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_4322623
_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](SO3CF3)2'
_chemical_formula_sum            'C38 H36 F6 Fe N8 O6 S2'
_chemical_formula_weight         934.72
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yc'
_symmetry_space_group_name_H-M   'P 1 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                 92.270(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.2360(10)
_cell_length_b                   10.1290(10)
_cell_length_c                   19.2510(10)
_cell_measurement_reflns_used    26
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.36
_cell_measurement_theta_min      10.93
_cell_volume                     1994.4(3)
_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         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0534
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            3964
_diffrn_reflns_theta_max         49.50
_diffrn_reflns_theta_min         4.32
_diffrn_standards_decay_%        8.08
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.771
_exptl_absorpt_correction_T_max  0.4506
_exptl_absorpt_correction_T_min  0.2946
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_description       fragment_of_plate
_exptl_crystal_F_000             960
_exptl_crystal_size_max          .40
_exptl_crystal_size_mid          .28
_exptl_crystal_size_min          .18
_refine_diff_density_max         0.325
_refine_diff_density_min         -0.494
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.010(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.016
_refine_ls_goodness_of_fit_obs   1.027
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     550
_refine_ls_number_reflns         3964
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.015
_refine_ls_restrained_S_obs      1.027
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_obs          0.0464
_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^)+(0.0894P)^2^+1.0759P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1205
_refine_ls_wR_factor_obs         0.1173
_reflns_number_observed          3709
_reflns_number_total             3964
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic971105e_4.cif
_cod_data_source_block           4-OTf(AD1230)
_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^)+(0.0894P)^2^+1.0759P] 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^)+(0.0894P)^2^+1.0759P] 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               4322623