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_4322624
_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)2](BPh4)2'
_chemical_formula_sum            'C84 H76 B2 Fe N8'
_chemical_formula_weight         1275.00
_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                 102.840(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.4890(10)
_cell_length_b                   14.1890(10)
_cell_length_c                   19.8430(10)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    299(2)
_cell_measurement_theta_max      28.58
_cell_measurement_theta_min      4.57
_cell_volume                     3428.4(4)
_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      299(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_sigmaI/netI    0.0623
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            5786
_diffrn_reflns_theta_max         56.73
_diffrn_reflns_theta_min         3.84
_diffrn_standards_decay_%        5.30
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.162
_exptl_absorpt_correction_T_max  0.3110
_exptl_absorpt_correction_T_min  0.2324
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.235
_exptl_crystal_description       prisms
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.150
_refine_diff_density_min         -0.183
_refine_diff_density_rms         0.036
_refine_ls_extinction_coef       0.0032(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.028
_refine_ls_goodness_of_fit_obs   1.096
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     431
_refine_ls_number_reflns         4553
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_restrained_S_obs      1.096
_refine_ls_R_factor_all          0.0813
_refine_ls_R_factor_obs          0.0494
_refine_ls_shift/esd_max         -0.008
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0495P)^2^+0.6403P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1257
_refine_ls_wR_factor_obs         0.1090
_reflns_number_observed          3146
_reflns_number_total             4553
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic971105e_5.cif
_cod_data_source_block           4-BPh4(AD1234c)
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0495P)^2^+0.6403P] 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^)+(0.0495P)^2^+0.6403P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4322624