A Tetrahedrally Coordinated L3Fe-Nx Platform that Accommodates Terminal Nitride (FeIV\τbN) and Dinitrogen (FeI-N2-FeI) Ligands
Theodore A. Betley; Jonas C. Peters; Journal of the American Chemical Society 126 (2004) 6252–6254; doi:10.1021/ja048713v

data_4112591
_publ_section_title
;
 A Tetrahedrally Coordinated L3Fe-Nx Platform that Accommodates Terminal
 Nitride (FeIV\\tbN) and Dinitrogen (FeI-N2-FeI) Ligands
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6252
_journal_page_last               6254
_journal_paper_doi               10.1021/ja048713v
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C39 H63 B Fe N P3'
_chemical_formula_weight         705.47
_chemical_name_common            '[PhBPiPr3]FeNPh2'
_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                87.377(2)
_cell_angle_beta                 75.6030(10)
_cell_angle_gamma                83.956(2)
_cell_formula_units_Z            2
_cell_length_a                   11.0240(9)
_cell_length_b                   13.4574(11)
_cell_length_c                   13.7499(11)
_cell_measurement_reflns_used    5743
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.97
_cell_measurement_theta_min      2.50
_cell_volume                     1964.4(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 0.899
_diffrn_measured_fraction_theta_max 0.899
_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  0.0855
_diffrn_reflns_av_sigmaI/netI    0.0762
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            44708
_diffrn_reflns_theta_full        30.76
_diffrn_reflns_theta_max         30.76
_diffrn_reflns_theta_min         1.52
_exptl_absorpt_coefficient_mu    0.533
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            dichroic
_exptl_crystal_density_diffrn    1.193
_exptl_crystal_density_meas      0
_exptl_crystal_description       blade
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.658
_refine_diff_density_min         -0.432
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.273
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     418
_refine_ls_number_reflns         11014
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.273
_refine_ls_R_factor_all          0.0841
_refine_ls_R_factor_gt           0.0448
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0797
_refine_ls_wR_factor_ref         0.0906
_reflns_number_gt                7304
_reflns_number_total             11014
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja048713vsi20040305_044107_2.cif
_cod_data_source_block           tab47
_cod_database_code               4112591