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_4327026
_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
'C36 H40 Cl4 Fe4 N20 O8, 2(Cl4 Fe), 4(C H4 O)'
_chemical_formula_sum            'C40 H56 Cl12 Fe6 N20 O12'
_chemical_formula_weight         1769.53
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_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                 117.171(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.5433(12)
_cell_length_b                   37.143(3)
_cell_length_c                   15.2818(14)
_cell_measurement_reflns_used    23752
_cell_measurement_temperature    158(2)
_cell_measurement_theta_max      24.86
_cell_measurement_theta_min      1.69
_cell_volume                     7344.0(11)
_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    '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      158(2)
_diffrn_detector_area_resol_mean 14.63
_diffrn_measured_fraction_theta_full 0.837
_diffrn_measured_fraction_theta_max 0.837
_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     0.71069
_diffrn_reflns_av_R_equivalents  0.0491
_diffrn_reflns_av_sigmaI/netI    0.0310
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13057
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.66
_exptl_absorpt_coefficient_mu    1.651
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.600
_exptl_crystal_description       Prism
_exptl_crystal_F_000             3568
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.876
_refine_diff_density_min         -1.139
_refine_diff_density_rms         0.182
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.160
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     856
_refine_ls_number_reflns         10828
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      1.166
_refine_ls_R_factor_all          0.1230
_refine_ls_R_factor_gt           0.1160
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0748P)^2^+178.1305P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2731
_refine_ls_wR_factor_ref         0.2774
_reflns_number_gt                10099
_reflns_number_total             10828
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201891h_si_001_04.cif
_cod_data_source_block           3a
_cod_original_cell_volume        7344.0(10)
_cod_database_code               4327026