Iron(II) Complexes with Tetradentate Bis(aminophenolate) Ligands: Synthesis and Characterization, Solution Behavior, and Reactivity with O2
Christopher J. Whiteoak; Rafael Torres Martin de Rosales; Andrew J. P. White; George J. P. Britovsek; Inorganic Chemistry 49 (2010) 11106–11117; doi:10.1021/ic1016998

data_4317175
_publ_section_title
;
 Iron(II) Complexes with Tetradentate Bis(aminophenolate) Ligands:
 Synthesis and Characterization, Solution Behavior, and Reactivity with O2
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11106
_journal_page_last               11117
_journal_paper_doi               10.1021/ic1016998
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C68 H108 Fe2 N4 O5, 2(C4 H8 O)'
_chemical_formula_sum            'C76 H124 Fe2 N4 O7'
_chemical_formula_weight         1317.49
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.16191(16)
_cell_length_b                   10.39828(9)
_cell_length_c                   27.96718(19)
_cell_measurement_reflns_used    29484
_cell_measurement_temperature    173
_cell_measurement_theta_max      71.2769
_cell_measurement_theta_min      1.5783
_cell_volume                     7608.16(10)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 8.2556
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'OD Xcalibur PX Ultra'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0438
_diffrn_reflns_av_sigmaI/netI    0.0308
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            89844
_diffrn_reflns_theta_full        71.42
_diffrn_reflns_theta_max         71.42
_diffrn_reflns_theta_min         3.16
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.456
_exptl_absorpt_correction_T_max  0.755
_exptl_absorpt_correction_T_min  0.589
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) 
(compiled Jan  5 2010,16:28:46) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
;
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.150
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             2864
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.836
_refine_diff_density_min         -0.385
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details
'Flack H D (1983), Acta Cryst. A39, 876-881, 6975 Friedel pairs'
_refine_ls_abs_structure_Flack   0.394(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     845
_refine_ls_number_reflns         14507
_refine_ls_number_restraints     319
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0690
_refine_ls_R_factor_gt           0.0581
_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^)+(0.1234P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1576
_refine_ls_wR_factor_ref         0.1645
_reflns_number_gt                11789
_reflns_number_total             14507
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1016998_si_001_4.cif
_cod_data_source_block           '[{Fe(SalantBu,tBu)}2(mu-O)]'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4317175