Two-Step Spin-Transition Iron(III) Compound with a Wide [High Spin-Low Spin] Plateau
Jinkui Tang; José Sánchez Costa; Simon Smulders; Gábor Molnár; Azzedine Bousseksou; Simon J. Teat; Yangguang Li; Gerard A. van Albada; Patrick Gamez; Jan Reedijk; Inorganic Chemistry 48 (2009) 2128–2135; doi:10.1021/ic801973x

data_4301574
_publ_section_title
;
Two-Step Spin-Transition Iron(III) Compound with a Wide [High Spin-Low
Spin] Plateau
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2128
_journal_page_last               2135
_journal_paper_doi               10.1021/ic801973x
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C26.5 H27 Cl Fe N6 O9'
_chemical_formula_weight         664.84
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                95.397(2)
_cell_angle_beta                 99.435(2)
_cell_angle_gamma                91.806(2)
_cell_formula_units_Z            4
_cell_length_a                   12.932(2)
_cell_length_b                   15.096(2)
_cell_length_c                   15.345(2)
_cell_measurement_reflns_used    4314
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.26
_cell_measurement_theta_min      2.75
_cell_volume                     2938.7(7)
_computing_cell_refinement       'Bruker SAINT v7.34a'
_computing_data_collection       'Bruker APEX 2'
_computing_data_reduction        'Bruker SAINT v7.34a'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL & local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX II CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Advanced Light Source station 11.3.1'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.77490
_diffrn_reflns_av_R_equivalents  0.0499
_diffrn_reflns_av_sigmaI/netI    0.0608
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            26158
_diffrn_reflns_theta_full        26.85
_diffrn_reflns_theta_max         26.85
_diffrn_reflns_theta_min         2.52
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.667
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.88
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2004/1 Bruker AXS Madison WI USA'
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1372
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.645
_refine_diff_density_min         -0.663
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     807
_refine_ls_number_reflns         9670
_refine_ls_number_restraints     75
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0981
_refine_ls_R_factor_gt           0.0555
_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^)+(0.0984P)^2^+1.1922P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1463
_refine_ls_wR_factor_ref         0.1729
_reflns_number_gt                6108
_reflns_number_total             9670
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic801973x_si_002.cif
_cod_data_source_block           jsc363
_cod_original_formula_sum        'C26.50 H27 Cl Fe N6 O9'
_cod_database_code               4301574