How Innocent are Potentially Redox Non-Innocent Ligands? Electronic Structure and Metal Oxidation States in Iron-PNN Complexes as a Representative Case Study.
Butschke, Burkhard; Fillman, Kathlyn L.; Bendikov, Tatyana; Shimon, Linda J. W.; Diskin-Posner, Yael; Leitus, Gregory; Gorelsky, Serge I.; Neidig, Michael L.; Milstein, David; Inorganic chemistry 54 (2015) 4909–4926; doi:10.1021/acs.inorgchem.5b00509

data_4342924
_publ_section_title
;
 How Innocent are Potentially Redox Non-Innocent Ligands? Electronic
 Structure and Metal Oxidation States in Iron-PNN Complexes as a
 Representative Case Study.
;
_journal_issue                   10
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4909
_journal_page_last               4926
_journal_paper_doi               10.1021/acs.inorgchem.5b00509
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         '2(C27 H37 Fe N2 O2 P), C5 H12'
_chemical_formula_sum            'C59 H86 Fe2 N4 O4 P2'
_chemical_formula_weight         1088.96
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 118.485(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   37.294(5)
_cell_length_b                   8.0360(10)
_cell_length_c                   21.344(3)
_cell_measurement_reflns_used    25799
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.48
_cell_measurement_theta_min      1.92
_cell_volume                     5622.3(13)
_computing_cell_refinement       APEX2
_computing_data_collection       'Bruker collect package'
_computing_data_reduction        APEX2
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEX - II KappaCCD'
_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  0.0474
_diffrn_reflns_av_sigmaI/netI    0.0679
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -49
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            25777
_diffrn_reflns_theta_full        28.48
_diffrn_reflns_theta_max         28.48
_diffrn_reflns_theta_min         2.71
_exptl_absorpt_coefficient_mu    0.622
_exptl_absorpt_correction_T_max  0.9393
_exptl_absorpt_correction_T_min  0.7462
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker APEX2'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.286
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2328
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.725
_refine_diff_density_min         -0.639
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         7033
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0790
_refine_ls_R_factor_gt           0.0407
_refine_ls_shift/su_max          0.026
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0354P)^2^+5.6057P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0798
_refine_ls_wR_factor_ref         0.0960
_reflns_number_gt                4946
_reflns_number_total             7033
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b00509_si_002.cif
_cod_data_source_block           compound2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 4342923--4342928.cif.
;
_cod_original_cell_volume        5622.4(13)
_cod_original_sg_symbol_Hall     -C2yc
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4342924