Cobalt-Dinitrogen Complexes with Weakened N-N Bonds
Keying Ding; Aaron W. Pierpont; William W. Brennessel; Gudrun Lukat-Rodgers; Kenton R. Rodgers; Thomas R. Cundari; Eckhard Bill; Patrick L. Holland; Journal of the American Chemical Society 131 (2009) 9471–9472; doi:10.1021/ja808783u

data_4104664
_publ_section_title
;
 Cobalt-Dinitrogen Complexes with Weakened N-N Bonds
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9471
_journal_page_last               9472
_journal_paper_doi               10.1021/ja808783u
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C70 H106 Fe2 N6, 0.5(C5 H12)'
_chemical_formula_sum            'C72.5 H112 Fe2 N6'
_chemical_formula_weight         1179.38
_chemical_name_common            holjs14
_chemical_name_systematic
; 
 ? 
;
_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                75.075(1)
_cell_angle_beta                 73.717(1)
_cell_angle_gamma                68.526(1)
_cell_formula_units_Z            2
_cell_length_a                   13.0850(10)
_cell_length_b                   13.9206(11)
_cell_length_c                   22.1213(18)
_cell_measurement_reflns_used    5054
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      23.17
_cell_measurement_theta_min      2.26
_cell_volume                     3544.8(5)
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 2003)'
_computing_data_reduction        'SAINT (Bruker, 2003)'
_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      193(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Siemens SMART CCD Platform'
_diffrn_measurement_method       'area detector, \w scans per \f'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0310
_diffrn_reflns_av_sigmaI/netI    0.0688
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            15251
_diffrn_reflns_theta_full        23.29
_diffrn_reflns_theta_max         23.29
_diffrn_reflns_theta_min         1.60
_exptl_absorpt_coefficient_mu    0.451
_exptl_absorpt_correction_T_max  0.9478
_exptl_absorpt_correction_T_min  0.8994
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Blessing, 1995)'
_exptl_crystal_colour            'dark red-brown'
_exptl_crystal_density_diffrn    1.105
_exptl_crystal_description       block
_exptl_crystal_F_000             1282
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.546
_refine_diff_density_min         -0.379
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     766
_refine_ls_number_reflns         9861
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.1103
_refine_ls_R_factor_gt           0.0750
_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^)+(0.0698P)^2^+0.9946P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1412
_refine_ls_wR_factor_ref         0.1540
_reflns_number_gt                7210
_reflns_number_total             9861
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja808783u_si_002_4.cif
_cod_data_source_block           LFeNNFeL-revised
_cod_database_code               4104664