H-H and Si-H Bond Addition to Fe\τbNNR2 Intermediates Derived from N2
Daniel L. M. Suess; Jonas C. Peters; Journal of the American Chemical Society 135 (2013) 4938–4941; doi:10.1021/ja400836u

data_4119544
_publ_contact_author_address
;Caltech Division of Chemistry and Chemical Engineering
1200 E. California Blvd.
Pasadena, CA 91125
;
_publ_contact_author_email       jpeters@caltech.edu
_publ_contact_author_name        'Jonas C. Peters'
_publ_contact_author_phone       626-395-3113
_publ_section_title
;
 H-H and Si-H Bond Addition to Fe\\tbNNR2 Intermediates Derived from N2
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4938
_journal_page_last               4941
_journal_paper_doi               10.1021/ja400836u
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C60 H82 B2 Fe2 N2 P4'
_chemical_formula_weight         1088.54
_chemical_name_systematic
;
 ?
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.3660(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.6080(5)
_cell_length_b                   22.6752(7)
_cell_length_c                   18.8057(7)
_cell_measurement_reflns_used    5086
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      35.83
_cell_measurement_theta_min      2.28
_cell_volume                     5645.6(3)
_computing_cell_refinement       'SAINT V7.68A (Bruker-AXS, 2007)'
_computing_data_collection       'APEX2 v2010.7-0 (Bruker-AXS, 2007)'
_computing_data_reduction        'SAINT V7.68A (Bruker-AXS, 2007)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker KAPPA APEX II'
_diffrn_measurement_method       '\w and \f 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  0.0684
_diffrn_reflns_av_sigmaI/netI    0.0406
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            485205
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         46.11
_diffrn_reflns_theta_min         1.43
_exptl_absorpt_coefficient_mu    0.667
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   none
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.281
_exptl_crystal_description       chunk
_exptl_crystal_F_000             2312
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.972
_refine_diff_density_min         -0.338
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     687
_refine_ls_number_reflns         48837
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0668
_refine_ls_R_factor_gt           0.0359
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0375P)^2^+1.2348P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0795
_refine_ls_wR_factor_ref         0.0916
_reflns_number_gt                35070
_reflns_number_total             48837
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja400836u_si_002_4.cif
_cod_data_source_block           4
_cod_database_code               4119544