A Cube in a Tetrahedron: Microwave-Assisted Synthesis of an Octametallic FeIIICluster
Gass, Ian A.; Milios, Constantinos J.; Whittaker, A. Gavin; Fabiani, Francesca P. A.; Parsons, Simon; Murrie, Mark; Perlepes, Spyros P.; Brechin, Euan K.; Inorganic Chemistry 45 (2006) 5281–5283; doi:10.1021/ic0607843

data_4332739
_publ_section_title
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 A Cube in a Tetrahedron:&#x00A0; Microwave-Assisted Synthesis of an
 Octametallic FeIIICluster
;
_journal_issue                   14
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5281
_journal_page_last               5283
_journal_paper_doi               10.1021/ic0607843
_journal_volume                  45
_journal_year                    2006
_chemical_compound_source        'I. Gass/E. Brechin'
_chemical_formula_moiety         'C76 H60 Fe8 N12 O20, 4(C5 H5 N)'
_chemical_formula_sum            'C96 H80 Fe8 N16 O20'
_chemical_formula_weight         2224.56
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             06-02-17
_audit_creation_method           CRYSTALS_ver_12.82
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.9096(3)
_cell_length_b                   28.9096(3)
_cell_length_c                   11.1722(3)
_cell_measurement_reflns_used    7933
_cell_measurement_temperature    150
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     9337.3(3)
_computing_cell_refinement       'SAINT (Siemens ,1995)'
_computing_data_collection       'SMART (Siemens, 1993)'
_computing_data_reduction        'SAINT (Siemens ,1995)'
_computing_molecular_graphics
'CAMERON (Watkin et al., 1996), XCIF, PLATON, ENCIFER'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SHELXS 86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'Bruker SMART'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.048
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            56039
_diffrn_reflns_theta_full        27.768
_diffrn_reflns_theta_max         28.925
_diffrn_reflns_theta_min         1.409
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.287
_exptl_absorpt_correction_T_max  0.85
_exptl_absorpt_correction_T_min  0.64
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_description       needle
_exptl_crystal_F_000             4544
_exptl_crystal_recrystallization_method
;
Slow cooling after solvothermal conditions.
;
_exptl_crystal_size_max          0.57
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.06
_refine_diff_density_min         -0.80
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.6355
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         5891
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0775
_refine_ls_R_factor_gt           0.0384
_refine_ls_shift/su_max          0.000207
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(F^2^) + ( 0.00P)^2^ + 0.00P] 
where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0867
_refine_ls_wR_factor_gt          0.0734
_refine_ls_wR_factor_ref         0.0867
_reflns_limit_h_max              27
_reflns_limit_h_min              -26
_reflns_limit_k_max              39
_reflns_limit_k_min              0
_reflns_limit_l_max              15
_reflns_limit_l_min              0
_reflns_number_gt                3808
_reflns_number_total             5891
_reflns_threshold_expression     I>2.00u(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_scale          0.097008(19)
_oxford_structure_analysis_title 'eb6020 in I4(1)/a'
_cod_data_source_file            ic0607843sup1.cif
_cod_data_source_block           eb6020
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'I 41/a '
_cod_database_code               4332739