High-Temperature Spin Crossover Behavior in a Nitrogen-Rich FeIII-Based System
Cyril Cook; Fatemah Habib; Tomoko Aharen; Rodolphe Clérac; Anguang Hu; Muralee Murugesu; Inorganic Chemistry 52 (2013) 1825–1831; doi:10.1021/ic301864d

data_4333800
_publ_section_title
;
 High-Temperature Spin Crossover Behavior in a Nitrogen-Rich FeIII-Based
 System
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1825
_journal_page_last               1831
_journal_paper_doi               10.1021/ic301864d
_journal_volume                  52
_journal_year                    2013
_chemical_compound_source        'Synthesized by the authors. See text'
_chemical_formula_moiety         'C15 H28 Fe N30 Na2 O5, H4 N'
_chemical_formula_sum            'C15 H32 Fe N31 Na2 O5'
_chemical_formula_weight         828.55
_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                77.327(4)
_cell_angle_beta                 71.974(4)
_cell_angle_gamma                78.734(4)
_cell_formula_units_Z            2
_cell_length_a                   10.9071(9)
_cell_length_b                   12.8656(10)
_cell_length_c                   13.8554(12)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    100
_cell_measurement_theta_max      69.95
_cell_measurement_theta_min      3.40
_cell_volume                     1786.7(3)
_computing_cell_refinement       'SAINT V7.68A(Bruker AXS, 2009)'
_computing_data_collection       'APEX2  (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT V7.68A(Bruker AXS, 2009)'
_computing_molecular_graphics    'SHELXTL v6.12 (Bruker AXS, 2001)'
_computing_publication_material  'UdMX (Maris, 2004)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.942
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_device_type  'Bruker APEX II'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'Quazar MX'
_diffrn_radiation_source         'Incoatec I\muS Microsource '
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.066
_diffrn_reflns_av_sigmaI/netI    0.0684
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            22948
_diffrn_reflns_theta_full        70.34
_diffrn_reflns_theta_max         70.34
_diffrn_reflns_theta_min         3.40
_exptl_absorpt_coefficient_mu    4.313
_exptl_absorpt_correction_T_max  0.9174
_exptl_absorpt_correction_T_min  0.6483
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Sheldrick, 2008)'
_exptl_crystal_colour            BLUE
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_description       PLATE
_exptl_crystal_F_000             854
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.035
_refine_diff_density_min         -0.846
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         6445
_refine_ls_number_restraints     52
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.1419
_refine_ls_R_factor_gt           0.1057
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1765P)^2^+7.6588P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2967
_refine_ls_wR_factor_ref         0.3259
_reflns_number_gt                4337
_reflns_number_total             6445
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic301864d_si_002.cif
_cod_data_source_block           murug2
_cod_database_code               4333800