Novel Square Arrangements in Tetranuclear and Octanuclear Iron(III) Complexes with Asymmetric Iron Environments Created by the Unsymmetric Bridging Ligand N,N,N'-Tris((N-methyl)-2-benzimidazolylmethyl)-N'-methyl-1,3-diamino-2-propanol
Joe H. Satcher,; Marilyn M. Olmstead; Michael W. Droege; Sean R. Parkin; Bruce C. Noll; Leopold May; Alan L. Balch; Inorganic Chemistry 37 (1998) 6751–6758; doi:10.1021/ic9802404

data_4323239
_publ_contact_author
; Dr. Alan L. Balch
  Department of Chemistry
  University of California
  One Shields Ave
  Davis, CA 95616-5295
  USA
;
_publ_contact_author_email       balch@chem.ucdavis.edu
_publ_section_title
;
 Novel Square Arrangements in Tetranuclear and Octanuclear Iron(III)
 Complexes with Asymmetric Iron Environments Created by the Unsymmetric
 Bridging Ligand
 N,N,N'-Tris((N-methyl)-2-benzimidazolylmethyl)-N'-methyl-1,3-diamino-2-propanol
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6751
_journal_page_last               6758
_journal_paper_doi               10.1021/ic9802404
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C136 H179 B3 F12 Fe8 N34 O29'
_chemical_formula_weight         3461.36
_chemical_name_common
;
[Fe~8~(\m-O)~4~(\m-BMDP)~4~(OH)~4~(OAc)~4~]{BF~4~]~3~[OH]^.^2CH~3~CN^.^8H~2~O
;
_chemical_name_systematic
; 
 ? 
;
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   38.555(3)
_cell_length_b                   38.555(3)
_cell_length_c                   11.865(2)
_cell_measurement_reflns_used    50
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      21.0
_cell_measurement_theta_min      9.0
_cell_volume                     17637(4)
_computing_cell_refinement       'Siemens P3'
_computing_data_collection       'Siemens P3'
_computing_data_reduction        'Siemens XDISK'
_computing_molecular_graphics    'SHELXTL 5.03, XP (Sheldrick, 1994)'
_computing_publication_material  'SHELXTL 5.03, XCIF (Sheldrick, 1994)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      130(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       2\q-\w
_diffrn_radiation_monochromator  'nickel filter'
_diffrn_radiation_source         'Siemens rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0387
_diffrn_reflns_av_sigmaI/netI    0.0848
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5803
_diffrn_reflns_theta_max         54.29
_diffrn_reflns_theta_min         2.29
_diffrn_standards_decay_%        <1.0
_diffrn_standards_interval_count 198
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    5.83
_exptl_absorpt_correction_T_max  0.91
_exptl_absorpt_correction_T_min  0.67
_exptl_absorpt_correction_type   XABS2
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             7184
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.413
_refine_diff_density_min         -0.602
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.017
_refine_ls_goodness_of_fit_obs   1.137
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     530
_refine_ls_number_reflns         5354
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.016
_refine_ls_restrained_S_obs      1.135
_refine_ls_R_factor_all          0.1759
_refine_ls_R_factor_obs          0.1175
_refine_ls_shift/esd_max         0.154
_refine_ls_shift/esd_mean        0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2390P)^2^+243.4101P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3837
_refine_ls_wR_factor_obs         0.3240
_reflns_number_observed          3129
_reflns_number_total             5354
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9802404_2.cif
_cod_data_source_block           sa08
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.2390P)^2^+243.4101P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.2390P)^2^+243.4101P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        17637.2(24)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               4323239