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_4113986
_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         'C13 H33 Fe N O P4, C3.5 H4 '
_chemical_formula_sum            'C16.5 H37 Fe N O P4'
_chemical_formula_weight         445.23
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_primary     direct
_audit_creation_date             'Fri Apr 18 10:51:38 2003'
_audit_creation_method           'by teXsan'
_cell_angle_alpha                90
_cell_angle_beta                 98.222(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   29.110(3)
_cell_length_b                   14.188(2)
_cell_length_c                   11.250(1)
_cell_measurement_reflns_used    2213
_cell_measurement_temperature    158.2
_cell_measurement_theta_max      22.5
_cell_measurement_theta_min      1.8
_cell_volume                     4598.6(9)
_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      158.2
_diffrn_measured_fraction_theta_full 0.9640
_diffrn_measured_fraction_theta_max 0.9640
_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  0.038
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3944
_diffrn_reflns_theta_full        24.72
_diffrn_reflns_theta_max         24.72
_diffrn_reflns_theta_min         0.00
_exptl_absorpt_coefficient_mu    0.938
_exptl_absorpt_correction_T_max  0.810
_exptl_absorpt_correction_T_min  0.650
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_description       tablet
_exptl_crystal_F_000             1904.00
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.210
_refine_diff_density_max         1.04
_refine_diff_density_min         -0.62
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.310
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         2031
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0800
_refine_ls_R_factor_gt           0.0371
_refine_ls_shift/su_max          0.0056
_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          0.0419
_refine_ls_wR_factor_ref         0.0475
_reflns_number_gt                2031
_reflns_number_total             3778
_reflns_threshold_expression     F^2^>3.0\s(F^2^)
_cod_data_source_file            ja035707asi20030613_111743.cif
_cod_data_source_block           djf2m_in_C2/c
_cod_original_cell_volume        4598.6(8)
_cod_original_sg_symbol_H-M      'C 2/c '
_cod_original_formula_sum        'C16.50 H37 Fe N O P4 '
_cod_database_code               4113986