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_4321308
_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            'C52.5 H63.5 Cl8.5 Fe N4 O14.5'
_chemical_formula_weight         1339.75
_chemical_name_systematic
;
 [Fe(TMCP)(OH2)(HOEt)](ClO4).[Fe(TMCP)(OH2)(HOEt)](H2O)(ClO4).(CHCl3)5
;
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                79.2150(10)
_cell_angle_beta                 76.4860(10)
_cell_angle_gamma                89.1730(10)
_cell_formula_units_Z            2
_cell_length_a                   13.1966(2)
_cell_length_b                   13.8900(2)
_cell_length_c                   17.810
_cell_measurement_temperature    193(2)
_cell_volume                     3116.66(7)
_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-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.787
_diffrn_measured_fraction_theta_max 0.787
_diffrn_measurement_method       '\w scans'
_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  0.0227
_diffrn_reflns_av_sigmaI/netI    0.0534
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13116
_diffrn_reflns_theta_full        25.95
_diffrn_reflns_theta_max         25.95
_diffrn_reflns_theta_min         1.20
_exptl_absorpt_coefficient_mu    0.670
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.428
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1386
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.8
_refine_diff_density_max         0.787
_refine_diff_density_min         -0.450
_refine_diff_density_rms         0.077
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.024(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1486
_refine_ls_number_reflns         11023
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_gt           0.0587
_refine_ls_shift/su_max          0.104
_refine_ls_shift/su_mean         0.010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1248P)^2^+1.8857P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1611
_refine_ls_wR_factor_ref         0.1664
_reflns_number_gt                10363
_reflns_number_total             11023
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000150a_2.cif
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 
;
_cod_original_cell_volume        3116.70(7)
_cod_original_formula_sum        'C52.50 H63.50 Cl8.50 Fe N4 O14.50'
_cod_database_code               4321308