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_4323238
_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            'C66 H89 Fe4 N19 O30'
_chemical_formula_weight         1851.96
_chemical_name_common
;
[Fe~4~(\m-O)~2~(\m-BMDP)~2~(\m-OAc)~2~][NO~3~]~3~[OH]^.^12H~2~O
;
_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
_cell_angle_alpha                115.99(2)
_cell_angle_beta                 108.02(2)
_cell_angle_gamma                95.73(2)
_cell_formula_units_Z            1
_cell_length_a                   12.228(3)
_cell_length_b                   13.915(3)
_cell_length_c                   14.120(3)
_cell_measurement_reflns_used    40
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      29.5
_cell_measurement_theta_min      8.0
_cell_volume                     1974.2(10)
_computing_cell_refinement       'Siemens P3'
_computing_data_collection       'Siemens P3'
_computing_data_reduction        'Siemens XDISK'
_computing_molecular_graphics    'SHELXTL V. 5.03, XP (Sheldrick, 1994)'
_computing_publication_material  'SHELXTL V. 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 Cu anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0160
_diffrn_reflns_av_sigmaI/netI    0.0553
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5118
_diffrn_reflns_theta_max         54.30
_diffrn_reflns_theta_min         3.68
_diffrn_standards_decay_%        <1.0
_diffrn_standards_interval_count 198
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    6.605
_exptl_absorpt_correction_T_max  0.718
_exptl_absorpt_correction_T_min  0.524
_exptl_absorpt_correction_type   XABS2
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.558
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             962
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.893
_refine_diff_density_min         -0.500
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.036
_refine_ls_goodness_of_fit_obs   1.059
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     529
_refine_ls_number_reflns         4814
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.122
_refine_ls_restrained_S_obs      1.061
_refine_ls_R_factor_all          0.1024
_refine_ls_R_factor_obs          0.0708
_refine_ls_shift/esd_max         0.022
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1108P)^2^+8.2250P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2250
_refine_ls_wR_factor_obs         0.1802
_reflns_number_observed          3585
_reflns_number_total             4829
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9802404_1.cif
_cod_data_source_block           sp46m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1108P)^2^+8.2250P] 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^)+(0.1108P)^2^+8.2250P] 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        1974.2(8)
_cod_original_formula_sum        'C66 H89 N19 O30 Fe4'
_cod_database_code               4323238