Hydrogenolysis of [PhBP3]Fe\τbN-p-tolyl: Probing the Reactivity of an Iron Imide with H2
Steven D. Brown; Jonas C. Peters; Journal of the American Chemical Society 126 (2004) 4538–4539; doi:10.1021/ja0399122

data_4112424
_publ_section_title
;
 Hydrogenolysis of [PhBP3]Fe\\tbN-p-tolyl: Probing the Reactivity of an
 Iron Imide with H2
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4538
_journal_page_last               4539
_journal_paper_doi               10.1021/ja0399122
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C52 H49 B Fe N P3'
_chemical_formula_weight         847.49
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                80.110(2)
_cell_angle_beta                 77.925(2)
_cell_angle_gamma                87.176(2)
_cell_formula_units_Z            2
_cell_length_a                   10.0087(9)
_cell_length_b                   14.8340(13)
_cell_length_c                   15.2850(13)
_cell_measurement_reflns_used    6347
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.25
_cell_volume                     2186.0(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_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      100(2)
_diffrn_measured_fraction_theta_full 0.915
_diffrn_measured_fraction_theta_max 0.915
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0567
_diffrn_reflns_av_sigmaI/netI    0.0548
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            38891
_diffrn_reflns_theta_full        28.36
_diffrn_reflns_theta_max         28.36
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    0.492
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            light
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_density_meas      0
_exptl_crystal_description       rough
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.121
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.956
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     524
_refine_ls_number_reflns         10010
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.956
_refine_ls_R_factor_all          0.0776
_refine_ls_R_factor_gt           0.0489
_refine_ls_shift/su_max          0.190
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0813
_refine_ls_wR_factor_ref         0.0846
_reflns_number_gt                7136
_reflns_number_total             10010
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0399122si20040306_051507_2.cif
_cod_data_source_block           sdb38
_cod_database_code               4112424