Reversible C-C Bond Formation between Redox-Active Pyridine Ligands in Iron Complexes
Thomas R. Dugan; Eckhard Bill; K. Cory MacLeod; Gemma J. Christian; Ryan E. Cowley; William W. Brennessel; Shengfa Ye; Frank Neese; Patrick L. Holland; Journal of the American Chemical Society 134 (2012) 20352–20364; doi:10.1021/ja305679m

data_4119019
_publ_section_title
;
 Reversible C-C Bond Formation between Redox-Active Pyridine Ligands in
 Iron Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              20352
_journal_page_last               20364
_journal_paper_doi               10.1021/ja305679m
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'C58 H66 Fe N4'
_chemical_formula_sum            'C58 H66 Fe N4'
_chemical_formula_weight         874.99
_chemical_name_common            holkcm01
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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     difmap
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                90
_cell_angle_beta                 92.150(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.783(2)
_cell_length_b                   17.156(3)
_cell_length_c                   18.848(3)
_cell_measurement_reflns_used    2499
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      20.12
_cell_measurement_theta_min      2.47
_cell_volume                     4776.8(13)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2012)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      100.0(5)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD Platform'
_diffrn_measurement_method       '\w scans'
_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  0.1798
_diffrn_reflns_av_sigmaI/netI    0.1407
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            38341
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.030
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         1.606
_exptl_absorpt_coefficient_mu    0.358
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6660
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.217
_exptl_crystal_description       needle
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.567
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     578
_refine_ls_number_reflns         8445
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.1425
_refine_ls_R_factor_gt           0.0666
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.0450P)^2^+2.5661P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1239
_refine_ls_wR_factor_ref         0.1513
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4714
_reflns_number_total             8445
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja305679m_si_002_3.cif
_cod_data_source_block           holkcm01
_cod_database_code               4119019
_shelx_estimated_absorpt_t_min   0.919
_shelx_estimated_absorpt_t_max   0.965