Structural, Magnetic, and Electronic Properties of a Pentacoordinated Intermediate-Spin (S=3/2) Iron(III) Complex with a Macrocyclic [N4]2-Ligand
Heike Keutel; Indira Käpplinger; Ernst-Gottfried Jäger; Michael Grodzicki; Volker Schünemann; Alfred Xaver Trautwein; Inorganic Chemistry 38 (1999) 2320–2327; doi:10.1021/ic981276z

data_4322020
_publ_contact_author
;
        Ernst-Gottfried Ja(e)ger
        Institute of Inorganic and Analytical Chemistry
        University of Jena
        August-Bebel-Str. 2
        D-07743 Jena
        Germany
;
_publ_contact_author_fax         '++49-3641 948102 '
_publ_contact_author_phone       '++49-3641 948130 '
_publ_section_title
;
 Structural, Magnetic, and Electronic Properties of a Pentacoordinated
 Intermediate-Spin (S=3/2) Iron(III) Complex with a Macrocyclic
 [N4]2-Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2320
_journal_page_last               2327
_journal_paper_doi               10.1021/ic981276z
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C21.5 H10 Fe I N4 O4'
_chemical_formula_weight         591.24
_chemical_name_systematic
; 
 6,13-Diethoxycarbonyl-7,12-dimethyl-1,4,8,11-tetraazacyclotetradeka-
 5,7,12,14-tetraenato-iron(III)-ioded
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 107.11(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.063(3)
_cell_length_b                   15.895(3)
_cell_length_c                   19.703(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      20.78
_cell_measurement_theta_min      10.50
_cell_volume                     4808.0(18)
_computing_cell_refinement       celdim
_computing_data_collection       CAD4
_computing_data_reduction        MolEN
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       CAD4
_diffrn_measurement_method       Omega-2Theta
_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  0.0218
_diffrn_reflns_av_sigmaI/netI    0.0487
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            7059
_diffrn_reflns_theta_max         30.56
_diffrn_reflns_theta_min         2.53
_diffrn_standards_decay_%        3.0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.946
_exptl_absorpt_correction_T_max  13.5
_exptl_absorpt_correction_T_min  4.3
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.634
_exptl_crystal_description       quader
_exptl_crystal_F_000             2384
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.680
_refine_diff_density_min         -0.525
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.094
_refine_ls_goodness_of_fit_obs   1.024
_refine_ls_hydrogen_treatment    isotrop
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         6843
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.213
_refine_ls_restrained_S_obs      1.024
_refine_ls_R_factor_all          0.0869
_refine_ls_R_factor_obs          0.0389
_refine_ls_shift/esd_max         0.009
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0368P)^2^+15.1622P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1201
_refine_ls_wR_factor_obs         0.0833
_reflns_number_observed          4723
_reflns_number_total             6894
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic981276z.cif
_cod_data_source_block           fo316i
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0368P)^2^+15.1622P] 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^)+(0.0368P)^2^+15.1622P] 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        4808.0(16)
_cod_database_code               4322020