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_4119541
_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            'C54 H45 B Fe P2'
_chemical_formula_weight         822.5
_chemical_name_systematic
;
 ?
;
_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                78.661(7)
_cell_angle_beta                 76.780(5)
_cell_angle_gamma                88.148(8)
_cell_formula_units_Z            2
_cell_length_a                   9.8333(19)
_cell_length_b                   11.167(3)
_cell_length_c                   19.774(3)
_cell_measurement_reflns_used    9879
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      39.42
_cell_measurement_theta_min      2.32
_cell_volume                     2072.4(8)
_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, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.19
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.928
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0617
_diffrn_reflns_av_sigmaI/netI    0.0894
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            88753
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         41.29
_diffrn_reflns_theta_min         1.08
_exptl_absorpt_coefficient_mu    0.479
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   none
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_description       block
_exptl_crystal_F_000             860
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.331
_refine_diff_density_min         -0.473
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     543
_refine_ls_number_reflns         25823
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.987
_refine_ls_R_factor_all          0.0929
_refine_ls_R_factor_gt           0.0505
_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^)+(0.0606P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1162
_refine_ls_wR_factor_ref         0.1311
_reflns_number_gt                16012
_reflns_number_total             25823
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja400836u_si_002_1.cif
_cod_data_source_block           5
_cod_original_cell_volume        2072.3(7)
_cod_original_formula_sum        'C54 H45 B1 Fe1 P2'
_cod_database_code               4119541