Tuning the nuclearity of iron(iii) polynuclear clusters by using tetradentate Schiff-base ligands
Abhervé, Alexandre; Clemente-Juan, Juan Modesto; Clemente-León, Miguel; Coronado, Eugenio; Boonmak, Jaursup; Youngme, Sujittra; New Journal of Chemistry 38 (2014) 2105–; doi:10.1039/c3nj01516e

data_7054061
_publ_section_title
;
 Tuning the nuclearity of iron(iii) polynuclear clusters by using
 tetradentate Schiff-base ligands
;
_journal_issue                   5
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              2105
_journal_paper_doi               10.1039/c3nj01516e
_journal_volume                  38
_journal_year                    2014
_chemical_formula_sum            'C91 H108 Cl5 Fe8 N59 O30 S11'
_chemical_formula_weight         3484.97
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           110
_space_group_name_Hall           'I 4bw -2c'
_space_group_name_H-M_alt        'I 41 c d'
_symmetry_space_group_name_Hall  'I 4bw -2c'
_symmetry_space_group_name_H-M   'I 41 c d'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   28.5279(3)
_cell_length_b                   28.5279(3)
_cell_length_c                   41.3731(6)
_cell_measurement_reflns_used    14623
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.4399
_cell_measurement_theta_min      2.8503
_cell_volume                     33671.1(7)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 16.0267
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
'SuperNova, Single source at offset), Sapphire3'
_diffrn_measurement_method       '\w scan'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1501
_diffrn_reflns_av_unetI/netI     0.1139
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_number            178800
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         2.856
_exptl_absorpt_coefficient_mu    0.960
_exptl_absorpt_correction_T_max  0.943
_exptl_absorpt_correction_T_min  0.890
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_description       Prism
_exptl_crystal_F_000             14112
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.239
_refine_diff_density_min         -0.596
_refine_diff_density_rms         0.135
_refine_ls_abs_structure_details
;
 Flack x determined using 3122 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.001(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     898
_refine_ls_number_reflns         19224
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.2154
_refine_ls_R_factor_gt           0.1109
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2758
_refine_ls_wR_factor_ref         0.3470
_reflns_Friedel_coverage         0.964
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.989
_reflns_number_gt                8631
_reflns_number_total             19224
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3nj01516e2.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        33671.1(9)
_cod_database_code               7054061
_shelx_estimated_absorpt_t_min   0.831
_shelx_estimated_absorpt_t_max   0.954
_shelxl_version_number           2013-4
_shelx_res_checksum              19310