Observation of the Structural Consequences of a Reversible S=3/2 and S=1/2 Spin Crossover in the Single Crystal
Yoshiki Ohgo; Takahisa Ikeue; Mikio Nakamura; Inorganic Chemistry 41 (2002) 1698–1700; doi:10.1021/ic015620v

data_4317823
_publ_contact_author_address
;
Department of Chemistry
Toho University
5-21-16 Omorinishi Ota-ku Tokyo 143 Japan
;
_publ_contact_author_email       yohgo@med.toho-u.ac.jp
_publ_contact_author_fax         '81 3 5493 5430'
_publ_contact_author_name        'Ohgo, Yoshiki'
_publ_contact_author_phone       '81 3 3762 4151 x2551'
_publ_section_title
;
 Observation of the Structural Consequences of a Reversible S=3/2 and
 S=1/2 Spin Crossover in the Single Crystal
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1698
_journal_page_last               1700
_journal_paper_doi               10.1021/ic015620v
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety         'C72 H36 Fe N6, C H Cl3, Cl O4'
_chemical_formula_sum            'C72 H74 Cl5 Fe N6 O4'
_chemical_formula_weight         1320.47
_chemical_name_common            porphyrin
_chemical_name_systematic
;
[(2,3,7,8,12,13,17,18-octaethyl-5,10,15,20-
tetraphenylporphyrinato)iron(III)bispyridine]
perchlorate
;
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.493(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.972(1)
_cell_length_b                   18.481(2)
_cell_length_c                   26.750(3)
_cell_measurement_reflns_used    133173
_cell_measurement_temperature    298
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.1
_cell_volume                     6768.8(12)
_computing_cell_refinement
;
MSC/AFC Diffractometer Control Software
;
_computing_data_collection
;
MSC/AFC Diffractometer Control Software
(Molecular Structure Corporation, 1992a)
;
_computing_data_reduction
;
MSC/AFC Diffractometer Control Software. Data Reduction:
TEXSAN (Molecular Structure Corporation, 1992b)
;
_computing_molecular_graphics    'SV (Nemoto & Ohashi, 1993)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-97(Altomare, A. et al., 1999)'
_diffrn_ambient_temperature      298
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.938
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_device_type  'RIGAKU RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_av_sigmaI/netI    0.0434
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            27327
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.50
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    0.473
_exptl_absorpt_correction_T_max  0.954
_exptl_absorpt_correction_T_min  0.907
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
ABSCOR(Higashi et al., 1968)
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2764
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.960
_refine_diff_density_min         -0.648
_refine_diff_density_rms         0.090
_refine_ls_extinction_coef       0.0097(10)
_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_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     832
_refine_ls_number_reflns         14992
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0970
_refine_ls_R_factor_gt           0.0759
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1659P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2262
_refine_ls_wR_factor_ref         0.2435
_reflns_number_gt                10628
_reflns_number_total             14992
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic015620v_1.cif
_cod_data_source_block           oetppfepy2-298
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1659P)^2^] 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^)+(0.1659P)^2^]
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        6769.0(10)
_cod_database_code               4317823