Complete and incomplete spin transitions in 1D chain iron(ii) compounds
Pfaffeneder, Toni M.; Thallmair, Sebastian; Bauer, Wolfgang; Weber, Birgit; New Journal of Chemistry 35 (2011) 691–; doi:10.1039/c0nj00750a

data_7052586
_publ_section_title
;
 Complete and incomplete spin transitions in 1D chain iron(ii)
 compounds
;
_journal_issue                   3
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              691
_journal_paper_doi               10.1039/c0nj00750a
_journal_volume                  35
_journal_year                    2011
_chemical_compound_source
;
A mixture of 0.29 g [FeL2(MeOH)~2~]\'b70.5(MeOH) (0.45 mmol) and 0.25 g
1,3-bis(pyridine-4-yl)propane (1.66 mmol) in 20 mL methanol was heated at
reflux for 1 h. After cooling, the black precipitate was filtered off, washed
with methanol (2 \\times 5 mL) and dried in vacuum. Single crystals of (I)
were slowly formed by diffusion techniques in methanol solution after several
weeks.
;
_chemical_formula_moiety         'C43 H40 Fe N4 O6, 0.54(C H4 O)'
_chemical_formula_sum            'C43.54 H42.17 Fe N4 O6.54'
_chemical_formula_weight         782.01
_chemical_name_common
;
(E,E)-((diethyl-2,2'-(1,2-
phenylenebis(iminomethylidyne))bis(3-oxo-3-phenyl-propanato)(2-)-
N,N',O$3!,O$3!')(1,3-bis(4-pyridyl) propane)iron(ii)
;
_chemical_name_systematic
;
(E,E)-[{diethyl-2,2'-[1,2-phenylenebis(iminomethylidyne)]bis[3-oxo-3-phenyl-
propanato](2-)-<i>N</i>,<i>N</i>',<i>O</i>^3^,<i>O</i>^3^'}(1,3-bis(4-pyridyl)
propane)iron(II)
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_code                Fe_L5f_bppa_oo008_Bauer
_audit_creation_date
;
'Tue Jan 19 07:37:29 2010'
;
_audit_creation_method           'form98_non/compatible with shelxl97-2'
_audit_update_record             24-Sep-10
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.3122(4)
_cell_length_b                   16.5116(3)
_cell_length_c                   25.1186(5)
_cell_measurement_reflns_used    10475
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.2489
_cell_measurement_theta_min      4.2044
_cell_volume                     8009.7(3)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May 6 2009,17:20:42)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May 6 2009,17:20:42)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May 6 2009,17:20:42)
;
_computing_molecular_graphics
;
ORTEP (M. N. Burnett, C. K. Johnson, ORTEP-III: Oak Ridge Thermal Ellipsoid
Plot Program for Crystal Structure Illustrations, Oak Ridge National
Laboratory Report ORNL-6895, 1996). Windows version (L. J. Farrugia, Univ.
Glasgow) used --- SCHAKAL (E. Keller, University of Freiburg (Breisgau),
Germany, 1995).
;
_computing_publication_material
;
PLATON (A. L. Spek, Acta Crystallogr, Sect. A, 1990, 46, C34, 1995 version).
;
_computing_structure_refinement
'SHELXL-97 (G. M. Sheldrick. University of G\"ottingen, 97-2 version)'
_computing_structure_solution
;
A. Altomare, M. C. Burla, M. Camalli, G. L. Cascarano, C. Giacovazzo, A.
Guagliardi, A. G. G. Moliterni, G. Polidori, R. Spagna: SIR97: a new tool for
crystal structure determination and refinement; J. Appl. Crystallogr. 1999,
32, 115-119.
;
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 15.9809
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
1 omega 59.00 101.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ frames
- 21.3869 179.0000 0.0000 42

2 omega -15.00 65.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ frames
- 21.3869 -97.0000 -172.0000 80

3 omega -37.00 95.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ frames
- 21.3869 0.0000 150.0000 132

;
_diffrn_measurement_device       'CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Oxford XCalibur'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0383986404
_diffrn_orient_matrix_UB_12      -0.0161967081
_diffrn_orient_matrix_UB_13      -0.0020737332
_diffrn_orient_matrix_UB_21      0.0161355777
_diffrn_orient_matrix_UB_22      0.0305201876
_diffrn_orient_matrix_UB_23      -0.0116273709
_diffrn_orient_matrix_UB_31      0.0104580283
_diffrn_orient_matrix_UB_32      0.0124995438
_diffrn_orient_matrix_UB_33      0.0256586400
_diffrn_radiation_collimation    '0.5 mm collimator'
_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  0.0379
_diffrn_reflns_av_sigmaI/netI    0.0604
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            33558
_diffrn_reflns_theta_full        26.28
_diffrn_reflns_theta_max         26.28
_diffrn_reflns_theta_min         4.20
_diffrn_source_current           40
_diffrn_source_power             2.00
_diffrn_source_type              'Spellman generator'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.430
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91951
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May 6 2009,17:20:42)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.297
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3278
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.283
_refine_diff_density_min         -0.346
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.841
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     509
_refine_ls_number_reflns         8121
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.841
_refine_ls_R_factor_all          0.0664
_refine_ls_R_factor_gt           0.0325
_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^)+(0.0380P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0701
_refine_ls_wR_factor_ref         0.0744
_reflns_number_gt                4814
_reflns_number_total             8121
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0NJ00750A.TXT
_cod_data_source_block           oo008
_cod_database_code               7052586