Bis(imino)pyridine Iron Dinitrogen Compounds Revisited: Differences in Electronic Structure Between Four- and Five-Coordinate Derivatives.
E Stieber, S Chantal; Milsmann, Carsten; Hoyt, Jordan M.; Turner, Zoë R; Finkelstein, Kenneth D.; Wieghardt, Karl; Debeer, Serena; Chirik, Paul J.; Organometallics 31 (2012) 2275–2285; doi:10.1021/om201212m

data_4076436
_publ_section_title
;
 Bis(imino)pyridine Iron Dinitrogen Compounds Revisited: Differences in
 Electronic Structure Between Four- and Five-Coordinate Derivatives.
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              2275
_journal_page_last               2285
_journal_paper_doi               10.1021/om201212m
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C34 H42 Cl2 F3 Fe N3, 0.5(C4 H10 O)'
_chemical_formula_sum            'C36 H47 Cl2 F3 Fe N3 O0.5'
_chemical_formula_weight         713.51
_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                 109.535(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.948(3)
_cell_length_b                   17.985(3)
_cell_length_c                   21.125(3)
_cell_measurement_reflns_used    16889
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.5
_cell_volume                     7501(2)
_computing_cell_refinement       'SHELXL--97 (Sheldrick, 2008)'
_computing_data_collection       'BRUKER APEX II software suite (Bruker AXS)'
_computing_data_reduction        'BRUKER APEX II software suite (Bruker AXS)'
_computing_molecular_graphics    'ORTEP 3 (Farrugia, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'Phi and omega 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  0.0612
_diffrn_reflns_av_sigmaI/netI    0.0543
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            83779
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    0.589
_exptl_absorpt_correction_T_max  0.9467
_exptl_absorpt_correction_T_min  0.8668
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.264
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3000
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.09
_refine_diff_density_max         2.099
_refine_diff_density_min         -1.049
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     822
_refine_ls_number_reflns         16889
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0962
_refine_ls_R_factor_gt           0.0565
_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^)+(0.0555P)^2^+13.2677P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1282
_refine_ls_wR_factor_ref         0.1468
_reflns_number_gt                11505
_reflns_number_total             16889
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om201212m_si_002.cif
_cod_data_source_block           jmd14
_cod_depositor_comments
;
Adding full bibliography for 4076435--4076439.cif.

2026-02-27
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C72 H94 Cl4 F6 Fe2 N6 O'
_cod_original_formula_weight         1427.03
_cod_original_formula_moiety         '2(C34 H42 Cl2 F3 Fe N3), C4 H10 O'
_cod_original_formula_units_Z            4
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4076436