Iron Diazoalkane Chemistry: N-N Bond Hydrogenation and Intramolecular C-H Activation
Suzanne C. Bart; Amanda C. Bowman; Emil Lobkovsky; Paul J. Chirik; Journal of the American Chemical Society 129 (2007) 7212–7213; doi:10.1021/ja070056u

data_4109495
_publ_section_title
;
 Iron Diazoalkane Chemistry: N-N Bond Hydrogenation and Intramolecular C-H
 Activation
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7212
_journal_page_last               7213
_journal_paper_doi               10.1021/ja070056u
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C37 H53 Fe N5 Si'
_chemical_formula_weight         651.78
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 111.727(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.3507(11)
_cell_length_b                   11.3702(7)
_cell_length_c                   18.7766(12)
_cell_measurement_reflns_used    8335
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      31.40
_cell_measurement_theta_min      2.23
_cell_volume                     3639.4(4)
_computing_cell_refinement       'Bruker SAINT+'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT+'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker X8 APEX II diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0348
_diffrn_reflns_av_sigmaI/netI    0.0385
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            55861
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         2.14
_exptl_absorpt_coefficient_mu    0.479
_exptl_absorpt_correction_T_max  0.9537
_exptl_absorpt_correction_T_min  0.8316
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.190
_exptl_crystal_density_meas      0
_exptl_crystal_description       plate
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.418
_refine_diff_density_min         -0.310
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     466
_refine_ls_number_reflns         11101
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0614
_refine_ls_R_factor_gt           0.0395
_refine_ls_shift/su_max          0.933
_refine_ls_shift/su_mean         0.013
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0666P)^2^+0.2696P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1078
_refine_ls_wR_factor_ref         0.1178
_reflns_number_gt                8270
_reflns_number_total             11101
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja070056usi20070104_104942.cif
_cod_data_source_block           scb42
_cod_database_code               4109495