One-electron oxidation chemistry and subsequent reactivity of diiron imido complexes.
Kuppuswamy, Subramaniam; Powers, Tamara M.; Johnson, Bruce M.; Brozek, Carl K.; Krogman, Jeremy P.; Bezpalko, Mark W.; Berben, Louise A.; Keith, Jason M.; Foxman, Bruce M.; Thomas, Christine M.; Inorganic chemistry 53 (2014) 5429–5437; doi:10.1021/ic403039x

data_4338434
_publ_section_title
;
 One-electron oxidation chemistry and subsequent reactivity of diiron
 imido complexes.
;
_journal_issue                   11
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5429
_journal_page_last               5437
_journal_paper_doi               10.1021/ic403039x
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C53 H66 F1 Fe2 N3 O3.50 P3'
_chemical_formula_sum            'C53 H66 F Fe2 N3 O3.5 P3'
_chemical_formula_weight         1024.74
_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   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             12-06-06
_audit_creation_method           CRYSTALS_ver_14.41
_cell_angle_alpha                91.606(3)
_cell_angle_beta                 95.472(3)
_cell_angle_gamma                90.287(3)
_cell_formula_units_Z            2
_cell_length_a                   10.5016(6)
_cell_length_b                   12.5484(8)
_cell_length_c                   19.7979(11)
_cell_measurement_reflns_used    9888
_cell_measurement_temperature    120
_cell_measurement_theta_max      30
_cell_measurement_theta_min      3
_cell_volume                     2595.9(3)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.048
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            48178
_diffrn_reflns_theta_full        26.245
_diffrn_reflns_theta_max         30.167
_diffrn_reflns_theta_min         2.546
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.700
_exptl_absorpt_correction_T_max  0.91
_exptl_absorpt_correction_T_min  0.80
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1078
_exptl_crystal_size_max          0.430
_exptl_crystal_size_mid          0.310
_exptl_crystal_size_min          0.130
_refine_diff_density_max         1.53
_refine_diff_density_min         -1.24
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     591
_refine_ls_number_reflns         14981
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0602
_refine_ls_R_factor_gt           0.0401
_refine_ls_shift/su_max          0.0011854
_refine_ls_shift/su_mean         0.0000458
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.03P)^2^ + 2.63P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0883
_refine_ls_wR_factor_gt          0.0826
_refine_ls_wR_factor_ref         0.0883
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              17
_reflns_limit_k_min              -17
_reflns_limit_l_max              27
_reflns_limit_l_min              0
_reflns_number_gt                11339
_reflns_number_total             14981
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0602
_oxford_refine_ls_scale          0.12423(2)
_oxford_reflns_number_all        14981
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'SK_527_0m in P-1'
_cod_data_source_file            ic403039x_si_002.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 4338432--4338435.cif.'
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C53 H66 F1 Fe2 N3 O3.50 P3'
_cod_database_code               4338434
_iucr_refine_instructions_details_constraints
;
BLOCK 
CONT SCALE 
CONT FE   (    1 ,X'S,U'S)  UNTIL C    (   52 ) 
CONT C    (   53 ,X'S,U[ISO])  UNTIL C    (   54 ) 
RIDE C   (   1,X'S) H   (  11,X'S) 
RIDE C   (   2,X'S) H   (  21,X'S) H   (  23,X'S) H   (  22,X'S) 
RIDE C   (   3,X'S) H   (  32,X'S) H   (  31,X'S) H   (  33,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) H   ( 173,X'S) H   ( 172,X'S) 
RIDE C   (  18,X'S) H   ( 182,X'S) H   ( 181,X'S) H   ( 183,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) 
RIDE C   (  27,X'S) H   ( 271,X'S) 
RIDE C   (  28,X'S) H   ( 281,X'S) 
RIDE C   (  29,X'S) H   ( 291,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) 
RIDE C   (  32,X'S) H   ( 323,X'S) H   ( 321,X'S) H   ( 322,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) H   ( 333,X'S) H   ( 332,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) 
RIDE C   (  37,X'S) H   ( 371,X'S) 
RIDE C   (  38,X'S) H   ( 381,X'S) 
RIDE C   (  39,X'S) H   ( 391,X'S) 
RIDE C   (  41,X'S) H   ( 411,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) 
RIDE C   (  43,X'S) H   ( 431,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) 
RIDE C   (  48,X'S) H   ( 481,X'S) H   ( 482,X'S) H   ( 483,X'S) 
RIDE C   (  49,X'S) H   ( 491,X'S) H   ( 492,X'S) 
RIDE C   (  50,X'S) H   ( 501,X'S) H   ( 502,X'S) 
RIDE C   (  51,X'S) H   ( 511,X'S) H   ( 513,X'S) H   ( 512,X'S) 
RIDE C   (  52,X'S) H   ( 522,X'S) H   ( 525,X'S) H   ( 524,X'S) 
CONT H   ( 521,X'S) H   ( 526,X'S) H   ( 523,X'S) 
RIDE C   (  53,X'S) H   ( 531,X'S) H   ( 532,X'S) 
RIDE C   (  54,X'S) H   ( 542,X'S) H   ( 541,X'S) 
END                                                                             
;
_iucr_refine_instructions_details_restraints
;
NO 
DISTANCE 1.420000 , 0.002000 = O(3) TO C(53) 
END                                                                             
;