The solvent effect in an axially symmetric FeIII4 single-molecule magnet
Yuan-Yuan Zhu; Ting-Ting Yin; Shang-Da Jiang; Anne-Laure Barra; Wolfgang Wernsdorfer; Petr Neugebauer; Raphael Marx; Maria Dorfel; Bing-Wu Wang; Zong-Quan Wu; Joris van Slageren; Song Gao; Chem.Commun. 50 (2014) 15090–; doi:10.1039/C4cc07580C

data_7116023
_publ_section_title
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 The solvent effect in an axially symmetric FeIII4 single-molecule magnet
;
_journal_name_full               Chem.Commun.
_journal_page_first              15090
_journal_paper_doi               10.1039/C4cc07580C
_journal_volume                  50
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_compound_source        no
_chemical_formula_moiety         C90H72Fe4N12O24
_chemical_formula_sum            'C90 H72 Fe4 N12 O24'
_chemical_formula_weight         1929.00
_chemical_name_common            Fe4L6-NO2-S
_chemical_name_systematic        Fe4-NO2(S)
_space_group_IT_number           155
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3 2"'
_symmetry_space_group_name_H-M   'R 3 2 :H'
_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            3
_cell_length_a                   29.778(4)
_cell_length_b                   29.778(4)
_cell_length_c                   13.885(3)
_cell_measurement_reflns_used    12535
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.4814
_cell_measurement_theta_min      1.3680
_cell_volume                     10663(3)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics
;
Mercury: visualization and analysis of crystal structures, C. F. Macrae,
 P. R. Edgington, P. McCabe, E. Pidcock, G. P. Shields, R. Taylor,
 M. Towler and J. van de Streek, J. Appl. Cryst., 39, 453-457, 2006.
;
_computing_publication_material  'SHELX-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'MM007HF + CCD (Saturn724+)'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0997
_diffrn_reflns_av_sigmaI/netI    0.0586
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            29068
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.37
_exptl_absorpt_coefficient_mu    0.452
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6930
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2008)'
_exptl_crystal_colour            'red brown'
_exptl_crystal_density_diffrn    0.901
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2976
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: DMA'
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.251
_platon_squeeze_details
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The disordered solvent molecules cannot be modeled and were treated 
by SQUEEZE,PLATON.
There are total 941e per unit cell were accumulated which corresponds 
to 314e per formula(C90H72Fe4N12O24). The 314e might come from solvent DMA molecules (calculated number is about 7) and were not included in the formula.
;
_refine_diff_density_max         0.365
_refine_diff_density_min         -0.684
_refine_diff_density_rms         0.079
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.003(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     197
_refine_ls_number_reflns         5438
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0616
_refine_ls_R_factor_gt           0.0607
_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^)+(0.1053P)^2^+8.1444P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1735
_refine_ls_wR_factor_ref         0.1743
_reflns_number_gt                5288
_reflns_number_total             5438
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc07580c2.cif
_cod_data_source_block           1S
_cod_original_sg_symbol_H-M      'R 3 2'
_cod_database_code               7116023