Highly selective hydroxylation of alkanes catalyzed by (μ-oxo)bis(μ-carboxylato)-bridged diiron(iii) complexes: involvement of mononuclear iron(iii) species in catalysis
Visvaganesan, Kusalendiran; Suresh, Eringathodi; Palaniandavar, Mallayan; Dalton Transactions  (2009) 3814–3823; doi:10.1039/b901508f

data_7001294
_publ_section_title
;
 Highly selective hydroxylation of alkanes catalyzed by
 (\m-oxo)bis(\m-carboxylato)-bridged diiron(iii) complexes: involvement
 of mononuclear iron(iii) species in catalysis
;
_journal_issue                   19
_journal_name_full               'Dalton Transactions'
_journal_page_first              3814
_journal_page_last               3823
_journal_paper_doi               10.1039/b901508f
_journal_year                    2009
_chemical_formula_sum            'C52 H48 Cl2 Fe2 N6 O13'
_chemical_formula_weight         1147.56
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                82.9990(10)
_cell_angle_beta                 87.5060(10)
_cell_angle_gamma                68.9290(10)
_cell_formula_units_Z            2
_cell_length_a                   12.1543(10)
_cell_length_b                   14.4925(12)
_cell_length_c                   15.7642(13)
_cell_measurement_temperature    100(2)
_cell_volume                     2571.8(4)
_computing_cell_refinement       'BRUKER SMART'
_computing_data_collection       'BRUKER SMART'
_computing_data_reduction        'BRUKER SAINT'
_computing_molecular_graphics    'ORTEP, PLATON'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.915
_diffrn_measured_fraction_theta_max 0.915
_diffrn_measurement_device_type  'BRUKER SMART APEX CCD DIFFRACTOMETER'
_diffrn_measurement_method       'OMEGA-PHI SCAN'
_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  0.0267
_diffrn_reflns_av_sigmaI/netI    0.0474
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22194
_diffrn_reflns_theta_full        28.25
_diffrn_reflns_theta_max         28.25
_diffrn_reflns_theta_min         1.30
_exptl_absorpt_coefficient_mu    0.739
_exptl_absorpt_correction_T_max  0.9036
_exptl_absorpt_correction_T_min  0.6654
_exptl_absorpt_correction_type   'SADABS MULTI-SCAN'
_exptl_crystal_colour            YELLOW
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       PLATES
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.552
_refine_diff_density_min         -0.355
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     676
_refine_ls_number_reflns         11641
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0452
_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^)+(0.0503P)^2^+1.6796P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1048
_refine_ls_wR_factor_ref         0.1096
_reflns_number_gt                9988
_reflns_number_total             11641
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b901508f.txt
_cod_data_source_block           14mpkvm
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'TRICLINIC' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0503P)^2^+1.6796P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0503P)^2^+1.6796P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7001294