Synthesis and Characterization of a New Family of Bi-, Tri-, Tetra-, and Pentanuclear Ferric Complexes
Colette Boskovic; Andreas Sieber; Grégory Chaboussant; Hans U. Güdel; Jürgen Ensling; Wolfgang Wernsdorfer; Antonia Neels; Gael Labat; Helen Stoeckli-Evans; Stefan Janssen; Inorganic Chemistry 43 (2004) 5053–5068; doi:10.1021/ic049600f

data_4311437
_publ_section_title
;
 Synthesis and Characterization of a New Family of Bi-, Tri-, Tetra-, and
 Pentanuclear Ferric Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5053
_journal_page_last               5068
_journal_paper_doi               10.1021/ic049600f
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety
'[Fe5(C15H13O2N)4(C7H5O2)4(OH)(O)](CH2Cl2)2(CH4O)0.5(H2O)1.5 '
_chemical_formula_sum            'C90.5 H82 Cl4 Fe5 N4 O20'
_chemical_formula_weight         1966.65
_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                87.069(11)
_cell_angle_beta                 79.397(10)
_cell_angle_gamma                69.702(10)
_cell_formula_units_Z            2
_cell_length_a                   14.4742(13)
_cell_length_b                   15.4790(15)
_cell_length_c                   21.1155(18)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      26.05
_cell_measurement_theta_min      1.65
_cell_volume                     4360.9(8)
_computing_cell_refinement       'CELL (Stoe IPDS Software, 2000)'
_computing_data_collection       'EXPOSE (Stoe IPDS Software, 2000)'
_computing_data_reduction        'INTEGRATE (Stoe IPDS Software, 2000)'
_computing_molecular_graphics    'PLATON99 (Spek, 1990)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 0.81\%A
_diffrn_measured_fraction_theta_full 0.925
_diffrn_measured_fraction_theta_max 0.925
_diffrn_measurement_device_type  'STOE IPDS'
_diffrn_measurement_method       'phi oscillation'
_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  0.0604
_diffrn_reflns_av_sigmaI/netI    0.0861
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            34634
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         2.38
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.008
_exptl_absorpt_correction_T_max  0.767
_exptl_absorpt_correction_T_min  0.346
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'DIFABS (PLATON, Spek, 1999)'
_exptl_crystal_colour            bordeaux
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2022
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.756
_refine_diff_density_min         -0.689
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1120
_refine_ls_number_reflns         15898
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.0918
_refine_ls_R_factor_gt           0.0584
_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^)+(0.1021P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1676
_refine_ls_wR_factor_ref         0.1802
_reflns_number_gt                10027
_reflns_number_total             15898
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049600fsi20040325_090813_7.cif
_cod_data_source_block           compound9
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

data name '_atom_site_symetry_multiplicity' was replaced with
'_atom_site_symmetry_multiplicity' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_original_cell_volume        4360.9(7)
_cod_original_formula_sum        'C90.50 H82 Cl4 Fe5 N4 O20'
_cod_database_code               4311437