Preparation, Structure, and Electronic Properties of a Low-Spin Iron(II) Hexaamine Compound
Heidi Börzel; Peter Comba; Hans Pritzkow; Achim F. Sickmüller; Inorganic Chemistry 37 (1998) 3853–3857; doi:10.1021/ic971552u

data_4322905
_publ_contact_author
;
        Hans Pritzkow
        Anorganisch-Chemisches Institut
        Universitaet Heidelberg
        Im Neuenheimer Feld 270
        D-69120 Heidelberg
        Bundesrepublik Deutschland
;
_publ_contact_author_email       hans@wasi0.aci.uni-heidelberg.de
_publ_contact_author_fax         '049 6221 54-5609'
_publ_contact_author_phone       '049 6221 54-8450'
_publ_section_title
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 Preparation, Structure, and Electronic Properties of a Low-Spin Iron(II)
 Hexaamine Compound
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3853
_journal_page_last               3857
_journal_paper_doi               10.1021/ic971552u
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C12 H32 F12 Fe N6 O P2'
_chemical_formula_weight         622.23
_chemical_name_systematic
;
 Exo-6,13-diamino-6,13-dimethyl-1,4,8,11-tetraazatetradecane
 iron bis(hexafluorophosphate)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 98.92(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.547(8)
_cell_length_b                   14.631(13)
_cell_length_c                   16.909(15)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      15.9
_cell_measurement_theta_min      15.2
_cell_volume                     2333(4)
_computing_cell_refinement       'DIF4 (Siemens-Stoe)'
_computing_data_collection       'DIF4 (Siemens-Stoe)'
_computing_data_reduction        'REDU4 (Siemens-Stoe)'
_computing_molecular_graphics    'ORTEP (C.K.Johnson, 1965)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measurement_device       'Siemens-Stoe AED2'
_diffrn_measurement_method       omega-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0361
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5634
_diffrn_reflns_theta_max         28.01
_diffrn_reflns_theta_min         1.85
_diffrn_standards_decay_%        2
_diffrn_standards_interval_time  90
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.898
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.833
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.771
_exptl_crystal_density_method    none
_exptl_crystal_description       plate
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.919
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.031
_refine_ls_goodness_of_fit_obs   1.071
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         5634
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_restrained_S_obs      1.071
_refine_ls_R_factor_all          0.0668
_refine_ls_R_factor_obs          0.0413
_refine_ls_shift/esd_max         -0.004
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0486P)^2^+1.5348P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1075
_refine_ls_wR_factor_obs         0.0961
_reflns_number_observed          4270
_reflns_number_total             5634
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic971552u_1.cif
_cod_data_source_block           comba9
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0486P)^2^+1.5348P] 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^)+(0.0486P)^2^+1.5348P] 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        2333.3(35)
_cod_database_code               4322905