the Reactive Allene-Bridged
 Intermediate [Fe2(CO)6(\m-PPh2){\m-\h1:\h1-(tert-BuNC)HCCCH2}]
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              3178
_journal_paper_doi               10.1021/om9901630
_journal_volume                  18
_journal_year                    1999
_chemical_formula_sum            'C25 H24 Fe2 N O6 P'
_chemical_formula_weight         577.12
_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 H1A&B coords freely refined'
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                91.276(2)
_cell_angle_beta                 99.797(2)
_cell_angle_gamma                103.431(2)
_cell_formula_units_Z            2
_cell_length_a                   8.5433(5)
_cell_length_b                   11.6773(7)
_cell_length_c                   13.4130(7)
_cell_measurement_reflns_used    8255
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.69
_cell_measurement_theta_min      2.29
_cell_volume                     1279.87(13)
_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_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  0.0156
_diffrn_reflns_av_sigmaI/netI    0.0264
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9461
_diffrn_reflns_theta_max         28.84
_diffrn_reflns_theta_min         1.54
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.236
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.686
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.540
_refine_diff_density_min         -0.370
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         5695
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0330
_refine_ls_R_factor_gt           0.0298
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0435P)^2^+0.6001P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0775
_refine_ls_wR_factor_ref         0.0804
_reflns_number_gt                5265
_reflns_number_total             5695
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om9901630.cif
_cod_data_source_block           5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0435P)^2^+0.6001P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0435P)^2^+0.6001P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4077786