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_4107768
_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         'C90 H136 Fe2 N10, 2(C6 D6)'
_chemical_formula_sum            'C102 H136 D12 Fe2 N10'
_chemical_formula_weight         1638.08
_chemical_name_common            holrc02
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.789(3)
_cell_length_b                   24.031(3)
_cell_length_c                   15.525(2)
_cell_measurement_reflns_used    3954
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      32.00
_cell_measurement_theta_min      2.70
_cell_volume                     9248(2)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.1214
_diffrn_reflns_av_sigmaI/netI    0.0724
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            158250
_diffrn_reflns_theta_full        32.58
_diffrn_reflns_theta_max         32.58
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    0.365
_exptl_absorpt_correction_T_max  0.9507
_exptl_absorpt_correction_T_min  0.9306
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2007)'
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_diffrn    1.176
_exptl_crystal_description       block
_exptl_crystal_F_000             3528
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.811
_refine_diff_density_min         -0.625
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     568
_refine_ls_number_reflns         16835
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.1014
_refine_ls_R_factor_gt           0.0641
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+15.3655P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1305
_refine_ls_wR_factor_ref         0.1440
_reflns_number_gt                11491
_reflns_number_total             16835
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja801375g-file002_1.cif
_cod_data_source_block           holrc02
_cod_database_code               4107768