Heptanuclear Antiferromagnetic Fe(III)-d-(-)-Quinato Assemblies with an S= 3/2 Ground State-pH-Specific Synthetic Chemistry, Spectroscopic, Structural, and Magnetic Susceptibility Studies
M. Menelaou; E. Vournari; V. Psycharis; C. P. Raptopoulou; A. Terzis; V. Tangoulis; Y. Sanakis; C. Mateescu; A. Salifoglou; Inorganic Chemistry 52 (2013) 13849–13860; doi:10.1021/ic401036e

data_4336944
_publ_section_title
;
 Heptanuclear Antiferromagnetic Fe(III)-d-(-)-Quinato Assemblies with an
 S= 3/2 Ground State-pH-Specific Synthetic Chemistry, Spectroscopic,
 Structural, and Magnetic Susceptibility Studies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              13849
_journal_page_last               13860
_journal_paper_doi               10.1021/ic401036e
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C42 H106 Fe7 N O68 S2'
_chemical_formula_weight         2168.35
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           182
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 6c 2c'
_symmetry_space_group_name_H-M   'P 63 2 2'
_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                120.00
_cell_formula_units_Z            2
_cell_length_a                   16.2964(3)
_cell_length_b                   16.2964(3)
_cell_length_c                   18.6865(3)
_cell_measurement_reflns_used    31564
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      72.06
_cell_measurement_theta_min      6.70
_cell_volume                     4297.76(13)
_computing_cell_refinement       'CrystalClear, Rigaku MSC, 2005'
_computing_data_collection       'CrystalClear, Rigaku MSC, 2005'
_computing_data_reduction        'CrystalClear, Rigaku MSC, 2005'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IPDS'
_diffrn_measurement_method       '\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_sigmaI/netI    0.0233
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            35313
_diffrn_reflns_theta_full        65.00
_diffrn_reflns_theta_max         65.00
_diffrn_reflns_theta_min         6.71
_exptl_absorpt_coefficient_mu    10.733
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.268
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'CrystalClear, Rigaku MSC, 2005'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.676
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             2246
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.607
_refine_diff_density_min         -0.509
_refine_diff_density_rms         0.085
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.021(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     216
_refine_ls_number_reflns         2392
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0446
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0838P)^2^+3.6495P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1273
_refine_ls_wR_factor_ref         0.1320
_reflns_number_gt                2168
_reflns_number_total             2392
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401036e_si_005.cif
_cod_data_source_block           salfeq309
_cod_database_code               4336944