Thermal Spin Crossover and LIESST Effect Observed in Complexes [Fe(LCh)2(NCX)2] [LCh= 2,5-Di(2-Pyridyl)-1,3,4-Chalcadiazole; Ch = O, S, Se; X = S, Se, BH3]
Julia Klingele; Dominic Kaase; Maximilian Schmucker; Yanhua Lan; Guillaume Chastanet; Jean-François Létard; Inorganic Chemistry 52 (2013) 6000–6010; doi:10.1021/ic400342m

data_4334899
_publ_contact_author             'Julia Klingele'
_publ_contact_author_email       julia.klingele@ac.uni-freiburg.de
_publ_section_title
;
 Thermal Spin Crossover and LIESST Effect Observed in Complexes
 [Fe(LCh)2(NCX)2] [LCh= 2,5-Di(2-Pyridyl)-1,3,4-Chalcadiazole; Ch = O, S,
 Se; X = S, Se, BH3]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6000
_journal_page_last               6010
_journal_paper_doi               10.1021/ic400342m
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety
;
 (Fe C26 H16 N10 O2 S2)
;
_chemical_formula_sum            'C26 H16 Fe N10 O2 S2'
_chemical_formula_weight         620.46
_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                 95.8981(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.5518(2)
_cell_length_b                   7.7916(2)
_cell_length_c                   17.7393(3)
_cell_measurement_reflns_used    6206
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      34.5
_cell_measurement_theta_min      2.3
_cell_volume                     1313.24(5)
_computing_data_collection       'Bruker APEX2'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.946
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_device_type  'Bruker APEX2 CCD area detector'
_diffrn_measurement_method       'f\ and \w scans'
_diffrn_radiation_monochromator  'multilayer mirror optics'
_diffrn_radiation_source         'microfused sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_sigmaI/netI    0.0351
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            20856
_diffrn_reflns_theta_full        34.85
_diffrn_reflns_theta_max         34.85
_diffrn_reflns_theta_min         2.31
_exptl_absorpt_coefficient_mu    0.780
_exptl_absorpt_correction_T_max  0.9846
_exptl_absorpt_correction_T_min  0.9260
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>SADABS</i>; Sheldrick, 1996)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.569
_exptl_crystal_description       block
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.596
_refine_diff_density_min         -0.416
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         5417
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0347
_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^)+(0.0374P)^2^+0.5155P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0813
_refine_ls_wR_factor_ref         0.0877
_reflns_number_gt                4294
_reflns_number_total             5417
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400342m_si_004.cif
_cod_data_source_block           dk_ms27
_cod_database_code               4334899