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_4336943
_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 H104 Fe7 O62.5'
_chemical_formula_weight         2000.20
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000(3)
_cell_angle_beta                 90.000(4)
_cell_angle_gamma                90.000(4)
_cell_formula_units_Z            4
_cell_length_a                   11.1003(2)
_cell_length_b                   21.0919(5)
_cell_length_c                   40.3401(8)
_cell_measurement_reflns_used    33412
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      3.03
_cell_volume                     9444.7(3)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0289
_diffrn_reflns_av_sigmaI/netI    0.0401
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            33383
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.07
_exptl_absorpt_coefficient_mu    1.144
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.453
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'CrystalClear, Rigaku MSC, 2005'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             4152
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.575
_refine_diff_density_min         -1.151
_refine_diff_density_rms         0.096
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.022(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1115
_refine_ls_number_reflns         16508
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0490
_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^)+(0.1043P)^2^+2.8522P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1435
_refine_ls_wR_factor_ref         0.1491
_reflns_number_gt                14897
_reflns_number_total             16508
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401036e_si_003.cif
_cod_data_source_block           salfe142
_cod_original_formula_sum        'C42 H104 Fe7 O62.50'
_cod_database_code               4336943