A New Family of Spin Crossover Complexes with a Tripod Ligand Containing Three Imidazoles: Synthesis, Characterization, and Magnetic Properties of [FeIIH3LMe](NO3)2.1.5H2O, [FeIIILMe].3.5H2O, [FeIIH3LMe][FeIILMe]NO3, and [FeIIH3LMe][FeIIILMe](NO3)2 (H3LMe= Tris[2-(((2-methylimidazol-4-yl)methylidene)amino)ethyl]amine)
Yuichi Ikuta; Makoto Ooidemizu; Yuichi Yamahata; Masahiro Yamada; Shutaro Osa; Naohide Matsumoto; Seiichiro Iijima; Yukinari Sunatsuki; Masaaki Kojima; Françoise Dahan; Jean-Pierre Tuchagues; Inorganic Chemistry 42 (2003) 7001–7017; doi:10.1021/ic034495f

data_4312402
_publ_contact_author_email       naohide@aster.sci.kumamoto-u.ac.jp
_publ_contact_author_fax         +81-96-342-3390
_publ_contact_author_name        'Naohide Matsumoto'
_publ_contact_author_phone       +81-96-342-3390
_publ_section_title
;
 A New Family of Spin Crossover Complexes with a Tripod Ligand Containing
 Three Imidazoles: Synthesis, Characterization, and Magnetic Properties of
 [FeIIH3LMe](NO3)2.1.5H2O, [FeIIILMe].3.5H2O, [FeIIH3LMe][FeIILMe]NO3, and
 [FeIIH3LMe][FeIIILMe](NO3)2 (H3LMe=
 Tris[2-(((2-methylimidazol-4-yl)methylidene)amino)ethyl]amine)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7001
_journal_page_last               7017
_journal_paper_doi               10.1021/ic034495f
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C42 H57 Fe2 N21 O3'
_chemical_formula_weight         1015.79
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           146
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   11.9031(18)
_cell_length_b                   11.9031(18)
_cell_length_c                   27.742(3)
_cell_measurement_temperature    90(2)
_cell_volume                     3404.0(8)
_computing_cell_refinement       'CRYSALISRED 169, Oxford-Diffraction, 2001'
_computing_data_collection       'CRYSALIS 169, Oxford-Diffraction, 2001'
_computing_data_reduction        'CRYSALISRED 169, Oxford-Diffraction, 2001'
_computing_molecular_graphics    'ZORTEP (Zsolnai, 1996)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.312
_diffrn_measured_fraction_theta_max 0.312
_diffrn_measurement_device_type  'Oxford-Diffraction Xcalibur'
_diffrn_measurement_method       '\w,\f scans'
_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  0.0441
_diffrn_reflns_av_sigmaI/netI    0.0473
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            10345
_diffrn_reflns_theta_full        31.70
_diffrn_reflns_theta_max         31.70
_diffrn_reflns_theta_min         3.42
_exptl_absorpt_coefficient_mu    0.706
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.487
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Parallelepiped
_exptl_crystal_F_000             1596
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.557
_refine_diff_density_min         -0.281
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.927
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         4609
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      0.928
_refine_ls_R_factor_all          0.0811
_refine_ls_R_factor_gt           0.0440
_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^)+(0.0495P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0914
_refine_ls_wR_factor_ref         0.1082
_reflns_number_gt                2495
_reflns_number_total             4609
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034495fsi20030510_090847_1.cif
_cod_data_source_block           '[FeIIH3LMe][FeIILMe]NO3at90K'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'None' changed to
'none' 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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0495P)^2^+0.0000P] 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^)+(0.0495P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               4312402