An Integrated Approach to the Mid-Spin State (S= 3/2) in Six-Coordinate Iron(III) Chiroporphyrins
Jean-Pierre Simonato; Jacques Pécaut; Laurent Le Pape; Jean-Louis Oddou; Claudine Jeandey; Maoyu Shang; W. Robert Scheidt; Jacek Wojaczyński; Stanisław Wołowiec; Lechosław Latos-Grażyński; Jean-Claude Marchon; Inorganic Chemistry 39 (2000) 3978–3987; doi:10.1021/ic000150a

data_4321307
_publ_section_title
;
 An Integrated Approach to the Mid-Spin State (S= 3/2) in Six-Coordinate
 Iron(III) Chiroporphyrins
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3978
_journal_page_last               3987
_journal_paper_doi               10.1021/ic000150a
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C157.46 H197.46 Cl7.36 Fe3 N12 O44'
_chemical_formula_weight         3390.83
_chemical_name_systematic
;
 [Fe(TMCP)(OH2)(HOEt)]2[Fe(TMCP)(HOEt)2](ClO4)3.(EtOH)2.(CHCl3)1.45
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 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                 97.353(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   47.576(2)
_cell_length_b                   12.9029(15)
_cell_length_c                   13.664(2)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     8318.9(16)
_computing_cell_refinement       MADNES
_computing_data_collection       MADNES
_computing_data_reduction        'MADNES (Messerschmitt & Pflugrath, 1987)'
_computing_molecular_graphics    'ORTEPIII (Burnett & Johnson, 1996)'
_computing_publication_material  'SHELXTL_V5 (Siemens, 1994)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      130(2)
_diffrn_measurement_device       'Enraf-Nonius FAST'
_diffrn_measurement_method       'Ellipsoid-mask fitting'
_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  0.0633
_diffrn_reflns_av_sigmaI/netI    0.0496
_diffrn_reflns_limit_h_max       59
_diffrn_reflns_limit_h_min       -58
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            25055
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.04
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.458
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.764
_exptl_absorpt_correction_type   refdelf
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.354
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate-like
_exptl_crystal_F_000             3563
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.716
_refine_diff_density_min         -0.788
_refine_diff_density_rms         0.079
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(2)
_refine_ls_extinction_coef       0.00022(13)
_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   1.022
_refine_ls_goodness_of_fit_obs   1.033
_refine_ls_hydrogen_treatment    'Idealized with riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1126
_refine_ls_number_reflns         10590
_refine_ls_number_restraints     249
_refine_ls_restrained_S_all      1.058
_refine_ls_restrained_S_obs      1.076
_refine_ls_R_factor_all          0.0849
_refine_ls_R_factor_obs          0.0671
_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^)+(0.0887P)^2^+27.4018P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1754
_refine_ls_wR_factor_obs         0.1604
_reflns_number_observed          8838
_reflns_number_total             10590
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000150a_1.cif
_cod_data_source_block           3
_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:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0887P)^2^+27.4018P] 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^)+(0.0887P)^2^+27.4018P] 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        8318.6(14)
_cod_database_code               4321307