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_4302185
_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, C4 H10 O'
_chemical_formula_sum            'C53 H81 Fe N6 O'
_chemical_formula_weight         874.09
_chemical_name_common            1
_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                 117.244(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.818(4)
_cell_length_b                   10.1533(18)
_cell_length_c                   23.453(4)
_cell_measurement_reflns_used    3830
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      32.92
_cell_measurement_theta_min      2.24
_cell_volume                     4830.8(15)
_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 0.985
_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  0.0667
_diffrn_reflns_av_sigmaI/netI    0.0617
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            82980
_diffrn_reflns_theta_full        32.57
_diffrn_reflns_theta_max         32.57
_diffrn_reflns_theta_min         1.69
_exptl_absorpt_coefficient_mu    0.356
_exptl_absorpt_correction_T_max  0.9721
_exptl_absorpt_correction_T_min  0.8562
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Blessing, 1995)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.202
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1900
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.594
_refine_diff_density_min         -0.522
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     574
_refine_ls_number_reflns         17333
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0955
_refine_ls_R_factor_gt           0.0528
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0423P)^2^+3.5745P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1163
_refine_ls_wR_factor_ref         0.1312
_reflns_number_gt                11621
_reflns_number_total             17333
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic900001y_si_001.cif
_cod_data_source_block           1
_cod_database_code               4302185