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_4327029
_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         'C22 H24 Fe N6 O8, C F3 O3 S, 2(C H4 O)'
_chemical_formula_sum            'C25 H32 F3 Fe N6 O13 S'
_chemical_formula_weight         769.46
_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                98.001(4)
_cell_angle_beta                 109.712(5)
_cell_angle_gamma                96.538(4)
_cell_formula_units_Z            2
_cell_length_a                   10.936(5)
_cell_length_b                   12.166(5)
_cell_length_c                   13.613(6)
_cell_measurement_reflns_used    5648
_cell_measurement_temperature    163(2)
_cell_measurement_theta_max      29.8
_cell_measurement_theta_min      1.6
_cell_volume                     1663.1(13)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_data_collection       'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_molecular_graphics    'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_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      163(2)
_diffrn_detector_area_resol_mean 14.63
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_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  0.0318
_diffrn_reflns_av_sigmaI/netI    0.0383
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14963
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.57
_exptl_absorpt_coefficient_mu    0.604
_exptl_absorpt_correction_T_max  0.979
_exptl_absorpt_correction_T_min  0.888
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(T. Higashi, 2000)'
_exptl_crystal_colour            'Olive Green'
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_description       Prism
_exptl_crystal_F_000             794
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.634
_refine_diff_density_min         -0.607
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     466
_refine_ls_number_reflns         7495
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0441
_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^)+(0.0937P)^2^+0.8784P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1273
_refine_ls_wR_factor_ref         0.1564
_reflns_number_gt                6578
_reflns_number_total             7495
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201891h_si_001_07.cif
_cod_data_source_block           6
_cod_database_code               4327029