A Bridging Hexazene (RNNNNNNR) Ligand from Reductive Coupling of Azides
Ryan E. Cowley; Jérôme Elhaïk; Nathan A. Eckert; William W. Brennessel; Eckhard Bill; Patrick L. Holland; Journal of the American Chemical Society 130 (2008) 6074–6075; doi:10.1021/ja801375g

data_4107769
_publ_section_title
;
 A Bridging Hexazene (RNNNNNNR) Ligand from Reductive Coupling of Azides
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6074
_journal_page_last               6075
_journal_paper_doi               10.1021/ja801375g
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         'C78 H112 Fe2 N10, 2(C H2 Cl2)'
_chemical_formula_sum            'C80 H116 Cl4 Fe2 N10'
_chemical_formula_weight         1471.33
_chemical_name_common            HOLRC04
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 90.204(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.2681(16)
_cell_length_b                   18.409(2)
_cell_length_c                   14.5166(16)
_cell_measurement_reflns_used    3909
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      32.85
_cell_measurement_theta_min      2.98
_cell_volume                     3812.9(7)
_computing_cell_refinement       'SAINT (Bruker, 2006)'
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        'SAINT (Bruker, 2006)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2000)'
_computing_publication_material  'SHELXTL (Bruker, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100.0(1)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD Platform'
_diffrn_measurement_method       'area detector, \w scans per \f'
_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  0.0403
_diffrn_reflns_av_sigmaI/netI    0.0329
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            67828
_diffrn_reflns_theta_full        32.58
_diffrn_reflns_theta_max         32.58
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    0.571
_exptl_absorpt_correction_T_max  0.8752
_exptl_absorpt_correction_T_min  0.8565
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2007)'
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_diffrn    1.282
_exptl_crystal_description       block
_exptl_crystal_F_000             1572
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.788
_refine_diff_density_min         -1.015
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         13782
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_gt           0.0420
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0508P)^2^+2.6839P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1088
_refine_ls_wR_factor_ref         0.1160
_reflns_number_gt                11160
_reflns_number_total             13782
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja801375g-file002_2.cif
_cod_data_source_block           holrc04
_cod_original_cell_volume        3812.8(7)
_cod_database_code               4107769