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_7054060
_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            'C93.5 H142 F3 Fe6.5 N46.5 O15 S10.5'
_chemical_formula_weight         2914.11
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 119.372(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   45.2573(13)
_cell_length_b                   27.5089(6)
_cell_length_c                   28.4547(9)
_cell_measurement_reflns_used    20892
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      20.1500
_cell_measurement_theta_min      3.0610
_cell_volume                     30871.7(19)
_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 0.997
_diffrn_measurement_device_type
'SuperNova, Single source at offset, Sapphire3'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1317
_diffrn_reflns_av_unetI/netI     0.0959
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       56
_diffrn_reflns_limit_h_min       -56
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            260859
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.408
_diffrn_reflns_theta_min         2.955
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.803
_exptl_absorpt_correction_T_max  0.946
_exptl_absorpt_correction_T_min  0.778
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.251
_exptl_crystal_description       prism
_exptl_crystal_F_000             12036
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.070
_platon_squeeze_details
;
The subroutine SQUEEZE from PLATON was used to remove the diffracting component of disordered solvents resulting in two voids of ca. 4163 Angstrom3 and 675 electrons/cell plus eight smaller voids of less than 25 Angstrom3 and 5 electrons/cell omitted. This corresponds to ca. 9 CH3OH + 1 H2O molecules per asymmetric unit. The contribution of these molecules has been included in the unit cell contents used in the refinement.
;
_refine_diff_density_max         2.251
_refine_diff_density_min         -1.068
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1306
_refine_ls_number_reflns         31587
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.1799
_refine_ls_R_factor_gt           0.1149
_refine_ls_shift/su_max          0.000
_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          0.3198
_refine_ls_wR_factor_ref         0.3644
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16529
_reflns_number_total             31587
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3nj01516e2.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        30871.7(18)
_cod_database_code               7054060
_shelx_estimated_absorpt_t_min   0.778
_shelx_estimated_absorpt_t_max   0.946
_shelxl_version_number           2013-4
_shelx_res_checksum              37491