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_4318585
_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_structural     '[C16 H29 Fe N5 O]2+, 2 (P F6)-'
_chemical_formula_sum            'C16 H29 F12 Fe N5 O P2'
_chemical_formula_weight         653.23
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 103.900(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.1945(6)
_cell_length_b                   15.8491(9)
_cell_length_c                   17.3321(12)
_cell_measurement_reflns_used    18339
_cell_measurement_temperature    100(2)
_cell_volume                     2451.8(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       'Nonius Kappa-CCD, rotating anode'
_diffrn_measurement_method       '287 images at 1 deg. in \w and 30 sec.'
_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  0.0549
_diffrn_reflns_av_sigmaI/netI    0.0812
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            18339
_diffrn_reflns_theta_max         31.00
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    0.858
_exptl_absorpt_correction_T_max  0.9166
_exptl_absorpt_correction_T_min  0.8709
_exptl_absorpt_correction_type   'Gaussian, Face Indexed'
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    1.770
_exptl_crystal_description       'opaque parallelepiped'
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.718
_refine_diff_density_min         -0.472
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.033
_refine_ls_goodness_of_fit_obs   1.125
_refine_ls_matrix_type           full
_refine_ls_number_parameters     337
_refine_ls_number_reflns         7732
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.103
_refine_ls_restrained_S_obs      1.125
_refine_ls_R_factor_all          0.0933
_refine_ls_R_factor_obs          0.0515
_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^)+(0.0500P)^2^+1.0350P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1363
_refine_ls_wR_factor_obs         0.1124
_reflns_number_observed          5179
_reflns_number_total             7783
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic020329g_1.cif
_cod_data_source_block           compound1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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^)+(0.0500P)^2^+1.0350P] 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^)+(0.0500P)^2^+1.0350P] 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               4318585