One- and Two-Step Spin-Crossover Behavior of [FeII(isoxazole)6]2+ and the Structure and Magnetic Properties of Triangular [FeIII3O(OAc)6(isoxazole)3][ClO4]
Wendy Hibbs; Petra J. van Koningsbruggen; Atta M. Arif; William W. Shum; Joel S. Miller; Inorganic Chemistry 42 (2003) 5645–5653; doi:10.1021/ic034226p

data_4314160
_publ_section_title
;
 One- and Two-Step Spin-Crossover Behavior of [FeII(isoxazole)6]2+ and the
 Structure and Magnetic Properties of Triangular
 [FeIII3O(OAc)6(isoxazole)3][ClO4]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5645
_journal_page_last               5653
_journal_paper_doi               10.1021/ic034226p
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C18 H18 B2 F8 Fe N6 O6'
_chemical_formula_weight         643.85
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_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                117.8195(8)
_cell_angle_beta                 90.5309(6)
_cell_angle_gamma                91.5231(6)
_cell_formula_units_Z            3
_cell_length_a                   7.51430(10)
_cell_length_b                   16.7481(2)
_cell_length_c                   17.0901(2)
_cell_measurement_reflns_used    6721
_cell_measurement_temperature    130(1)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      1.018
_cell_volume                     1900.97(4)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'WinGX, Ortep3'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      130(1)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Nonius KappaCCD Diffractometer'
_diffrn_measurement_method       'Phi plus Omega scan'
_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  0.0154
_diffrn_reflns_av_sigmaI/netI    0.0367
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            13550
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.60
_diffrn_standards_decay_%        <2.0
_exptl_absorpt_coefficient_mu    0.702
_exptl_absorpt_correction_T_max  0.8441
_exptl_absorpt_correction_T_min  0.7913
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO-SMN (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.687
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             972
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.653
_refine_diff_density_min         -0.732
_refine_diff_density_rms         0.052
_refine_ls_extinction_coef       0.0028(8)
_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   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     693
_refine_ls_number_reflns         8523
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0328
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0135P)^2^+1.5315P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0734
_refine_ls_wR_factor_ref         0.0779
_reflns_number_gt                7444
_reflns_number_total             8523
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034226p_s1.cif
_cod_data_source_block           '[FeII(oxazole)6][BF4]2_130K'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' 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        1900.96(4)
_cod_database_code               4314160