Synthesis, Magnetism, and 57Fe Mössbauer Spectroscopic Study of a Family of [Ln3Fe7] Coordination Clusters (Ln = Gd, Tb, and Er)
Ghulam Abbas; Yanhua Lan; Valeriu Mereacre; Gernot Buth; Moulay T. Sagrati; Fernande Grandjean; Gary J. Long; Christopher E. Anson; Annie K. Powell; Inorganic Chemistry 52 (2013) 11767–11777; doi:10.1021/ic401011d

data_4336407
_publ_contact_author
; 
'Annie K. Powell'
;
_publ_contact_author_email       annie.powell@kit.edu
_publ_contact_author_phone       '+49 721 608 42135'
_publ_section_title
;
 Synthesis, Magnetism, and 57Fe M\"ossbauer Spectroscopic Study of a
 Family of [Ln3Fe7] Coordination Clusters (Ln = Gd, Tb, and Er)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11767
_journal_page_last               11777
_journal_paper_doi               10.1021/ic401011d
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C63 H99 Fe7 Gd3 N25 O26, 4(C2 H3 N), (H2 O)'
_chemical_formula_sum            'C71 H113 Fe7 Gd3 N29 O27'
_chemical_formula_weight         2667.60
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                91.229(3)
_cell_angle_beta                 93.576(3)
_cell_angle_gamma                98.440(3)
_cell_formula_units_Z            2
_cell_length_a                   14.443(2)
_cell_length_b                   17.383(3)
_cell_length_c                   21.268(3)
_cell_measurement_reflns_used    10168
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.56
_cell_measurement_theta_min      2.05
_cell_volume                     5269.0(14)
_computing_cell_refinement       'Apex2 (Bruker AXS Inc., 2005)'
_computing_data_collection       'Apex2 (Bruker AXS Inc., 2005)'
_computing_data_reduction        'Apex2 (Bruker AXS Inc., 2005)'
_computing_molecular_graphics    'Diamond 2.1 (Crystal Impact, 1998)'
_computing_publication_material  'SHELXTL 6.14 (BrukerAXS Inc., 2003)'
_computing_structure_refinement  'SHELXTL 6.14 (BrukerAXS Inc., 2003)'
_computing_structure_solution    'SHELXTL 6.14 (BrukerAXS Inc., 2003)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'Bruker SMART Apex'
_diffrn_measurement_method       'CCD area detector'
_diffrn_radiation_monochromator  silicon
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.80000
_diffrn_reflns_av_R_equivalents  0.0546
_diffrn_reflns_av_sigmaI/netI    0.0230
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            44236
_diffrn_reflns_theta_full        29.00
_diffrn_reflns_theta_max         29.59
_diffrn_reflns_theta_min         2.42
_exptl_absorpt_coefficient_mu    3.921
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.468
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS 1.05 (Bruker AXS Inc., 2006)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.681
_exptl_crystal_description       plate
_exptl_crystal_F_000             2664
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.04
_refine_diff_density_max         3.137
_refine_diff_density_min         -3.247
_refine_diff_density_rms         0.213
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1203
_refine_ls_number_reflns         20831
_refine_ls_number_restraints     69
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.1063
_refine_ls_R_factor_gt           0.0910
_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^)+(0.1323P)^2^+65.2193P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2329
_refine_ls_wR_factor_ref         0.2492
_reflns_number_gt                17657
_reflns_number_total             20831
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401011d_si_001_1.cif
_cod_data_source_block           fe7gd35
_cod_original_cell_volume        5269.1(13)
_cod_database_code               4336407