Catalytic N-N Coupling of Aryl Azides To Yield Azoarenes via trigonal Bipyramid Iron-Nitrene Intermediates
Neal P. Mankad; Peter Müller; Jonas C. Peters; Journal of the American Chemical Society 132 (2010) 4083–4085; doi:10.1021/ja910224c

data_4102167
_publ_section_title
;
 Catalytic N-N Coupling of Aryl Azides To Yield Azoarenes via trigonal
 Bipyramid Iron-Nitrene Intermediates
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4083
_journal_page_last               4085
_journal_paper_doi               10.1021/ja910224c
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C46 H69 Fe N3 P3 Si, 1.5(C5 H12) '
_chemical_formula_sum            'C53.5 H87 Fe N3 P3 Si'
_chemical_formula_weight         949.11
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           167
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            12
_cell_length_a                   15.0449(8)
_cell_length_b                   15.0449(8)
_cell_length_c                   81.101(6)
_cell_measurement_reflns_used    9647
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.24
_cell_measurement_theta_min      2.55
_cell_volume                     15897.7(17)
_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 8.3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0557
_diffrn_reflns_av_sigmaI/netI    0.0169
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       115
_diffrn_reflns_limit_l_min       -115
_diffrn_reflns_number            136582
_diffrn_reflns_theta_full        30.50
_diffrn_reflns_theta_max         30.50
_diffrn_reflns_theta_min         1.51
_exptl_absorpt_coefficient_mu    0.435
_exptl_absorpt_correction_T_max  0.8284
_exptl_absorpt_correction_T_min  0.8120
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.190
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6168
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.45
_refine_diff_density_max         0.429
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.210
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         5406
_refine_ls_number_restraints     331
_refine_ls_restrained_S_all      1.223
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0516
_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^)+(0.0176P)^2^+85.9117P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1168
_refine_ls_wR_factor_ref         0.1200
_reflns_number_gt                4807
_reflns_number_total             5406
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja910224c_si_001_1.cif
_cod_data_source_block           09172
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Rhombohedral' changed to
'rhombohedral' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        15897.8(17)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_original_formula_sum        'C53.50 H87 Fe N3 P3 Si'
_cod_database_code               4102167