Iron(II) Complexes with Redox-Active Tetrazene (RNNNNR) Ligands
Ryan E. Cowley; Eckhard Bill; Frank Neese; William W. Brennessel; Patrick L. Holland; Inorganic Chemistry 48 (2009) 4828–4836; doi:10.1021/ic900001y

data_4302186
_publ_contact_author             'Prof. Dr. Patrick L. Holland'
_publ_contact_author_email       holland@chem.rochester.edu
_publ_section_title
;
Iron(II) Complexes with Redox-Active Tetrazene (RNNNNR) Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4828
_journal_page_last               4836
_journal_paper_doi               10.1021/ic900001y
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C49 H71 Fe N6, C18 H36 K N2 O6'
_chemical_formula_sum            'C67 H107 Fe K N8 O6'
_chemical_formula_weight         1215.56
_chemical_name_common            2
_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                73.691(1)
_cell_angle_beta                 88.752(1)
_cell_angle_gamma                73.527(1)
_cell_formula_units_Z            2
_cell_length_a                   14.0308(10)
_cell_length_b                   14.1616(10)
_cell_length_c                   20.6650(15)
_cell_measurement_reflns_used    9705
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      37.95
_cell_measurement_theta_min      2.46
_cell_volume                     3771.6(5)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      100.0(1)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.0316
_diffrn_reflns_av_sigmaI/netI    0.0461
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            81559
_diffrn_reflns_theta_full        34.97
_diffrn_reflns_theta_max         34.97
_diffrn_reflns_theta_min         1.03
_exptl_absorpt_coefficient_mu    0.304
_exptl_absorpt_correction_T_max  0.9473
_exptl_absorpt_correction_T_min  0.8985
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2007)'
_exptl_crystal_colour            orange-black
_exptl_crystal_density_diffrn    1.070
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1316
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.511
_refine_diff_density_min         -0.356
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     758
_refine_ls_number_reflns         32672
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0612
_refine_ls_R_factor_gt           0.0412
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0605P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1041
_refine_ls_wR_factor_ref         0.1113
_reflns_number_gt                23268
_reflns_number_total             32672
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic900001y_si_002.cif
_cod_data_source_block           2
_cod_original_cell_volume        3771.7(5)
_cod_database_code               4302186