Iron(II) Polyamine Chemistry: Variation of Spin State and Coordination Number in Solid State and Solution with Iron(II) Tris(2-pyridylmethyl)amine Complexes
Alain Diebold; Karl S. Hagen; Inorganic Chemistry 37 (1998) 215–223; doi:10.1021/ic971105e

data_4322621
_publ_section_title
;
 Iron(II) Polyamine Chemistry: Variation of Spin State and Coordination
 Number in Solid State and Solution with Iron(II)
 Tris(2-pyridylmethyl)amine Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              215
_journal_page_last               223
_journal_paper_doi               10.1021/ic971105e
_journal_volume                  37
_journal_year                    1998
_chemical_formula_moiety         Fe(TPA)(SO3CF3)2
_chemical_formula_sum            'C20 H18 F6 Fe N4 O6 S2'
_chemical_formula_weight         644.35
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 113.290(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.636(2)
_cell_length_b                   9.6590(10)
_cell_length_c                   16.004(2)
_cell_measurement_reflns_used    26
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      12.44
_cell_measurement_theta_min      5.25
_cell_volume                     2504.1(5)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0304
_diffrn_reflns_av_sigmaI/netI    0.0368
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            5532
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.26
_diffrn_standards_decay_%        10.42
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.859
_exptl_absorpt_correction_T_max  0.8857
_exptl_absorpt_correction_T_min  0.6513
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            pale_yellow
_exptl_crystal_density_diffrn    1.709
_exptl_crystal_description       aggregate_of_cryst
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          .65
_exptl_crystal_size_mid          .50
_exptl_crystal_size_min          .50
_refine_diff_density_max         0.360
_refine_diff_density_min         -0.602
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.117
_refine_ls_goodness_of_fit_obs   1.088
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         4406
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.117
_refine_ls_restrained_S_obs      1.088
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_obs          0.0392
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0645P)^2^+1.3648P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1143
_refine_ls_wR_factor_obs         0.1036
_reflns_number_observed          3855
_reflns_number_total             4406
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic971105e_2.cif
_cod_data_source_block           2(AD1154c)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0645P)^2^+1.3648P] 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^)+(0.0645P)^2^+1.3648P] 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               4322621