Polynuclear Fen Complexes (n= 1, 2, 4, 5) of Polytopic Hydrazone Ligands with Fe(II), Fe(III) and Mixed Oxidation State Combinations
Muhammad U. Anwar; Konstantin V. Shuvaev; Louise N. Dawe; Laurence K. Thompson; Inorganic Chemistry 50 (2011) 12141–12154; doi:10.1021/ic201891h

data_4327024
_publ_contact_author_address
;
Department of chemistry
Memorial University of Newfoundland
St. Johns, NL, A1B 3X7, Canada
;
_publ_contact_author_email       lk.thompson@mun.ca
_publ_contact_author_fax         1-709-864-3702
_publ_contact_author_name        'Laurence K. Thompson'
_publ_contact_author_phone       1-709-864-8750
_publ_section_title
;
 Polynuclear Fen Complexes (n= 1, 2, 4, 5) of Polytopic Hydrazone Ligands
 with Fe(II), Fe(III) and Mixed Oxidation State Combinations
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12141
_journal_page_last               12154
_journal_paper_doi               10.1021/ic201891h
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety
'C66 H54 Fe5 N36 O6, 4(C F3 O3 S), 2(C H4 O), 5(H2 O)'
_chemical_formula_sum            'C72 H78 F12 Fe5 N36 O25 S4'
_chemical_formula_weight         2483.09
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                99.829(7)
_cell_angle_beta                 93.742(7)
_cell_angle_gamma                99.903(7)
_cell_formula_units_Z            2
_cell_length_a                   14.235(5)
_cell_length_b                   14.512(6)
_cell_length_c                   26.039(10)
_cell_measurement_reflns_used    17116
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      30.7818
_cell_measurement_theta_min      2.2362
_cell_volume                     5196(3)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_molecular_graphics    'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)'
_computing_publication_material  'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)'
_computing_structure_refinement  'SHELXL-97 (Acta Cryst.2008, A64, 112-122)'
_computing_structure_solution    'SHELXS-97 (Acta Cryst.2008, A64, 112-122)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 14.63
_diffrn_measured_fraction_theta_full 0.840
_diffrn_measured_fraction_theta_max 0.840
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'graphite - Rigaku SHINE'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0430
_diffrn_reflns_av_sigmaI/netI    0.1794
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            38706
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         2.50
_exptl_absorpt_coefficient_mu    0.870
_exptl_absorpt_correction_T_max  0.9131
_exptl_absorpt_correction_T_min  0.7291
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(T. Higashi, 2000)'
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.587
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2528
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.13
_refine_diff_density_max         5.152
_refine_diff_density_min         -1.690
_refine_diff_density_rms         0.253
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1389
_refine_ls_number_reflns         18092
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      2.046
_refine_ls_R_factor_all          0.1773
_refine_ls_R_factor_gt           0.1659
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4369
_refine_ls_wR_factor_ref         0.4705
_reflns_number_gt                15080
_reflns_number_total             18092
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201891h_si_001_02.cif
_cod_data_source_block           2
_cod_database_code               4327024