Octahedral (cis-Cyclam)iron(III) Complexes with O,N-Coordinatedo-Iminosemiquinonate(1-) π Radicals and o-Imidophenolate(2-) Anions
Hyungphil Chun; Eckhard Bill; Eberhard Bothe; Thomas Weyhermüller; Karl Wieghardt; Inorganic Chemistry 41 (2002) 5091–5099; doi:10.1021/ic020329g

data_4318587
_publ_contact_author_address
;     Max-Planck-Institute of Radiation Chemistry
        Stiftstrasse 34-36
        D-45470 Muelheim an der Ruhr
        Germany
;
_publ_contact_author_email       wieghardt@mpi-muelheim.mpg.de
_publ_contact_author_fax         49-208-306-3952
_publ_contact_author_name        'Dr. Karl Wieghardt'
_publ_contact_author_phone       49-208-306-3609
_publ_section_title
;
 Octahedral (cis-Cyclam)iron(III) Complexes with
 O,N-Coordinatedo-Iminosemiquinonate(1-) \p Radicals and
 o-Imidophenolate(2-) Anions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5091
_journal_page_last               5099
_journal_paper_doi               10.1021/ic020329g
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety         '[C30 H49 Fe N5 O]2+, 2 (P F6)-'
_chemical_formula_sum            'C30 H49 F12 Fe N5 O P2'
_chemical_formula_weight         841.53
_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                78.370(10)
_cell_angle_beta                 87.670(10)
_cell_angle_gamma                69.010(10)
_cell_formula_units_Z            2
_cell_length_a                   9.5149(9)
_cell_length_b                   9.8258(9)
_cell_length_c                   21.244(2)
_cell_measurement_temperature    100(2)
_cell_volume                     1815.2(3)
_computing_cell_refinement       'DENZO, Nonius Collect Software'
_computing_data_collection       'DENZO, Nonius Collect Software'
_computing_data_reduction        'DENZO, Nonius Collect Software'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measurement_device_type  'Nonius Kappa-CCD'
_diffrn_measurement_method       '770 images at 0.5 deg. in \w and 30 sec.'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0997
_diffrn_reflns_av_sigmaI/netI    0.1034
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            13763
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.27
_exptl_absorpt_coefficient_mu    0.599
_exptl_absorpt_correction_T_max  0.9646
_exptl_absorpt_correction_T_min  0.8513
_exptl_absorpt_correction_type   'Gaussian, face-indexed'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'transparent platelet'
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.989
_refine_diff_density_min         -0.624
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.061
_refine_ls_goodness_of_fit_obs   1.119
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         8047
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_restrained_S_obs      1.119
_refine_ls_R_factor_all          0.0968
_refine_ls_R_factor_obs          0.0680
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0438P)^2^+3.9291P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1792
_refine_ls_wR_factor_obs         0.1593
_reflns_number_observed          6027
_reflns_number_total             8093
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic020329g_3.cif
_cod_data_source_block           compound3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0438P)^2^+3.9291P] 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^)+(0.0438P)^2^+3.9291P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4318587