A Low-Spin d5 Iron Imide: Nitrene Capture by Low-Coordinate Iron(I) Provides the 4-Coordinate Fe(III) Complex [PhB(CH2PPh2)3]Fe\τbN-p-tolyl
Steven D. Brown; Theodore A. Betley; Jonas C. Peters; Journal of the American Chemical Society 125 (2003) 322–323; doi:10.1021/ja028448i

data_4113387
_publ_section_title
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 A Low-Spin d5 Iron Imide: Nitrene Capture by Low-Coordinate Iron(I)
 Provides the 4-Coordinate Fe(III) Complex [PhB(CH2PPh2)3]Fe\\tbN-p-tolyl
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_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              322
_journal_page_last               323
_journal_paper_doi               10.1021/ja028448i
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C71 H69 B Fe P4'
_chemical_formula_weight         1112.80
_space_group_IT_number           61
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_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.2596(6)
_cell_length_b                   17.7356(6)
_cell_length_c                   33.4617(11)
_cell_measurement_reflns_used    37660
_cell_measurement_temperature    98(2)
_cell_measurement_theta_max      28.42
_cell_measurement_theta_min      2.28
_cell_volume                     12023.3(7)
_computing_cell_refinement       'Bruker SAINT v6.022'
_computing_data_collection       'Bruker SMART v5.054'
_computing_data_reduction        'Bruker SAINT v6.022'
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_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      98(2)
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       '\w scans at 5 \f settings'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
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_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            174637
_diffrn_reflns_theta_full        28.58
_diffrn_reflns_theta_max         28.58
_diffrn_reflns_theta_min         1.58
_exptl_absorpt_coefficient_mu    0.399
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'Pale orange'
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_description       Plate
_exptl_crystal_F_000             4688
_exptl_crystal_size_max          0.29
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_refine_ls_R_factor_gt           0.0713
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     w=1/s^2^(Fo^2^)
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.1170
_refine_ls_wR_factor_ref         0.1190
_reflns_number_gt                10408
_reflns_number_total             14706
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja028448i-2_s2.cif
_cod_data_source_block           sdb16
_cod_depositor_comments
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The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'direct methods' was changed to
'direct'.

'_atom_sites_solution_secondary' value 'Difference Fourier map' was
changed to 'difmap'.

'_atom_sites_solution_hydrogens' value 'Geometric positions' was
changed to 'geom'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
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_cod_database_code               4113387