Synthesis of a First-Row Transition Metal Parent Amido Complex and Carbon Monoxide Insertion into the Amide N-H Bond
Daniel J. Fox; Robert G. Bergman; Journal of the American Chemical Society 125 (2003) 8984–8985; doi:10.1021/ja035707a

data_4113985
_publ_section_title
;
 Synthesis of a First-Row Transition Metal Parent Amido Complex and Carbon
 Monoxide Insertion into the Amide N-H Bond
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8984
_journal_page_last               8985
_journal_paper_doi               10.1021/ja035707a
_journal_volume                  125
_journal_year                    2003
_chemical_formula_moiety         'C12 H35 Fe N P4 '
_chemical_formula_sum            'C12 H35 Fe N P4'
_chemical_formula_weight         373.16
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_primary     direct
_audit_creation_date             'Fri Apr 18 11:07:42 2003'
_audit_creation_method           'by teXsan'
_cell_angle_alpha                90
_cell_angle_beta                 91.736(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.5433(3)
_cell_length_b                   12.2238(4)
_cell_length_c                   16.8938(5)
_cell_measurement_reflns_used    2526
_cell_measurement_temperature    154.2
_cell_measurement_theta_max      22.5
_cell_measurement_theta_min      1.8
_cell_volume                     1969.85(11)
_computing_cell_refinement       'Bruker SAINT v5.04'
_computing_data_collection       'Bruker SMART v5.0'
_computing_data_reduction        'Bruker SAINT v5.04'
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      154.2
_diffrn_measured_fraction_theta_full 0.9669
_diffrn_measured_fraction_theta_max 0.9669
_diffrn_measurement_device_type  'SMART CCD'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.043
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            3383
_diffrn_reflns_theta_full        24.62
_diffrn_reflns_theta_max         24.62
_diffrn_reflns_theta_min         0.00
_exptl_absorpt_coefficient_mu    1.077
_exptl_absorpt_correction_T_max  0.850
_exptl_absorpt_correction_T_min  0.590
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.258
_exptl_crystal_description       tablet
_exptl_crystal_F_000             800.00
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.77
_refine_diff_density_min         -0.64
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.745
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         1911
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0822
_refine_ls_R_factor_gt           0.0469
_refine_ls_shift/su_max          0.0005
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00022|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0516
_refine_ls_wR_factor_ref         0.0553
_reflns_number_gt                1911
_reflns_number_total             3218
_reflns_threshold_expression     F^2^>3.0\s(F^2^)
_cod_data_source_file            ja035707asi20030613_111731.cif
_cod_data_source_block           DJF276_for_Dan_Fox_@_-117C
_cod_original_cell_volume        1969.8(1)
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_original_formula_sum        'C12 H35 Fe N P4 '
_cod_database_code               4113985